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Dental Materials (2004) 20, 873–880

www.intl.elsevierhealth.com/journals/dema

Immediate performance of self-etching

versus system adhesives with multiple
light-activated restoratives
M. Iriea,*, K. Suzukia, D.C. Wattsb

a
Department of Biomaterials, Okayama University Graduate School of Medicine and Dentistry,
2-5-1 Shikata-cho, Okayama 700-8525, Japan
b
University of Manchester Dental School, Manchester, UK

Received 28 July 2003; received in revised form 26 January 2004; accepted 1 April 2004

KEYWORDS
Marginal gap formation;
Bond strength; Adhesive
technique; Resin
composite; Compomer
Summary Objectives: The purpose of this study was to evaluate the performance of
both single and double applications of (Adper Prompt L-Pop) self-etching dental
adhesive, when used with three classes of light-activated restorative materials, in
comparison to the performance of each restorative system adhesive. Evaluation
parameters to be considered for the adhesive systems were (a) immediate marginal
adaptation (or gap formation) in tooth cavities, (b) free setting shrinkage-strain
determined by the immediate marginal gap-width in a non-bonding Teflon cavity, and
(c) their immediate shear bond-strengths to enamel and to dentin.
Methods: The maximum marginal gap-width and the opposing-width (if any) in the
tooth cavities and in the Teflon cavities were measured immediately (3 min) after
light-activation. The shear bond-strengths to enamel and to dentin were also
measured at 3 min.
Results: For light-activated restorative materials during early setting (, 3 min),
application of Adper Prompt L-Pop exhibited generally superior marginal adaptation to
most system adhesives. But there was no additional benefit from double application.
The marginal-gaps in tooth cavities and the marginal-gaps in Teflon cavities were
highly correlated (r ¼ 0:86 – 0:89; p , 0:02 – 0:01). For enamel and dentin shear bond-
strengths, there were no significant differences between single and double
applications, for all materials tested except Toughwell and Z 250 with enamel.
Significance: Single application of a self-etch adhesive was a feasible and beneficial
alternative to system adhesives for several classes of restorative. Marginal gap-widths
in tooth cavities correlated more strongly with free shrinkage-strain magnitudes than
with bond-strengths to tooth structure.
Q 2004 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Introduction

*Corresponding author. Tel.: þ81-86-235-6668; fax: þ81-86- Marginal adaptation and bonding of restorative
235-6669. filling materials to the tooth cavity may not be
E-mail address: mirie@md.okayama-u.ac.jp

0109-5641/$ - see front matter Q 2004 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.dental.2004.04.003
874
secure in the initial stage. It has been suggested
that restoration failure might occur immediately
after setting or during the initial stage of restor-
ation [1] and early gaps may lead to bacterial
penetration and pulpal damage [2,3]. Therefore,
protocols for measuring marginal gap formation
were developed to evaluate the marginal adap-
tation of resin composite restorations [1,4,5]. When
a resin composite is used to restore a dental cavity,
any gap resulting at the cavity margin may be the
result of an interaction between its’ setting
shrinkage, bond strength and material flow during
the setting period [4].
Contemporary self-etching adhesives and the
recently introduced all-in-one adhesives are attrac-
tive additions to the clinician’s bonding procedures.
They are user-friendly in that the number of steps
required in the bonding protocol is reduced. As the
smear layer is not removed prior to the application
of the adhesive, the potential for post-operative
sensitivity that is caused by incomplete resin
infiltration of patent dentinal tubules can be
substantially reduced. Moreover, as water is an
essential component of these systems to enable
ionization of the acidic monomers for deminerali-
zation of hard dental tissues, the technique
sensitivity associated with variations in the state
of hydration of a demineralized collagen matrix is
also eliminated. These self-etching adhesives vary
in their acidity by differences in the composition
and concentration of polymerizable acids and/or
acidic resin-monomers in these systems. Moreover,
self-etching adhesives are generally less technique
sensitive compared with systems that utilizes
separate acid conditioning and rinsing steps [6 – 8].
Clinically, self-etching adhesives not only simplify
the bonding process by eliminating steps, but also
eliminate some of the technique-sensitivity of
total-etch systems [9].
The version of Adper Prompt L-Pop (3M ESPE,
Seefeld, Germany) designed for use with compomer
or resin composite contains methacrylated phos-
phoric acid esters as the acidic components and is an
all-in one, self-etching adhesive. Strong self-etch
adhesives, such as Adper Prompt L-Pop have been
documented as producing an interfacial ultra-
morphology at dentin resembling that produced
typically by total-etch adhesives [8]. Consequently,
the mechanism of bonding strong self-etch
adhesives to dentin is more like that of total-etch
adhesives. This means that nearly all apatite
minerals are removed from surface layers of
collagen and thus any chemical interaction between
apatite minerals and functional monomers is
excluded. These strong self-etch adhesives exhibit
the typical hybridization features of total-etch
M. Irie et al.
adhesives along with the formation of abundant
resin tags. Concern is often raised however regard-
ing the bonding effectiveness of self-etch adhesives
to enamel. Numerous recent laboratory studies
provide data that suggest either equal or reduced
enamel bonding effectiveness as compared to
conventional phosphoric acid etching [6,10].
Previous studies have evaluated the effect of
multiple applications of self-etching or self-priming
adhesives. Although manufacturers suggested a
double application technique of the adhesives to
improve their bonding ability, no significant benefit
was reported from this application technique
[11,12]. For Clearfil Liner Bond 2 V, bond strengths
increased significantly as the thickness of bonding
layer increased ðp , 0:05Þ; whereas bond strengths
of Single Bond decreased significantly with
increased thickness of the bonding layer ðp ,
0:05Þ: Thus the effect of the thickness of the
adhesive layer on bond strength was evidently
material-dependent [13].
All light-activated resin-based biomaterials
shrink upon photo-polymerization and this is a
major problem in light-activated restorative pro-
cedures [14,15], such that the restorative/tissue
bond may be disrupted [16]. Previous studies have
suggested that setting shrinkage-strain has a
greater effect on the marginal adaptation than
two other factors, namely: bond strength or flow of
the restorative material [13 – 19]. Our method for
measuring the relative setting shrinkage-strain, for
comparison with marginal gaps in tooth cavities,
was described previously [18 –20]. This method is
based upon determining marginal gap-widths in
non-bonding Teflon cavities. These showed a
significant correlation with marginal gap-widths in
tooth cavities [18,19]. The effect of water-storage
on gap-widths in both Teflon and tooth cavities was
also studied [20].
This investigation was, therefore, carried out
with multiple types of light-activated restorative
materials to evaluate their system adhesives versus
both single and double applications of a self-etching
adhesive (Adper Prompt L-Pop). Performance was
to be assessed with regard to: (a) their immediate
marginal adaptation (or gap formation) in tooth
cavities; (b) their immediate free setting shrinkage-
strain, determined by the marginal gap-width in a
non-bonding Teflon cavity; (c) their immediate
shear bond-strengths to enamel and to dentin.
The first hypothesis to be tested was that the single
or double application of Adper Prompt L-Pop would
have no adverse effect on marginal integrity,
compared to the system adhesives. The second
hypothesis to be tested was that, amongst the set
of materials studied, trends in one or more of
Marginal-gap formation of light-activated restoratives 875

properties (b) and (c) would correlate with trends in
property (a).
Materials and methods
Seven light-activated restorative materials, includ-
ing three compomers, one giomer and three compo-
sites, used in this study are listed in Table 1. This
range of materials was not only representative of
major clinical types, but provided a range of values
for the parameters under investigation. Tooth
preparation procedures, mixing and handling were
carried out according to the manufacturers’ rec-
ommendations (Table 2). A visible-light curing unit
(New Light VL-II, GC, Tokyo, Japan; irradiated
diameter: 8 mm) was used for light-activated
materials with an irradiation time of 30 s. The light
intensity was checked immediately before each
application of the adhesive resin and restorative
material, using a radiometer (Demetron/Kerr,
Danbury, CT, USA). During the experiment the light
intensity was maintained at 450 mW/cm2. Human
premolars, extracted for orthodontic reasons, were
used throughout this study. After extraction and
cleaning, teeth were immediately stored in cold
distilled water at 4 8C for 1 – 2 months before testing,
then mounted in a holder using a slow setting epoxy
resin (Epofix Resin, Struers, Copenhagen, Denmark).
Marginal gap in the tooth cavity
A flat enamel surface was obtained by grinding the
tooth with a wet 220 grit silicon carbide paper, until
at least a 4 mm diameter area was exposed. With
the tooth held rigidly in a custom-made drill press, a
cylindrical cavity was prepared to a depth of
approximately 1.5 mm, with a diameter of 3.5 mm,
using a tungsten carbide bur (200,000 rpm) and a
custom bur rotating at 4000 rpm under wet con-
ditions. One cavity preparation was made in each
tooth in the coronal region and on the mesial
surface. A total of 210 cavities were prepared in 210
teeth for this study. The cavity walls and surround-
ing enamel margin were pretreated according to
the manufacturers’ instruction as described in
Table 2. Each cavity was filled with various
restorative materials using a syringe tip (Centrix
C-R Syringe System, Centrix, CT, USA). The slightly
overfilled cavity was covered with a plastic strip
and allowed to harden. Excess filling material
and approximately 0.1 mm of enamel were
removed by wet grinding on carborundum paper
#1000, followed by polishing with linen using an
aqueous slurry of Alfa Micropolish (0.3 mm) (Buehler
Ltd, Chicago, USA) immediately after setting. Each
restoration margin was inspected under a traveling
microscope (400 £ ) (XY-B, D-Type, Nikon, Tokyo,
Japan) for the presence, location, and extent of
marginal gaps. The maximum gap-width and
the opposing width (if any) between the material
and the cavity wall were measured using the
optical microscope, as previously described
[5,11,12,17,18], at a time of 3 min from start of
light-activation. The sum of these two measure-
ments was defined as the marginal gap in the tooth
cavity. For each material, 10 specimens were
prepared.

Table 1 Light-activated restorative materials investigated.

Product (type) Composition Manufacturer Batch No.

F 2000 (A) Fluoro-aluminosilicate-glass (84 wt%), CDMA oligomer, 3M ESPE, St Paul, MN, USA F2990825
GDMA, photo-initiators, stabilisers
Dyract AP(A) Strontium-fluoro-silicate glass (47 vol%, 73 wt%) Dentsply/DeTrey Konstanz Germany DA990826
polymerisable resins, TCB, strontium fluoride photo-
initiators, stabilisers
Hytac(A) Ca–Al– Zn–fluoride glass (66 wt%) organic monomers, photo- 3M ESPE AG Seefeld, Germany FW0054808
initiators, stabilisers
Reactmer(B) F-PRG þ glass filler (77–78 wt%), UDMA, HEMA Shofu, Kyoto, Japan 099900
Unifil F(C) Fluoro-aluminosilicate-glass þ silica (77 wt%), UDMA, GC, Tokyo, Japan 101181
dimethacrylate,, photo-initiators, stabilizer
Toughwell(C) Silica/zirconia filler (83 wt%) Bis-MPEPP, TEGDMA, UDMA, Tokuyama Dental Tokyo, Japan 323
photo-initiators
Z 250(C) Zirconia/silica filler (60 vol%) TEGDMA, UDMA, Bis-EMA 3M ESPE, St Paul, MN, USA ABJ

A: compomer, B: Giomer, C: Composite, CDMA oligomer: dimethacrylate functional oligomer derived from citric acid, GDMA:
glyceryl dimethacrylate, TCB: butane tetracarboxylic acid and hydroxyethylmethacrylate, HEMA: 2-hydroxyethyl methacrylate,
PENTA: dipentaerythritol pentaacrylate phosphate, UDMA: urethane dimethacrylate, Bis-GMA: bisphenol A glycidyl methacrylate,
TEGDMA: tri-ethylene-glycol dimethacrylate, Bis-MPEPP: 2,2-bis(4-methacryloyloxypolyethoxyphenyl)propane, Bis-EMA: bisphenol
A polyethellene glycol diether dimethacrylate, F-PRG: full reaction type of prereacted glass-ionomer.
876 M. Irie et al.

Table 2 System adhesive and self-etching adhesive components.

Adhesive Composition and surface treatment Manufacturer Batch No.

Primer/adhesive Side A: HEMA, Methacrylated polycarboxylic acid water, 3M ESPE, St Paul, MN, USA ALAR
ethanol, Photo-initiator
Side B: Maleic acid, water primer/adhesive (30 s)-air-light
(10 s)
Prime and Bond 2.1 PENTA, Elastomeric resin, short chain cross-linking resins, Dentsply/DeTrey Konstanz, DA990826
amine hydrofluoride, initiator, stabilisers, acetone Prime and Germany
bond 2.1 (30 s)-air-light (10 s)
Hytac OSB Co-momomer, initiator, acetone, stabiliser Hytac OSB (30 s)- 3M ESPE AG Seefeld, Germany FW0054808
air-light (10 s)
Reactmer bond A: water, acetone, F-PRG filler, FASG filler, initiator Shofu, Kyoto, Japan IB 515
B: 4-AET, 4-AETA, HEMA, UDMA, initiator A þ B (20 s)-air
(5 s)-light (20 s)
UniFil bond Self-etching primer: ethanol, water, HEMA,4-MET, GC, Tokyo, Japan 090491
photo-initiator
Bonding agent: UDMA, HEMA, TEGDMA, silica filler
photo-initiator
Self-etching primer (20 s)-air-bonding agent-light (10 s)
One-up bond F Bonding A: methacryloyloxyalkyl phosphate, MAC-10, Tokuyama Dental Tokyo, Japan 454720
bifunctional dimethacrylate, co-catalyst
One-up Bond F (20 s)-air-light (10 s)
Scotchbond Echant (7EE): 10% maleic acid, water 3M, St Paul, MN USA
multi-purpose
Primer (7AC): HEMA, polyalkenoic acid, copolymer, water
Adhesive (7AB): bis-GMA, HEMA, photo-initiator
Echant (15 s)-rinse and dry-primer (30 s)-dry-adhesive-light
(30 s)
Prompt L-Pop Methacrylated phosphoric acid ester, water, phosphine 3M ESPE, Seefeld, Germany FW66757
oxide, stabilizer, fluoride complex
Single application: Prompt L-Pop (15 s)-air-light (10 s)
Double application: Prompt L-Pop (15 s)-air-Prompt L-Pop
(15 s)-air-light (10 s)

HEMA: 2-hydroxyethyl methacrylate, PENTA: dipentaerythritol pentaacrylate phosphate, GPDM: glycerol phosphate dimethacry-
late, UDMA: urethane dimethacrylate, Bis-GMA: bisphenol A glycidyl methacrylate, TEGDMA: tri-ethylene-glycol dimethacrylate,
4-MET: 4-methacryloxyethyl trimellitic acid, MAC-10: 11-methacryloyloxy-1, 1-undecanedicarboxylic acid, F-PRG filler: full-
reaction-type pre-reacted glass-ionomer filler:, FASG filler: fluoro-aluminosilicate glass filler, 4-AET: 4-acryloxyethyltrimellitic
acid, 4-AETA: 4-acryloxyethyltrimellitate anhydride.

Marginal gap in the teflon cavity
Since the Teflon material does not react with the
restorative materials, it was used as a mold to
measure the degree of shrinkage-strain (immedi-
ately after setting). For direct comparison with the
width of the marginal gap in the tooth cavity, a
Teflon cavity of the same diameter as the tooth
cavity was used. The prepared Teflon mold was
placed on a glass plate covered with silicone oil, so
that the glass plate did not react or bond to the
filled material. Making and measuring a specimen
involved the same procedure as described above,
but without adhesive application, again at a time of
3 min from start of light-activation. The sum of two
measurements was expressed as the marginal gap-
width in the Teflon cavity. For each material,
10 specimens were prepared.
Shear bond-strength to enamel and to dentin
Wet grinding of the buccal surfaces was performed
with up to 1000 grit silicon carbide abrasive paper
until a flat enamel or superficial dentin area of at
least 4 mm in diameter was exposed. The surface
was pretreated as described above. A split Teflon
mold with a cylindrical hole (diameter, 3.6 mm;
height, 2 mm) was clamped to the prepared enamel
or dentin surface. The Teflon mold was filled with
various restorative materials using a Centrix syringe
Marginal-gap formation of light-activated restoratives 877

Table 3 Immediate marginal gaps (mm).

Restorative In the tooth cavity (mean (SD))a In the Teflon cavity

(mean (SD))a
Adhesive technique

Single application Double application System adhesive

of Prompt L-Pop of Prompt L-Pop

F 2000 11.2 (1.2)*A 10.1 (1.3)*A 12.9 (1.9)A 20.7 (2.1)A

Dyract AP 7.2 (2.3)*B 7.0 (2.0)*B 11.7 (5.2)AB 18.1 (1.7)ABCD
Hytac 8.9 (2.3)*AB 7.3 (1.9)*B 12.0 (2.4)AB 18.7 (4.5)ABC
Reactmer 7.2 (2.3)*B 6.8 (2.3)*B 9.9 (2.8)ABC 14.9 (1.8)D
UniFil F 7.1 (2.1)*#B 6.4 (1.5)*B 8.6 (2.2)#BC 15.3 (2.6)CD
Toughwell 6.9 (1.7)*B 6.2 (1.5)*B 7.6 (2.4)*C 15.7 (2.2)BCD
Z 250 8.5 (1.3)*B 8.2 (2.1)*AB 11.7 (1.5) AB 18.8 (1.8) AB

With each adhesive technique and Teflon cavity, mean values designated with the same letters (A, B, C, D) were not significantly
different ðp . 0:05Þ: With each product, means designated with the same symbols (*, #) were not significantly different ðp . 0:05Þ:
a
N ¼ 10:

tip (Centrix C-R Syringe System, Centrix, CT, USA).
It was covered with a plastic strip and the material
was hardened by light irradiation, as described
above. This prepared specimen was secured in a
mounting jig. At a time of 3 minutes from start of
light irradiation, the shear force was transmitted
by a flat (blunt) 1 mm broad shearing edge making a
908 angle to the direction of the load (or the back of
the load plate). The shear force was applied using a
testing machine (Autograph DCS-2000, Shimadzu,
Kyoto, Japan) at a cross-head speed of 0.5 mm/min
[19]. For each material, 10 specimens were
prepared. The stress at failure was calculated and
recorded as the shear bond-strength. The failed
specimens were examined under a light microscope
(4 £ ) (SMZ-10, Nikon, Tokyo, Japan) to determine
the total number of adhesive failure surfaces
[11,18].
All procedures, except for testing, were per-
formed in an air-conditioned room at 23 ^ 0.5 8C
and 50 ^ 2% RH. The data-sets for marginal gaps in
tooth cavities and shear bond-strength were each
subjected to one-way ANOVA to examine the
influence of the adhesive techniques and the
system adhesive. Significant differences at
p , 0:05 were determined using Duncan’s new
multiple-range test. Possible correlations between
pairs of parameters were analyzed by linear
regression.
Results
system adhesive. There was no significant differ-
ence between the single and the double appli-
cations of Prompt L-pop for all the materials
tested. With both the single and the double
applications of Prompt L-Pop, F 2000 showed
significantly wider marginal gaps than with the
other materials. The marginal-gap data for the
tooth cavities separated into three groups, whereas
the marginal-gap data for the Teflon cavities
separated into four groups. All resin-composites
showed significantly smaller marginal gaps than all
compomers. For the set of restorative materials
studied, the marginal-gaps in tooth cavities with
each adhesive technique were highly correlated
with the marginal-gaps in Teflon cavities (Table 4).
These three correlation coefficients ðrÞ were
approximately the same for each technique. Thus,
in general, a restorative material with a smaller
marginal-gap in the tooth cavity showed a smaller
marginal-gap in the Teflon cavity.
The values of shear bond-strength to enamel are
presented in Table 5. Single and double applications
of Prompt L-Pop to enamel with all restorative
materials, except Toughwell and Z 250, showed
significantly higher strengths than with the corres-
ponding system adhesive. There was no significant
difference between the single application and
Table 4 The linear regression relationships between the
marginal gaps in the tooth cavities and the marginal gaps in
Teflon cavities.
Adhesive technique r p Value

The data for marginal gaps in the tooth and Teflon

Single application of prompt L-Pop 0.86 ,0.02
cavities are presented in Table 3. Single and double Double application of prompt L-Pop 0.86 ,0.02
applications of Prompt L-Pop with all restorative System adhesive 0.89 ,0.01
materials, except Toughwell, showed significantly
N ¼ 7:
smaller gaps than when using the corresponding
878 M. Irie et al.

Table 5 Immediate shear bond-strength to enamel (MPa, Mean (SD, F)).

Restorative Adhesive technique

Single application of Prompt L-Pop Double application of Prompt L-Pop System adhesive

F 2000 16.1 (3.5, 0)*A 15.6 (2.9, 0)*ABC 7.7 (1.1, 2)#A
Dyract AP 10.5 (2.3, 0)*B 12.2 (2.3, 0)*B 7.1 (5.2, 0)#A
Hytac 16.9 (2.8, 0)*A 18.8 (3.0, 0)*A 10.2 (2.9, 1)#AB
Reactmer 16.8 (3.2, 0)*A 18.3 (3.4, 0)*A 11.9 (2.8, 4)#B
UniFil F 11.8 (1.4, 0)*BC 12.8 (2.3, 0)*BC 9.6 (2.3, 1)#AB
Toughwell 10.1 (1.5, 0)*B 14.0 (1.5, 0)#BC 20.1 (2.6, 0) þ
Z 250 14.7 (2.9, 0)*AC 17.8 (3.3, 0)#AC 25.0 (3.0, 0) þ

N ¼ 10: F: number of adhesive failure modes; Within each adhesive technique, mean values designated with the same letters are not
significantly different ðp . 0:05Þ: With each restorative, means designated with the same symbols (*, #, þ ) are not significantly
different ðp . 0:05Þ:

the double application with all materials tested,
except with Toughwell and Z 250. The system
adhesives for Toughwell and Z 250 showed the
highest values amongst the data-set (Table 5). With
the single and double applications of Prompt L-Pop,
the enamel bond-strength data separated into
three groups. With the system adhesives, the
strength data separated into four groups. No single
or double applications of Prompt L-Pop showed
adhesive failures. With its system adhesive, the
proportion of adhesive failures of specimens using
Reactmer was 40%. No relationship was observed
between the marginal gaps in tooth cavities with
each of three kinds of adhesive technique and the
corresponding shear bond-strength to enamel
(p . 0:10; n ¼ 7).
The values of shear bond-strength to dentin are
presented in Table 6. There was no significant
difference between the single and the double
applications of Prompt L-pop with all materials
tested, except with Z 250. Single and double
applications of Prompt L-Pop with Hytac showed
significantly higher strengths than with the corre-
sponding system adhesive. However, the system
adhesive of Toughwell showed significantly higher
strengths than with either single or double appli-
cations of Prompt L-Pop. With the single and double
applications of Prompt L-Pop, the dentin bond-
strength data separated into two groups. With the
system adhesives, the strength data separated into
three groups. No single or double applications of
Prompt L-Pop showed adhesive failure. With the
system adhesive, the proportion of adhesive fail-
ures using Dyract AP was only 10%. No relationship
was observed between the marginal gaps in tooth
cavities with each of three kinds of adhesive
technique and the corresponding shear bond-
strengths to dentin (p . 0:10; n ¼ 7).
Discussion
With the aim of simplifying restorative procedures,
a new self-etching all-in-one adhesive (Adper
Prompt L-Pop) was developed, with the ability to
completely solubilize the smear layer and smear
plugs, even with thick smear layers. Thus
hybrid layers could be formed with a thickness

Table 6 Immediate shear bond-strength to dentin (MPa, Mean (SD, F)).a

Restorative Adhesive technique

Single application of Prompt L-Pop Double application of Prompt L-Pop System adhesive

F 2000 10.0 (1.6, 0)*A 11.5 (1.8, 0)*A 10.5 (2.6, 0)*B
Dyract AP 8.9 (2.0, 0)*A B 10.0 (1.6, 0)*AB 10.5 (4.5, 1)*B
Hytac 8.5 (1.9, 0)*AB 10.1 (2.1, 0)*AB 5.7 (2.6, 0)#C
Reactmer 8.9 (1.5, 0)*AB 10.5 (2.4, 0)*A 8.8 (2.0, 0)*BC
UniFil F 8.0 (1.6, 0)*AB 9.6 (1.8, 0)*#A 11.4 (2.8, 0)#AB
Toughwell 7.1 (1.9, 0)*B 7.5 (2.5, 0)*B 15.1 (3.6, 0)#A
Z 250 7.8 (1.6, 0)*AB 10.2 (2.5, 0)#AB 9.8 (1.7, 0)#B

F: Number of adhesive failure modes; Within each adhesive technique, mean values designated with the same letters (A, B, C) are
not significantly different ðp . 0:05Þ: With each restorative, means designated with the same symbols (*, #) are not significantly
different ðp . 0:05Þ:
a
N ¼ 10:
Marginal-gap formation of light-activated restoratives
approaching those of phosphoric-acid-conditioned
dentin [7]. A similar difference in aggressiveness
could also be seen on unground enamel.
This self-etching adhesive was studied with both
compomer and resin-composite restorations [8]. It
was demonstrated that a double application of
Adper Prompt L-Pop did not improve performance,
relative to single application, when evaluated by
marginal-gaps in the tooth cavities, and by enamel
and dentin shear bond-strengths. Clearfil Mega
Bond, the least aggressive system had a pH value
of 2.0, while Non-Rinse Conditioner/Prime and
Bond NT that produced moderate etching, had a pH
value of 1.2. Adper Prompt L-Pop, the most
aggressive system at etching unground enamel,
had a pH value of 1.0 [8]. Dental adhesive resins
penetrate the subsurface microporosity created in
etched enamel and the underlying layer of hybri-
dized enamel tissue has been credited with produ-
cing the strong resin-enamel bond. It is possible
that the more hydrophilic resins that are employed
in contemporary adhesive systems produce deeper
penetration into the interprismatic substance of
the etched enamel tissue.
The present data, concerning gap-formation in
enamel margins and enamel and dentin bond-
strength values, showed that in most cases when
using Adper Prompt L-Pop significant improvements
occurred in comparison with the performance of
system adhesives. An exception occurred with One-
up Bond F, where the action of the self-etching
system primer resulted in the formation of a thin
hybridized complex, consisting of a surface zone of
hybridized smear layer and a subsurface authentic
hybrid layer [7,21]. Under such circumstances, the
strength of the resin-dentin bond would depend on
the strength of the polymerized resin components.
This study demonstrated that double-appli-
cations of Adper Prompt L-Pop caused no additional
improvement in performance. However, manufac-
turers of other adhesive systems often advise
double primer applications, which may be entirely
appropriate. For example, the manufacturer
(Dentsply/Caulk, Milford, DE) of Prime and Bond
NT states that if the first application of the adhesive
does not leave a uniform glossy appearance, a
second application is indicated. The manufacturer
of OptiBond Solo Plus Self-Etch Adhesive system
(Kerr, Orange, CA) recommends the use of two
coats of adhesive. However, multiple applications
of one-bottle adhesives had little effect on compo-
site shear bond-strength to dentin [11]. Double
applications had no effect with OptiBond Solo
(Kerr, Orange, CA) or with One-step (Bisco,
Schaumburg, IL) adhesives [12]. The effect of
the adhesive-layer thickness on bond-strength is
879
evidently material-dependent, and care should be
taken to avoid excess adhesive [13]. Increase in the
adhesive-layer thickness by double application of
Adper Prompt L-Pop may affect its stress distri-
bution during polymerization, since shrinkage-
stresses may be concentrated at the interface
during polymerization [16,17]. Since volatile sol-
vents may be removed within Adper Prompt L-Pop
by gently air-drying prior to light-activation (3M
ESPE data), there may be little effect on bonding if
the double adhesive-layer was not too thick. Thus
we observed that the fracture patterns for both a
single and double applications were the same.
These were mostly of interfacial failure between
dentin and adhesive.
The shrinkage behavior of a light-activated
direct restorative material depends on many
intrinsic factors, as well as the host temperature
and environment and the irradiation regime [22].
Examples of these intrinsic factors are the mono-
mer system, the concentration of the catalyst and/or
initiating system, amount of filler, filler type, size
and silane coating. All materials studied incorpor-
ated a light-activated monomer system (Table 1).
Shrinkage of the polymerized restorative materials
has a great effect on their marginal adaptation
[14 – 20].
A marginal shrinkage-gap was created in the
Teflon cavity mold margin during the initial setting
process. The sum of the maximum marginal-gap
width and the opposing width in the Teflon cavity
was taken as a measure of the net setting shrinkage-
strain [18,19] as was the same property measured
after water-storage [20].
The range of marginal-gap values measured
using Teflon molds was generally similar to the
range of results for the same materials placed in
same-size tooth cavities. However, with each
material, the actual values for the Teflon cavities
were distinctly greater than for the tooth cavities.
Restorative materials in Teflon molds are not
susceptible to strong interaction with the cavity
walls due to the non-reactivity of Teflon. The
smaller marginal-gaps observed in natural teeth
than in Teflon molds, confirmed the important
influence of interfacial adhesion. Nevertheless, a
highly significant correlation was found (Table 4)
between the Teflon marginal-gaps and the mar-
ginal-gap in the identically-sized tooth-cavities.
Therefore, it appeared that the immediate shrink-
age-strain of materials had a significant effect on
marginal-gap formation in tooth cavities. The
empirical regression approach to the magnitudes
of marginal gap-widths in Teflon cavities has also
been suggested as a predictor of marginal leakage
in tooth cavities [18,19].
880
Perhaps surprisingly, the trends in shear bond-
strength values to enamel and to dentin were not
determinative at all for the trends in the marginal
gap-width in tooth cavities. As noted above, early
adhesion probably influences the magnitude of
marginal-gaps, making them smaller than they
would otherwise be [18,19].
The values of shear bond-strength to enamel and
to dentin were significantly different for the
restorative materials used this study, even though
the tooth substrate was pretreated by the same
self-etching adhesive system. The mechanical
properties of the adhesive layers may be critical
as most fractured surfaces showed interfacial fail-
ure between dentin and adhesive, and some
cohesive failures in the adhesive layers. Thus the
reasons betanin this result may be complex.
The Gluma-system previously showed a corre-
lation between the marginal gap and bond strength,
when the intermediate resin was changed [5]. In
that study, however, bond-strength was measured
after 24 h, and when there were a number of
common conditions. Therefore, the test conditions
were different from those of the present study.
Further studies on the formation of marginal
gaps, with light-activated restorative materials,
require careful analysis and comparison of the
competing shrinkage and bond-formation abilities.
In conclusion, for light-activated direct restora-
tive materials during the early stage of setting
(, 3 min), application of Adper Prompt L-Pop
exhibited generally superior performance to most
system adhesives. But there was no additional
benefit from double application. The free shrink-
age-strain, measured, by marginal gap-widths in
Teflon cavities, had a greater correlation with
marginal gap-widths in tooth cavities than the
bond-strengths to tooth structure.
Acknowledgements
The authors thank Dr Makoto Okamoto, of the
Department of Removable Prosthodontics, for help
in editing the manuscript and the manufacturers for
supplying the materials.
References
[1] Asmussen E. A microscopic investigation of the adaptation
of some plastic filling materials to dental cavity walls. Acta
Odontol Scand 1972;30:3—21.
[2] Brännström M. Communication between the oral cavity and
the dental pulp associated with restorative treatment. Oper
Dent 1984;9:57—68.
M. Irie et al.
[3] Brännström M, Torstenson B, Nordenvall K-J. The initial gap
around large composite restorations in vitro: the effect of
etching enamel walls. J Dent Res 1984;63:681—4.
[4] Asmussen E. Composite restorative resins. Composition
versus wall-to-wall polymerization contraction. Acta Odon-
tol Scand 1975;33:337—44.
[5] Munksgaard EC, Irie M, Asmussen E. Dentin-polymer bond
promoted by Gluma and various resins. J Dent Res 1985;64:
1409—11.
[6] Van Meerbeek B, Vargas M, Inoue S, Yoshida Y, Peumans M,
Lambrechts P, Vanherle G. Adhesives and cements to
promote preservation dentistry. Oper Dent 2001;Suppl 6:
119—44.
[7] Tay FR, Pashley DH. Aggressiveness of contemporary self-
etching systems. I. Depth of penetration beyond dentin
smear layers. Dent Mater 2001;17:296—308.
[8] Pashley DH, Tay FR. Aggressiveness of contemporary self-
etching systems. II. Etching effects on unground enamel.
Dent Mater 2001;17:430—44.
[9] Gordan VV, Vargas MA, Cobb DS, Denehy GE. Evaluation of
acidic primers in microleakage of Class V composite resin
restorations. Oper Dent 1998;23:244—9.
[10] Miyazaki M, Iwasaki K, Onose H. Adhesion of single
application bonding systems to bovine enamel and dentin.
Oper Dent 2002;27:88—94.
[11] Swift Jr EJ, Wilder Jr AD, May Jr KN, Waddell SL. Shear bond
strengths of one-bottle dentin adhesives using multiple
applications. Oper Dent 1997;22:194—9.
[12] Platt JA, Almeida J, Gonzalez-Cabezas C, Rhodes B, Moore
BK. The effect of double adhesive application on the shear
bond strength to dentin of compomers using three one-
bottle adhesive systems. Oper Dent 2001;26:313—7.
[13] Zheng L, Pereira PNR, Nakajima M, Sano H, Tagami J.
Relationship between adhesive thickness and microtensile
bond strength. Oper Dent 2001;26:97—104.
[14] Feilzer AJ, de Gee AJ, Davidson CL. Curing contraction of
composites and glass-ionomer cements. J Prosthet Dent
1988;59:297—300.
[15] de Gee AJ, Feilzer AJ, Davidson CL. True linear polymeriz-
ation shrinkage of unfilled resins and composites deter-
mined with a linometer. Dent Mater 1993;9:11—14.
[16] Davidson CL, de Gee AJ, Feilzer AJ. The competition
between the composite-dentin bond strength and the
polymerization contraction stress. J Dent Res 1984;63:
1396—9.
[17] Feilzer AJ, de Gee AJ, Davidson CL. Setting stresses in
composites for two different curing modes. Dent Mater
1993;9:2—5.
[18] Irie M, Suzuki K. Marginal gap formation of light-activated
base/liner materials: effect of setting shrinkage and bond
strength. Dent Mater 1999;15:403—7.
[19] Irie M, Suzuki K, Watts DC. Marginal gap formation of light-
activated restorative materials: effect of immediate setting
shrinkage and bond strength. Dent Mater 2002;18:203—10.
[20] Irie M, Suzuki K. Marginal seal of resin-modified glass
ionomers and compomers: effect of delaying polishing
procedure after one-day storage. Oper Dent 2000;25:
488—96.
[21] Watanabe I, Nakabayashi N, Pashley DH. Bonding to ground
dentin by a phenyl-P self-etching primer. J Dent Res 1994;
73:1212—20.
[22] Pananakis D, Watts DC. Incorporation of the heating effect
of the light source in a non-isothermal model of a visible-
light-cured resin composite. J Mater Sci 2000;35:4589—600.
View publication stats
 Necessity of bevels for box only Class II composite restorations
Niek J. M. Opdam, DMD, PhD,a Joost J. M. Roeters, DMD, PhD,b Ruud Kuijs, DMD,c and
Rob C. W. Burgersdijk, DMD, PhDd
University of Nijmegen, Nijmegen, The Netherlands
Statement of problem. The tooth preparation of a bevel is recommended to improve marginal quality of
a composite restoration. However, in small Class II restorations, it is unclear if a bevel also contributed to a
better marginal fit.
Purpose. This study investigated the influence of tooth preparation design on microleakage of minimal
posterior Class II composite restorations.
Material and methods. Box-shaped Class II tooth preparations for posterior composite restorations in
maxillary premolars were restored with a total etch technique. The tooth preparations were beveled or non-
beveled and the box prepared at a right angle cervically or additionally excavated. The facial and lingual box
margins were also either beveled or unbeveled. The teeth were thermocycled and immersed in a dye solu-
tion. After sectioning specimens, dye penetration at the facial and palatal margins was recorded.
Results. A bevel-reduced microleakage both at the cervical and ascending walls. Enamel cracks were
observed along certain unbeveled margins as recorded in this study. The additional excavation did not con-
tribute to reduction of microleakage.
Conclusions. Tooth preparation of a bevel is recommended for an optimal marginal seal in small box-type
Class II composite restorations. (J Prosthet Dent 1998;80:274-9.)

CLINICAL IMPLICATIONS
It is recommended to place a bevel at the margins of small box-type Class II composite
restorations to control marginal leakage.

W hen a tooth is restored for the first time, an

adhesive restoration can preserve sound tooth tissue
compared with conventional silver amalgam.1 This is
particularly true when a tooth is initially restored.
Therefore small carious lesions for the proximal sur-
faces of premolars and molars should conserve sound
tooth tissue.
Tunnel restorations or box-type (saucer-shaped)
restorations are viable alternatives. However, the tunnel
restoration has been difficult to control because of a
limited access to the cavity and poor clinical perfor-
mance.2,3 Although clinical studies have been limited,
current investigations have demonstrated a suitable
clinical performance for box-type restorations.4,5
Considerable effort has been made to reduce the
microleakage of restorations. The inability of restora-
tive materials to seal the interface with tooth structure
encouraged microleakage of intraoral irritants. 6
Bergenholtz et al.7 stated positively that microleakage
This investigation was financially supported by the Dutch Dental
Association (NMT)-Nieuwegein, The Netherlands.
aAssistant Professor, Department of Cariology and Endodontology.
bAssistant Professor, Department of Cariology and Endodontology.
cAssistant Professor, Department of Cariology and Endodontology.
dProfessor, Department of Cariology and Endodontology.
of restorative materials has great clinical significance.
Sensitivity, bacterial infiltration, and secondary caries
may develop from microleakage. An adhesive restora-
tion technique can reduce microleakage particularly
when advanced adhesive systems are selected.8,9 The
dentist has the opportunity to modify the tooth prepa-
ration design of the carious surface with minimal
removal of sound tooth tissue, especially with previous-
ly unrestored teeth. During removal of dental caries of
a Class II defect, the dentist has the opportunity to
either extend the cervical outline of the tooth prepara-
tion to the carious-free dentinoenamel junction or
restrict the tooth preparation to sound enamel. The
dental caries is later removed at the dentinoenamel
junction with a round bur.
Tooth preparation of a bevel is recommended to
improve the bonding surface and reduce microleakage.
However, tooth preparation of a bevel is arduous in
small cavity preparations when the approximal margins
are in contact with the adjacent tooth. In extensive loss
of tooth structure, tooth preparation of a bevel at a cer-
vical margin may result in removal of remaining enam-
el. Another effect of beveling is an enlargement of the
tooth preparation, unless unsupported enamel is pre-
served.

274 THE JOURNAL OF PROSTHETIC DENTISTRY VOLUME 80 NUMBER 3

OPDAM ET AL
Fig. 1. Unbeveled tooth preparation (group 1).
The purpose of this study was to investigate the
influence of a bevel on microleakage of minimal Class
II composite restorations.
MATERIAL AND METHODS
Box-shaped Class II tooth preparations were com-
pleted for 20 extracted sound maxillary premolars,
which were stored in a 1% chloramine solution after
extraction. Each tooth received 2 box tooth prepara-
tions at the mesial and distal surfaces, which were per-
formed with a diamond stone (Meisinger 836012).
The width of the box was 3 mm buccolingual and
the axial depth was 1.5 mm at the cervical margin. The
axial wall was prepared in a parallel direction with the
SEPTEMBER 1998
THE JOURNAL OF PROSTHETIC DENTISTRY
Fig. 2. Beveled tooth preparation (group 2).
tooth long axis. The cervical margin ended 2 mm supe-
rior to the enamel-cement junction.
Teeth were divided into 4 groups of cavity designs,
according to tooth preparations:
Group 1: Tooth preparation remained as described,
which resulted in a butt-joint outline at the cervical
margin and a concave-shaped margin at facial and lin-
gual walls of the box because of the shape of the dia-
mond stone (Fig. 1).
Group 2: Tooth preparation was beveled at the
facial, lingual, and cervical margins. The 45-degree
bevel, 1 mm in width, was made with a fine diamond
stone (Horico FG 539 F 007) (Fig. 2).
Group 3: Same procedures as group 1, except at the
275
THE JOURNAL OF PROSTHETIC DENTISTRY
Fig. 3. Unbeveled tooth preparation combined with excava-
tion (group 3).
cervical wall of the tooth preparation, excavation was
simulated with a round bur (Meisinger HM 1012)
(Fig. 3).
Group 4: Same procedures as group 3; however, the
tooth preparation was beveled at the facial, lingual, and
cervical margins according to the procedure in group 2
(Fig. 4).
The teeth were mounted in an artificial jaw and were
in contact with adjacent teeth to simulate clinical con-
ditions. A Lucifix transparent matrix with light-reflect-
ing Luciwedges material (Hawe Neos, Bioggio,
Switzerland) was placed around each tooth. Tooth
preparations were etched with 35% phosphoric acid
(DMG, Hamburg, Germany) for 15 seconds, rinsed
276
OPDAM ET AL
Fig. 4. Beveled tooth preparation combined with excavation
(group 4).
with water spray for 20 seconds, then gently dried with
a stream of air. Clearfil Photo Bond material (Kuraray,
Osaka, Japan) was mixed and applied to the cavity,
thinned with a gentle stream of air, and cured during
10 seconds of light polymerization (Translux, Kulzer,
Wehrheim, Germany) at an intensity of 600 mW/cm2.
Composite (Clearfil Ray Posterior, Kuraray, Osaka,
Japan) was injected in the cavity with a Centrix tip
(Hawe Neos, Bioggio, Switzerland), in a composite
delivery gun (Caulk - DeTrey Dentsply, Konstanz,
Germany).
Composite was applied in 2 layers. The first layer was
inserted on the floor of the cavity and carefully shaped
against the palatal wall of the cavity. This layer was
VOLUME 80 NUMBER 3
OPDAM ET AL THE JOURNAL OF PROSTHETIC DENTISTRY

Table I. Results for dye penetration

0 1 2 3 4

Cervical dye penetration

Group 2–bevel 10
Group 4–bevel with 5 4 1 *
excavation
Group 3–no bevel with 2 3 2 1 2
excavation
Group 1–no bevel 1 1 6 2
Approximal dye penetration
Group 1/3–no bevel 6 12 2
Group 2/4–bevel 19 1
*Results within same level of significance are marked.

cured for 30 seconds through the light-reflecting

wedge and palatal cusp. Subsequently, a second layer
was injected in the cavity to complete the restoration.
This layer was cured for 30 seconds from the buccal
side through the cusp. Finally, the restoration was
cured for an additional 30 seconds from the occlusal
surface (Fig. 5).
The restorations were removed from the artificial
jaw and finished occlusally with a fine grit diamond
stone (830 C 016, Meisinger, Düsseldorf, Germany)
and approximally with Soflex disks (3M, St. Paul,
Minn.). After 24 hours storage in tap water, the teeth
were thermocycled (500 cycles at 5° to 55°C) and coat-
ed with 2 layers of nail varnish with the surfaces of
restorations remaining free. The teeth were then
immersed in a dye solution (basic fuchsin) for 24 hours.
After embedding the teeth in an acrylic resin (Fas-
tacryl), the teeth were sectioned with a 0.5-mm thick
diamond saw (Bronwill, Rochester, N.Y.).
Teeth were sectioned horizontally so the cervical
half of the restorations remained intact. The section
was inspected from the occlusal surface with a micro-
scope. Dye penetration at the facial and palatal margins
was scored on a 5-point ordinal rating scale: 0, no leak-
age; 1, leakage restricted to enamel; 2, leakage in
dentin not reaching axial cavity wall; 3, leakage to axial
cavity wall; 4, leakage beyond axial cavity wall into the
pulp. Each tooth was subsequently sectioned mesiodis-
tally along the fissure system, and cervical dye penetra-
tion was also scored according to the identical ordinal
rating scale.
Dye penetration at the palatal and facial margins
was statistically compared by using a Mann-Whitney
U-test at P<.05. The data for cervical dye penetration
were statistically compared by using a Kruskal-Wallis
analysis of variance (ANOVA) at P<.05. Statistically
significant differences in microleakage between sepa-
rate groups were computed with the Mann-Whitney
U-test at P<.05, corrected to .01 for multiple group
testing.
Fig. 5. Restorative procedure. A, Application and polymer-
ization of first layer. B, Application and polymerization of
second layer.
RESULTS
Table I presents the microleakage values for various
tooth preparation designs. The Kruskal-Wallis ANOVA
revealed a significant influence of tooth preparation
design on cervical microleakage. The differences in
microleakage between groups were statistically signifi-
cant (Mann-Whitney U-test; P<.05) (Table I).
A bevel at the facial and palatal margins resulted in
95% of restorations without microleakage. The absence
of a bevel resulted in 30% restorations without leakage
and these differences were statistically significant
(Mann-Whitney U-test, P<.05). Microleakage at the
ascending wall extended into the dentin in 10% of the
restorations.
For microleakage at the cervical margin, the cervical
bevel used in groups 2 and 4 resulted in 75% of the
restorations without microleakage at the cervical mar-
gins. Group 2 without microleakage produced the best
results. However, an unbeveled cervical outline result-
ed in only 15% of restorations without leakage and 70%
of the restorations exhibited microleakage in dentin.

SEPTEMBER 1998 277

THE JOURNAL OF PROSTHETIC DENTISTRY
The differences of the groups with additional excava-
tion (3 and 4) with comparable groups without excava-
tion (1 and 2) were not statistically significant. The pat-
tern of microleakage recorded for groups with excava-
tion was commonly dye penetration through a
horizontal fracture between enamel prisms adjacent to
the cervical margin of the restoration. Enamel cracks
inducing microleakage were also observed in restora-
tions of group 1.
DISCUSSION
Research has focused on alternatives to dental silver
amalgam in the treatment of dental caries. Composites
are available that have recorded satisfactory results in
clinical studies. A 3-year clinical study with the same
composite selected for this study demonstrated excel-
lent responses of the restorations without signs of post-
operative sensitivity.10
Insertion of a composite restoration has become less
complicated because of the development of total etch
adhesives that can be applied to dentin and enamel.
The adhesive in our study has demonstrated adequate
performance in other in vitro and in vivo studies.8-10
Therefore, in our study, excellent results were possibly
restricted to small Class II cavities. The beveled restora-
tions recorded virtually no leakage. The experimental
tooth preparation designs in this study were used to
investigate the influence of either a simplification of
tooth preparation design (no bevel) or a design that
preserved cervical enamel.
Tooth preparation of a bevel appeared to reduce the
microleakage both at the cervical and ascending walls.
This was in agreement with other studies that also
observed the phenomenon of enamel cracks along an
unbeveled margin11,12; these cracks were also reported
by Crim and Chapman.13 The additional excavation
did not contribute to a reduction of microleakage. In
similar research, a retentive groove at the cervical wall
was discovered beneficial to reduce microleakage.14
This experimental tooth preparation with a cavosurface
design resembling the cavity preparation of group 4
reduced microleakage.15 However, in one study, a
chemical-curing composite was selected, with a differ-
ent shrinkage pattern.15 Another factor may be that, in
this study, more unsupported enamel remained, as frac-
tures in the enamel close to the margin of the restora-
tion were observed. These fractures were also verified
by Oilo and Jørgensen.16
Marginal leakage in the ascending walls in this study
was restricted to enamel in 95% of the cases, but a bevel
did affect diminished microleakage. Evidently,
microleakage was more pronounced along the cervical
margin. The results may also have been influenced by
the consistency of the composite selected and the mode
of application. Excessive manipulation of the compos-
ite may have also resulted in a reduced adaptation to
278
OPDAM ET AL
the cavity wall.17 In addition, the narrow-shaped area
of the bevel may have hindered the flow of composite
to the cervical outline. However, a suitable adaptation
to the cavity wall was discovered in this study because
the selected composite had a medium consistency and
was injected in the cavity.18,19
This study indicated that a bevel is recommended
when a tooth preparation is made for a minimal Class
II composite restoration. However, in a 5-year clinical
study, different responses were not recorded for Class
II composite restorations with or without a bevel.20 An
11-year clinical study of beveled and nonbeveled Class
III restorations reported no difference in survival
rate.21 Therefore a clinical study that compares beveled
and nonbeveled small Class II box-restorations is nec-
essary to establish the clinical relevance of this study.
CONCLUSIONS
The following conclusions were drawn from this
study.
1. Tooth preparation of a bevel-reduced microleak-
age at both the cervical and ascending walls of a small
Class II box-type composite resin restoration.
2. Tooth preparation of a bevel is recommended for
both cavity designs in this study.
REFERENCES
1. Walls AW, Murray JJ, McCabe JF. The management of occlusal caries in
permanent molars. A clinical trial comparing a minimal composite
restoration with an occlusal amalgam restoration. Br Dent J 1988;164:
288-92.
2. Do Amaral Zenkner JE, Baratieri LN, Monteiro S, Caldeira De Andrada
MA, Vieira LCC. Clinical and radiographic evaluation of cermet tunnel
restorations on primary molars. Quintessence Int 1993;24:783-91.
3. Strand GV, Nordbø H, Tveit AB, Espelid I, Wikstrand K, Eide GE. A 3-year
clinical study of tunnel restorations. Eur J Oral Sci 1996;104:384-9.
4. Nordbø H, Leirskar J, Von der Fehr FR. Saucer-shaped cavity preparation
for composite resin restorations in Class II carious lesions: three-year
results. J Prosthet Dent 1993;69:155-9.
5. Kreulen CM. A study on assessing quality aspects of class II restorations.
[Thesis.] Amsterdam: ACTA; 1992. p. 75-81.
6. Brännström M. Infection beneath composite resin restorations: Can it be
avoided? Oper Dent 1987;12:158-63.
7. Bergenholtz G, Cox CF, Loesche WJ, Syed SA. Bacterial leakage around
dental restorations: its effect on the dental pulp. J Oral Pathol 1982;11:
439-50.
8. Abdalla AI, Davidson CL. Comparison of the marginal integrity of in vivo
and in vitro Class II composite restorations. J Dent 1993;21:158-62.
9. Abdalla AI, Davidson CL. Comparison of the marginal axial wall integrity
of in-vivo and in-vitro made adhesive class V restorations. J Oral Rehabil
1993;20:257-69.
10. Wendt SL, Leinfelder KF. Clinical evaluation of Clearfil photo posterior: 3-
year results. Am J Dent 1992;5:121-5.
11. Lösche GM, Neuerburg CM, Roulet JF. Die adhäsive Versorgung konserv-
ativer Klasse II Kavitäten. Deutsch Zahn Zeitschr 1993;48:26-30.
12. Hilton TJ, Schwartz RS, Ferracane JL. Microleakage of four Class II resin
composite insertion techniques at intraoral temperature. Quintessence Int
1997;28:135-44.
13. Crim GA, Chapman KW. Reducing microleakage in Class II restorations:
an in-vitro study. Quintessence Int 1994;25:781-5.
14. Shahani DR, Menezes JM. The effect of retention grooves on posterior
composite resin restorations: an in vitro microleakage study. Oper Dent
1992;17:156-64.
15. Porte A, Lutz F, Lund MR, Swartz ML, Cochran MA. Cavity designs for
composite resins. Oper Dent 1984;9:50-6.
VOLUME 80 NUMBER 3
OPDAM ET AL THE JOURNAL OF PROSTHETIC DENTISTRY

16. Oilo G, Jørgensen KD. Effect of beveling on the occurrence of fracture in Reprint requests to:
the enamel surrounding composite resin fillings. J Oral Rehabil 1977;4: DR. N. J. M. OPDAM
305-8. DEPARTMENT OF CARIOLOGY AND ENDODONTOLOGY
17. Hansen EK, Asmussen E. Efficacy of dentin-bonding agents in relation to UNIVERSITY OF NIJMEGEN
application technique. Acta Odontol Scand 1989;47:117-20. PO BOX 9101
18. Opdam N, Roeters JJ, Peters TC, Burgersdijk RC, Teunis M. Cavity wall NL 6500 NIJMEGEN
adaptation and voids in adhesive Class I resin restorations. Dent Mater THE NETHERLANDS
1996;12:230-5.
19. Opdam N, Roeters JJ, Peters TC, Burgersdijk RC, Kuyijs RH. Consistency Copyright © 1998 by The Editorial Council of The Journal of Prosthetic
of resin composites for posterior use. Dent Mater 1996;12:350-4. Dentistry.
20. Wilson NH. Performance of occlusion in butt-joint and bevel-edged 0022-3913/98/$.500 + 0. 10/1/91495
preparations: five-year results. 4. Dent Mater 1991;7:92-8.
21. Qvist V, Strøm C. Eleven-year assessment of Class-III resin restorations
completed with two restorative procedures. Acta Odontol Scand
1993;51:253-62.

Effect of heating delay on conversion and strength of a

Noteworthy Abstracts post-cured resin composite
of the Loza-Herrero MA, Rueggeberg FA, Caughman WF, Schuster
Current Literature GS, Lefebvre CA, Gardner FM. J Dent Res 1998;77:426-31.

Purpose. This investigation examined the effect of delayed and post-cure heating (after initial
light-polymerization) on the strength and monomer conversion of 1 commercially available com-
posite.
Material and Methods. A total of 160 disk-shaped specimens (10 × 1 mm thick) were fabricat-
ed from a commercially available composite material (Herculite XRV, Shade A3, Kerr/Sybron).
All specimens were initially light-polymerized for 60 seconds on each side in an aluminum mold
using a controlled light source. Two types of specimens were fabricated. One type was used as a
“light-polymerized only” control, and the other was subjected to post-cure heat treatment for
7 minutes at 100°C. All specimens were coded and stored at room temperature in a light tight
container until needed. The following time intervals between initial light-polymerization and
post-cure treatment of the specimens were 5 and 30 minutes, and 6, 24, 48, 72, 96, and
120 hours. Ten test specimens and 10 control specimens were used for each time interval. After
the designated time delay, the unheated and post-cured composite specimens were subjected to
testing to determine biaxial flexural strength. Ten specimens per test group were then analyzed
for monomer conversion using infrared spectroscopy. Analyses of variance (α = 0.05), Fischer’s
Protected LSD tests, Dunnett’s t tests, and Student’s t tests were used to analyze the data.
Results. Both delay time and type of treatment revealed a significant effect upon the biaxial flex-
ure strength of the specimens, as did the interaction of these parameters. Control specimens
seemed to gain strength with increasing time. This was confirmed by linear regression analysis.
No such correlation existed between strength and delay time for post-cure heated specimens. The
only time intervals that demonstrated greater strength values for the post-cured specimens com-
pared with the unheated control group specimens were the 5- and 30-minute delays. Both delay
time and type of treatment significantly affected the observed cure values (monomer conversion)
and the interaction of these variables. Cure values of unheated specimens were observed to
increase with time after initial light-polymerization. Monomer conversion of heated specimens
also declined with delay in heat application.
Conclusions. Post-cure heating did not significantly affect the biaxial flexural strength of the
composite tested, and time delay of heat application was not a significant factor in strength. Post-
cure heating of the composite significantly affected the increase in monomer conversion, and the
time after which heat was applied following initial light-polymerization was influential. Early
application of heat, after initial light-polymerization, resulted in higher monomer conversion val-
ues. For the greatest amount of polymerization, post-cure heating should be applied within
6 hours after light-polymerization. 17 References.—DL DIXON

SEPTEMBER 1998 279

Nonretentive Bonded Ceramic Partial Crowns:
Concept and Simplified Protocol for Long-lasting Dental
Restorations
Gianfranco Politanoa / Bart Van Meerbeekb / Marleen Peumansc

Purpose: Adhesively luted partial ceramic crowns have been documented to be clinically more durable than direct
composite restorations when minimally invasively restoring large defects (replacing two cusps or more) in posterior
teeth. The clinical longevity of such restorations is largely determined by the tooth-preparation design, material se-
lection and adhesive luting procedure. The most frequently recorded failure in medium- to long-term clinical trials is
fracture of the restoration. The clinical protocol of adhesively luted partial ceramic crowns can be optimized by tak-
ing the etiology of these restoration fractures into account. In this article, a simplified nonretentive bonded ceramic
partial crown concept is presented that aims to achieve an adhesively luted ceramic restoration – composite ce-
ment – residual tooth structure biomechanical unit that maximally resists functional aging. Therefore, the three pri-
mary components of the bonded restoration-cement-tooth complex must function in synergy.
Methods, Results and Discussion: The clinical protocol starts with a tooth preparation designed to optimally absorb
chewing stress. A stable, internally rounded and gently sloping tooth-preparation design with all outer margins in-
clined towards the tooth center assures a favorable and homogenous stress distribution with low cyclic fatigue sub-
jected to the adhesive interface. This preparation form additionally enables the dental technician to fabricate a
well-seating and -fitting ceramic restoration of uniform thickness. As restoration material, monolithic lithium-disilicate
glass ceramic is sufficiently strong for the partial crown indication and preferred in order to decrease the fracture risk.
Clinically essential for a long-lasting restoration is the optimal bond that can be obtained by combined micromechani-
cal interlocking and chemical bonding of composite cement to hydrofluoric acid-etched and silanized glass ceramic.
Conclusion: The clinical effectiveness of this nonretentive bonded ceramic partial crown concept is confirmed by the
overall high success rate as well as the very low fracture and debonding rate, as was recorded in long-term clinical trials.
Keywords: overlay, onlay, tooth preparation, glass ceramic, indirect restoration.

J Adhes Dent 2018; 20: 495–510. Submitted for publication: 26.10.18; accepted for publication: 19.11.18
doi: 10.3290/j.jad.a41630

R estoring posterior teeth exhibiting large defects (replac-

ing two cuspids or more) with directly bonded restor-
ative composite is possible, but can be very challenging for
a Dentist in Private Practice, Rome, Italy. Developed the concept, constructed
the figures, proofread the manuscript.
b Full Professor; KU Leuven (University of Leuven), Department of Oral Health Sci-
ences, BIOMAT & UZ Leuven (University Hospitals Leuven), Dentistry, Leuven,
Belgium. Proofread the manuscript.
c Associate Professor; KU Leuven (University of Leuven), Department of Oral
Health Sciences, BIOMAT & UZ Leuven (University Hospitals Leuven), Den-
tistry, Leuven, Belgium. Wrote the manuscript.
Correspondence: Professor Marleen Peumans, KU Leuven (University of Leuven),
Department of Oral Health Sciences, BIOMAT & UZ Leuven (University Hospitals
Leuven), Dentistry, Kapucijnenvoer 7, B-3000, Leuven, Belgium. Tel: +32-16-
332744; e-mail: marleen.peumans@kuleuven.be
the dentist, in particular in busy clinical practices where
treatment time should be as short as possible.69 Upon a
detailed biomechanical analysis of the remaining tooth
structure, the tooth should be prepared minimally inva-
sively, preserving as much sound tissue as possible, while
removing any tooth parts with doubtful stability. In this
sense, thin unsupported cusps must be reduced, as this
will increase the durability of the restoration. The most dif-
ficult steps in the fabrication of large direct posterior com-
posite restorations are the creation of a correct form with
good occlusal anatomy as well as of well-contoured proxi-
mal surfaces with strong and correctly positioned contact
points with the neighboring teeth. A posterior tooth restored
in this direct composite workflow can function quite well in
the medium term (ca 3-5 years).27,54,85 Bruxism and high
caries risk seriously affect the durability of extensive com-
posite restorations.68,92 Bonded indirect ceramic partial

Vol 20, No 6, 2018 495

Politano et al
a b
Biomechanical tooth
preparation analysis
c tioned obliquely to give good mechanical support to the restoration.
d e
partial crown
luting composite
tooth
Fig 2 SEM photograph of a cross-sectioned molar restored with a
bonded lithium-disilicate glass-ceramic partial crown. The section
shows the different components of the bonded ceramic restoration-
luting composite-tooth complex. The three components must func-
tion in synergy in order to restore the tooth in a durable way.  Cement-Tooth Complex
crowns, often also being referred to as “onlays” and “over-
lays”, have been documented to be more durable when
posterior teeth with large defects need to be minimally inva-
sively restored (Fig 1).5-8,20,25,31,40,52,67,93 Of the different
factors that contribute to the success of a restoration, in
particular the material properties and adhesive luting tech-
niques have frequently been studied in the literature, result-
ing in fairly uniform guidelines for the dental practitio-
ner. 17,78 However, no consensus has been reached
regarding a proper preparation form for this restoration
type.2,10,21,22,41,53,78,88,89 Nevertheless, the tooth-prepara-
tion design is a very important factor determining the suc-
cess of bonded indirect ceramic partial crowns.2,3 In this
496
Fig 1 a. Initial situation. The patient complained of pain in the first
mandibular molar during biting. This tooth showed an unacceptable
amalgam restoration with caries underneath and a crack at the dis-
tal side. b. After removal of the amalgam filling, infectious dentin
underneath became visible. The crack at the distal side ran towards
the tooth center. The cusps were undermined by caries. c. The tooth
was prepared for a lithium-disilicate glass-ceramic partial crown. All
infectious dentin was removed. Due to the heavy loading on the buc-
cal and lingual cusps and caries undermining the cusps, the cusps
were reduced (minimum 1.5 mm) to a level at which enamel was
supported by dentin. d. Final simplified preparation for a bonded
nonretentive lithium-disilicate glass-ceramic partial crown. The prep-
aration area is antifragile. The dentin surface was protected by im-
mediate dentin sealing (IDS) and the undercuts were blocked out
with a highly filled flowable composite. The enamel prisms were sec-
e. The bonded lithium-disilicate glass-ceramic restoration shows a
perfect integration with the surrounding tooth structure. An optimal
bond of the ceramic restoration via the luting composite to the tooth
is required to ensure a long-lasting restoration. 
article, a simplified nonretentive tooth-preparation concept
is presented for these restorations. The aim of this simpli-
fied preparation concept is to create an adhesively luted
ceramic restoration–composite cement–residual-tooth-struc-
ture biomechanical unit that functions in the most favorable
way and results in a long-lasting restored tooth.
The basic principles of the bonded restoration-cement-
tooth complex and their contribution to the durability of the
restored tooth will be discussed first. Second, a correct bio-
mechanical analysis before and during tooth preparation
will determine the amount of tooth and cusp reduction.
Third, the clinical protocol for restoring teeth with bonded
ceramic partial crowns will be described step by step. Fi-
nally, the clinical durability of nonretentive bonded ceramic
partial crowns will be discussed based on literature data.
1. Basic Principles of the Bonded Restoration-
After restoring the tooth with a bonded partial ceramic
crown, a strong biomechanical unit consisting of the resto-
ration bonded to the remaining tooth structure is created
(Fig 2). The three components of this complex should work
in synergy to result in a long-lasting restoration.
1a. Tooth preparation
Today, bonded ceramic partial crowns are scientifically rec-
ognized as adequate tooth restorations for the posterior
region. Despite the good medium- to long-term results, it is
important to draw correct conclusions from failures that
have occurred in clinical trials.6,31,40,52,67,80,93 The main
reason for failure in all these clinical trials is (partial/total)
fracture. A higher frequency of fractures is recorded for the
older feldspar ceramics and leucite-reinforced glass-ceram-
ics, compared to the newer and stronger lithium-(di-)silicate
glass-ceramics, possibly reinforced with zirconia, that today
The Journal of Adhesive Dentistry

a b
c d
Fig 3 a. Initial situation. The old composite restorations with car-
ies recurrence on both mandibular molars needed replacement. b.
Removal of the existing restorations and caries resulted in deep,
wide cavities. When kept, the lingual and buccal cusps would func-
tion as long cantilever arms. Reduction of all cusps was therefore
indicated. c. The cusps were reduced (minimum 1.5 mm) to a level
at which enamel was fully supported by dentin. The dentin surface
was smoothed. All margins were located in enamel. The prepared
tooth surface was then ready for IDS and out-blocking of the under-
cuts. d. Two lithium-disilicate glass-ceramic partial crowns were
bonded with a light-curing restorative composite.
can be used for this indication.6,8,67,74 It should be noted
that the geometry of the tooth preps in these clinical trials
did not often match well with the material-specific proper-
ties of hard and brittle ceramic materials. Nonetheless, the
fracture resistance of the bonded ceramic restorations
should be increased. New guidelines for the preparation
form of bonded all-ceramic restorations were formulated by
Ahlers et al2 and Arnetzl and Arnetzl.3,4 These guidelines
describe eight points of interest. First, cavities designed for
ceramics must have the simplest possible basic geometry.
Second, an appropriate and uniform layer thickness of the
restoration is recommended (minimum 1.5 to 2 mm). Third,
corners and sharp edges must be avoided. Fourth, high ten-
sile stresses should be avoided and must be transformed
whenever possible into compressive stresses by changing
the prep design. Fifth, stress peaks and sudden changes in
cross-section should be avoided by soft and smooth transi-
tions. Sixth, notch stresses must be minimized. Seventh,
the contact surface with the ceramic restoration must be
made as large as possible. Finally, enamel bordered resto-
ration margins facilitate a stable and adhesive bond of the
ceramic restoration via the luting composite to the remain-
ing tooth structure and will thus permanently guarantee bet-
ter marginal quality.
Fairly similar geometrically simplified preparation designs
were tested in vitro4,10,60,62,83 and in vivo.5,7,40,64,75 In
some laboratory studies, the teeth were prepared for the
treatment of occlusal wear with so-called occlusal ve-
neers.10,41,60,62,83 It must be emphasized that in all in vitro
studies intact natural teeth were prepared, while in daily
clinical practice moderate to heavily destroyed teeth are
Vol 20, No 6, 2018
Politano et al
most often prepared for ceramic partial crowns. Therefore,
in this article the preparation design will be described start-
ing from a real clinical situation, ie, a moderately compro-
mised tooth (Fig 3). In addition, the nonretentive tooth-prep-
aration design will be considered as part of an entire
concept, resulting in the most favorable biomechanical
loading of the bonded restoration-cement-tooth complex.
The main features of this modified tooth-preparation de-
sign are fourfold and described in Fig 4. After biomechani-
cal analysis (see below), the preparation phase starts with
removal of the existing defective restoration and selective
removal of decayed and infected tissues (Figs 3a and 3b).
Next, a smooth dentin surface is created with gradual and
soft transitions between concavities and convexities
(Fig 3c). No resistance and retention form is required. The
preparation outline follows a smooth and fluid curve, with
open angles to increase and ensure the mechanical stabil-
ity of the restoration.
The tooth preparation consists of a dentin part that is
(ideally) completely surrounded by enamel. As mentioned
above, the prepared dentin surface should be clean and
may not show sharp irregularities. This increases the inter-
nal adaptation and marginal fit of the partial crown when
compared with a retentive tooth-preparation design, as was
demonstrated in vitro by Kim et al.50 The better the adapta-
tion, the lower the thickness of the cement layer, the easier
the restoration can be positioned onto the prepared tooth
surface, the easier the cement will flow during seating and
cementation, and the more precise the occlusion. If the ce-
ment layer can be reduced to the thinnest possible layer,
there is less risk of interference with occlusion and articula-
tion after cementation of the restoration. Poor marginal fit
can exacerbate degradation of the cement in the oral envi-
ronment, resulting in microleakage, marginal discoloration,
recurrent caries, and periodontal disease.26,46 Although
there is no consensus on the optimal internal cement
space for adhesively luted ceramic restorations, an internal
space of 50-100 µm has been advocated for good perfor-
mance of composite cements65,86 (Fig 4b). A large internal
cement space can cause higher polymerization shrinkage of
luting cement and less optimal support to the ceramic res-
toration. In addition, bond strength of composite cements
to glass ceramics was postulated to decrease with an in-
crease of composite-cement film thickness.9
A flat surface also results in a lower C-factor, decreasing
the polymerization stress of the luting composite compared
to a cavity prep with a complex configuration.24 However,
one has to take into account that there is limited relaxation
of polymerization stress due to flow because the luting
composite is bonded at all sides. Feilzer et al23 reported
that when the thickness of the resin composite is thinned
down, as when used as luting agent, the wall-to-wall polym-
erization shrinkage may be three times the normal linear
contraction of bulk resin composite. This is one of the rea-
sons why it is advisable to use a light-curing restorative
composite for cementation, as the polymerization shrinkage
is lower compared to a dual-curing luting composite with
lower filler content.
497
Politano et al
partial crown
luting composite
enamel IDS + flowable
dentin
a plication of IDS and blocking out the undercuts with a flowable
partial crown
50–100 micron
enamel
dentin
b 100 µm (small white arrows). Ideally, the prep margins are located
eccentric centric
partial
crown
maximum
eccentric
stress
stress dissipation preparation
c platform
The prep margin is very precise and defined, allowing the
dental technician to read the prep margin very clearly. Ide-
ally, the prep margin must be located in enamel in order to
obtain an optimal marginal seal and to give long-term stabil-
ity to the large dentin adhesive surface.15,22 The prepara-
tion in enamel also follows the antifragile concept and is
able to support the restoration well. The enamel prisms
must be sectioned obliquely (Figs 4b and 4c). As was
shown by Giannini et al,33 bonding to obliquely sectioned
enamel results in a significantly higher bond strength than
to horizontally cut enamel. This obliquely sectioned enamel
will be completely supported by dentin. The stresses will be
relocated in a centripetal way inside the tooth, not outside
(Fig 4c). The restoration will benefit from the most stable
support in the areas where the maximum eccentric stress
is concentrated (Fig 4c). Final preparation of the enamel
margin should be carried out after application of “immedi-
ate dentin sealing” (IDS).
Once the dentin surface has been adequately prepared,
IDS is performed as part of the indirect two-visit workflow.
This includes the formation of a high-quality hybrid layer
upon preferential application of either a mild 10-MDP-based
2-step self-etch adhesive (ie, Clearfil SE Bond 2, Kuraray
Noritake; Tokyo, Japan) or a 3-step etch-and-rinse adhesive
(ie, Optibond FL, KerrHawe; Orange, CA, USA), each accord-
ing to the instructions of the respective manufacturer. IDS
immediately seals dentin and blocks water uptake through
osmosis from dentin underneath. Placing a highly filled flow-
able composite on top of the adhesive layer enables to mi-
cro-selectively block out potential tooth-preparation under-
498
Fig 4 a. SEM photographs of the ceramic restoration-luting com-
posite-tooth complex showing the four requirements of the tooth-
preparation design. (1) The preparation area (white small-dotted
line) must be antifragile, as during occlusion and articulation, the
working and non-working occlusal forces are mainly concentrated in
the lower half of the tooth. (2) The prepared surface must be
smooth without any abrupt transitions to decrease stress concentra-
tion at the restoration-luting composite-tooth complex. (3) After ap-
composite, a stress dissipation area is created (white long-dotted
line). This means that the forces, absorbed by the restoration, are
transferred in the most favorable way to the adhesive interface and
the tooth, by converting the tensile stress in the ceramic and at the
interface as much as possible into compressive stress. b. A fourth
requirement is that the prep margins are precisely defined and the
preparation allows for the best possible internal and marginal fit of
the ceramic partial restoration. The luting area varies between 50-
in enamel (large white arrows), although this is determined by the
extent of lesion. The enamel prisms must be cut obliquely to ensure
maximum bond strength and to create optimal mechanical stability
for the restoration (blue arrows). c. By sectioning the enamel prisms
in an oblique way, the stresses will be mainly relocated in a centrip-
etal way inside the tooth, not outside the tooth. The restoration will
have the most stable support in the areas where the maximum ec-
centric stress is concentrated.
cuts (Figs 1d and 4a). IDS protects the freshly cut dentin
surface, awaiting that the ceramic restoration is made by
the dental technician. Post-operative sensitivity is thus pre-
vented.63,76 Furthermore, IDS allows a stress-free dentin-
bond development, which even in vitro has been docu-
mented to result in a significantly higher dentin-bond
strength compared to delayed bonding (adhesive procedure
just before cementation).18,39,58 Finally, the IDS layer (hy-
brid layer + adhesive layer + flowable composite) forms a
stable and strong platform for stress dissipation during oc-
clusal loading (Fig 4c). The micro-buildup with the well-stabi-
lized hybrid layer creates a smooth and regular surface that
allows for the most favorable stress distribution (mainly
compressive stress) during occlusion and articulation.
A composite macrocore buildup is not indicated as this
increases the stress on the recently formed hybrid layer. In
addition, such a bonded core buildup has a lower elastic
modulus and thus will flex more than the overlying ceramic
restoration, by which high tensile stresses may develop in
the ceramic at the interface with the cement, just below the
loaded area. This can cause the formation of cracks in the
ceramic at the interface, which may grow towards a total
bulk fracture at a later stage.47,48 An exception can be
made for an endodontically treated premolar when little
amount of tooth structure is remaining. In this situation, a
macrocore buildup can be made to provide more retention
to the restoration and to achieve a better resistance form
against lateral forces (Fig 5).
Regarding this new simplified tooth-preparation concept, it
must be emphasized that this concept works only on the con-
The Journal of Adhesive Dentistry

a b
Fig 5 Macrocore buildup on an endodontically treated premolar. A
fiber-reinforced composite (EverX Posterior, GC; Tokyo, Japan) is
used to fill the pulp chamber and to constitute the macrocore
buildup. It was covered with a highly filled flowable composite. This
macrocore buildup was needed to provide retention to the restora-
tion and to resist lateral forces during articulation.  to the center of the tooth. b. The buccal surface of the overlay on
dition that a high-quality bond is obtained with the existing
tooth structure. If application errors are made in this regard,
failures of the restoration can be expected in the short term.
1b. Ceramic restoration
Regarding the ceramic materials for bonded indirect restora-
tions, the most favorable results in vivo and in vitro are
obtained with the strongest etchable ceramics nowadays
available on the dental market, ie lithium-disilicate glass
ceramics.7,8,10,40,56,60,62,64,75,83,95 Today, so-called zirco-
nium-reinforced lithium-silicate glass ceramics are also
available. Lithium-(di)silicate glass ceramics present with a
similar wear behavior as enamel.81 At the moment, the
commercial glass ceramic e.max CAD/e.max Press (Ivoclar
Vivadent; Schaan, Liechtenstein) is the most studied lith-
ium-disilicate glass ceramic in the literature.
The thickness of the ceramic restoration (minimum
1.5 mm) must be as uniform as possible, in order to have a
more homogeneous distribution of stresses and forces in-
side the restoration, the prepared tooth surface and across
the adhesive interface during occlusal loading. This is real-
ized if the guidelines for this preparation design as de-
scribed above are followed. Promising results were recorded
in vitro with “occlusal veneers” for the treatment of occlusal
wear in thicknesses of 0.5 -1 mm, especially when the res-
torations were bonded to enamel.10,41,62,84 At the moment,
no in-vivo studies are available that show that these mini-
mally invasive occlusal veneers work well in the medium- to
long-term. The main indication for a partial ceramic crown
presented in this article is to restore moderately to severely
compromised teeth. As it is the aim to make a durable res-
toration with a proven clinical performance, the restoration
must have a minimum thickness of 1.5 mm.3,56 In addition,
the partial crown must restore the natural anatomy of the
tooth (Fig 6). This means correct inclination of the buccal
and lingual cusps (outer and inner inclination), just in order
to have a loading that will be transferred to the tooth cor-
rectly. During occlusal loading the stresses must be relo-
cated in a centripetal way from the periphery to the center
of the tooth, in order to allow the tooth to work like a natu-
Vol 20, No 6, 2018
Politano et al
a b
Fig 6 a. The partial crown must restore the natural anatomy of the
tooth (blue arrows). The buccal and lingual cusps must have the cor-
rect inclination in order to induce loading that is transferred cor-
rectly to the tooth (red arrow). This means that during occlusal
loading, the stresses are relocated centripetally from the periphery
the maxillary first molar has a correct inclination (white arrow) for
optimal stress distribution in the restored tooth. 
ral, intact tooth and to be able to dissipate the loads much
better along the long axis of the roots.
In this proposed concept, the retention of the restoration
mainly relies on bonding. Hence, the quality of the bond to
the restoration is of key importance and is a dominant factor
required for the long-term success of the bonded lithium-(di)
silicate glass-ceramic restoration. Composite cements pro-
vide the strongest and most durable bonding of ceramics to
tooth structure and contribute to a higher ceramic strength.91
It is generally accepted that adhesion of composite ce-
ments to ceramics is provided by two major mechanisms:
micromechanical interlocking and chemical bonding. Micro-
mechanical interlocking or micro-retention can be provided
upon hydrofluoric-acid (HF) etching, whilst a silane coupling
agent increases the wettability of the ceramic surface and
provides a primary chemical bond.91 Various glass ceramics
differ in chemical composition and microstructure, by which
it is necessary to establish bonding procedures according
to the glass-ceramic type.19,55,73 Lithium-disilicate glass
ceramic requires a shorter HF acid-etching time (20 s) com-
pared to feldspatic and leucite-reinforced glass ceramics.
Regarding etching time, it is important to follow the instruc-
tions of the manufacturer.
1c. Luting composite
The strongest luting composite must be selected to create
a good support for the partial ceramic crown; the antifragile
margin preparation (Fig 4b) is a key determinant as well.
Therefore, a light-curing restorative composite is preferred
to be used as luting agent. A restorative composite is more
wear-resistant and has better physico-mechanical proper-
ties than a conventional dual-curing luting composite with
lower filler content. In two in vitro studies, feldspatic ce-
ramic blocks (Vita Mark II, Vita; Bad Säckingen, Germany)
with a 4-mm thickness and lithium-disilicate glass-ceramic
blocks (e.max CAD HT, Ivoclar Vivadent) with even an 8-mm
thickness were bonded to flat dentin surfaces using differ-
ent luting composites.45,82 Both studies showed that the
micro-tensile bond strength of the light-curing restorative
composite applied in combination with a 2-step self-etch
499
Politano et al
enamel-dentin thickness of the remaining cusps: amount of cusp reduction
cut = critical unsupported
dental structure
prepare = reduction of the height
save = hybridization &
micro-build-up
a dentin. However, if there is a little wall left where enamel is not com-
b c
d e
adhesive (Clearfil SE Bond, Kuraray Noritake) was signifi-
cantly higher compared to the tested conventional dual-
curing luting composites applied with their accompanying
adhesives. Similarly, other in vitro studies showed that a
light-curing restorative composite can be used to lute thick
ceramic/composite restorations.35,38 To obtain this result,
it is important that the restorations transmit light suffi-
ciently, sufficiently powerful LED light-curing units are used,
light curing is conducted from different sites and that the
curing time is prolonged extensively and sufficiently. The
curing time should be 60 seconds per surface (vestibular,
lingual/palatal, occlusal for premolars, occlusal at mesial
and distal side for molars). In all the above-mentioned in
vitro studies, fairly translucent ceramics/composites were
used (with an opacity of about 50%). In general, for the
fabrication of ceramic partial crowns, translucent lithium-
disilicate glass ceramics are used as they give the most
natural outcome. Several clinical trials have also shown
that inlays/onlays bonded with a light-curing restorative
composite function well in the long term.12,31,40,52,80
Cement excess removal is easier thanks to the higher
viscosity of the restorative composite as compared to the
significantly more fluent and thinner luting composites. Spe-
cific restorative composites such as Clearfil AP-X (Kuraray
Noritake) were for instance found to have near-ideal vis-
cosities for luting, even when used at room temperature.
Preheating stiffer restorative composite might be indicated
to decrease viscosity; preheating composite in turn facili-
tates the seating of the restorations and contributes to a
higher degree of conversion.1,71 Clinically, luting with a
500
Fig 7 a. The enamel-dentin thickness of the remaining cusps and
the cavity depth determine the amount of flexure of the cavity walls.
For a bonded indirect lithium-disilicate glass-ceramic restoration: (1)
the non-undermined cusp (right side) is reduced with 1.2-1.5 mm if
the cavity is deep and wide. The long cantilever arm would otherwise
flex too much during occlusal loading and can result in fracture after
long-term clinical functioning. (2) The greatly undermined cusp (left
side) should be reduced to the level at which enamel is supported by
pletely supported by dentin (yellow arrow), this little wall can be kept,
as the flexure arm is dramatically reduced by reducing the cusp to
this level. It is preferable to block out the undercuts with a flowable
composite (green arrow) and to keep the margin in enamel in the
cervical area in order to obtain an optimal bond at that cervical mar-
gin. b. Shortcoming in the preparation on the first molar. The inten-
tion was to be less invasive by keeping the two cusps. These cusps
were, however, not stable enough to resist flexure during occlusion
and articulation, having resulted in rapid mechanical degradation of
the adhesive interface. c. After cementation of the lithium-disilicate
glass-ceramic partial crown with a light-curing restorative composite,
the larger luting area at the buccal side can be noticed. This will be
a weak area in this restoration. d. The thick cusps on the prepared
molar can be kept. The remaining cusps are able to resist the forces
during occlusion and articulation and will not flex easily. Conse-
quently, the interface will be less stressed. e. The thick buccal cusp
of the maxillary premolar was maintained for esthetic reasons.
light-curing restorative composite gives the practitioner
much more control on complete removal of cement excess
and substantially increases the work time to accurately re-
move cement excess, especially in the difficult interdental
areas. Good radio-opacity of the luting composite (higher
than that of dentin) is required in order to visualize poten-
tial residual excess of composite after cementation. Having
a nearly unlimited work time (when the dental unit light is
moved away and/or an orange light filter is used on a den-
tal operating microscope or the light source connected to
magnifying glasses), multiple ceramic restorations in light
of a quadrant restorative treatment is clinically feasible.
2. Biomechanical Analysis
Dental tissues respond biologically to stresses and strains
imposed during mastication. Teeth compromised due to ex-
tensive carious lesions or large restorations tend to weaken
the tooth. The stresses in teeth associated with these condi-
tions may lead to cusp fracture. It is essential to prevent
fractures by starting from a clear concept with a sound tooth-
preparation design and by anticipating the stresses of masti-
cation that may be imposed to the remaining tooth structure.
For these reasons, the restorative procedure of a bonded
(direct/indirect) restoration in the posterior region always has
to start with a profound biomechanical analysis of the tooth.
This includes analysis of the forces and loading on the tooth
during occlusion and articulation, as well as analysis of the
amount and quality of the remaining tooth structure.
The chewing forces and occlusal loading imposed on a
tooth are determined by the anatomic position of the tooth
The Journal of Adhesive Dentistry

in the arch, the patient’s occlusion and musculature, and
the functional and parafunctional load on the tooth. The oc-
clusal loads increase from anterior towards posterior, from
mesial towards distal, and from premolars towards molars.
Increasing loads will automatically increase the risk of frac-
ture. The occlusion and articulation on the tooth to be re-
stored should beforehand be registered with articulation
paper, in order to analyse the strength and location of the
occlusal contacts at the future restoration margins and on
the remaining cusps.
The amount and quality of the remaining tooth structure
is analysed by evaluating the size of the existing restoration
and the presence of decay, defects, cracks and wear facets.
The type, size and depth of the cavity preparation deter-
mines the reduction in fracture resistance of the tooth to a
great extent. The fracture resistance of intact teeth, teeth
with a cavity prep and restored teeth was studied in several in
vitro studies using different methods such as finite element
analysis, measuring cuspal deflection or cusp stiffness during
occlusal loading, and by fracture tests.34,36,42,59,66,70,77
These studies show that increasing the depth of the cavity,
increasing the isthmus width and loss of the marginal
ridges resulted in the largest reduction in fracture strength.
The fracture resistance of teeth with cavities gradually de-
creases for teeth having solely an occlusal class-I cavity, to
teeth undermined by a two-surface class-II cavity, and finally
teeth exhibiting a three-surface MOD cavity preparation hav-
ing the lowest fracture resistance. Large MOD cavities re-
sulted in a decrease in fracture resistance by 59% to 76%,
compared to that of intact teeth.13,16,77,87 Other in vitro
studies recorded that occlusal loading (150 N) of premolars
with an MOD cavity resulted in a widening of the cusps over
a distance of 114-179 µm.36,59 After direct restoration of a
tooth with composite, a cusp deflection of about 7-9 µm
was still measured. One also has to take into account the
changes that take place at the cusps due to polymerization
shrinkage of the composite, as was shown by Tantbirojn et
al90 and González-López et al.37 The adhesive is also a de-
termining factor. The observed effects will be magnified if
the bond is inadequate. According to Reeh et al,77 end-
odontic procedures alone (access preparation, instrumenta-
tion and obturation) have only a small effect on the tooth,
reducing its relative stiffness by 5%. This reduction in stiff-
ness did not depend on the sequence of the endodontic
treatment before or after cavity preparation. Other in vitro
studies recorded a more pronounced decrease in fracture
resistance after endodontic treatment.42,70 The least favor-
able situation regarding fracture resistance of the prepared
tooth is an endodontically treated premolar/molar with a
large MOD cavity.32,36,42,70,77 In these teeth, complete
cusp coverage (overlay) is needed to increase the fracture
resistance of the restored tooth.
In summary, the reduction in fracture resistance will be
most pronounced in teeth with large, wide and deep cavi-
ties. Bonding of a restoration to these cavity walls rein-
forces the tooth, but flexure will still occur during occlusal
loading. This results in mechanical degradation of the adhe-
sive interface. Along with hydrolytic and enzymatic bond
Vol 20, No 6, 2018
Politano et al
degradation, loss of adhesion will occur with time, leading
to open coronal margins, marginal discoloration, secondary
caries, increased flexure of the cavity walls, and possible
fracture of the cusp. In these kind of large, wide and deep
cavities, where the cusp functions as a long cantilever arm,
cusp reduction followed by cusp coverage increases the
fracture resistance of the tooth and the clinical longevity of
the restoration4,42,57 (Fig 7a). For a bonded indirect ceramic
partial crown, one should avoid keeping cusps that flex dur-
ing occlusal loading, as they will negatively influence the
longevity of the restoration (Figs 7b and 7c). Hence, a cusp
can be maintained in the following situations:
1. A very thick cusp that is able to support occlusion and
articulation (Fig 7d). The cusp contributes to a great ex-
tent to the fracture resistance of the tooth. Keeping this
part of the tooth structure does not provide many prob-
lems of instability to the residual dental structure. The
remaining cusp is able to resist the forces during occlu-
sion and articulation and will not flex easily. Conse-
quently, the interface will be less stressed. A shortcom-
ing in these situations is that the occlusal margin is not
protected. Enhanced exposure of the restoration margin
to occlusal wear results in more extensive marginal dis-
crepancies.88 In addition, as enamel wears more than
ceramic in these areas, positive ceramic steps will be
formed after long-term clinical functioning. If these
steps are not adjusted, initial cracks may be initiated at
exactly these points.31,51 Therefore, when making a par-
tial crown that does not cap all cusps, the fit and adap-
tation at the occlusal surface must be perfect and the
luting marginal gap must be kept as small as possible.
2. A thick buccal cusp of a maxillary premolar can be main-
tained for esthetic reasons, but the strength of the fi-
nally restored tooth will not be the same as that of one
restored with a circumferential preparation (Fig 7e). In
these situations, we need to evaluate the latero-trusive
path and the guidance of the premolars. In case of a
missing first molar, the premolars are often overloaded
during occlusion and articulation.
In all other situations, the cusps are better reduced as this
allows the ceramic restoration to function in the best pos-
sible condition, namely under compression. Reducing the
cusps contributes to the antifragile preparation form. In
general, for bonded indirect lithium-disilicate glass-ceramic
restorations, the cusps, where enamel is supported by den-
tin, are reduced with 1.2 to 1.5 mm. This is a slightly more
invasive approach than what is often described in the litera-
ture, where cusps 2.0 to 2.5 mm thick are kept.5,53 The
main goal of this minimally hazardous dentistry is to create
a long-lasting restoration-cement-tooth complex.
3. Clinical Protocol, from Concept to Clinic
The different steps of the clinical protocol are explained in
detail and documented with clinical pictures (Figs 8-20).
501
Politano et al
a b c
Fig 8 a. Initial situation. Maxillary molar with unacceptable amal-
gam restoration. Large marginal defects are noticed. b. Biomechani-
cal analysis of the buccal part of the tooth. The presence of cracks
decreases the fracture resistance of the tooth. The wear facets indi-
cate heavy loading during occlusion and articulation. One can expect
the buccal cusps to be undermined. Cracks are noticed at enamel
surrounding the amalgam restoration. c. Biomechanical analysis of
the palatal side of the tooth. Similar as at the buccal side, open
margins and wear facets can be observed. A crack line is noticed at
the distal marginal ridge.  gins. Gingival correction without or with removal of the sup-
a b
c d
Fig 9 a. The unacceptable amalgam restoration was removed in a
minimally invasive way with a multiblade tungsten carbide bur. An ul-
trasonic device with water cooling can be used to remove the last
pieces of amalgam at a low biological cost. b. Caries-infected dentin
was removed with a round tungsten carbide bur (Komet H1SEM,
Brasseler; Lemgo, Germany) dry and at low speed (7000 rpm). A cen-
tripetal approach was followed. This included starting at the periph-
ery towards the critical points. In this way, possible pulp exposure
would have been programmed. It is very important that all caries-in-
fected dentin be removed in order to realize a good-quality hybrid
layer that will remain stable in the long term. c. After removal of the
restoration and all infected tissues, a more detailed biomechanical
analysis takes place. The thickness and quality of the cusps, the
thickness of marginal ridge and the presence of crack lines was con-
trolled. At the buccal side, the cusps were undermined. Cusp reduc-
tion was needed. d. At the palatal cups, enamel was supported by
dentin. Because of the heavy occlusal loading (wear facets) and the
crack line at the distal side, the palatal cusps were also reduced.
502
3a. Biomechanical analysis of the tooth before removal of
the defective restoration (Fig 8)
See Fig 8.
3a. 1. Evaluation of the quality and amount of remaining tooth
structure
Size and depth of the existing restoration, decay and de-
fects will inform the dentist about the most optimal restora-
tion type (direct versus indirect; cusp capping or no cusp
capping).
A radiograph shows the depth of the existing restoration
and caries, and the risk of pulp exposure.
Evaluate the future location of the proximal prep margin.
Take correct measures in case of deep subgingival mar-
porting bone can relocate the margins iuxta- or supragingi-
val.94 Removal of the supporting bone is indicated when the
biologic width has been invaded. A non-invasive alternative
of surgical crown lengthening to bring the margins supra-
gingivally is deep margin elevation (DME). This technique
proposes the application of composite resin in the deepest
part of the proximal areas in order to reposition the cervical
margin supragingivally, which is expected to facilitate isola-
tion and improve impression-taking and adhesive luting of
the indirect restoration.17,49,61 Several in-vitro studies show
promising results with DME.29,43,79,96 However, the influ-
ence of the DME technique on clinical performance, longev-
ity of the restorations and periodontal health is not yet
known.44 A 12-month clinical trial showed that DME is a
clinically sensitive technique, especially when performed on
deep subgingival margins.28 A higher incidence of bleeding
on probing was recorded on teeth treated with DME and in
coincidence with deep margins placed at or closer than
2 mm to the bone crest.
Next, the tooth to be restored is analysed for presence
of cracks and fractures. These critical areas decrease the
tooth’s fracture resistance. The presence of wear facets
indicates heavy loading during occlusion and articulation.
Cusp capping in these regions will be needed in case of a
bonded indirect lithium-disilicate partial crown.
3a. 2. Analysis of forces and loading on the tooth to be
restored
Attention should be paid to the patient’s musculature, func-
tional/parafunctional activities, intensity and direction of
the forces, location and strength of the contact points, and
loading of the cusps.
3b. Rubber-dam isolation
Strict rubber-dam isolation is required in order to perform a
high quality adhesive procedure (IDS and blocking out the
undercuts). It is preferable to isolate 4-5 teeth under rub-
ber-dam before starting the preparation as isolation at this
moment is easier than after prepping. In addition, the den-
tist will have a better visibility during prepping when the
teeth are isolated under rubber-dam.
The Journal of Adhesive Dentistry

a b
c d
e f
g h
Fig 10 After thorough biomechanical analysis, it was decided to re-
duce all cusps. This contributes to a more equal and favorable load-
ing on the tooth and interface, and increases the longevity of the
restoration. a. Before reduction. b. Depth grooves (±1.4 mm) were
made on each cusp and the marginal ridge. An olive shaped dia-
mond bur (833G314014; Hager and Meisinger; Neuss, Germany)
was used as a calliper. c. The same bur was used to cut the cusps
circumferentially, guided by the depth grooves prepared with the ol-
ive-shaped diamond bur. d. After cusp reduction, the dentin support
was analysed cusp by cusp. e. The tooth preparation was finalized
using the same olive bur. Smooth transitions were created inside
the preparation to remove sharp irregularities. f. Also the prep out-
line was made smooth with the same bur. g and h. Final tooth prep
before (g) and after (h) sandblasting with Al2O3 (30 µm).
3c. Tooth preparation
After removal of the restoration and all infected tissues, the
remaining tooth structure is evaluated (Fig 9). A more de-
tailed biomechanical analysis is then performed to control
the thickness and quality of the cusps (enamel supported
by dentin), the thickness of the marginal ridges and to de-
tect the possible presence of crack lines. Thin, unsupported
cusps behave like a cantilever wall and must be reduced
with at least 1.5 mm. By reducing the cusps (Fig 10), the
flexural behavior of the cantilever wall is dramatically re-
Vol 20, No 6, 2018
Politano et al
a b
c d
Fig 11 a. Initial situation: amalgam restoration that needed re-
placement because of the presence of several severe cracks in the
surrounding tooth structure. b. After removal of the existing restora-
tion, the cracks are clearly visible at the base of the lingual and buc-
cal cusps (blue arrows). c. The mechanical resistance of the cusp
walls was tested with an excavator. At the buccal side, the cusp
fractured spontaneously at the level of the crack line. At the lingual
side, the crack lines are clearly visible. The lingual cusp resisted the
pressure executed with the excavator. d. Reduction of the lingual
cusps more or less at the level of the crack. The preparation margin
was kept in enamel.
duced and the geometry of the forces is changed. Compres-
sive instead of tensile forces will work mainly on the resid-
ual dental structure. Guidelines to treat teeth with crack
lines are demonstrated by clinical cases (Figs 11 and 12).
3d. Immediate dentin sealing (IDS) using a gold-standard
adhesive and microselective out-blocking of undercuts
Documented gold-standard adhesives are the 3-step etch-
and-rinse adhesive Optibond FL (KerrHawe) and the mild
2-step self-etch adhesive Clearfil SE Bond (Kuraray Nori-
take).14,72 The adhesive is applied according to the instruc-
tions of the respective manufacturer (Fig 13). After polymer-
ization of the adhesive, a highly filled flowable composite is
applied to micro-selectively block out undercuts in the dentin
preparation (Fig 14). At the same time, deep, tight and com-
plex cavities are corrected geometrically. The application of
the flowable composite will stabilize and protect the newly
formed hybrid layer and increase its degree of conversion.
3e. Re-preparation of the enamel margins (Fig 15)
See Fig 15.
3f. Cementation of the lithium-disilicate ceramic partial
crown (Figs 16–19)
Check the fit and marginal adaptation of the ceramic par-
tial crown (Fig 16).
Adhesive treatment of the lithium-disilicate glass-ceramic
partial crown (Fig 17).
503
Politano et al

a b a b

c c d

d e e f

f g h
Fig 13 a. A 3-step etch-and-rinse adhesive (Optibond FL, Ker-
rHawe) was applied according to the instructions of the manufac-
turer. First, the dentin surface was etched with phosphoric acid
(35%) gel for 15 s. b. The etch gel was rinsed for 15 s. c. A wet den-
tin surface is visible. d. The dentin surface was gently air dried for 5
s. e. Immediately after drying, the dentin was rehydrated by gener-
ous application of the water-ethanol based primer, while gently rub-
g bing the primer into the dentin surface with a microbrush for at least
for 20 s. f. Gentle evaporation of the solvent contained in the primer
Fig 12 a. Initial situation. Old, large, unacceptable class-I compos- by air drying for 5 s. g. The particle-filled bonding agent was applied.
ite restoration. Cracks are present at the mesial, distal and palatal A uniform adhesive layer was created by moving the bonding gently
side. b. Residual dental structure after removal of the existing resto- over the whole surface. h. The adhesive was light-cured for 20 s
ration and infected dentin. Crack lines are running from the mesial with a high-intensity light-curing unit (1200 mW/cm2). The tip of the
and palatal side towards the center of the cavity. In this deep, wide light-curing unit must be placed as close as possible to the surface. 
cavity with completely undermined cusps, total cusp reduction is
needed. c. Detailed analysis of the cracks in the tooth (blue ar-
rows). d. The cusps were circumferentially reduced until a level that
enamel was completely supported by dentin. e. The crack was sand-
blasted with Al2O3 powder (30 µm). f. After sandblasting, the crack
line is contaminated with the non-hydrosoluble Al2O3 powder parti-
cles. g. Cleaning of the crack line with sodium bicarbonate (40 µm)
air polishing, followed by generously rinsing with an air-water spray.
The prepared tooth was ready for immediate dentin sealing.

504 The Journal of Adhesive Dentistry


a b
c d
e f
Fig 14 a. Hybridized dentin surface, having used a 3-step etch-
and-rinse adhesive. b. Microselective out-blocking of all undercuts
with a highly filled flowable composite. The flowable composite was
applied centripetally, ie, from periphery to the center of the dentin
surface. c. The flowable composite was light cured for 40 s with a
high-intensity light-curing unit (1200 mW/cm2). The tip of the light-
curing unit must be placed as close as possible and perpendicular
to the surface. d. After IDS and blocking out the undercuts with a
highly filled flowable composite, a perfect adhesive surface was cre-
ated: smooth and without undercuts. e. Application of glycerine gel
on the layer of flowable composite to remove the oxygen-inhibited
layer at the surface. f. Complete polymerization throughout the glyc-
erine gel for at least 20 s.
Adhesive treatment of the tooth prep to lute the ceramic
partial crown (Fig 18).
Cementation of the ceramic partial crown (Fig 19).
3g. Finishing and polishing of the restoration margins (Fig 20)
See Fig 20.
4. Durability of Bonded Ceramic Partial Crowns
The durability of bonded ceramic partial crowns is deter-
mined by several factors, ie patient, operator, materials,
amount and quality of the tooth structure to be bonded to
and the restoration maintenance.
Regarding the patient factor, high caries risk, heavy oc-
clusion/bruxism and poor oral hygiene have a considerable
influence on the clinical performance of restorations. Caries
recurrence is rarely seen in clinical trials, as these restora-
tions are commonly placed in motivated patients with low
Vol 20, No 6, 2018
Politano et al
a b
c d
Fig 15 a. The gel was rinsed off with an air-water spray, upon
which the prepared tooth surface was air dried. b. The enamel mar-
gins were re-prepared with a fine-grit olive-shaped diamond bur
(833F314012, Hager and Meisinger) at medium speed without
water. The bur was inclined 45 degrees to section the prisms
obliquely. c. The interproximal areas were finished with a medium-
grit metal strip. d. The final antifragile tooth preparation, just before
impression taking. A large dissipation platform was created. The
preparation margins in enamel were well defined.
Fig 16 Monolithic lithium-disilicate glass-ceramic partial crowns
made in e.Max Press (HT, Ivoclar Vivadent).
caries risk. Because of the higher cost of the restoration,
most of the patients have a high socio-economic status and
maintain good oral hygiene.
Bruxism also has a negative effect on the durability of
bonded indirect ceramic partial crowns, as restoration frac-
ture is more frequently recorded in patients with brux-
ism.5,6,67,93 In these clinical trials, feldspatic or leucite-re-
inforced glass ceramics were used. In the retrospective
analysis of Belli et al,8 the fracture rate of lithium-disilicate
glass-ceramic onlays (e.Max CAD, Ivoclar Vivadent) was sig-
nificantly lower compared to that of leucite-reinforced glass-
ceramic onlays (Empress CAD, Ivoclar Vivadent). Lifetime
estimations showed that only 10% of the e.Max CAD (Ivo-
clar Vivadent) onlays will fail due to catastrophic fracture
after 30 years, while Empress CAD (Ivoclar Vivadent) onlays
were estimated to reach a 10% fracture rate already at
10 years of service.
505
Politano et al

a b c a b

c d e
Fig 18 a. Strict isolation under rubber-dam is required. After re-
d e f moval of the temporary restoration, the prepared surface is contami-
nated. b. The surface was slightly roughened by air abrasion (30
µm) for 5 to 10 s. c. Phosphoric-acid (35%) etch gel was applied on
the whole prepared tooth surface. The gel creates a microretentive
etch pattern on the prepared enamel and cleans the dentin surface
covered with the IDS layer. d. The phosphoric acid-etch gel was
scrubbed onto the tooth surface with a microbrush for 30 s. e. After
rinsing and drying, a drop of the particle-filled bonding agent was ap-
plied on the whole prepared tooth surface with smooth movements.
h Premature polymerization by the operatory light must be prevented.
g i
Fig 17 a. The inner side of the lithium-disilicate glass-ceramic par-
tial crown was etched with HF acid-etch gel (9.6% buffered porcelain
etch, Ultradent; South Jordan, UT, USA) for 20 s. The gel was applied
over the whole inner surface. The action of the acid was increased by
rubbing with a microbrush. b. The HF acid-etch gel was rinsed off very
carefully with an air-water spray for 60 s. c. Next, the surface was
dried with air. d. A drop of fresh silane (Monobond Plus, Ivoclar Viva-
dent) was applied onto the etched ceramic surface. e. It must wet the
whole inner surface. f. After 60 s, the silanated surface was actively
air dried to remove residual solvent. g and h. The particle-filled bond-
ing agent was applied on the whole silanized surface. Premature po-
lymerization by the operatory light must be prevented. i. A light-curing
restorative composite was applied at the inner surface. It was spread
out with a smooth instrument over the whole surface, until the com-
posite covered the margins.

Next, the operator also co-determines the durability of
the restoration to a large extent. He has to ensure that the
clinical procedure is carried out accurately and correctly.
Placement of bonded indirect restorations requires the clin-
ical execution of a highly technique-sensitive protocol. Pro-
found knowledge of adhesive techniques by the operator is
required. This was shown in a 4-year clinical trial of Fran-
kenberger et al,30 who evaluated ceramic inlays/onlays
placed by two operators with different levels of experience
in placing adhesive restorations. Significantly more failures
were recorded for the unexperienced operator (24.6%),
compared to the experienced operator (2.6%). Therefore, in
order to reduce the number of application errors during the
clinical procedure, the protocol must be simplified, stan-
dardized and easily reproducible as proposed in this article.
Regarding the amount and quality of the remaining tooth
structure, a deep cervical cavity outline ending in dentin is
reported as a risk factor for the survival of bonded indirect
ceramic restorations.11,93 One has to keep in mind that
these teeth are often heavily compromised with a low
amount of sound tooth structure available to bond the res-
toration to. In addition, strict isolation is more difficult to
obtain when restoring teeth with deep cervical margins.
Tooth vitality is another factor determining the restora-
tion survival in several clinical trials. Vital teeth perform sig-
nificantly better than non-vital teeth.6,67,93 Here too, one
has to be aware that non-vital teeth are in general more
heavily destroyed with less tooth structure available to bond
the restoration to.
As described in our protocol, the most optimal bond to
dentin is obtained using either a 3-step etch-and-rinse or a
2-step self-etch gold-standard adhesive. This is confirmed

506 The Journal of Adhesive Dentistry


a b c gentle to strong. c. During positioning of the partial crown, a mixture
d e
g tal, mesio-occlusal and disto-occlusal) was polymerized again for 2
f h
i j
in a practice-based study of Collares et al,11 where bonded
ceramic inlay/onlays bonded with a simplified adhesive (2-
step etch-and-rinse and 1-step self-etch adhesive) pre-
sented a risk of failure that is 142% higher than restora-
tions bonded with adhesives that come with a bonding resin
that is applied separately (3-step etch-and-rinse and 2-step
self-etch adhesive). A similar conclusion was drawn by van
Dijken and Hasselrot.93
Finally, regular maintenance of the bonded ceramic resto-
rations will lengthen their life span. The occlusion and articu-
lation must be checked during recalls and corrected if
needed. Rough areas must be re-polished to a high surface
gloss, as they result more easily in the formation of cracks
with a possible catastrophic failure as a long-term conse-
quence. In addition, the ceramic-tooth interface must be care-
fully monitored, corrected and re-polished if needed.31,51,52,74
Three clinical trials were found in the literature that evalu-
ated the performance of nonretentive ceramic partial crowns
after long-term clinical functioning (Table 1).5,7,40 The clinical
protocols (preparation, adhesives, luting materials) were
slightly different than the ones presented in this article. The
survival rates varied between 96% and 100% after 7 to
10 years. Very few fractures occurred and almost any resto-
Vol 20, No 6, 2018
Politano et al
Fig 19 a. The partial crown filled with luting composite was gently
positioned on the prepared tooth surface. b. The right path of inser-
tion was searched and partially adapting the restoration was started.
Premature polymerization by the operatory light must be prevented.
Uniform pressure was applied on the occlusal surface, going from
of bonding agent and composite was squeezed out at the margins.
d. The excess of composite was removed at the margins with a
probe. This push-squeeze procedure was repeated 2-3 times. e. The
partial crown was stabilized with a finger. The margins were checked
with a probe and the last composite excess was removed. If the
margins disappear, the partial crown adapted well. f. Before polymer-
ization, floss was placed interproximally to further remove excess
luting composite. The restoration was stabilized with a finger. The
floss was moved from the lingual towards the buccal side. This must
be repeated until all composite excess is removed interproximally. g.
A bit of composite was left on the easily accessible surfaces (buc-
cal, palatal) but never in the interproximal area. h. The partial crown
was stabilized with a smooth, rounded instrument. Each surface was
polymerized for 20 s with a light intensity of 1200 mW/cm2: buccal,
palatal, mesio-occlusal and disto-occlusal. i. Glycerine gel was ap-
plied at the margins. j. Re-polymerization of the luting composite
after glycerine-gel application. Each accessible surface (buccal, pala-
cycles of 20 s with a light intensity of 1200 mW/cm2.
ration was lost. Next to the high success rate in these clini-
cal trials, a very good long-term clinical performance is re-
ported by Milichich.64 He has bonded more than 3000
lithium-disilicate glass-ceramic partial crowns over a period
of 9 years using a nonretentive prep design. Only 2 fractured
restorations and no debonding incidents were reported.
CONCLUSION
All the above-mentioned positive results confirm the clinical
effectiveness of the concept advanced in this article for the
placement of bonded indirect ceramic restorations. Never-
theless, long-term controlled clinical trials are necessary to
evaluate the proposed restoration type.
ACKNOWLEDGMENTS
The authors would like to express their gratitude to Mr. Claudio Tinti
(MDT) for his meticulous work with the fabrication of the lithium-dis-
ilicate glass-ceramic partial crowns.
507
Politano et al

Fig 20 a. The interproximal margins were checked for composite

excess with a sharp scaler from the occlusal towards the cervical re-
gion. b. A small excess of composite was left at the buccal and
lingual margin (blue arrows), just to be sure that the whole marginal
gap was filled with luting composite. This excess of composite was
removed with polishing rubbers. c. A rubber polishing point, Brownie
FG (Shofu Dental; Kyoto, Japan), was used under water cooling at
low pressure and 15,000-20,000 rpm. The point removed the com-
a b posite excess, which became visible by producing a brown powder.
d. When powder production was no longer visible during the finish-
ing procedure, all composite excess was removed. e. Polishing the
margins to a high gloss was realised using a silicon yellow cup
(Identoflex C9, KerrHawe) at a speed of 5000-7000 rpm, dry and
with very low pressure. f. In a last step, the margins were cleaned
and glossed with a soft synthetic brush. g. Using a sharp probe, the
adaptation of the margins was checked. h and j. The restoration
margins were invisible and non-probable.
c c

e f

g h i

Table 1 Overview of clinical trials that evaluated nonretentive ceramic partial crowns

Authors Patient/resto- Material Adhesive and Duration Survival (%) Fracture/

ration number luting composite (years) debonding
Arnetzl et al5 264/310 Vita Mark II Syntac Classic & 8 96.5% 2 fractures
Variolink (patient with
bruxism); no
debondings

Belleflamme et al7 94/137 84 e.Max CAD IDS: Optibond FL 1-10 99% e.Max CAD 2 debondings
12 Vita Enamic Excite & (±4.5) 89.9% Vita (all restorations
3 Composite Variolink Enamic included)
(not specified)

Guess et al40 25/80 40 ProCAD Syntac Classic & 7 97% ProCAD 1 bulk fracture;
40 e.Max Press Tetric Ceram 100% e.Max no debondings
Press

e.Max CAD, e.Max Press, ProCAD, Syntac Classic, Tetric Ceram, Excite, Variolink: Ivoclar Vivadent, Schaan, Liechtenstein; Vita Mark II, Vita Enamic:
VITA Zahnfabrik, Bad Säckingen, Germany; Optibond FL: KerrHawe, Orange, CA, USA.

508 The Journal of Adhesive Dentistry


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procedure.
The Journal of Adhesive Dentistry
 CLINICAL RESEARCH

Posterior indirect adhesive

restorations (PIAR):
preparation designs and
adhesthetics clinical protocol
Federico Ferraris, DDS
Private Practice, Alessandria, Italy

Correspondence to: Dr Federico Ferraris

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Abstract
Posterior indirect adhesive restorations

-
-

-
-

-
-
-

(Int J Esthet Dent 2017;12:482–502)

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- -

and their predictability6

1,2 -
-
-

-
7 In

clean and prepared: inlay (a cavity that -

-

-
-

-
and the
-
-

-
-

-
-

Fig 1 Posterior indirect adhesive restorations

-
-
-

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Indications

-
Fig 2

-
-
-

Fig 3
Generally, in the adhesthetics proto-
col, indirect restorations are not chosen

considered in order to restore an inlay

- -
rect restorative inlay approaches have
-
-

-
-
-

- -

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rehabilitations on abraded and/or erod-

-
- -

-
direct inlay in order to better seal the -

10

-
11

-
-

an indirect restorative approach in the -

- -

16,17 the
-

-
-
-

- -

In the adhesthetics protocol, it is be-

-
rect partial posterior restorations are:

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-
-
ation: clinical protocol

or endodontic treat-
20

the physical prop-

and, -
-

-
26,27 -
ation approach:
- -
-
-

-
-

- -

- In order to preserve the tooth, the hierar-

are 16,17

-
-

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Fig 4 Fig 5 -

For

preparation:

-
-

The

-
tin,

and

-
-

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-
or

- Fig 6 -

On the contrary, it has been

-
the clinical in- -
-

- -
-

- the post to the canal and not the other

-
-
-

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Fig 7
-

-
-

Fig 8

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Fig 9 Fig 10 -

Fig 11 Fig 12 -

-
-

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to adhesion

-
-
Fig 13

Fig 14
-

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Fig 15 Fig 16

The butt joint -

-
-
-

-
The bevel

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-
-

-
-
-
-

The shoulder

Fig 17 Fig 18
-

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Fig 19 Fig 20

adhesthetics protocol: slot, bevel, and -

Slot: -
Bevel: a less invasive preparation
-

Fig 21 Fig 22 -
-

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Fig 23 Fig 24

Ridge up:

Fig 25

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Fig 26 - Fig 27
-

Fig 28

non-vital tooth,

Fig 29

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clinical protocol

First preparation Peripheral preparation

Analysis and choice of preparation

Occlusal preparation

preparation

-
-

- -
-

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-
- -
-

-
Other protocol steps

-
-

-
-
-

-
7 -

- -
-

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-
-
-

in restorative dentistry and 6-year retrospective clin-

- -
-

- -

-
posite inlays in relation to

roottreated teeth prepared

so -
Uçta -

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- -
-

- -

-
- -

Randspaltverhalten von

- -
-

Int J Periodontics Restorative

-
-
-

endodontically treated teeth

-
-
-

tooth-colored posterior res-

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-
-

Júnior PC, Soares CJ, Nori- -

-
-

Evidence-based concepts

- -
Historical perspectives
-

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➞
 The Effect of Secondary Curing of Resin
Composite on the Adherence of Resin
Cement
Erik Asmussen^/Anne Peutzfeldt''

Purpose: The aim of this study was to measure the adherence between a resin cement and a resin com-
posite polymeNzed with and without an additional secondary cure of tiie resin composite.
Materials and Methods: The resin cement was 3M Opai Luting Composite and the resin composite was Z-
100, The resin composite was either poiymerized by iight only, or given an additional secondary cure at
110°C for 10 min. For each curing mode, the composite was either ground on carborundum paper #1000
or sandblasted with alumina powder. The adherence was determined as bond strength and as bond en-
ergy.
Results: Without sandblasting of the resin composite, the heat treatment resuited in reduced adherence
both in the bond strength and the bond energy mode of measurement. With sandblasting, only the bond
energy was reduced as a consequence of the heat treatment.
Conclusion: On the basis of the experiments conducted, it may be concluded that secondary cure of resin
composites takes place at the expense of the adherence to the resin cement.

J Adhesive Dent 2000:2:315-318. Submitted for oublication:04.04.00:accepted forpubiicavon:13.10.00.

esin composite was introduced as an
R iniay/onlay material in an attempt to improve
the mechanicai properties in comparison with di-
rect fiiiing composites."'31 A reduced risk of mar-
ginai gaps also promoted the deveiopment of
inlay/onlay materials: with an inlay materiai, the
poiymerization contraction takes piace outside the
mouth, and oniy the contraction of a reiativeiy thin
iayer of resin cement may cause marginai
gaps.19.21.28
The retention of the resin iniay is provided by a
resin cement. The cement is bonded to the enamel
' Professor, Department of Dental Materials, School of Dentistry, Fac-doubie bonds in the polymer at the surface of the
ulty of Health Sciences, University oí Copenhagen, Copenhagen,
Denmark.
" Associate Professor, Department of Dental Materiais, Scbooi of
Dentistry, Facuity of Heair/i Sciences, University of Copenhagen, reduction in remaining doubie bonds of tiie mater-
Copenhagen, Denmark.
Heprtnt requests: Erii< Asmussen, Department of Dentai Materiais, tential for favorabie mechanical properties, al-
Schooi of Dentistry, 20 Narre MIe, DK-2200 Copenhagen N, Den-
mark. Tel: ^45-3532-6580, Fax: +45-3532-6505. e-mail:
ea%ddont.ku.rSk
and dentin of the tooth by the acid-etch technique
and by means of dentin bonding agents. The adher-
ence of the cement to the iniay has a mechanical
and a chemicai component. Regarding the mechan-
icai component, a number of studies have investi-
gated surface treatments that would give rise to
optimum adherence between resin cement and
iniay materiai.12,16,29 n was found that microabra-
sion (sandbiasting) of the iniay surface is a prere-
quisite for optimai bonding. The retention of
oemented iniays has been measured and was
found to vary with the type of resin composite.22
Regarding the chemicai component of adherence,
bonding is brought about by a ccpolymerization of
the monomer of the resin cement and unreacted
inlay. Severai studies have demonstrated that the
secondary cure of resin inlays causes a significant
¡al_5,i3,25 The reiativeiy few remaining doubie bonds
of a secondariiy cured resin composite imply a po-
though significant or iong-iasting improvements

315
Vol 2, No A, 2000
Asmussen et al
Fig 1 Schematic representation of the method used for
measuring bond energy, A wedge is introduced between the
cemented beams of resin composite to create a fissure. From
the length of the fissure L, the thickness of the beams a, and
the wjdth of the fissure d, the bond energy W is caiculated as
W = (3E/16Ka3dz/L'^), E is the modulus of elasticity of the
composite beams-
were not always found.^'^'^^'^^ A less beneficial
consequence of the few remaining double bonds
may be the effect on bonding to the resin cement.
Fewer remaining double bonds will presumably re-
sult in less copolymerization of the monomer of the
resin cement with the polymer of the inlay material.
This means that the potential for bonding may be
compromised. Thus, an uncertain gain in mechani-
cal properties may be offset by a reduced capability
of adhering to the resin cement. Although this re-
duced capability for bonding has been mentioned
in numerous papers,i-i'i''.20.26,27 ^ the knowledge
of the authors, the effect of secondary curing on
adherence has been but little investigated, and
with contradictory results.^o.^s
It was the aim of the present study to measure
the adherence between resin cement and resin
composite polymerized with and without secondary
cure. It was hypothesized that the adherence of
resin cement to resin composite would decrease as
a result of the secondary curing.
MATERIALS AND METHODS
The adherence between resin composite {Z-100,
3M, St Paul, MN, USA) and resin cement {3iV) Opal
Luting Composite) was measured in two modes. In
one mode, the bond strength was measured, and in
the other, bond energy.
316
Bond Strengtii
The measurements were carried out as previously
described in detail,^'i The resin composite was ap-
plied in a cylindrical brass mold ( 0 = 6 mm, h = 3
mm) and covered on both sides with a transparent
matrix. The resin composite was polymerized by
means of a light curing unit (XL3000, 3M, St Paul,
MN, USA) with an output energy of 450 mW/cm^ as
measured by an intensity meter (Demetron Re-
search, Danbury, CT, USA), The specimen was irradi-
ated for 40 s on each side and then separated from
the mold. In one series of measurements, the spec-
imen was given a secondary cure in a normal heat
oven at 11O''C for 10 min. Our previous work
showed that this heat treatment gave rise to maxi-
mum conversion.2^ The specimen was stored in air
at room temperature for 6 days to complete poly-
merization and was then embedded in epoxy resin.
After another day in air at room temperature, the
embedded specimen was abraded to a smooth pla-
nar surface on carborundum paper #1000. In one
series of measurements, the specimen was then
sandblasted with 50-pm alumina at 0.2 MPa for
5 s, rinsed with water, and dried with a blast of air.
The surface received a thin coat of Scotchbond
Multi-Purpose Catalyst #3.5 (3iVI), and the speci-
men was now mounted in a holder with a cylindrical
teflon mold ( 0 = 3.6 mm, h = 2,5 mm). Equal
amounts of resin cement paste A and B were mixed
for 30 s, applied in the mold to the dentin surface,
and illuminated for 40 s with the light curing unit.
After 1 day in water at 37°0, the bonded specimen
was thermocycled 6000 times between two water
baths maintained at 5''C and 55°C, respectively.
The dwell time per immersion was 30 s. After 1 h in
water at 37°C, the bond strength was measured in
shear with an Instron Universal Testing Machine
(Canton, MA, USA). There were S specimens in each
of the 4 series.
Bond Energy
The resin composite was applied in a box-shaped
brass mold (I = 60 mm, w = 6 mm, h = 2 mm) and
covered on both sides with transparent matrices.
The material was irradiated by means of the light
curing unit first on one side for 180 s, and then on
the other, also for 180 s. The specimen was sepa-
rated from the mold and, in one series of experi-
ments, subjected to the same secondary cure as
The Journal of Adhesive Dentistry

Table 1 Bond strength and bond energy of resin cement in relation to
secondary cure of resin composite (mean values ± SD)
Secondary cure Bond strengtb (MPa)
Sandblasting
None 1 21 ± 1.4 ^c 23 ± 1.0
110°C for 10 min ^17 4 1.3 =^2412.3
Values designatefl üy the same superscript letter are rot statisticaliy different at p = 0.05.
above: 110°C for 10 min. The beam was now
stored in air for 7 days, after wbich time it was
abraded on carborundum paper #1000 to give a
parallel-sided beam as described earlier." In one
series of measurements, the beam was sand-
blasted on one side as described above, A pair of
beams was now fixed in a bolder to ensure parallel
alignment.'^ The bonding surfaces of the beams
were treated with Scotchbond Multi-Purpose Cata-
lyst #3.5 and cemented with freshly mixed resin ce-
ment to a cement film thickness of 100 pm. Tbe
cement line was irradiated for 60 s, the bonded
specimen freed from tbe holder, and irradiated
from tbe other tbree sides for 60 s on each side.
The specimen was then stored for 1 day in air at
37"C, and abraded and poiished to make the ce-
ment iine visible. Subsequently, a wedge was in-
serted to produce a fissure^.'i (Eig 1). The assembly
was now stored in water at 37''C for another day,
after which time the length and width of tbe fissure
were determined microscopically. From the lengtb
of the fissure L, the thickness of the beams a, tbe
modulus of elasticity of tbe beams E determined
earlier,25 and the width of the fissure d, tbe bond
energy W was calculated^ as W = (3E/16) (aSdVL")-
There were 6 specimens in eacb of tbe four groups.
Statistical Anaiysis
The data were treated statistically by analysis of
variance and by Neuman-Keuis' multiple range
tests at a level of significance of p = 0.05,
RESULTS
The results of the adherence measurements are
presented in Table 1. It can be seen that the sec-
ondary cure was not refiected in the bond strengths
Voi 2, No 4, 2000
Asmussen et al
Bond energy (J/
Sanúbiasting
a 9 ± i.g ^ 22 ± 5.5
"510.7 ^ 10 +1.3
when the substrate was sandblasted. Without sand-
blasting, the secondary cure resulted in a bond
strength that was significantly lower than without
the secondary cure. On the other hand, both in the
sandbiasted and nonsandblasted groups, the sec-
ondary cure resulted m bond energies of about balf
of tbe vaiues obtained with resin composite that
was oniy light cured. Finally, sandblasting increased
the adherence in three out of the four comparisons
made in Tabie 1.
DISCUSSION
The secondary cure of composite resins has been
found to give rise to increased conversion of tbe
resin monomer.5.13 In agreement with this, the
resin composite of the present investigation was
also found to contain fewer remaining double
bonds as a consequence of heat treatment.^^ This
implies a reduced potentiai for copciymerization of
the monomer of the resin cement with the poiymer
of the inlay material. When assessing the adher-
ence by way of bond strength measurements, the
reduced potential for bonding was not evident in
the sandblasted group. A possible explanation is
that in this group, the adherence is of such strength
that it is not the bond strength which is mea-
sured,30 but ratber the cohesive strength of embed-
ded inlay composite. This was supported by the
observation tbat all specimens fractured cohesively
in the resin composite. In the group without sand-
blasting, where adherence was lower, assessing the
bonding potentiai by bond strength measurements
is iess problematic, in the group without secondary
cure, oniy half the specimens fractured cohesively;
in tbe heat-cured group, aii specimens fractured ad-
besively. The ambiguous resuits of eariier studies^o
may tentatively be expiained by differences in sur-
face roughness, strength of the substrate, and
317
 Asmussen et al
whether the specimens fractured cohesiveiy or ad-
hesively.
Bond energy has previously been measured with
metal as the substrate and various resin cements
as adhesive.^'^'-i Clinicai studies have indicated
that the bond energy is e parameter which is re-
iated to clinical performance of adhesive restora-
tions.^ In the present work, the differences in
adherence as a consequence of sandblasting and
secondary cure of a resin composite were cleariy
displayed by use of measurements of bond energy.
The resuits corroborate the notion that improve-
ments in mechanical properties by the process of
secondary cure take place at the expense of bond-
ing to the resin oement.^^
In view of the reduced bonding resulting from the
secondary cure, it wouid seem bénéficiai to sand-
blast composite iniays before cementation.12,16,29
Additionally, silanization of the sandblasted inlay
has been found to increase the adherenoe.^^
ACKNOWLEDGMENTS
The study was supported by the 3M Company, whicii is gratefully
acknowledged.
REFERENCES
1. Asmussen E, Peutzfeldt A. Mechanical properties of heat
treated restorative resins for use in the inlay/onlay tech-
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2. Asmussen E, Attal J.p, Degrange M, Adherence of resin-based
luting cements assessed by the energy of fracture. Aota
Odcntol Scand 1993;51:235-240,
3. Asmussen E, Attai J-P, Degrange M. Factors affecting the en-
ergy of adherence of expérimentai cements bonded to a
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4. Asmussen E, Peutzfeidt A. The roie cf maleic anhydride in ad.
hesive resin cements. Eur J Orai Soi 1998; 106;882-886.
5. Bagis VH, Rueggeberg FA. Effect of post-cure and heat dura-
tion on monomer conversion of photo-activated dental resin
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6. Bruning JL, Kintz BL Computationai Handbook of Statistics.
Gienview, iL, USA; Scott, Foresman & Co,1997.
7. Cognard J. The mecrianics of the wedge test. J Adhesion
1986;2C:1-13.
8. Degrange M, Charrier JL, Attal J.p, Asmussen E. Bending of
luting materials for resin-bonded bridges; clinical relevance
of in vitro tests. J Dent 1994;22;528-532.
9. Ferracane JL, Hopkin JK, Condon JR. Properties of heat-
treated composites after aging in water. Dent Mater 1995;
11:354-358.
10. Haller B, Kiaiber B, Tarenz 0, Hofmann N. Zur Verbundfes.
tigi<eit zwischen Kompositinlay und ßefestigungskcmposit.
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11. Heyman HO. indirect composite resin veneers; clinicai tech.
nique and two-year observations. Quintessence Int 1987;18:
111-llB.
12. Hummel SK, Marker V, Pace L, Goldfogle M. Surface treat-
ment of indirect resin composite surfaces before cementa,
tien. J Prosthet Dent 1997;77;568-572.
13. Kildai KK, Ruyter iE. Hcw different curing methods affect the
degree cf conversion of resin-based inlay/oniay materials.
Acta Odontol Scand 1994:52 ;315-322.
14. Krejci I, Picco Ü, Lutz F. Dentinhaftung bei zahnfarbenen ad-
hlsiven MOD-Sofortinlays aus Komposit. Schv^eiz Monatsciir
Zahnmed 1990; 100:1151-1159.
15. Kuiimann W. Extraorale Photopolymerisatian zur Optimierung
physikaiisch-technischer Meri<male von Füiiungskunststof.
fen. Dtsch Zahnarzt Z 1988;43;383-386.
16. Latta MA, Barkmeier WW. Bond strength of a resin cement to
a cured oomposite inlay materiai, J Prosthet Dent 1994;72;
189-193.
17. Lutz F, Krejci I, Merman W. Die zahnfarbene Seitenzahn-
Restauration. PhiilipJ 1987;4:127-137.
18. McCabe JF, Kägi S. Mechanicai properties of a composite
inlay material following postcuring. Brit Dent J 1991:171:246-
248.
19. Mörmann W, Ameye C, Lutz F. Komposit-lnlays: Marginaie
Adaptation, Randdichtigkeit, Porosität und okkiusaier Ver-
schleiß. Dtsch Zahnarzti Z 1982;37;438-441.
2C. Noack MJ, Le devenir ciiniqye des inlays composites et
céramiques coliés. Rev d'Odonto Stomatoi 1995;24;305-
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21. Peutzfeidt A, Asmussen E. A comparison of accuracy in seat-
ing and gap formation for three iniay/onlay techniques. Oper
Dentl990;15:129-135.
22. Peutzfeldt A, Asmussen E, Retention of composite resin in.
iays in enamel/dentin cavities. Dent Mater 1991;7:11-14,
23. Peutzfeldt A, Asmussen E. Mechanical properties of three
composite resins for the inlay/oniay technique. J Prosthet
Dent 1991;66:322-324.
24. Peutzfeidt A. Asmussen E. Influence of eugenol-ccntaining
temporary cement on efficacy of dentin-bonding agents. Eur
J Oral Sei 1999; 107:65-69.
25. Peutzfeidt A, Asmussen E. The effect of postcuring on quan-
tity of remaining double bonds, mechanical properties, and
in vitro wear of two resin composites. J Dent 2OD0;28:447-
452.
26. Reinhardt K-J. Seitenzahnrestaurationen mit Composite-Fiii-
iung Oder -inlay? Phiiiip J 1994; 11:465-472.
27. Rouiet J-F, Degrange M. Iniay restorations. J Canad Dent
Asscc 1996;24;48-62.
28. Shortaii AC, Baylis RL, Baylis MA, Grundy JR. Marginal seal
comparisons between resin-bonded Class II porcelain iniays,
posterior composite restorations, and direct composite resin
iniays. Int J Prosthodont 1989;2:217-223.
29. Swift Jr EJ, Brodeur C, Ovitko E, Pires JA. Treatment of com-
posite surfaces for indirect bonding. Dent Mater 1992:8; 193-
196.
30. Van Noort R, Norcozi S, Howard IC, Oardew G, A critique of
bond strength measurements. J Dent 1989; 17;61-76.
31. Wendt SL. The effect of heat used as secondary cure upon
the physicai properties of three composite resins, li. Wear,
hardness, and coior stability. Quintessence Int 1987;18-351-
356,
The Journal of Adhesive Dentistry
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Composite-to-Composite Microtensile Bond Strength t es

i
se nz
in the Repair of a Microfilled Hybrid Resin: Effect of
Surface Treatment and Oxygen Inhibition
Federica Papacchinia/Susanna Dall’Ocaa/Nicoletta Chieffib/Cecilia Goraccic/
Fernanda Tranchesi Sadekd/Byoung I. Suhe/Franklin R. Tayf/Marco Ferrarig

Purpose: To compare the 24-h microtensile bond strength of a microfilled hybrid composite to the same material after
mechanical and/or chemical treatment and assess the effect of oxygen inhibition on the composite-composite bond.

Materials and Methods: Forty composite cylinders of Gradia Direct Anterior (GC) were prepared and stored 24 h prior
to the following surface treatments: 50-µm aluminum oxide air abrasion and 37% phosphoric acid etching (group 1); hy-
drochloric acid and 6.9% hydrofluoric acid etching (group 2); diamond bur roughening and 37% phosphoric acid etching
(group 3); diamond bur roughening (group 4). In all groups, Prime & Bond NT (Dentsply De Trey) was applied and light
cured in air or under a nitrogen atmosphere, prior to layering a buildup of the repairing resin composite. Microtensile
bond strength measurements were performed. Data were statistically analyzed with two-way ANOVA and Tukey’s test
(α = 0.05).

Results: The curing atmosphere did not significantly influence the interfacial strength (p < 0.05). Surface treatment sig-
nificantly affected the composite-composite bond (p > 0.05). Air abrasion, regardless of curing atmosphere, resulted in
the strongest bond (p < 0.05). The other treatments were comparable.

Conclusion: Air abrasion and the application of a bonding agent offer satisfactory bond strengths for composite repair.
The oxygen inhibition layer on a light-cured adhesive is not crucial to the success of the 24-h composite-composite bond.

Keywords: composite repair, surface treatment, oxygen-inhibited layer, microtensile bond strength.

J Adhes Dent 2007; 9: 25-31. Submitted for publication: 28.02.06; accepted for publication: 09.06.06.

a PhD Student, Department of Dental Materials and Restorative Dentistry, Uni-

versity of Siena, Policlinico “Le Scotte” Viale Bracci, Siena, Italy.
b Private Practitioner, Siena, Italy.
c Assistant Professor, Department of Dental Materials and Restorative Den-
tistry, University of Siena, Policlinico “Le Scotte” Viale Bracci, Siena, Italy.
d PhD Student, Department of Dental Materials, University of São Paulo, São
Paulo, Brazil; Department of Dental Materials and Restorative Dentistry, Uni-
versity of Siena, Policlinico “Le Scotte” Viale Bracci, Siena, Italy.
e President, Bisco Inc, Schaumburg, IL, USA.
f Research Scientist, Department of Oral Biology and Maxillofacial Pathology,
School of Dentistry, Medical College of Georgia, Augusta, Georgia, USA; De-
partment of Dental Materials and Restorative Dentistry, University of Siena,
Policlinico “Le Scotte” Viale Bracci, Siena, Italy.
g Dean and Professor, Department of Dental Materials and Restorative Den-
tistry, Policlinico “Le Scotte”, University of Siena, Viale Bracci, Siena, Italy.
Reprint requests: Prof. Marco Ferrari, University of Siena, School of Dental
Medicine, Department of Dental Sciences, Policlinico Le Scotte, Viale Bracci,
Siena, 53100, Italy. Tel: +39-0577-233131, Fax: +39-0577-233117. e-mail:
md3972@mclink.it
T he advent of adhesive techniques and bioactive restora-
tive materials has paved the way for minimally invasive
operative dentistry, aimed at preserving tooth structure as
opposed to cavity preparation for mechanical retention.35 In
light of this operative philosophy, the complete removal and
remaking of a defective composite restoration is frequently
neither necessary nor desirable, as it is time consuming16
and involves the risk of removing sound tooth substance as
well as injuring the pulp tissue. Selective replacement or ve-
neering of the unsatisfactory part, be it worn, discolored or
inadequate in color matching or in outline form, can be con-
sidered the most conservative approach.
A large amount of research data has been collected on
composite repairs. This essentially includes results from
conventional scanning electron microscopy,3,20,27 mi-
croleakage tests,6 and bond strength measurements. In par-
ticular, the composite-to-composite strength has been eval-
uated with flexural,27,28 fatigue,10 shear,2,3,14,19,20,27,32,33
and conventional tensile tests.27 In recent years, although

Vol 9, No 1, 2007 25

Papacchini et al
Table 1 Composition, batch numbers, and manufacturers of the materials used in this study
Materials Composition
Gradia Direct Anterior UDMA, dimethacrylate co-monomers, silica, prepolymerized
Batch #: filler, pigments, catalysts
A3-0305231
B3-0305221
Total Etch 37% H3PO4
Batch #: E25773
Prime&Bond NT Di- and trimethacrylate resins; PENTA, nanofillers, amorphous Dentsply DeTrey; Konstanz, Germany
Batch #: 0311002148 silicon dioxide, photoinitiators, stabilizers, cetylamine
hydrofluoride, acetone
Chelagess 6.9% hydrofluoric acid, > 10% hydrochloric acid
Batch #: 00328
Abbreviations: H3PO4: phosphoric acid; UDMA: urethane dimethacrylate; PENTA: dipentaerythritol penta acrylate monophosphate.
an increasing number of researchers have adopted the mi-
crotensile technique as a more accurate method for the as-
sessment of the interfacial strength,22 only a few studies
have evaluated the composite-to-composite microtensile
bond strength.21,29,30
The bond strength necessary for a clinically satisfactory
composite repair in vivo has never been assessed. On the
other hand, many in vitro studies have investigated the po-
tential variables affecting the composite-composite bond
strength: surface roughness,2-4,17,27 intermediary material
applied,4,17,27,32,33 repairing material used,12,21,27 and time
after repair.21,27 Divergent results were reported considering
the contribution of surface roughness to the interfacial bond
strength. Some investigators, by conducting SEM observa-
tions27 and bond strength measurements,17,27 concluded
that mechanical interlocking is the most significant factor
improving the repair strength. However, other studies re-
ported that grinding of the composite surface decreased the
tensile bond strength as a consequence of filler exposure.3,4
For this reason, the use of an intermediary layer, whether an
adhesive agent alone or in combination with a previous ap-
plication of a silane primer, has been proposed on a me-
chanically-treated composite to improve surface wetting and
chemical bonding, irrespective of the texture created by the
previous surface treatment.4,14,20,21,32 As the operator is
sometimes unable to identify the material to be repaired, the
compatibility between the repaired and repairing materials
is also of interest. It has been reported that repairs of com-
posite resins with identical resin matrix chemistry did not
produce bond strengths significantly greater than those of
different matrix chemistry.12,21 A tendency for composite-
composite bond strength to decrease after aging and stor-
age of the substrate material in water or saliva has also been
reported.21,27
26
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Manufacturer e ss e n z
GC; Tokyo, Japan
Ivoclar Vivadent; Schaan, Liechtenstein
Techim, Arese, Milano, Italy
Clinically, bonding between two composite layers is
achieved in the presence of an oxygen-inhibited zone of un-
reacted monomers and oligomers11,25 that would act as an
adhesive medium binding the overlying applied material via
a chemical bond. The influence of the oxygen-inhibited lay-
er on bond strength has already received some attention, al-
though there is no consensus in the literature on how this in-
completely polymerized surface can affect the layer-layer in-
teraction. Divergent reports on the existence of a positive
correlation between the oxygen-inhibited layer and the ad-
hesive strength,34 and other studies that reported no sig-
nificant differences9,17,30 or even a detrimental correla-
tion8,24,37 further contributed to the controversy of this is-
sue.
Based on these premises, the objectives of this study
were: (1) to compare the 24-h microtensile bond strength of
a composite to the same material after mechanical and/or
chemical treatment; (2) to assess the influence of oxygen in-
hibition on the 24-h composite-to-composite bond.
The null hypotheses to be tested were: (a) surface treat-
ment has no effect on the 24-h bond strength of a resin com-
posite repaired with the same type of material; (b) there is
no difference in the 24-h repair strength of a composite re-
gardless of the presence or absence of an oxygen-inhibited
layer.
MATERIALS AND METHODS
Specimen Preparation
The materials used in this study are listed in Table 1. Forty
cylinder-shaped composite substrates, 4 mm in height and
8 mm in diameter, were made by layering 2-mm-thick incre-
ments of Gradia Direct Anterior (GC; Tokyo, Japan, shade A3)
The Journal of Adhesive Dentistry

in a split aluminum mold. Each increment was carefully con-
densed with a clean plastic filling instrument in order to
avoid contamination and/or incorporation of voids, then
cured for 20 s with the tip of the light-polymerizing unit (VIP,
Bisco; Schaumburg, IL, USA, output: 500 mW/cm2) placed
in contact with the surface of the mold. The last increment
was covered with a Mylar strip and compressed with a glass
slide in order to obtain a flat surface of the specimen after
light curing. After the top surface had been cured, the spec-
imen was removed from the mold and irradiation was per-
formed for a further 20 s on the portions of the specimens
that were in contact with the metallic parts of the mold, in
order to ensure uniform and complete polymerization.
All composite cylinders were stored in a saline solution at
37°C for 24 h before the repair procedures were performed,
then randomly assigned to 4 groups of 10 specimens each.
Each group differed in the chemical and/or mechanical sur-
face treatment that preceded the repairing procedure, as de-
scribed below.
• Group 1: An air spray of 50-µm aluminum oxide particles
(Microetcher II, Danville Engineering; San Ramon, CA,
USA) was used for 10 s from a distance of approximately
5 mm perpendicular to the specimen surface at a pres-
sure of 60 to 100 psi. 37% phosphoric acid (Total Etch,
Ivoclar-Vivadent; Schaan, Liechtenstein) was applied to
the treated surfaces for 30 s, then washed off with water
for 30 s to remove debris, and dried using an air syringe
for 10 s from a distance of 5 mm.
• Group 2: A mix of hydrochloric acid (HCl, >10%) and hy-
drofluoric acid (HF, 6.9%) (Chelagess, Techim; Arese, Mi-
lano, Italy) was applied to the experimental surface for 60
s, then rinsed with a water spray for 20 s, and dried with
compressed air for 10 s from a distance of 5 mm.
• Groups 3 and 4: A 770-8P fine-grit diamond bur was used
for 10 s to roughen the specimens surface. In group 3,
37% phosphoric acid (Total Etch, Ivoclar-Vivadent;
Schaan, Liechtenstein) was also applied to the treated
surfaces for 30 s, then washed off with water for 30 s to
remove debris, and dried using an air syringe for 10 s
from a distance of 5 mm.
In all groups, the self-priming etch-and-rinse adhesive
Prime&Bond NT (Dentsply DeTrey; Konstanz, Germany) was
then applied with a microbrush on the treated composite
substrate, lightly air dried, and light cured for 20 s with the
above mentioned light-curing device in an air atmosphere
(subgroup A, n = 5) or under a nitrogen atmosphere (sub-
group N, n = 5). In the nitrogen chamber, oxygen was com-
pletely removed through 6 to 8 purge cycles prior to intro-
ducing nitrogen by opening an inlet valve.
Each specimen was then replaced into the mold and
fresh Gradia Direct Anterior shade B3 was packed against
the treated side of the substrate specimen in 2-mm-thick in-
crements, which were incrementally cured for 20 s each, cre-
ating a repaired composite-composite specimen 8 mm in
height and 8 mm in diameter with (A) or without (N) a pre-ex-
isting oxygen-inhibited interface. Different shades were in-
tentionally chosen for the substrate and for the repairing ma-
terial, in order to facilitate the visual identification of the
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composite-composite interface and an accurate and easierhalt
n interface en
mounting of the repaired specimens at the repair t
i
in the testing machine. e ss e n z
After a 24-h storage in a 37°C saline solution, each bond-
ed specimen was secured with sticky wax (Micerium, Aveg-
no; Genova, Italy) on an acrylic resin cylinder, which was
mounted on a cutting machine (Isomet, Buehler; Lake Bluff,
IL, USA). By means of a water-cooled diamond blade, each
repaired specimen was serially sectioned to obtain multiple
beam-shaped sticks, according to the nontrimming tech-
nique.22 The cross-sectional area ranged between 0.78 and
0.81 mm2. For about one-half of its length, each stick was
composed of the treated substrate composite material, and
for the remaining half, the repairing material. The two halves
were joined together at their interface by the bonding agent
Prime & Bond NT with or without a pre-existing oxygen-in-
hibited interface, depending on the subgroup.
For microtensile testing, each beam was secured at the
ends with cyanoacrylate adhesive (Zapit, Dental Ventures of
America; Corona, CA, USA) to a Gerardeli’s jig,23 designed to
transmit purely tensile forces to the specimen when mount-
ed on a universal loading machine (Controls; Milano, Italy).
The test was conducted at a cross-head speed of 0.5
mm/min until failure. The load at failure was recorded in N,
and the specimen’s fragments were carefully removed from
the fixtures with a scalpel blade. The cross-sectional area at
the site of fracture was measured to the nearest 0.01 mm
with a digital caliper, in order to calculate the bond strength
at failure in MPa.
For each specimen, the failure mode was classified as co-
hesive within the substrate or the repairing composite, ad-
hesive, or mixed, by examining the fractured stick with an op-
tical microscope (Nikon SMZ645; Tokyo, Japan) at 50X mag-
nification. All the sticks that failed prematurely while being
cut or glued were included and considered in the statistical
calculations as null bond strength values.
SEM Evaluation
Three additional composite substrates were prepared and
surface treated similarly to those in groups 1 to 4. The spec-
imens were mounted on aluminum stubs, sputter coated
with gold (SC7620 Sputter Coater, Polaron Range, Quorum
Technologies; Newhaven, UK), and observed using a scan-
ning electron microscope (JEOL, JSM-6060LV; Tokyo, Japan).
Micrographs were taken at standardized magnifications
(150X, 500X, 2000X) in order to document the surface tex-
ture created by the different mechanical and/or chemical
treatments performed in each study group.
Statistical Analysis
The bond strength data were first analyzed for normality with
the Kolmogorov-Smirnov test and the Levene’s test for ho-
mogeneity of variances. As data were normally distributed,
a two-way ANOVA was applied with “bond strength” as the
dependent variable, and “surface treatment” and “atmos-
phere” as factors. Tukey’s test was then used for multiple
comparisons among surface treatments. All analyses were
processed using SPSS 11.0 software (SPSS; Chicago, IL,
USA), with significance set at the 95% probability level.
27
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Table 2 Means and standard deviations of the microtensile bond strengths (µTBS) measured in each experimental group
a
nt lte
n

i
Groups Atmosphere µTBS (MPa) Failure mode Number ofess e n z
of curing (stereomicroscopy) premature failures
cohesive adhesive mixed

1 A 43.2 (13.5) [65]a 15 45 5 0

2 35.2 (12.0) [73]b 3 63 1 6
3 37.8 (9.9) [60]b 8 48 3 1
4 37.3 (14.4) [72]b 12 53 4 3

1 N 42.4 (14.0) [64]a 18 43 3 0

2 33.5 (11.4) [64]b 4 60 0 0
3 36.3 (11.7) [67]b 10 53 4 0
4 36.2 (10.9) [66]b 7 58 1 0

The failure modes and the number of specimens that failed prematurely during cutting or gluing are reported. Numbers in square brackets represent the
number of tested sticks. Subgroups (A, N) labelled with the same superscript letter are not statistically different (p > 0.05). A: air; N: nitrogen.

RESULTS Chemical treatment with a mix of HCl and 6.9% HF (Fig

Microtensile Bond Strengths
The means and standard deviations of the microtensile bond
strengths measured for all the tested subgroups are presen-
ted in Table 2. The failure modes are also reported.The statis-
tical analysis showed that the atmosphere under which the
adhesive was cured did not have a significant influence on
the interfacial strength (p > 0.05), whereas the surface treat-
ment significantly affected composite-composite strength (p
< 0.05). Tukey’s post-hoc test revealed that aluminum oxide
abrasion (group 1) produced significantly higher bond
strengths (p < 0.05) than all the other surface treatments.
Irrespective of the presence (A: 43.2 ± 13.5 MPa) or ab-
sence (N: 42.4 ± 14.0 MPa) of a pre-existing oxygen-inhibit-
ed layer at the composite-composite interface, aluminum ox-
ide abrasion achieved the statistically significantly (p < 0.05)
highest bond strength of all the subgroups. All other surface
treatments in the tested subgroups showed comparable
bond strength results.
The interaction between surface treatment and atmos-
phere was statistically significant (p < 0.05). According to the
Tukey’s test, the bond strength values achieved following air
abrasion in either atmosphere were significantly higher than
those measured in any other subgroup.
As regards the failure modes, in the majority of loaded
specimens, fractures developed at the composite-compos-
ite interface; however, the highest number of cohesive and
mixed failures was recorded for air-abraded subgroups and
the lowest for HF/HCl-acid treated subgroups.
SEM Observations
SEM examination of the mechanically and/or chemically
treated composite substrates revealed different surface tex-
tures. Air abrasion with 50-µm aluminum oxide particles
and etching with 37% phosphoric acid (Fig 1A) produced a
roughened, highly irregular surface topography, with resin
composite block asperities created among numerous mi-
croretentive fissures.
1B) resulted in an extensive dissolution of the upper layer of
the composite substrate, exposing both the glass fillers and
the resin matrix. In addition, numerous irregular and ran-
domly distributed gaps and pores could be identified.
Scratches and grooves covered with streaks of smeared
matrix can be observed on the composite substrate after
roughening with a fine-grit diamond bur (Fig 1C). Etching with
37% phosphoric acid did not cause any morphological change
in the retentive pattern of the similarly-treated composite sur-
face, apart from producing a cleaning effect (Fig 1D).
DISCUSSION
In all groups, the treated surface was coated with a thin lay-
er of a bonding agent, as it has been well documented that
the repairing material does not wet the etched composite
surface at all locations.28 The poor wettability could be ex-
plained by the high viscosity of the uncured repairing com-
posite or by the polymerization shrinkage that pulls the ma-
terial away from the treated surface during the curing
process.
The use of an intermediate low viscosity resin can be con-
sidered a necessary step in composite repair in order to en-
hance the composite-composite bond by promoting chemi-
cal coupling to the resin matrix, chemical bonds to the ex-
posed filler particles, or micromechanical retention through
monomer penetration into the matrix microcracks.20 Differ-
ent composite surface treatments are likely to generate dif-
ferences in smearing and matrix cracking,28 and thus influ-
ence the repair bond strength.
The results of our investigation, in agreement with other
studies,4,17,27 confirm that surface abrasion with 50-µm alu-
minum oxide particles significantly improves the composite-
to-composite repair bond strength. It has been reported that
this surface pretreatment, followed by the application of a
bonding agent, can result in an intraoral repair strength that
is nearly identical to the cohesive strength of the original

28 The Journal of Adhesive Dentistry

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B D

Fig 1A Scanning electron micrograph of the composite surface air abraded with 50-µm aluminum oxide
particles and etched with 37% phosphoric acid. A roughened, highly irregular topography was produced,
with resin composites asperities appearing besides areas of numerous microretentive fissures (bar = 50
µm).
Fig 1B Scanning electron micrograph of the composite substrate etched with a mix of hydrochloric and
6.9% hydrofluoric acid. Extensive dissolution of the upper layer of the composite substrate could be iden-
tified, involving both the glass fillers and the resin matrix. Gaps and pores were extensively distributed on
the chemically-treated surface (bar = 50 µm).
Fig 1C Scanning electron micrograph of the composite surface roughened with a fine-grit diamond bur.
Scratches and grooves covered with streaks of smeared matrix could be observed (bar = 50 µm).
Fig 1D Scanning electron micrograph of the composite substrate roughened with a fine-grit diamond bur
and etched with 37% phosphoric acid. The etching procedure did not produce morphological changes in
the retentive pattern of the composite surface, but only a cleaning effect (bar = 50 µm).

composite.17,27 SEM observations in previous studies20,27
showed that aluminum oxide sandblasting is able to pro-
duce microretentive features, increasing the surface area
available for wetting and bonding by the adhesive resin. This
may account for the strong interfacial bond achieved in this
experiment following air abrasion.
The composite-to-composite bond achieved after grinding
the substrate surface with a diamond bur was significantly
weaker, regardless of the use of 37% phosphoric acid to
clean the composite surface. These differences in bond
strength as compared with the air-abraded specimens are
probably related to the different microscopic pattern pro-
duced by the rotating instrument, which results in scratches
and a tenacious smear layer that can decrease the strength
of the composite-to-composite bond.27
The acid etching procedure, also performed in similar re-
search protocols,2,20,27 was unable to produce any signifi-
cant morphological changes in the retentive pattern of the
resin matrix, as confirmed by the similar bond strengths in
comparison to the unetched groups. Lucena-Martín et al20
found clinically unacceptable repair bond strengths in sec-
ondarily cured microhybrid and microfilled composites after
treating an unground resin surface with 37% phosphoric
acid and an adhesive agent. Their study agrees with our re-
sults, confirming both that mechanical retention plays the
most important role in repair bond strength and that 37%
phosphoric acid probably exercises a superficial cleaning ef-
fect on the composite surface.
The lowest bond strength was obtained by chemically
treating the composite surface with a mix of HCl and 6.9%

Vol 9, No 1, 2007 29

Papacchini et al
HF for 60 s. This product has a different aggressiveness de-
pending on the concentration. When diluted to 50%, it is
able to clean investments from cast restorations. When
used undiluted, the solution is effective in dissolving glass
and porcelain by corrosion, and cleaning titanium or resin
composites. In this study we applied the acid solution for 60
s only for etching, taking care to completely wash and dry the
treated surface before performing the bonding procedure. In
contrast to 37% phosphoric acid, this solution appears to
have a more aggressive effect on a direct composite restora-
tion. When hydrofluoric acid is applied on resin composites,
it has been reported that this etching agent, traditionally
used to etch porcelain, would act by lightly dissolving the
glass particles of the composite filling, leaving gaps or pores
and allowing micromechanical retention by the bonding
agent.31 Nevertheless, some studies20,32 reported that a
30- to 120-s application of hydrofluoric acid not only result-
ed in complete dissolution of exposed glass particles, but al-
so produced softening and porosity of the composite resin
matrix. This may have accounted for the lower bond
strengths, depending on the chemical composition of the
material being repaired. For this reason, the routine use of
hydrofluoric acid in a repair procedure is not recommended
by Brosh et al,4 especially when the exact composition of the
old composite is unknown. A similar combined action either
on the glass fillers or in the resin matrix can be assumed to
have occurred for the 6.9% HF used in the present study, as
confirmed by the SEM evaluation. The combined action of
two strong acids, such as hydrofluoric and hydrochloric acid,
had a great impact on the structure of the resin composite,
possibly including a cleavage of the filler particles from the
resin matrix. Clinically, rubber-dam isolation and suction of
vapors will be effective at preventing hazardous effects ei-
ther using intraoral air abrasion or strong acids such as
those applied in this study.
Another topic of interest of the present research is the
bonding ability of the oxygen-inhibited layer on the compos-
ite surface. Oxygen from the ambient atmosphere can inhibit
any free-radical-initiated, addition polymerization reaction.11
It has been reported that oxygen inhibition results from
quenching the free radicals generated via light activation of
the photoinitiator in its excited triplet states, thus limiting the
initiation stage of the polymerization reaction.1 The peroxy
radicals that form in the presence of oxygen are more stable
and less reactive towards carbon-carbon double bonds than
the propagating radical. As a consequence, polymerization
is strongly compromised, and the surface of the polymerized
layer may remain undercured and tacky.25 The degree of oxy-
gen inhibition during polymerization can potentially be af-
fected by several factors such as monomer functionality and
structure,9,18 bis-GMA:HEMA ratio,9 the type and concen-
tration of photoinitiators, polymerization conditions,11,13,15
and the surface-to-volume ratio of the resin coating.9,25
An interesting and controversial aspect that remains un-
resolved is whether this sticky surface is really necessary for
bonding of composite resins. Some studies have shown that
the presence of an oxygen-inhibited layer is crucial for im-
proving the adhesive strength between two composite layers
by means of remaining unreacted acrylate groups, forming
chemical covalent bonds within an interpenetrating net-
30
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work.19,34,36 ha
Based on these findings, the oxygen-inhibited
n lte
layer has traditionally been assumed to be necessary before n
t
i
e ss e n
adding more layers of bonded composite. Conversely, z
a neg-
ative correlation has also been reported in the litera-
ture,8,24,37 indicating37 that the oxygen-inhibited layer cor-
responds to a soft and undercured interface; local con-
sumption of the photoinitiator on the substrate surface
would be responsible for imperfect bonding with the overly-
ing resin composite after polymerization. Moreover, the pres-
ence of an oxygen-inhibited layer in acidic, self-etching ad-
hesives resulted in their incompatibility with self-cured com-
posites.26,29
In the present study, bond strength data obtained from
specimens cured in nitrogen atmosphere, in which the con-
tact of the adhesive layer with oxygen was completely avoid-
ed, and those from specimens cured in the air were statisti-
cally comparable. These results confirmed that, contrary to
the common perception, the oxygen-inhibition layer is not
necessary for bonding additional layers of resin composites,
at least for the initial 24-h period in which incomplete decay
of the existing free radicals within the polymerized dentin ad-
hesive enables its chemical coupling to the repair compos-
ite. Similarly, in recent studies,17,30 comparable results were
found in the composite-to-composite bond strength, with or
without an oxygen-inhibited layer on the composite surface
requiring repair. It can be speculated that the amount of re-
maining active free radicals available for reacting with resin
composite monomers, even in absence of oxygen, is the
most important factor for the coupling of a 24-h direct com-
posite veneering or repair.
As free radicals have half-lives and slowly decay with
time,5 we can assume that for an adhesive layer that is light
cured and bonded with the repairing material after 24 h,
such as those that were examined in this study, a maximum
amount of remaining active free radicals is still available for
bonding with the overlying composite increment. Thus, the
longevity of free radicals appears to be an important factor
affecting the outcome of bonding to a light-cured composite
surface or a light-cured adhesive layer even several days af-
ter photopolymerization, without using a resin activator. Fur-
ther studies should be performed to evaluate how long these
existing free radicals can remain available for bonding with-
out adversely affecting bond strength. Clinically, this will pro-
vide important information, for example, on how long the op-
erator can leave a direct composite restoration before cor-
recting defects or a provisional restoration on adhesive-de-
sensitized dentin,7 without compromising bond strength of
the final restoration.
CONCLUSION
In conclusion, within the limits of this study, the first null hy-
pothesis that surface treatment has no effect on the 24-h
bond strength of a resin composite repaired with the same
type of material has to be rejected. Regardless of the pres-
ence or absence of an oxygen inhibited layer, air abrasion of
a cured composite surface with 50-µm aluminum oxide pro-
duces statistically higher bond strengths than those ob-
tained by treating the same material with a diamond bur or
The Journal of Adhesive Dentistry

a mixture of hydrochloric (> 10%) and hydrofluoric acid
(6.9%). 37% phosphoric acid does not improve composite-to-
composite bond strength when the composite surface is
roughened with a diamond bur, and has only a cleaning ef-
fect. The second null hypothesis that there is no difference
in the 24-h repair strength of a composite regardless of the
presence or absence of an oxygen inhibited layer must be ac-
cepted. The presence of an oxygen-inhibition layer on a light-
cured resin composite or adhesive layer is not necessary for
additional resin coupling, at least up to 24 h after polymer-
ization, due to the presence of incompletely decayed, active,
remnant free radicals within the cured composite or adhe-
sive.
ACKNOWLEDGMENTS
This study was based on a dissertation to be submitted by Dr. Federica
Papacchini for partial fulfilment of the requirements of the degree of
Doctor of Philosophy at the University of Siena, Italy. The materials em-
ployed in this study were generously donated by Bisco, Dentsply Detrey,
GC and Ivoclar-Vivadent.
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2. Bonstein T, Garlapo D, Donarummo J Jr, Bush PJ. Evaluation of varied repair
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3. Bouschlicher MR, Reinhardt JW, Vargas MA. Surface treatment techniques
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4. Brosh T, Pilo R, Bichacho N, Blutstein R. Effect of combinations of surface
treatments and bonding agents on the bond strength of repaired composites.
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5. Burtscher P. Stability of radicals in cured composite materials. Dent Mater
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6. Cavalcanti AN, Lobo MM, Fontes CM, Liporoni P, Mathias P. Microleakage at
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7. Chieffi N, Sadek FT, Monticelli F, Goracci C, Grandini S, Davidson CL, Tay FR,
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8. Eliades GC, Caputo AA. The strength of layering technique in visible light-
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9. Finger WJ, Lee KS, Podszun W. Monomers with low oxygen inhibition as
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10. Frankenberger R, Krämer N, Ebert J, Lohbauer U, Käppel S, ten Weges S,
Petschelt A. Fatigue behavior of the resin-resin bond of partially replaced
resin-based composite restorations. Am J Dent 2003;16:17-22.
11. Gauthier MA, Stangel I, Ellis TH, Zhu XX. Oxygen inhibition in dental resins. J
Dent Res 2005;84:725-729.
12. Gregory WA, Pounder B, Bakus E. Bond strengths of chemically dissimilar re-
paired composite resins. J Prosthet Dent 1990;64:664-668.
13. Guillot G, Nunes TG, Ruaud JP, Polido M. Aspects of photopolymerization of
a commercial dental resin studied by 1H magnetic resonance imaging. Poly-
mer 2004;45:5525-5532.
14. Kallio TT, Lastumaki TM, Vallittu PK. Bonding of restorative and veneering
composite resin to some polymeric composites. Dent Mater 2001;17:80-86.
15. Kim JS, Choi YH, Cho BH, Son HH, Lee IB, Um CM, Kim CK. Effect of light-cure
time of adhesive resin on the thickness of the oxygen-inhibited layer and the
microtensile bond strength to dentin. J Biomed Mater Res Part B: Appl Bio-
mater 2006;78:115-123.
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16. ha
Krejci I, Lieber CM, Lutz F. Time required to remove totally bonded tooth-col-
ored posterior restorations and related tooth substance loss. Dent Mater lte
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1995;11:34-40.
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17. Kupiec KA, Barkmeier WW. Laboratory evaluation of surface treatments for
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18. Lee TY, Guymon CA, Sonny Jönsson E, Hoyle CE. The effect of monomer struc-
ture on oxygen inhibition of (meta)acrylates photopolymerization. Polymer
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19. Li J. Effects of surface properties on bond strength between layers of newly
cured dental composites. J Oral Rehabil 1997;24:358-360.
20. Lucena-Martín C, González-López S, Navajas-Rodríguez de Mondelo JM. The
effect of various surface treatments and bonding agents on the repaired
strength of heat-treated composites. J Prosthet Dent 2001;86:481-488.
21. Papacchini F, de Castro FL, Goracci C, Sardella TN, Tay FR, Polimeni A, Fer-
rari M, Carvalho RM. An investigation of the contribution of silane to the com-
posite repair strength over time using a double-sided microtensile test. Int
Dent South Africa 2006;1:26-36.
22. Pashley DH, Carvalho RM, Sano H, Nakajima M, Yoshiyama M, Shono Y et al.
The microtensile bond test: a review. J Adhes Dent 1999;1:299-309.
23. Perdigão J, Gerardeli S, Carmo ARP, Dutra HR. In vivo influence of residual
moisture on microtensile bond strengths of one-bottle adhesives. J Esthet
Restor Dent 2002;14:31-38.
24. Rueggeberg FA, Margeson DH. The effect of oxygen inhibition on an un-
filled/filled composite system. J Dent Res 1990;69:1652-1658.
25. Ruyter IE. Unpolymerized surface layers on sealants. Acta Odontol Scand
1981;39:27-32.
26. Sanares AME, Itthagarun A, King NM, Tay FR, Pashley D. Adverse surface in-
teractions between one-bottle light-cured adhesives and chemical-cured
composites. Dent Mater 2001;17:542-556.
27. Shahdad SA, Kennedy JG. Bond strength of repaired anterior composite
resins: an in vitro study. J Dent 1998;26:685-694.
28. Söderholm K-JM, Roberts MJ. Variables influencing the repair strength of
dental composites. Scand J Dent Res 1991;99:173-180.
29. Suh BI, Feng L, Pashley DH, Tay FR. Factors contributing to the incompatibil-
ity between simplified-step adhesives and chemically-cured or dual-cured
composites. Part III. Effect of acidic resin monomers. J Adhes Dent
2003;5:283-291.
30. Suh BI. Oxygen-inhibited layer in adhesion dentistry. J Esthet Restor Dent
2004;16:316-323.
31. Swift EJ Jr, Le Valley BD, Boyer DB. Evaluation of new methods for compos-
ite repair. Dent Mater 1992;8:362-365.
32. Swift EJ, Cloe BC, Boyer DB. Effect of a silane coupling agent on composite
repair bond strength. Am J Dent 1994;7:200-202.
33. Tezvergil A, Lassila LVJ, Vallittu PK. Composite-composite repair bond
strength: effect of different adhesion primers. J Dent 2003;31:521-525.
34. Truffier-Boutry D, Place E, Devaux J, Leloup G. Interfacial layer characteriza-
tion in dental composite. J Oral Rehabil 2003;30:74-77.
35. Tyas MJ, Anusavice KJ, Frencken JE, Mount GJ. Minimal intervention dentistry
– a review. Int Dent J 2000;50:1-12.
36. Vankerckhoven H, Lambrechts P, Van Beylen M, Davidson CL, Vanherle G. Un-
reacted methacrylate groups on the surfaces of composite resins. J Dent Res
1982;61:791-795.
37. von Beetzen M, Li J, Nicander I, Sundstrom F. Factors influencing shear
strength of incrementally cured composite resins. Acta Odontol Scand
1996;54:275-278.
Clinical relevance: Air abrasion with aluminum oxide rep-
resents a useful technique for improving composite repair
bond strength. The oxygen inhibition layer on a light-cured
adhesive is not crucial to the 24-h composite-composite
bond.
31
!
Operative Dentistry, 2015, 40-4, 372-378

Influence of Etching Protocol and

Silane Treatment with a Universal
Adhesive on Lithium Disilicate Bond
Strength
VK Kalavacharla ! NC Lawson ! LC Ramp
JO Burgess

Clinical Relevance
Optimal bond strength to lithium disilicate is achieved by exposure to at least 20 seconds of
5% hydrofluoric acid (HF) followed by a coat of silane and then a universal adhesive. If an
additional silane step is not taken prior to applying a universal adhesive, the use of 9.5%
HF for 60 seconds can increase bond strength.

SUMMARY based on surface pretreatments, as follows: 1)

Objectives: To measure the effects of hydro-
fluoric acid (HF) etching and silane prior to the
application of a universal adhesive on the bond
strength between lithium disilicate and a resin.
Methods and Materials: Sixty blocks of lithium
disilicate (e.max CAD, Ivoclar Vivadent) were
sectioned into coupons and polished. Speci-
mens were divided into six groups (n=10)
Vamsi K Kalavacharla, BDS, MS, UAB, Birmingham, AL,
USA
*Nathaniel C Lawson, DMD, MS, University of Alabama at
Birmingham, Clinical and Community Sciences, Birming-
ham, AL, USA
Lance C Ramp, DMD, PC, UAB School of Dentistry,
Comprehensive Dentistry, Birmingham, AL, USA
John O Burgess, DDS, University of Alabama at Birmingham,
Prosthodontics and Biomaterials, Birmingham, AL, USA
*Corresponding author: SDB 603, 1720 2nd Avenue S,
Birmingham, AL 35294-0007, USA; e-mail: nlawson@uab.
edu
DOI: 10.2341/14-116-L
no treatment (control); 2) 5% HF etch for 20
seconds (5HF); 3) 9.5% HF etch for 60 seconds
(9.5HF); 4) silane with no HF (S); 5) 5% HF for
20 seconds + silane (5HFS); and 6) 9.5% HF for
60 seconds + silane (9.5HFS). All etching was
followed by rinsing, and all silane was applied
in one coat for 20 seconds and then dried. The
universal adhesive (Scotchbond Universal, 3M
ESPE) was applied onto the pretreated ceram-
ic surface, air thinned, and light cured for 10
seconds. A 1.5-mm-diameter plastic tube filled
with Z100 composite (3M ESPE) was applied
over the bonded ceramic surface and light
cured for 20 seconds on all four sides. The
specimens were thermocycled for 10,000 cycles
(58C-508C/15 s dwell time). Specimens were
loaded until failure using a universal testing
machine at a crosshead speed of 1 mm/min. The
peak failure load was used to calculate the
shear bond strength. Scanning electron mi-
croscopy images were taken of representative
e.max specimens from each group.
Kalavacharla & Others: Bond Strength to Lithium Disilicate
Results: A two-way analysis of variance
(ANOVA) determined that there were signifi-
cant differences between HF etching, silane
treatment, and the interaction between HF
and silane treatment (p,0.01). Silane treat-
ment provided higher shear bond strength
regardless of the use or concentration of the
HF etchant. Individual one-way ANOVA and
Tukey post hoc analyses were performed for
each silane group. Shear bond strength values
for each etch time were significantly different
(p,0.01) and could be divided into significant-
ly different groups based on silane treatment:
no silane treatment: 0 HF , 5% HF , 9.5% HF;
and RelyX silane treatment: 0 HF , 5% HF and
9.5% HF.
Conclusions: Both HF and silane treatment
significantly improved the bond strength be-
tween resin and lithium disilicate when used
with a universal adhesive.
INTRODUCTION
Lithium disilicate is a dental ceramic that mimics
the esthetics and strength of natural tooth structure.
The 70% crystal phase of this unique glass-ceramic
material refracts light naturally and provides supe-
rior structural reinforcement, imparting a greater
flexural strength than is associated with traditional
feldspathic porcelain or leucite-reinforced glass
ceramics.1,2 Lithium disilicate crowns may be placed
by either traditional cementation techniques or
adhesive bonding. One clinical trial has shown
similar survival of lithium disilicate crowns cement-
ed with resin-modified glass ionomer cements and
bonded with resin cements.3,4 In clinical situations
involving short clinical crowns or overtapering of the
crown preparation, adhesive bonding is recommend-
ed.5 In vitro studies6,7 have shown superior bond
strength when lithium disilicate is bonded to tooth
as compared to traditional cementation. Additional-
ly, bonding with a resin composite cement may also
improve the fracture strength of lithium disilicate
crowns.8
Prior to bonding lithium disilicate crowns,
etching with hydrofluoric acid (HF) is recommend-
ed.9 The action of HF etching on the microstruc-
ture of these ceramics is by dissolution of the
glassy phases of porcelain.5,6 This phase is partial-
ly dissolved to create an appropriate microstruc-
ture that increases surface area for bonding.7-10
Studies11-15 have shown that HF etching with
lithium disilicate improved bond strength. These
studies have etched with 9.5%-10% HF for 60
373
seconds13,15 or 20 seconds11,12 and with 5% HF for
20 seconds.14 Since there has not been an evalu-
ation on the effect of HF concentration on bond
strength, this study will compare two reported
etching protocols: 9.5% HF for 60 seconds13,15 and
5% HF for 20 seconds.14 Silanes are a class of
organic molecules that contain one or more silicon
atoms. The specific silane used in dentistry is 3-
methacryloxypropyltrimethoxysilane. It is used as
a chemical coupler, linking organics (resin-based
materials) to inorganics (eg, porcelain, some oxi-
dized metals, and glass fillers in resin-based
composites).16 Infrared spectroscopy has shown
that silane has the potential to react with hydroxyl
(-OH) groups present on the surface of silica in
ceramics and the methacrylate group of a bonding
agent or resin cement.17,18 A study by Panah and
others15 demonstrated that the bond strength to
lithium disilicate was significantly improved with
silane treatment and further improved with HF
etching and then use of silane. Nagai and others14
concluded that silane improved the bond strength
to lithium disilicate. Additionally, they discovered
that HF etching improved bond strength more in
unsilanated specimens than in those that were
silanated.14
The introduction of universal adhesives presents a
new simplified approach for bonding ceramic to resin
cements. Universal adhesives contain silane and a
monomer called 10-methacryloxydecyl dihydrogen
phosphate (MDP) that help bond ceramic to the resin
in a cement. A study by Amaral and others19 has
shown the ability of a universal adhesive to bond
zirconia to a resin; however, the effectiveness of the
adhesive has not been thoroughly investigated with
lithium disilicate.
This study examined how surface treatment (HF
and silane) affects shear bond strength between a
resin composite and lithium disilicate treated with
a universal adhesive (Scotchbond Universal, 3M
ESPE, St Paul, MN, USA). The purpose of this
study was to determine if it is necessary to apply
silane prior to a universal adhesive. Additionally,
we wished to determine if HF etching improves
bond strength to lithium disilicate and to compare
the effectiveness of 5% HF (20 seconds) and 9.5%
HF (60 seconds). The null hypotheses of this study
were that there is no difference in the bond strength
when silane is applied prior to a universal adhesive
and that there is no difference in bond strength
with two different etching protocols prior to a
universal adhesive application.
374
Table 1: Materials Used in this Study
Material
Lithium disilicate
5% Hydrofluoric acid etchant
9.5% Hydrofluoric acid etchant
Silane
Universal adhesive
Resin composite
METHODS AND MATERIALS
All materials used for specimen preparation are
described in Table 1. Blocks of lithium disilicate
(e.max CAD, Ivoclar Vivadent, Amherst, NY, USA)
in bisque (blue, metasilicate) form were sectioned
into rectangular coupons using a low-speed cutting
device (Isomet, Buehler Ltd, Lake Bluff, IL, USA)
and sintered according to the recommended proto-
col. To establish a uniform surface, each specimen
was polished with a rotational polishing device
using 180- and 320-grit silica carbide abrasive
paper under a steady stream of water. The polish-
ing was done by rotating the specimen 908 every one
minute with each grit, for a total of four minutes.
The specimens were finished with 0.5-lm Al2O3
slurry, rotating the specimens 908 every 30 seconds
for a total of two minutes. All specimens were
subjected to ultrasonic cleaning in distilled water
for 15 seconds.
The specimens were divided into groups (n=10)
based on surface pretreatments, as follows (Table 2):
1) no treatment (control); 2) 5% HF etch for 20
seconds (5HF); 3) 9.5% HF etch for 60 seconds
(9.5HF); 4) silane (S); 5) 5% HF for 20 seconds þ
silane (5HFS); and 6) 9.5% HF for 60 seconds þ
silane (9.5HFS).
Groups 5HF, 9.5HF, 5HFS, and 9.5HFS were
etched with HF. For the etching procedure using
5% HF (Ceramic etching gel, Ivoclar), a drop of
etchant was evenly spread for 20 seconds over the
Table 2: Etching, Silane, and Adhesive Procedure
Group Etch Concentration, % Etching Time, s
Control None
5HF 5 20
9.5HF 9.5
S None
5HFS 5 20
9.5HFS 9.5
Abbreviations: 5HF, 5% hydrofluoric acid (HF) etch for 20 s; 9.5HF, 9.5% HF etch for 60 s; S silane with no HF; 5HFS, 5% HF for 20 s þ silane; 9.5HFS, 9.5% HF for 60
s þ silane.
Operative Dentistry
Brand Name Manufacturer Lot No.
e.max Ivoclar Vivadent —
Ceramic etching gel Ivoclar Vivadent R05638
Porcelain etchant Bisco 1200006564
RelyX Ceramic Primer 3M ESPE N371615
Scotchbond Universal 3M ESPE 472585
Z100 3M ESPE N352896
bonding surface of the ceramic using a microbrush.
The surface was cleaned with water for 10 seconds.
The 9.5% HF (Porcelain etchant, Bisco, Schaum-
burg, IL, USA) was applied for 60 seconds and
cleaned with water for 10 seconds. Groups S,
5HFS, and 9.5HFS then received one coat of silane
(RelyX Ceramic Primer, 3M ESPE), which was
applied for 20 seconds using a microbrush and
then air dried for 10 seconds with room-tempera-
ture air. Scotchbond Universal adhesive (3M
ESPE) was applied onto all pretreated ceramic
surfaces for 20 seconds using a microbrush,
followed by air thinning for 10 seconds. The
adhesive was cured for 10 seconds with an LED
curing light (1200 mW/cm2; Elipar S10, 3M ESPE).
Curing light output was tested after finishing
every 10 specimens to check for uniformity of light
output using a radiometer (Power Max, Molectron
Detector Inc, Portland, OR, USA).
A 5-mm-long, transparent, plastic tube with an
internal diameter of 1.5 mm was filled with Z100
composite (shade A2, 3M ESPE). Z100 composite was
chosen to represent an adhesive resin cement, such
as Rely X Unicem (3M ESPE), as both materials are
composed of a methacrylate-based monomer rein-
forced with silanated inorganic fillers (70 wt% for
RelyX Unicem and 85 wt% for Z100). Z100 resin
composite was used instead of a cement in order to
prevent cohesive fractures within the bonded post.
The composite filled tube was affixed to the surface
of each ceramic specimen and light cured (Elipar
Silane Treatment Duration, s Universal Adhesive Treatment Duration, s
— — 20
— 20
60 — 20
— 20 20
20 20
60 20 20
Kalavacharla & Others: Bond Strength to Lithium Disilicate
Figure 1. Composite tube affixed to the coupon of lithium disilicate.
S10, 3M ESPE) on four sides for 20 seconds per side
(Figure 1). After storage in deionized water for 24
hours at 378C, the specimens were thermocycled for
10,000 cycles (six days) between 58C and 508C water
baths (15-second dwell time). Prior to shear bond
strength testing, the plastic tube was removed to
reveal a cylinder of composite. The specimens were
mounted into a steel fixture in a universal testing
machine (Instron 5565, Canton, MA, USA). A
sharpened stylus applied a shear load to the side of
the composite cylinder until failure at a crosshead
speed of 1 mm/min (Figure 2). The peak failure load
and surface area of the composite cylinder were used
to calculate the shear bond strength (MPa). An
additional specimen from both etching conditions
was sputter-coated and imaged under a scanning
electron microscope (SEM) for observation of the
etching pattern.
A two-way analysis of variance (ANOVA) and
Tukey post hoc analysis were used to analyze the
differences in the bond strength values based on HF
etching and silane treatment (a=0.05).
Table 3: Bond Strength of Lithium Disilicate to Composite
Resin with Different Surface Treatments (Mean
6 Standard Deviation [Group Abbreviation])a
Bond Strength, MPa
No Silane Application Silane Application
No HF 1.82 6 2.0 A (control) 12.55 6 5.0 A (S)
5% HF 19.08 6 3.0 B (5HF) 40.47 6 4.2 B (5HFS)
9.5% HF 24.93 6 2.6 C (9.5HF) 37.50 6 5.1 B (9.5HFS)
Abbreviations: 5HF, 5% hydrofluoric acid (HF) etch for 20 s; 9.5HF, 9.5% HF
etch for 60 s; S silane with no HF; 5HFS, 5% HF for 20 s þ silane; 9.5HFS,
9.5% HF for 60 s þ silane.
a
Groups in each column with similar capital letters are not statistically
different.
375
Figure 2. Lithium disilicate specimen mounted in the universal
testing device.
RESULTS
The means and standard deviations of the bond
strength values for each group are presented in
Table 3. The two-way ANOVA determined that there
were significant differences between HF etching,
silane treatment, and the interaction between the
HF and silane groups (p,0.01). As the factor ‘‘silane
treatment’’ was found to be significant, silane
treatment was shown to provide higher shear bond
strength without HF etching and at both concentra-
tions of HF etching. Individual one-way ANOVA and
Tukey post hoc analyses were performed for the
silane and no silane groups. Shear bond strength
values for each etch concentration were significantly
different (p,0.01) and could be divided into signif-
icantly different groups based on silane treatment:
no silane treatment: no HF , 5% HF , 9.5% HF; and
RelyX silane treatment: no HF , 5% HF and 9.5%
HF. Therefore, the significant interaction could be
explained by the fact that without silane treatment,
9.5% HF etching produced higher bond strength
than did 5% HF etching, whereas this was not the
case if the material was treated with silane. The
SEM images of the 5% HF etched lithium disilicate
showed the presence of elongated crystals after
partial disintegration of the silica matrix (Figures
3A and 3B). The 9.5% HF etched surface showed a
more distinct etching pattern with more dissolved
matrix (Figures 3C and 3D).
DISCUSSION
The use of HF etching improved resin-lithium
disilicate bond strength regardless of whether or
not silane was applied. Therefore, we can reject the
null hypothesis that HF etching will not affect the
376
Figure 3. Etching pattern of lithium disilicate etched for 20 seconds with 5% HF acid at 30003 (A) and 10,0003 (B) and for 60 seconds with 9.5% HF
acid at 30003 (C) and 10,0003 (D).
bond strength of resin bonded to lithium disilicate
pretreated with a universal composite. The concen-
tration/application time of HF etchant did not have a
significant effect on bond strength for the specimens
that were given a coat of silane. The specimens that
were not silanated, however, showed significantly
greater bond strength with 60 seconds of 9.5% HF
than with 20 seconds of 5% HF. Although the study
clearly demonstrates that optimal bonds are
achieved by HF etching and silanating, if an
additional silane step is not taken prior to applying
a universal adhesive, the use of 9.5% HF for 60
Operative Dentistry
seconds can increase bond strength. Perhaps the
explanation for this difference is that the specimens
that did not receive silane were more dependent on
the micromechanical retention provided by the etch
pattern in the ceramic. The SEM images show that
there is considerably deeper etching pattern present
on the specimen etched for 60 seconds at 9.5% HF
(Figure 3A-D). Therefore, the nonsilanated speci-
mens could achieve higher bond strengths with a
deep etching pattern in the 9.5% HF. The specimens
that were silanated, on the other hand, could rely on
the chemical bond facilitated by the silane molecules.
Kalavacharla & Others: Bond Strength to Lithium Disilicate
The choice to etch for 20 seconds with 5% HF and
for 60 seconds with 9.5% HF was based on the
manufacturer’s recommendations. Previous studies
have suggested that etching with 4.9% HF for over
90 seconds20 or with 9% HF for 120 seconds21
decreases the strength of the lithium disilicate. As
the bond strength in this study did not improve
when increasing the etching concentration from 5%
HF (20 seconds) to 9.5% HF (60 seconds), it is
beneficial to adopt a regimen of 5% HF at 20
seconds. This etching protocol will save the clinician
time and preserve the strength of the lithium
disilicate.
The results of this study also reveal that silane
treatment prior to application of a universal adhe-
sive significantly improved the bond strength re-
gardless of the method of etching. We can therefore
reject the null hypothesis that there is no difference
in bond strength between resin and lithium disilicate
when a silane treatment is applied. This result
suggests that the constituent silane in the universal
adhesive was not effective in optimizing the ceramic-
resin bond. Clinicians should therefore pretreat
lithium disilicate with a coat of silane prior to
applying the universal adhesive. A study by Panah
and others15 showed that microshear bond strength
between lithium disilicate and composite resin
improved from 4.10 MPa to 14.58 MPa when silane
was applied. Additionally, the microshear bond
strength improved from 14.04 MPa to 24.70 MPa
when silane was applied to lithium disilicate that
had been HF etched.15 This study further confirms
that lithium disilicate should undergo both sufficient
etching and silanization prior to bonding.
One limitation of this study is that only one brand
of universal adhesive was tested. There are several
commercially available universal adhesives that
have unique compositions. The specific chemicals
and concentrations used in each brand of adhesive
may have different interactions with the method of
surface pretreatment.
CONCLUSIONS
Optimal bonds are achieved by HF etching and
application of silane to lithium disilicate prior to
application of a universal adhesive. When using the
universal adhesive in conjunction with silane, it is
beneficial to adopt a regimen of 5% HF at 20 seconds
in order to minimize surface damage to the ceramic
while preserving the bond strength. If an additional
silane step is not taken prior to applying a universal
adhesive, the use of 9.5% HF for 60 seconds can
increase bond strength. As the constituent silane
377
and MDP in the universal adhesive were not
effective in optimizing the ceramic-resin bond, silane
should always be applied to lithium disilicate prior to
bonding.
Conflict of Interest
The authors of this manuscript certify that they have no
proprietary, financial, or other personal interest of any nature
or kind in any product, service, and/or company that is
presented in this article except for the following: Dr Burgess
has, through the University of Alabama at Birmingham,
contracts and research grants from the following: GC, 3M
ESPE, Ivoclar, Dentsply, Septodont, Glidewell, Discus, VOCO,
Shofu, Ultradent, Noritake, and DMG. However, Dr Burgess
received no honoraria, nor did he collect any fee, for the
submission of this manuscript.
(Accepted 20 August 2014)
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 CLINICAL RESEARCH

Luting of inlays, onlays, and overlays

with preheated restorative composite
resin does not prevent seating
accuracy
Pascal Magne, DMD, PhD, PD
The Don & Sybil Harrington Professor of Esthetic Dentistry, Division of Restorative Sciences,
Herman Ostrow School of Dentistry, University of Southern California, Los Angeles,
California, USA

Mehrdad Razaghy, DDS

Student, Herman Ostrow School of Dentistry, University of Southern California, Los Angeles,
California, USA

Marco Aurelio Carvalho, DDS, MS, PhD

Luciana Mara Soares, DDS, MS

Correspondence to: Dr Luciana Mara Soares

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Abstract
Purpose: To evaluate in vitro the verti-
cal seating of computer-assisted de-
sign/computer-assisted manufacturing
(CAD/CAM) composite resin inlays, on-
lays, and overlays luted with two differ-
Materials and methods: Sixty plastic ty-
podont molars were prepared for medi-
the central groove with similar morphol-
- (P
ations were milled using Lava Ultimate
- difference when compared to baseline
ispherical occlusal concavity for seating
measurements with an electromechan-
were luted either with preheated com-
of restorations was first evaluated at
-
ated after airborne-particle abrasion
(Step 1), after seating with luting agent
the Wilcoxon post hoc test were used to
compare the seating among steps, and
Mann-Whitney post hoc test were used
to compare the seating between luting
agents at P
Results: Seating differences varied sig-
nificantly from baseline (P
MAGNE ET AL
particle abrasion (Step 1) (P
Except for cement-luted inlays, the try-in
-
(P
using RelyX (P
with RelyX seated higher than during try-
2 (P
the seating of inlays with no statistical
(P
Conclusion: Airborne-particle abrasion
significantly deepens the seating of
CAD/CAM composite resin restorations,
torative composite resin luting agent
perfectly compensates for this discrep-
and overlays seat deeper compared
The latter, however, resulted in a slightly
Clinical significance: With the least
variation compared to baseline seating
(try-in), restorative composite resin used
as luting agent resulted in the seating of
CAD/CAM inlays, onlays, and overlays
closer to baseline when compared to
(Int J Esthet Dent 2018;13:318–332)
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Introduction 3-6 These authors all

-
The use of computer-assisted design/ ation can be compensated for by ex-
computer-assisted manufacturing (CAD/
CAM) posterior bonded restorations has
- cements still require efficient light curing
ations are classically delivered with an 7,8

adhesive protocol, including dual-cure Another potential advantage of re-

- storative composite resins used as a
clude the use of immediate dentin seal- luting agent is their resistance to wear,
which proved to be superior to meth-
only composite resins used as a luting acrylate or phosphate-based resin ce-
- 9,10 Using light-curing restorative
materials for luting tooth-colored inlay,
Friedman1 demonstrated the success onlays or overlays should therefore no
for over 15 years of porcelain veneers 11

bonded with a microhybrid restorative Despite the aforementioned, clini-

2 cians are still concerned about the pos-
may have been the first to propose the sibility of incomplete restoration seating
use of a restorative composite resin as due to the viscosity of the restorative ma-

authors demonstrated that, with respect resin through ultrasonic devices12 or a

- small composite heater13 has been pro-
vantages of dual-curing resin compared posed to increase the flow and facilitate
- -
all handling of the light-curing compos- tion, preheating proved to have posi-
ite resin was judged to be easier than 14,15

conclusions were drawn by Krämer and 16-18 however, this might

3 who added that less not happen during a luting procedure
luting composite overhangs were found because of the rapid cooling of the ma-
- 13,14

posite resin because the clinician has The same syringe of material can be
more time for excess removal prior to preheated up to 20 times without affect-
ing the mechanical properties or poly-
Remaining concerns about the depth 19,20

Some authors, however, have claimed

-
lays and overlays have been resolved
by several studies showing that even resins were higher than those of veneer
- cements and flowable composite resins,
priate mechanical performance when 21 Although
restorative composite resins might not

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 MAGNE ET AL

a b c

Inlay Anatomical onlay Flat overlay

Groups INcr INcem ONcr ONcem OVcr OVcem

Preheated Dual-cure Preheated Dual-cure Preheated Dual-cure

Luting
restorative resin restorative resin restorative resin
agent
composite resin cement composite resin cement composite resin cement

Fig 1 (a) (b) (c) Overlay

Materials and methods

-
face of composite resin inlays or onlays
needs to be air abraded with aluminum
oxide before bonding,22-25 this might
create the additional clearance space
- molar typodont teeth (Columbia Dento-
portance is that different parameters of
pressure, and time of abrasion could af-
of this study was to evaluate in vitro the
vertical seating of CAD/CAM composite
resin inlays, onlays, and overlays luted
null hypothesis was that restorations
would seat similarly, independent of the
type of luting agent (restorative mater-
ial vs dual-cure cement) or preparation
Tooth preparation
with an isthmus width of 4 mm, pulpal
floor depth of 3 mm, and proximal box
forms was applied to 20 mandibular first
form) by using chamfer round-ended
-
larly, 20 additional teeth were prepared
with identical isthmus width and pulpal
floor depth measurements as those of
the inlay, but with an extra 2-mm reduc-
that was to be connected to the proximal
box forms, to receive anatomic onlay res-
tion with an occlusal reduction of 3 mm
and flattened cusps was performed on

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 CLINICAL RESEARCH

Fig 2

proximal box forms were developed -

preparations presented soft internal an-
All typodont teeth were sectioned at
the root base 3 mm below the artificial
cementoenamel junction (CEJ), and the
sectioned surfaces were accurately flat-
tened and smoothened with sandpaper
pression scanning of each prepared
tooth was performed, aided with a con-
trast powder (Cerec Optispray, Sirona),
and restorations were designed using
were milled in nanofilled composite
resin (Lava Ultimate A2, 3M ESPE), and
carefully adjusted to the preparations

box forms of 1-mm depth were created

in the center of the buccal and lingual
root surfaces to guide the positioning of
the specimens during all the measure-
Design and manufacturing
of the restorations
All specimens were restored using the
One unprepared tooth was scanned to
generate a master for the biogeneric
hemispherical occlusal concavity (load
fossa) of 1-mm depth was created by
on all the restorations, to precisely per-
form the vertical seating measurement
The 60 teeth were divided into six
groups according to preparation design
composition and properties of the luting
materials used in the study are shown in

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 MAGNE ET AL

Table 1 Material application, brand name, manufacturer, and composition of the materials used for lut-
ing in the study

Application Preheated restora- Dual-cure self- Total-etch adhe- Universal adhe-

tive composite adhesive universal sive system sive system
resin for restor- resin cement for
ation luting restoration luting

Brand name RelyX Ultimate Optibond FL (Ad- Scotchbond Uni-

versal Primer and
Adhesive

Manufacturer 3M ESPE, St Paul, 3M ESPE, Seefeld, Kerr, Orange, USA 3M ESPE, Seefeld,
USA Germany Germany

Composition Base paste: Adhesive: MDP phosphate

TEG-DMA methacrylate 2-hydroxyethyl -
Inorganic matrix: monomers con-
taining (or not) 3-trimetho-
(71%) phosphoric acid xysilylpropyl

2-hydroxy-1,3-
initiator compo- propanediyl

rheological addi- -
tives cates (n/a)

Catalyst paste:
methacrylate
-

initiator compo-

-
logical additives

Flexural 300 98 n/a n/a

strength (MPa)

Mean particle 13 n/a

size (µm)

Filler content 85 48
(% wt)

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 CLINICAL RESEARCH

a b c

Fig 3
(a) (b) (c)

Vertical seating test At baseline (dry try-in)

All specimens were placed on a flat
stainless steel base and the contour of
their root base was drawn on the sur-
face with a pencil to guide and repeat
the precise position of the specimen at
- The inner surfaces of all the restorations
ually subjected to a maximum 30 N of
load (Acumen III, MTS Systems), axially
applied by a spherical stainless steel tip
Restorations were initially seated without
any surface treatments or luting agent
(Fig 2), and the vertical axial positioning
was recorded as a baseline measurement
After airborne-particle abrasion (Step 1)
modified aluminum oxide (Rocatec, 3M
ESPE) for 10 s at a distance of 10 mm

of the occlusal surface of the restor- cleaning was performed by immersion

values were recorded for each step of
the vertical seating test (baseline, after
airborne-particle abrasion, after seating
with luting agent, and after light polymer-
the root base of the tooth and the surface
of the stainless steel base were cleaned
out after each measurement to remove
in distilled water using an ultrasonic bath
-
itioned on the stainless steel base for the
second step of the vertical seating test,
following the same parameters as pre-
-

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a b
Fig 4
(b)
After seating with luting agents (Step 2)
The bonding surfaces of the restorations
for groups 1, 3, and 5 were subsequently
treated according to the following luting
protocol for preheated restorative com-
posite resin: 1) Application of silane (Si-
lane, Ultradent) for 20 s and heat drying
-
in (Optibond FL, bottle 2, Kerr), without
the restorations onto the preparations
with the restorative composite resin (Fil-
in a heating device (Calset, AdDent)
- curing light, Ultradent) while the speci-
ite resin excesses, the specimens were
placed on the stainless steel device to
perform the second step of the test, fol-
lowing the same parameters previously
all the restorations for groups 2, 4, and 6,
luted with dual-cure resin cement (RelyX
Ultimate), were treated according to the
- surface to perform the third step of the
tion of Scotchbond Universal Primer and
MAGNE ET AL
c
(a) Application of
(c)
Adhesive (3M ESPE) to the inner surface
of the restorations for 20 s, followed by
2) Application of the resin cement into
-
ing of the restorations onto the prepar-
The specimens were then loaded in
Testing was then performed, and axial
After light polymerization (Step 3)
Each surface of the restorations was ulti-
mens were maintained under 30 N of
from the device and all margins covered
Personal Products Company) for an
-
placed in the same position on the flat
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 CLINICAL RESEARCH

Statistical analysis compare the seating among the differ-

ent steps for each preparation design
Statistical analysis was performed with
SPSS (version 23) statistical software

difference in seating after airborne-par- Results

ticle abrasion (Step 1) for each type of
preparation (inlay, onlay, and overlay), The measured mean vertical displace-
ments and standard deviations of the
with P seated restorations are presented in Ta-

during the seating with the luting agent
(Step 3), the Mann-Whitney U test was
used to compare two-by-two the means
obtained according to the luting agent
- of inlays compared to onlays (P
posite resin, and RelyX Ultimate dual-
cure resin cement) within each type of
The Friedman test, followed by the
airborne-particle abrasion (Step 1) are
presented in Figure 5, according to the
Whitney U test revealed the presence
of significant differences in the seating
and overlays (P -
ence was found between onlays and
overlays (P
During the seating with unpolymer-

correction (P the Wilcoxon post hoc test, the baseline

-1

-2

-3

-4

-5
a
Fig 5 Vertical measurement
means and standard deviation
-6
(n = 20) after airborne-particle
b b
abrasion (Step 1) for each type
-7
Inlay Onlay Overlay followed by Mann-Whitney U post
hoc test (P

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 MAGNE ET AL

Table 2 Vertical measurement data during Steps 1, 2, and 3

Step 1: Verti- Step 2: Vertical Step 3: Vertical

cal measure- measurements measurements
Groups ments in µm in µm with unpo- P value in µm after luting P value
after air abra- lymerized luting agent polymeriza-
sion (SD) agent (SD) tion (SD)

INcr (1) Aa Aab

Ab 0 0

INcem (2)

ONcr (3) Aa Ac

ONcem (4) Aa

OVcr (5) Aab Ab

OVcem (6) Aa

try-in position was recovered for all res- hand, inlays luted with RelyX Ultimate
torations (P - (INcem) seated close to their unpo-
P
higher compared to the baseline try-in
above the baseline try-in, P (P -
Mann-Whitney U test presented no differ-
ence between the luting agents for onlays
(P P

- Discussion
coxon post hoc test showed that onlays
The use of preheated restorative com-
posite resin (instead of resin cement)
- as a luting agent for inlays, onlays, and
ite resin (P overlays was investigated, especially
deeper when using RelyX Ultimate dual- -
cure composite resin cement (OVcem ation seating due to the viscosity of the

respectively) (P rejected because all restorations seated

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 CLINICAL RESEARCH

15

10

a
a a
a
0

-5

INcr INcem ONcr ONcem OVcr OVcem

Fig 6

15

10

a
-5

b b
-10
INcr INcem ONcr ONcem OVcr OVcem

Fig 7

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closer to baseline with the restorative
material when compared to the dual-
cure cement, in addition to the fact that
the onlays and overlays seated deeper
Typodont plastic teeth were chosen
because of their availability but also be-
cause tooth preparations, restorations,
and positioning in the measuring device
was applied consistently through the
accurate electromechanic system in the
exact same location at each step of the
after simulating the luting pressure in a
- Apart from this surprising finding about
vided highly precise load and motion
resolution digital encoder to ensure ac-
curate control and measurement of the
- ness might not have an influence on the
confirm the exact vertical positioning,
Airborne-particle abrasion is neces-
sary to enhance resin-to-resin bond-
ing of both laboratory and CAD/CAM
22-25 This
potentially creates an additional gap in
confirms this fact because air abrasion
with Rocatec sand (3M ESPE) resulted in
significantly deeper seating into the tooth
subjecting the restoration to sandblast-
ing, so as to preserve marginal adapta-
tion (such as protecting the margins with
a finger pressed onto the occlusal surface
sandblasting was slightly stronger in on-
MAGNE ET AL
Once inserted with the luting com-
posite resin, the seating of all the res-
higher than baseline, were an excep-
-
-
As most of the preparation is formed by
the vertical walls in inlays, it is expected
that the seating would be more affected
inlays, no statistically significant differ-
ence was found between the cement
and the restorative material for onlays
-
composite resins might not present the
21 this did not pre-
vent the appropriate seating of the res-
Prior to light curing, the viscosity af-
fects the application and manipulation
-
ity of restorative composite resins var-
ies significantly between brands, even
though they might be included in the
26 In addition, as tempera-
ture increases, the viscosity of the com-
material responded differently, with a
27
Hence, many composite resins are not
suitable for luting because their viscos-
-
28
resin was selected for luting purposes
329
THE INTERNATIONAL JOURNAL OF ESTHETIC DENTISTRY
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 CLINICAL RESEARCH

- -
26 ing to the positional changes of onlays/
In order to understand the effects of overlays) are also in accordance with

seating, it needs to be borne in mind that -

clusion is perfectly preadjusted during
the light but rather toward the surfaces try-in, the positional change (deeper
29 Therefore, seating) during adhesive delivery will

As expected, the seating of all the in- The present results are clearly in favor
lays remained very similar after light of the use of preheated restorative ma-
terials as a luting agent for inlays, on-

clear, practical advantages to using pre-

lingual) being perpendicular to the long heated composite resin over traditional
resin cements11 such as ease of excess
et al,30 removal because of the firm consisten-

contraction of the composite resin ce-

ment is non-destructively compensated
for by an inward flexing of each cavity
- Conclusions
The use of preheated restorative com-
vectors are along the axis of the tooth, posite resin as a luting agent for inlays,
hence they pull the restoration against onlays, and overlays can be recom-
-
torations demonstrated significant posi- incomplete restoration seating due to the
tional changes (deeper seating) after viscosity of the composite are not justi-

Airborne-particle abrasion significantly

- deepens the seating of CAD/CAM com-
posite resin restorations, but the pres-

composite resin luting agent perfectly

31

The difference between luting agents the least variation compared to baseline
- seating (try-in), the restorative compos-
tolotto et al32 that showed significantly ite resin resulted in a more predictable
- seating of the CAD/CAM inlays, onlays,
tion forces when restorative materials and overlays when compared to the du-
were used as a luting agent compared

330
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AUTUMN 2018
 MAGNE ET AL

The authors wish to express their grati-
tude to 3M ESPE (St Paul, MN, USA), Kerr
(Orange, CA, USA), Ultradent (South
Jordan, UT, USA), Patterson Dental (Los
Angeles, CA, USA), and Sirona Dental
Enciso, PhD (Associate Professor of Clin-
ical Dentistry, Herman Ostrow School of
Dentistry, University of Southern Cali-
fornia), for guidance with the statistical

References
-

Curr Opin Cosmet Dent cured cements under com-

Kawano Y, Francci C, Reis

-
of composites under Cerec Conversion of dual cure lut- ite pre-heating: effects on
- marginal adaptation, degree
of conversion and mechani-

bonded leucite-reinforced -
glass ceramic inlays and version of pre-heated com-

cements for bonding esthetic

ceramic inlays and onlays
luted with a solely light-cur-
-
Current clinical concepts
for adhesive cementation of
tooth-colored posterior res-

Onisor I, Ardu S, Krejci I, Effect of pre-heating on the

viscosity and microhardness
of light- and dual-polymer-
- Curr Opin Cosmet Dent

- and extending heating on

cally relevant issues related

J Esthet Restor Dent

CAM Composite Resin
- -
heating cycles on flexural
The effect of resin composite
pre-heating on monomer

331
THE INTERNATIONAL JOURNAL OF ESTHETIC DENTISTRY
AUTUMN 2018
 CLINICAL RESEARCH
of cementation materials
for veneers: An in vitro 3D
microcomputed tomography
of composite surfaces for
cement to post-cured hybrid
cement to a cured compos-
332
THE INTERNATIONAL JOURNAL OF ESTHETIC DENTISTRY
AUTUMN 2018
of Different Surface Treat-
ments on Luting CAD/CAM
Composite Resin Overlay
-
a vertical oscillation rheom-
of resin composites accord-
ing to variations in composi-
temperature on unpolymer-
toward the light? J Dent Res
-
ginal adaptation in bonded
-
metric method for measuring
-
age in light cured dental
Gutemberg D, Veuthey JL,
resin cement for luting of
indirect restorations: com-
parison of solubility and
 CLINICAL ARTICLE

Semidirect Composite Onlay With Cavity Sealing:

A Review of Clinical Procedures
AMAL ALHARBI, BDS, MAS*, GIOVANNI TOMMASO ROCCA, DR. MED. DENT.†,
DIDIER DIETSCHI, DR. MED. DENT., PhD, PD‡, IVO KREJCI, PROF. DR. MED. DENT.§

ABSTRACT
The evolution in adhesive dentistry has broadened the indication of esthetic restorative procedures especially with
the use of resin composite material. Depending on the clinical situation, some restorative techniques are best indicated.
As an example, indirect adhesive restorations offer many advantages over direct techniques in extended cavities. In
general, the indirect technique requires two appointments and a laboratory involvement, or it can be prepared
chairside in a single visit either conventionally or by the use of computer-aided design/computer-aided manufacturing
systems. In both cases, there will be an extra cost as well as the need of specific materials. This paper describes the
clinical procedures for the chairside semidirect technique for composite onlay fabrication without the use of special
equipments. The use of this technique combines the advantages of the direct and the indirect restoration.

CLINICAL SIGNIFICANCE
The semidirect technique for composite onlays offers the advantages of an indirect restoration and low cost, and can
be the ideal treatment option for extended cavities in case of financial limitations.
(J Esthet Restor Dent ••:••–••, 2013)

INTRODUCTION options depends mainly on the number, extension, and

The trend toward conservative esthetic dentistry has
become very popular because of patient awareness of
esthetic restorations and improvements in materials’
properties. Composite resin is the material of choice in
many dental treatments because of improved esthetics,
strength, and durability.1,2 It also allows conservative
preparation and easy addition/reparation of the
restoration.3
When using composite resin restoration, the choice of
the proper restorative technique plays an important
role in the longevity of the restoration.4 Three main
restorative techniques are available, direct, semidirect,
and indirect2,5 (Figure 1). The selection between those
location of the restoration.2 In large cavities, the
indirect technique allows the achievement of a good
occlusal and interproximal anatomy.6 In addition, it
provides theoretically better marginal adaptation
because of the lower polymerization stresses between
the restoration, and the tooth as shrinkage is normally
confined to the thin layer of resin cement.7–9 Moreover,
the restoration’s physical and mechanical properties
may be improved due to the effect of the post-curing
procedure.10–12 However, this technique requires two
appointments, the fabrication of a provisional
restoration, and the contribution of a lab technician
that lead to an increase of time and costs. With
the introduction of the computer-aided design/
computer-aided manufacturing (CAD/CAM) system

*PhD student, Department of Cariology and Endodontics, University of Geneva, Geneva, Switzerland
†
Doctor, Department of Cariology and Endodontics, University of Geneva, Geneva, Switzerland
‡
PD and doctor, Department of Cariology and Endodontics, University of Geneva, Geneva, Switzerland
§
Professor and doctor, Department of Cariology and Endodontics, University of Geneva, Geneva, Switzerland

© 2013 Wiley Periodicals, Inc. DOI 10.1111/jerd.12067 Journal of Esthetic and Restorative Dentistry Vol •• • No •• • ••–•• • 2013 1
 SEMIDIRECT COMPOSITE ONLAY WITH CAVITY SEALING Alharbi et al.
in 1985,13 the treatment time and the laboratory steps
were reduced. Nevertheless, the cost is still high
compared with the direct restoration, and the
technology remains expensive.
A simplified chairside method called “semidirect
technique” was introduced and developed in the
1980s.14–17 In this technique, the dentist himself
fabricates the restoration with an intraoral or extraoral
procedure during a single appointment.4 In the intraoral
approach, the restoration is fabricated by placing
directly the composite increments on the isolated
tooth’s cavity. After in-mouth polymerization, the
workpiece is removed and finished/polished extraorally,
followed by the luting of the restoration. Although the
intraoral approach could be the most accurate18 in
respect to marginal fit, as the restoration is made
directly in the cavity, the main disadvantage of this
approach is the difficulty of removing the restoration
after composite resin hardening. This is mainly due to
the cavity configuration and the microretentions
created by the diamond burs used for preparation.4
That confines its use to simple cavities (occlusal,
mesio-occlusal, or disto-occlusal) with a regular design
and highly divergent walls. In the extraoral approach, a
silicon-working model is fabricated from the impression
of the cavity in order to build-up the restoration
chairside extraorally. This approach offers an advantage
over the intraoral one as less divergent cavity walls are
2 Vol •• • No •• • ••–•• • 2013 Journal of Esthetic and Restorative Dentistry
FIGURE 1. General classification of
dental restorations. CAD/CAM =
computer-aided design/
computer-aided manufacturing.
required; thus, a more conservative preparation can be
realized.4,19 However, the freehand semidirect technique
is more sensitive to the cavity configuration design than
the CAD/CAM technique, e.g., the mesial-occlusal
-distal (MOD) cavity may cause a problem because of
the polymerization shrinkage that tends to be directed
toward the axial walls leading to lock of the restoration
that will prevent its removal.2,4
The major advantage of the semidirect technique is that
the dentist can provide his patient with a low-cost
indirect restorationt in a single visit.
The aim of this paper is to describe step by step the
extraoral semidirect technique with cavity sealing20 in
two clinical cases.
MATERIALS AND METHODS
Case 1
The first case was a 33-year-old female with a large
defective occlusal-buccal amalgam restoration on the
mandibular first molar that needed replacement
(Figure 2). The patient could not tolerate long dental
appointments because of a limited mouth opening. In
addition to that, patient presented some financial
limitations.
DOI 10.1111/jerd.12067 © 2013 Wiley Periodicals, Inc.
 SEMIDIRECT COMPOSITE ONLAY WITH CAVITY SEALING Alharbi et al.
FIGURE 2. Preoperative view of the mandibular first molar
showing the defective amalgam restoration.
All these elements brought the therapeutic solution to
the semidirect technique. With this option, cavity was
prepared first, the workpiece was then fabricated
chairside extraorally, while the patient was waiting, and
then the restoration was luted within the same
appointment. Thus, the patient received restoration
that combined the advantages of the direct and the
indirect technique.
Cavity Preparation
A particular attention was drawn to the intraoral steps
in respect to the low tolerance of the patient for long
dental appointment.
Before starting the treatment, occlusal contacts were
checked with a contact-point paper in order to evaluate
the occlusal space available for the future restoration.
Then, shade was selected based above all on
neighboring teeth color, as the presence of a metallic
restoration with recurrent caries may affect the tooth
color. Alternatively, shade selection can be done after
removing old restoration.
Rubber dam was placed, and cavity preparation was
completed in a very conservative manner using
diamond bur. Cavity preparation was strictly confined
to the removal of decayed tooth structure (Figure 3A).
In order to seal the free dentin in the cavity, a self-etch
adhesive system was used (Syntac Classic, Ivoclar
Vivadent, Schaan, Liechtenstein) according to the
© 2013 Wiley Periodicals, Inc. DOI 10.1111/jerd.12067
manufacturer’s instructions. Then, a thin layer of
restorative nanohybrid composite resin (Tetric
EvoCeram, IvoclarVivadent) was used to achieve an
ideal cavity geometry with minimal preparation (no
undercuts, regular surface, and correct taper)20
(Figure 3B). Composite resin light-curing was
accomplished with a high-power light-emitting diode
(LED) curing light for 40 seconds per curing area.
Finishing of enamel margins and of the composite
surface was done with the use of fine diamond bur
before taking the impression of the cavity to clean the
enamel and to remove the oxygen inhibition layer on
the composite surface and to achieve a slightly beveled
surface21 (Figure 3C). Rubber dam was removed, and
the preparation was carefully isolated using cotton
pellet to be ready for the impression.
Impression and Working Model Fabrication
The working model should be fabricated with a
material characterized by a fast setting time, high
rigidity, and prompt easy separation from the
impression.2 Most of the silicones, which can be
potentially used for model fabrication, are addition-type
materials, so ideally, the impression should be done
using a condensation-type silicone material. Speedex
(Coltene/Whaledent, Altstätten, Switzerland) was used
for this purpose, together with a simple sectional tray.
Then, in order to have a certain precision on the
working model, a thin layer of light body impression
material (Affinis, Coltene/Whaledent) was applied
before the completion of the working model by the
application of the body mass (Jet Bite,
Coltene/Whaledent) (Figure 4)
Work Piece Fabrication
The restoration was completed through several
increments of nanohybrid composite resin material
(Tetric EvoCeram) of about 1.5-mm thickness; each
layer was light-cured by LED lamp for 40 seconds. The
first increment was done with dentin shade.
Subsequently, enamel and incisal layers were placed and
shaped to achieve an ideal anatomy. The final
characterization was accomplished by the use of
intensive color resin (Kolor+plus, Kerr, Orange, CA,
USA). Once the onlay has been completed, its
adaptation was checked intraorally (Figure 5).
Journal of Esthetic and Restorative Dentistry Vol •• • No •• • ••–•• • 2013 3
 SEMIDIRECT COMPOSITE ONLAY WITH CAVITY SEALING Alharbi et al.
FIGURE 3. Cavity preparation. A, Old restoration and the secondary caries were removed, and the cavity was cleaned. B,
Immediate Dentin Sealing and composite coating. C, Finishing of the enamel margins with fine diamond bur.
Moreover, in order to achieve a maximum monomer
conversion of the resin, dimensional stability, and
improved mechanical properties,22 the semidirect onlay
was post-cured in a special oven (D.I. 500,
Coltene/Whaledent) for 7 minutes at 120°.2,6
Luting of the Restoration
First, the internal surface of the restoration was cleaned
with soft air abrasion to remove any contamination
during the intraoral try-in. Then, a thin layer of
bonding resin was spread over the surface and left
uncured. The restoration was placed under light
protection23 (Figure 6).
Under rubber-dam protection, the cavity was cleaned
with air abrasion (30 microns Al2O3) for about 5
seconds. Enamel was selectively etched with 37%
4 Vol •• • No •• • ••–•• • 2013 Journal of Esthetic and Restorative Dentistry
FIGURE 4. Impression and flexible
model fabrication. A,B, Sectional final
impression (Speedex
Coltene/Whaledent). C, First part of
the flexible model fabrication was
fabricateddone using alight body
additional silicons (Affinis,
Coltene/Whaledent). D, Flexible
model was completed by the body
mass silicon (Jetbite,
Coltene/Whaledent).
phosphoric acid for 30 seconds, rinsed with water spray
for 30 seconds, and air dried. The bonding agent was
applied on the entire cavity surface without being
light-cured. (Figure 7). Finally, an adequate amount of
preheated restorative composite resin (Tetric
EvoCeram) was spread all over the cavity surface. The
onlay was inserted into the cavity and fixed in place by
applying a finger pressure on the occlusal surface. A
dental probe was used to remove the excess of luting
composite. The restoration was then seated in its final
position with the help of ultrasonic energy, and the final
removal of the excess was done using a soft brush. A
spot cure of 5 seconds per surface was effectuated to fix
the restoration in place using high-power LED curing
unit, then full polymerization was achieved by light
curing for at least 60 seconds per surface from the
buccal, oral, and occlusal each. Fine diamond burs
DOI 10.1111/jerd.12067 © 2013 Wiley Periodicals, Inc.
 SEMIDIRECT COMPOSITE ONLAY WITH CAVITY SEALING Alharbi et al.

FIGURE 5. Restoration build-up.

A–C, Restoration build-up with a
restorative hybrid composite resin.
D, Try-in of the onlay in the mouth.

FIGURE 6. Adhesive treatment of

the onlay. A, Internal surface of the
onlay was cleaned with soft air
abrasion. B–D, A thin layer of
adhesive resin was placed and left
unucured, the restoration was
covered in a light protective box.

(Composhape, Intensiv, Grancia, Switzerland) was used
to finish the margins, and then the restoration was
polished with a diamond-coated discs (PopOn, 3M
ESPE, St. Paul, MN, USA) and silicone points
(Identoflex, Kerr, Bioggio, Switzerland)
(Figures 8 and 9).
Case 2
The second case was a 69-year-old female who
presented a Cl II MOD amalgam restoration on the
mandibular second molar, which needed replacement
(Figure 10A). The tooth was vital with no history of
pain. The wide extension of the cavity and the position
of the tooth limiting the accessibility to obtain a good
anatomy were a clear indication for an indirect
restoration, but as the patient had financial limitations,
a semidirect technique was chosen.
During the cavity preparation, the lingual cusps were
reduced due to the presence of important dentinal
fissures. The treatment procedures were the same as

© 2013 Wiley Periodicals, Inc. DOI 10.1111/jerd.12067 Journal of Esthetic and Restorative Dentistry Vol •• • No •• • ••–•• • 2013 5
 SEMIDIRECT COMPOSITE ONLAY WITH CAVITY SEALING Alharbi et al.
described for the 1st case, except for some steps in the
model fabrication (Figure 10B–F).
DISCUSSION
The main reason to replace posterior composite
restoration is secondary caries24 mainly related to the
failure on the bond interface. This failure develops
during the polymerization shrinkage of the resin.25
This phenomenon will create internal stresses on the
restoration, which may lead to marginal failure. Various
techniques have been described in the literature to
overcome this problem,26–29 e.g., the incremental
method, the use of glass-ionomer bases and the indirect
technique. The indirect technique in particular allows
the initial polymerization contraction, and the following
post-curing shrinkage to occur before cementation.30
Various in-vitro studies have shown that tensile
strength, elastic modulus, fracture toughness,
hardness, and wear resistance are improved by
post-curing.10–11,31–32 Also marginal adaptation of resin
composite inlays has been reported in some studies to
be superior to direct fillings, showing less microleakage
and better marginal quality.33–35
Nevertheless, the cost and the time needed to fabricate
indirect restorations remains an important concern of
6 Vol •• • No •• • ••–•• • 2013 Journal of Esthetic and Restorative Dentistry
FIGURE 7. Adhesive treatment of
the cavity. A, Cleaning of the cavity
with soft air abrasion. B, Conditioning
of the enamel margin with
orthophosphoric acid-etching.
C,D, A thin layer of adhesive resin
was applied and left uncured.
the technique. The use of the chairside semidirect
technique overcomes this issue without affecting the
restoration quality. In an 11-year clinical trial, Van
Dijken concluded that semidirect composite resin
inlays/onlays showed a promising clinical longevity with
improved marginal adaptation and low incidence of
secondary caries.36 A 3.5-year evaluation for
medium-size cavity showed that there were no
significant differences for direct and semidirect
composite restoration in respect to clinical evaluation
and scanning electron microscopy marginal adaptation.
These two studies confirm that this technique could be
of benefit for large cavites.6
Despite the elimination of the lab involvement in the
restoration fabrication, the procedure allows the
realization of a predictable final result from the esthetic
point of view as the restoration is fabricated and
corrected chairside.
In contrast with the chairside CAD/CAM system, the
free-hand semidirect technique does not need special
expensive tools or equipment. However, care should be
taken in respect to the choice of the material for
impression and model fabrication. These materials
should have different chemical composition in order to
insure easy separation between the model and
impression. During model fabrication, the use of a thin
DOI 10.1111/jerd.12067 © 2013 Wiley Periodicals, Inc.
 SEMIDIRECT COMPOSITE ONLAY WITH CAVITY SEALING Alharbi et al.

FIGURE 8. Luting procedure of the

onlay. A, The warm hybrid composite
resin was placed into the cavity.
B, The composite resin was spread
over all the cavity surfaces. C, The
onlay was seated and held in place
with a plugger, then the excess
material was removed with a probe.
D, Complete seating of the
restoration was accomplished by the
use of ultrasonic tip. E, Final removal
of the excesses was done with a soft
brush. F, Light-curing of the
restoration with the light-emitting
diode lamp. G,H, Finishing of the
restoration with a fine diamond bur
and abrasive discs.

FIGURE 9. Final restoration.

A, Occlusal view of the mandibular
first molar 1 week after the luting.
B, Two years follow up.

© 2013 Wiley Periodicals, Inc. DOI 10.1111/jerd.12067 Journal of Esthetic and Restorative Dentistry Vol •• • No •• • ••–•• • 2013 7
 SEMIDIRECT COMPOSITE ONLAY WITH CAVITY SEALING Alharbi et al.

FIGURE 10. Case 2. A, Preoperative view of the mandibular second molar showing the large MOD old amalgam restoration,
which needs to be changed. B, During cavity preparation, the lingual cusps were undermined by horizontal fissure and therefore
removed. C, Immediate dentin sealing procedure and cavity resin coating. D,E, Silicon working model. The model is partially cut in
the interproximal region to facilitate the build up of the marginal ridge and the proximal surface, as in this way, the model can be
opened giving a better access for the sculpturing. F, Postoperative view after the luting of the onlay. MOD = mesial-occlusal-distal.

layer of light body silicon was introduced to have a
certain precision in the working model. However, the
excessive use of light body material may affect the
rigidity of the working model. Thus, deformation may
occur during the restoration’s build up because of the
increased model flexibility.
Although the semidirect restoration is done in a single
appointment, meaning that the so-called immediate
dentin sealing procedure37,38 would not be necessary,
dentin was sealed to eliminate any risk of sensitivity
during the period between the two phases of the
treatment. Moreover, by using immediate dentin
sealing, anesthesia is often not necessary during the
second phase. It is well proven that the use of self-etch
adhesive system will insure sealing of the freshly cut
dentinal tubules, thus reducing the postoperative
sensitivity and preventing bacterial contamination.37
Furthermore, the application of the composite resin
layer over the sealed dentin eliminates cavity undercuts,
thus allow minimally invasive preparation.20 The use of
sandblasting associated with the subsequent application
of a silane solution is employed in the indirect
technique to reactivate the composite resin layer before
luting.39 However, its use is probably not essential in the
semidirect technique as the composite resin is still
chemically reactive.40 During the adhesive treatment,
composite resin of both the restoration and cavity was
cleaned with soft air abrasion to remove any potential
contamination that could occur during the intraoral
try-in or during the break between the two phases.
Restorative hybrid composite resin was used in adhesive
luting procedure23 as it provides rather low
polymerization shrinkage and rather low coefficient of
thermal expansion compared with low-filled resins (as
the common dual-cured resin luting cements).41 The
use of preheated composite resin improved the
handling characteristics of the material by decreasing its
viscosity, which aided to the attainment of excellent
restoration margins.42 In addition, this treatment
enhances the adaptation of the material, decreases the
potential of voids formation, and increases monomer
conversion, thus resulting in better physical and
mechanical properties.43 Finally, it is important to note
that the use of the described technique allows for
fabrication of the restoration using the same restorative
hybrid composite resin that was used to seal the cavity

8 Vol •• • No •• • ••–•• • 2013 Journal of Esthetic and Restorative Dentistry DOI 10.1111/jerd.12067 © 2013 Wiley Periodicals, Inc.
 SEMIDIRECT COMPOSITE ONLAY WITH CAVITY SEALING Alharbi et al.
FIGURE 11. General features of
the different restorative techniques.
and then to lute the restoration. This leads to perfect
chemical compatibility and identical biomechanical
properties between the different layers of the
restoration, which may offer an additional advantage for
this technique.
CONCLUSIONS
The use of the semidirect technique overcomes the
disadvantages of the indirect technique, e.g., lab
involvement, extra time and cost. It combines the
advantages of the direct and the indirect approaches
(Figure 11).
DISCLOSURE
The authors do not have any financial interest in the
companies whose materials are included in this article.
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application of dentin bonding agents: effect on bond
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40. Papacchini F, Dall’Oca S, Chieffi N, et al.
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the repair of a microfilled hybrid resin: effect of surface
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Reprint requests: Amal Al-Harbi, BDS, MAS, Section de Médecine
dentaire, Division de Cariologie et d’Endodontie, Université de Genève,
19, rue Barthélemy-Menn, Genève 1205, Switzerland; Tel.: 022-379-41-00;
Fax: 022-379-41-02; email: amal.alharbi@unige.ch
DOI 10.1111/jerd.12067 © 2013 Wiley Periodicals, Inc.
J Dent Res 77(2): 426-431, February, 1998
Effect of Heating Delay on Conversion and
Strength of a Post-cured Resin Composite
MA Loza-Henrerol, FA RueggebergZ3*, W.F. Caughmanz3, G.S. Scduster32, CA. Lefebvr3, and EM Gardnei3
lPrivate prosthodontic practice, Caguas, Puerto Rico; 'Assistant Professor, Restorative Sciences Department, School of Dentistry, University
of Puerto Rico; 2Department of Oral Rehabilitation, Medical College of Georgia, School of Dentistry; 3Department of Oral Biology, Medical
College of Georgia, School of Dentistry; and *Section Director, Dental Materials, Department of Oral Rehabilitation, Medical College of
Georgia, School of Dentistry, Augusta, Georgia 30912-1260; *corresponding author
Abstract Physical property enhancement in light-cured resin
composites from post-cure heating is attributed to free radicals
created during initial photocuring, the number of which
decreases following initial light-curing. Clinically, it is
important to know when the number of remaining free
radicals is too low to provide for additional conversion of
monomer in post-cure-heated specimens. The hypothesis
tested is that the potential for additional conversion in post-
cure-heated resin composite restorations is dependent upon
the time after initial light-curing at which the specimen is
exposed to heat treatment. This research examined the effect of
delay in post-cure heating after initial photo-activation on
strength and monomer conversion of a commercial resin
composite material. Discs (10 x 1 mm) of Herculite XRV
(Kerr/Sybron, Orange, CA) were photocured at standardized
conditions. One group was left unheated, and another was
subjected to post-cure heating (Brilliant DI-500, Coltene AG,
Altstatten, Switzerland) at the following times after being light-
cured: 5 and 30 min, and 6, 24, 48, 72, 96, and 120 hrs. After the
appropriate delay time, unheated and heated specimens (n =
10) were tested for biaxial flexural strength at a constant
stressing rate. Recovered, fractured strength specimens (n = 10)
were analyzed for cure by means of IR spectroscopy. Post-cure
heating increased strength over that of the unheated specimens
only for the shortest delay times: 5 or 30 min. Thereafter,
strength values were statistically equivalent (p < 0.05). Delay in
heating did not significantly enhance strength of post-cure-
heated specimens, but delay in time did improve strength of
the unheated groups. The greatest monomer conversion was
obtained when post-cure heating was applied within 6 hrs
following light-curing. The difference in cure between
unheated and heated specimens remained significant up to 96
hrs of delay. Flexural strength of post-cure-heated specimens
remained unchanged with time delay for heating specimens.
Maximal monomer conversion of post-cured specimens is
obtained only within 6 hrs of light-curing. The potential for
additional conversion arising from post-cure heat treatment is
dependent upon the time following initial curing at which heat
is applied following initial light-curing. However, delay in heat
application has no influence on flexural strength.
Key words: post-cure, composite strength, composite cure.
Received February 11, 1997; Last Revision August 7,1997;
Accepted August 11, 1997
426
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Introduction
Post-curing is the exposure of a previously polymerized
resin composite restoration to elevated temperatures which
produces further activation of the polymerization reaction.
Several mechanisms have been proposed to explain the
further polymerization of the post-cure-heated composite.
Wu and Fanconi (1983) suggested that decay of free radicals
in the presence of oxygen and water might compromise the
ability to post-cure. They found that immediate post-curing
yielded a higher monomer conversion with fewer residual
carbon double-bonds than post-cure heating 25 min after
the initial light-cure treatment. Burtscher (1993) reported
free radical half-life in a commercial light-cured composite
to be greatly reduced by aging, by an increase in tempera-
ture, and by the amount of filler particles present.
Research has demonstrated physical property enhance-
ment as a result of composite post-curing. Bausch et al.
(1981), Wendt (1987), and Covey et al. (1992) reported im-
proved diametral tensile strength by heat treatment after
initial cure. Dionysopoulos and Watts (1989), Asmussen and
Peutzfeldt (1990), and Gregory et al. (1992) reported an in-
crease in flexural strength from post-cure heating. Ferracane
and Condon (1992) demonstrated an increase in fracture
toughness from post-cure treatment. These property
increases were attributed to the enhancement of monomer
conversion which accompanied the post-cure process.
Surprisingly, no decrease in material wear associated
with post-cure treatment has been noted when compared
with conventional light-cure composites (Wendt and
Leinfelder, 1992). De Gee et al. (1990) reported that wear of
unheated specimens improved in time (70 days) to a point
where it equaled that of post-cured-treated specimens. They
explained this result as a slow homogenization of polymeri-
zation shrinkage stress in conventionally cured specimens.
Thus, immediate increase in wear resistance of post-cure-
heated specimens could be attributed to heat annealing
more than to the effect of additional curing.
Assuming that free radicals decay with time after initial
photocuring (Wu and Fanconi, 1983; Burtscher, 1993), it
would be desirable to know the time constraints within
which post-cure heating must be performed to optimize
mechanical and physical properties. It seems reasonable
j Dent Res 77(2) 1998 Delay in Post-cure Heating 427

that, if post-cure properties are

related to enhanced cure values Controlled intensity
and there is a logarithmic decay light source Disk of composite
of free radicals, then the time to be cured
interval between initial light-
curing and application of heat Aluminum
may have significant influence
on post-cure properties. mold \ 7 Mylar
The purpose of this study
was to examine the influence of
time delay between initial light-
curing and subsequent post- Thin layer of -
cure heating on biaxial flexural optical oil
strength and monomer con- Myla r
version values of a commercial
resin composite restorative Cured composite disc for providing
material. constant reflective backing
Figure 1. Schematic diagram of resin composite disc fabrication.
Materials and methods
Disc-shaped specimens (10 mm x
1 mm thick) were made of a com-mercial resin composite
Determination of biaxial flexural strength
material (lot #503709, Herculite XRV, Shade A3, Kerr/Sybron, All specimens were made by the same operator to minimize
Orange, CA). Specimens were initially light-cured for 60 s on variability encountered by multiple operators. Following
each side in an aluminum sheet mold between two Mylar sheets appropriate delay, both cured composite specimens (unheated
(0.07 mm thick, Du Pont, Wilmington, DE) with a controlled and post-cured) were subjected to testing. Specimen thickness
light source (Optilux 401, Demetron Research Corp., Danbury, was measured (digital micrometer model #331-711-10,
CT) with a 13-mm-diameter straight light guide (item #20474, Mitutoyo, Paramas, NJ) and entered into the computer
Demetron Research Corp.) emitting 500 mW/cm2 as measured controlling the universal testing machine (model 8562, Instron
by means of a hand-held dental radiometer (model 100, Corporation, Canton, MA). The specimen was placed in a
Demetron Research Corp.). specially designed loading device which supported it on three
When specimens were fabricated, care was taken to ensure a equally spaced balls (ASTM, 1978; Fairhurst et al., 1992). The
reproducible light-curing environment. Composite was placed upper member of the universal testing machine was lowered,
in the mold in one increment and pressed with standardized subjecting the specimen to biaxial loading at a constant
pressure (200 pounds) (Carver laboratory press, model C, Fred stressing rate of 10 MPa/s until failure.
S. Carver, Inc., Menomonee Falls, WI). The assembly was then
placed on a 6-mm-thick disc of cured composite of similar Determination of monomer conversion
shade and lot number. Between the outer, lower Mylar face and A remnant of fractured strength specimen was recovered and
the top of the thick underlying composite, a thin layer of optical pulverized in a stainless steel percussion mortar (cat. #12-990,
oil was placed (Type B, R.P. Cargille Laboratories, Cedar Grove, Fisher Scientific, Norcross, GA). A small amount of the powder
NJ). This oil eliminated an air interface between the Mylar and (0.01 g) was mixed with 0.10 g of potassium bromide (cat.
the underlying thick layer of cured composite. In this manner, #P227-25, Fisher Scientific), and a pellet was made by means of
the curing composite disc would "see" a consistent backing of a hand press (Model MKD-S13, Harrick Scientific Corp.,
material similar in optical nature to itself. Thus, this method Ossining, NY). The pressed specimen was placed in a micro-
simulated curing the disc as if it were one tall cylinder of transmission holder (Model TSH-OLG, Harrick Scientific Corp.)
composite, with the exception that the top 1 mm could be of a beam-condensing unit (Model 4XF-CLO, Harrick Scientific
removed easily for testing. Fig. 1 presents the curing apparatus Corp.). The infrared spectrum of the specimen was obtained
schematically. with a Fourier transform infrared spectrometer (FTIR) (FTS-40,
Two types of specimens were made. One specimen was used Digilab, Cambridge, MA), with 16 scans at a resolution of 2 cm-1.
as a light-cured-only control (unheated), and the other was The spectrum of the uncured resin was obtained by means of a
subjected to post-cure heat treatment for 7 min at 100"C (DI-500 transmission technique of paste between ZnSe windows.
oven, Coltene/Whaledent, Switzerland). The specimens were To determine monomer conversion stability after post-cure
coded and stored at room temperature in a light-tight container heat treatment, we made five additional specimens. All
until the appropriate time elapsed. The time intervals between specimens were post-cure-heated at a five-minute delay and
initial light cure and post-cure treatment were 5 and 30 min, tested for monomer conversion 72 hrs after the post-cure
and 6, 24, 48, 72, 96, and 120 hrs. Ten test specimens and ten heating. The testing protocol was identical to that described
control specimens were made for each time interval, resulting in above.
160 specimens: 10 replications x 2 type specimens per condition Spectral absorption peak heights were analyzed (Spectra
x 8 post-cure time delays. Calc, version 2.23, Galactic Industries Corp., Salem, NH), and
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428 Loza-Herrero et al. J Dent Res 77(2) 1998
It was assumed that monomer
A aI- II l- A -- I
250 -0- I'UPI-GUMH HFAItU conversion and strength of speci-
mens not exposed to post-cure
0*11%FG FG F FG F G FG FG heating would increase with time
co from the initial light-curing. The
amount of time that passed after
200 initial light-curing when mono-
mer conversion (or strength) of
unheated specimens equaled or
exceeded (mean 2 control) the
value obtained immediately fol-
IL 150 lowing light-curing (five-minute-
delay value) was tested by a one-
tailed Dunnett's t test. This test
CD was performed to determine at
which delay after initial light-
100
I--a- UNHEATED CONTROLI curing the strength (or monomer
conversion) value of specimens
CD receiving no post-cure heat
treatment becomes significantly
A* AB AB C CDE CDE CD E greater than that of the specimen
50- , . . . . group tested 5 min after light-
Cl D curing (used as control value).
E co co
Thus, this test used the unheated
LO) 0
L To five-minute-delay group as the
control and compared it with
unheated specimens of each time
delay.
DELAY TIME IN POST-CURING It was also assumed that the
Figure 2. Influence of delay in heat application and post-cure treatment on biaxial flexural strength. potential for additional cure as a
Vertical bar = ± 1 standard deviation. N = 10 specimens per test group. *Similar letters indicate result of post-cure heating de-
statistically equivalent groupings by ANOVA and Fisher's PLSD test. Horizontal axis is not a linear clines with time after initial light-
scale. curing. We performed a one-
tailed Dunnett's t test to deter-
the data were recorded in spread-sheet format (Microsoft Excel, mine when cure values (or strength values) of post-cured
v5.0a, Microsoft Corporation, Redmond, WA). Using calibration specimens become significantly lower than those when post-
graphs relating absorption ratio to molar ratio of aliphatic and cure heating was performed with the shortest time delay (5
aromatic carbon double-bonds, we determined the monomer min). Therefore, this test used the shortest time delay that post-
conversion of each treated specimen using methods previously cure heating was applied (5 min) and statistically compared the
described (Ruyter and Svendsen, 1978; Ferracane and Greener, values of post-cure-treated specimens at the subsequent delay
1984; Rueggeberg et al., 1990). These methods determine the times (mean < control).
amount of C=C available prior to curing and then calculate the A two-tailed Dunnett's t test was used to determine when
amount remaining after the curing process. monomer conversion (or strength) of the unheated sample
equaled or exceeded that of the post-cure-heated sample. It was
Statistical analysis expected that the latter group would have maximal properties
Two, two-way ANOVAs were performed to test the presence of because it was heated the soonest after initial light-curing (five-
significant difference (p < 0.05) on the dependent variables minute-delay group). This test used the cure (or strength) value
(flexural strength or monomer conversion) with respect to delay observed for the five-minute post-cure-heated specimen and
in post-curing time, the use of post-cure heating (control or compared it with values obtained for the unheated specimens at
post-cure-heated), as well the interaction between the each time delay interval (mean < control 2 mean).
independent variables. We performed two-tailed Student's t tests to determine at
When examining either the unheated or post-cured what given time delay, after initial light-curing, the value of
specimens individually, we performed two, one-way ANOVAs, monomer conversion (or strength) for the post-cure-heated
followed by Fisher's Protected LSD test, to compare between specimen exceeded that of the corresponding unheated
mean parameter values for significant difference (p < 0.05). The specimen. This test was used to compare the differences in
independent variable was heating delay time (8 levels), and the strength and monomer conversion between unheated and post-
dependent variable was strength or monomer conversion. This cured specimens at each time delay. The relationship between
test was used to observe the effect of time-delay on each type of post-cure delay time and monomer conversion (or strength) for
treatment (unheated or post-cured), and also separated the data either unheated or for post-cure-heated specimens was obtained
into equivalent groups. by linear regression.
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j Dent Res 77(2) 1998 Delay in Post-cure Heating 429

We performed a two-tailed 75-

-IV r-

Student's t test to determine the

stability of monomer conversion of
post-cure-heated specimens over
time. This test compared monomer
conversion values of specimens post-
cure-heated at a five-minute delay
and tested either immediately or 72
hrs later.
Results
Biaxial flexural strength
The relationship between biaxial z 0
flexural strength and time delay of
post-cured heating is expressed in
Fig. 2. The two-way ANOVA indi- 1f--n.- UNHEATED CONTROLf
cated that the main independent A*
variables (delay time, p = 0.0001,
and type of treatment, p = 0.0002)
each had a significant impact upon
strength values, as did the inter-
action of these parameters (p =
0.0007). Unheated control speci-
mens appear to gain strength with
increasing time. This trend was
AXL%-. %_"OIAL e A.LL%.,. A ALIO LA I-XL VV UO
confirmed by linear regression Figure 3. Influence of delay in heat application and post-cure treatment on monomer conversion.
(slope = 0.451, p = 0.0001, R2 = Vertical bar = ± 1 standard deviation. N - 10 specimens per test group. *Similar letters indicate
0.331). With unheated specimen statistically equivalent groupings by ANOVA and Fisher's PLSD test. Horizontal axis is not a
strength at the five-minute time as linear scale.
the control, the strength of un-
heated specimens significantly increaised above this value
after 6 hrs. There appeared to be no such correlation
between strength and delay time fFor post-cure-heated
specimens. This observation was confirmed by linear
regression (slope = 0.074, p = 0.2867, R2 = 0.015). With the
five-minute-delay post-cure-heated strength value as the
control, there was no significant dif:ference between this p = 0.0001, R2 = 0.397). When the cure value of the post-cure-
value and any other post-cured stren1 gth value of the other
times. With this group as the control1 once again, but this
time compared with values of unheaited specimens at the
various time delays, we found that,,at 6 hrs from initial
light-curing, the unheated specimerns had demonstrated
strength equivalent to that of the ezarliest time in which
specimens were subjected to post-ct ire heating. The only
time intervals demonstrating greater s trength values for the
post-cured specimens compared with the unheated control
group were the five- and 30-minute de!lays.
Monomer conversion
Fig. 3 indicates change in monomer c-onversion when time
delay between initial light-curing anid subjection to post-
cure heating was varied. The two-wEay ANOVA indicated
that both independent variables (delayy time, p = 0.0002, and
type of treatment, p = 0.0001) had a significant impact upon
observed cure values, as well as on their interaction (p =
0.0001). Cure values of unheated speccimens increased with
time after initial curing. Linear regri ession confirmed this
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Z E E E G F FG FG G
0
7-- . POST-CURE HEATED
w
z
o 65-
w
60
0s
AB AB AB BC D AB CD
500
DELAY TIME IN POST-CURING
trend (slope = 0.021, p = 0.0006, R2 = 0.139). With the cure of
the unheated five-minute-delay group as the control, only
the cure values of the unheated specimens at 72- and 120-
hour delay provided higher values. Monomer conversion of
heated specimens also declined with delay in heat applica-
tion. Regression analysis confirmed this trend (slope = -0.43,
heated five-minute-delay group was used as the control,
only post-cured specimens from 30-minute and six-hour
delay times yielded equivalent values. Specimens in which
heating was delayed for longer than 6 hrs had conversion
values lower than that of the five-minute control group. The
cure of unheated specimens was always significantly lower
than that of the post-cure-heated five-minute-delay group.
In the comparison of cure values between unheated speci-
mens and their post-cure-heated equivalents at similar time-
delay intervals, the conversion of heated specimens was al-
ways greater than that of the unheated group, except for the
120-hour-delay group, which was equivalent (p = 0.6840).
Student's t test was used for the comparison of con-
version values of the five-minute-delay post-cure-heated
specimens tested immediately against the cure values of
five-minute-delay post-cure-heated specimens tested 72 hrs
after being heated. The conversion values were equivalent
(p = 0.7209). Thus, once post-cure heating had taken place,
no further increase in conversion was seen over time.
Correlations of specific conversion values were made
with their respective flexural strength values (Fig. 4), where
430 Loza-Herrero et al. j Dent Res 77(2) 1998
2U0
A-k Al% A%
conversion, and thus maximal
Non-Heated - Post-cure Heated strength. Interestingly, strength
co Specimens Specimens of post-cure-heated specimens
120HCG did not change with delay in
* 72HP
heat application. Thus,
w
180 24HP strength enhancement during
the shorter time delays for the
*48HC ,*l' IA 20HP INO 0 30MP post-cure-heated specimens
z *10 @ *96HP %%%* 5MP
may be the result of increase in
160 96HC M 24HC 72HC * 48HP #* monomer conversion arising

I
-J ,," e 6HP
from post-cure heating. This
hypothesis was validated by
information presented in Fig. 3.
LU
x This Fig. shows that the
-J
m 140- QD
greatest difference in cure
@6HC values, when unheated and
w
-j post-cure-heated specimens
* 30MC were compared at equivalent
120 delay times, was during inter-
* 5MC vals up to the 30-minute delay.
Conversion values for post-
y = -0.973x2 + 124.115x- 3779.159 r 2 = 0.579 cure-heated significantly
specimens were
greater than those
1 nn I I
for the unheated group at each
I

55 60 65 time delay, with the exception

of the 120-hour period, for
% MONOMER CONVERSION which the values were equi-
valent. It is important to note,
Figure 4. Relationship between the specific monomer conversion value and biaxial flexural strength of however, that the difference in
an identical specimen. Coding for data points: number and first letter = time delay (i.e., 5M = five- cure between unheated and
minute delay); second letter = specimen treatment; C = control, no heat application; P = post-cure- heated specimens decreased
heated.
with increasing time delay. This
result validated two previously
tracking of correlated data could be made. Specimens with hypothesized phenomena. First, it was reported that the
conversions less than 62% were associated with the amount of free radicals remaining after initial curing
unheated group, whereas conversion values greater than declined to a point that few, if any, were left after a period of
this value belonged to the post-cure-heated discs. The 5 days (120 hrs) (Burtscher, 1993). If post-cure heating used
relationship between the two variables seemed to be linear these remaining radicals to enhance polymer cure, then it is
at first, and then plateaued, or declined as the extent of expected that a decline in radical presence would also result
conversion increased. in a decrease in potential for further curing to be obtained as
a result of heat application. The experimental results
Discussion validated this assumption. Second, it is known that there is a
slow, continual increase in conversion of conventionally
It is important to recognize that the results observed in this light-cured resin composite after initial photo-activation
research are applicable only to the specific brand of resin (Johnston et al. 1985). Again, experimental results validated
composite tested. However, since post-cure heating affects these findings (Fig. 3). However, post-cure-heated
the remaining methacrylate groups, it is thought that the composite did not demonstrate this increase in monomer
observations made may be applicable to photocured conversion value over time (72 hrs). Thus, post-cure heating
composites in general. If assumptions are made with respect was found to have effectively increased monomer
to other composite materials, it is important to note that conversion even after 96 hrs following the initial light-
adequate photo-activation (at least 300 mW/cm2) would curing. However, the extent of increase declined with time
have to be applied to those materials, as was the case in the of heat application.
present research. Correlation between monomer conversion and specimen
This study indicated that post-cure heating of resin strength showed a distinction between unheated and post-
composites increased strength over that of unheated cure-heated specimens. However, for delay times greater
specimens in the first 30 min following initial photo- than 6 hrs for the unheated group, all strength values
polymerization. Six hrs after initial curing and thereafter, spanned a conversion range from 58% to 68%. Regression of
strength of unheated specimens rose to equal that of the the data by means of a second-order polynomial indicated
five-minute delay for post-cure heating-the time delay that there may be a parabolic relationship between cure and
which should provide the greatest opportunity for maximal biaxial tensile strength. Those specimens demonstrating
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J Dent Res 77(2) 1998
lowest cures (unheated specimens from the five- and 30-
minute- and six-hour-delay groups) also demonstrated the
lowest strength. However, as conversion increased, strength
values tended to plateau, or even to decline. This result
implied that once a threshold conversion value was reached,
polymer network strength did not markedly increase with
additional curing. In fact, strength may even decline, as a
result of increasing brittleness, where the effect of surface
flaws becomes a significant strength factor.
Strength enhancement cannot be totally attributed to an
increase in monomer conversion. This fact is evidenced by
data in Fig. 4. The conversion value for an unheated
specimen with a five-minute delay (56.9%) was found to be
statistically equivalent to that of the unheated 96-hour delay
(58.1%). Yet, biaxial strength of the unheated 96-hour-delay
specimen (161.4 MPa) was 36% greater than the strength
value of the unheated five-minute-delay group (118.5 MPa).
The additional factor affecting this strength increase may be
the slow homogenization of internal stresses. This stress is
initiated as a result of polymerization shrinkage. Post-cure
heating increases monomer conversion, but it also
immediately subjects the specimen to an annealing process
which can relieve internal stresses through increased
molecular segmental movement. This concept was
developed by De Gee et al. (1990) to explain why wear
resistance of unheated resin composite specimens gradually
increased and became similar to that of the post-cure-heated
specimens. Thus, at oral temperatures and upon subjection
of conventionally cured restorations to elevated
temperatures of hot foodstuffs, it is expected that a similar
annealing effect would be present, but would require a
much longer time to relieve polymerization stresses than
would immediate heating following light-curing.
The clinical significance of this research indicates that if
one merely waited long enough, strength of a resin
composite would eventually increase to a level where it was
comparable with that of the post-cure-heated product. Only
6 hrs were required for this equivalence to occur. Thus, post-
cure heating did not significantly affect biaxial flexural
strength, and time delay of heat application was not a
significant factor in strength. However, post-cure heating
significantly affected the ability to increase monomer
conversion, and the time after which heat was applied
subsequent to initial light-curing had an influential role. The
earlier heat was applied after initial light-curing, the higher
was the overall conversion value. The greatest level of
conversion was obtained when heat was applied within the
first 6 hrs following light-curing. After that time, the
increase in conversion from heating became significantly
lower than that of a short delay time. Optimization of
monomer conversion may significantly reduce the amount
of leachable components from a restoration, enhancing its
biocompatibilty. Therefore, to optimize the extent of resin
curing, post-cure heating should be applied within 6 hrs
after light-curing.
Acknowledgments
The Kerr/Sybron Corporation is thanked for its supply of
composite material. This research was supported by
Downloaded from jdr.sagepub.com at UNIV OF UTAH on October 15, 2014 For personal use only. No other uses without permission.
Delay in Post-cure Heating 431
NIH/NIDR grant DE 09418, the Medical College of Georgia
School of Graduate Studies, and the Department of Oral
Biology. Participation of the MCG Biocompatibility Program
is acknowledged. This paper is based on a thesis submitted
to the graduate faculty, Medical College of Georgia, in
partial fulfillment of the requirements for the MS degree.
References
Asmussen E, Peutzfeldt A (1990). Mechanical properties of heat
treated restorative resins for use in the inlay/onlay
technique. Scand J Dent Res 98:564-567.
ASTM Designation F394-78 (1978). American standard test
method for biaxial flexure strength (modulus of rupture) of
ceramic substrates. In: Annual book of ASTM standards.
Philadelphia, PA: American Society for Testing and
Materials (re-approved, 1984).
Bausch JR, de Lange C, Davidson CL (1981). The influence of
temperature on some physical properties of dental
composites. J Oral Rehabil 8:309-317.
Burtscher P (1993). Stability of radicals in cured composite
materials. Dent Mater 9:218-221.
Covey DA, Tahaney SR, Davenport JM (1992). Mechanical
properties of heat-treated composite resin restorative
materials. J Prosthet Dent 68:458-461.
De Gee AJ, Pallav P, Werner A, Davidson CL (1990). Annealing
as a mechanism of increasing wear resistance of
composites. Dent Mater 6:266-270.
Dionysopoulos P, Watts DC (1989). Dynamic mechanical
properties of an inlay composite. I Dent 17:140-144.
Fairhurst CW, Lockwood PE, Ringle RD, Thompson WO (1992).
The effect of glaze on porcelain strength. Dent Mater 8:203-
207.
Ferracane JL, Condon JR (1992). Post-cure heat treatments for
composites: properties and fractography. Dent Mater 8:290-
295.
Ferracane JL, Greener EH (1984). Fourier transform infrared
analysis of degree of polymerization in unfilled resins-
methods comparison. J Dent Res 63:1093-1095.
Gregory WA, Berry S, Duke E, Dennison JB (1992). Physical
properties and repair bond strength of direct and indirect
composite resins. J Prosthet Dent 68:406-411.
Johnston WM, Leung RL, Fan PL (1985). A mathematical model
for post-irradiation hardening of photoactivated composite
resins. Dent Mater 1:191-194.
Rueggeberg FA, Hashinger DT, Fairhurst CW (1990).
Calibration of FTIR conversion analysis of contemporary
dental resin composites. Dent Mater 6:241-249.
Ruyter IE, Svendsen SA (1978). Remaining methacrylate groups
in composite restorative materials. Acta Odontol Scand
36:75-82.
Wendt SL Jr (1987). The effect of heat used as a secondary cure
upon the physical properties of three composite resins. I.
Diametral tensile strength, compressive strength and
marginal dimensional stability. Quintessence Int 18:265-271.
Wendt SL Jr, Leinfelder KF (1992). Clinical evaluation of a heat-
treated resin composite inlay: 3-year results. Am J Dent
5:258-262.
Wu W, Fanconi BM (1983). Post-curing of dental restorative
resin polymer. Polymer Eng & Sci 23:704-707.
 COSMETIC & R E S T O R AT I V E C A R E ABSTRACT
Background. Polymerization shrinkage
is one of dental clinicians’ main
concerns when placing A D A
J
direct, posterior, resin-

An alternative
✷ ✷
based composite restora- 

N
tions. Evolving improve-

CON

IO
method to reduce ments associated with

T
T

A
N

I
C
resin-based composite A UING EDU 3
materials, dental adhesives,
R TICLE
polymerization filling techniques and light
curing have improved their predictability,

shrinkage in direct but shrinkage problems remain.

Methods. The authors propose restoring
enamel and dentin as two different sub-
posterior composite strates and describe new techniques for
placing direct, posterior, resin-based com-

restorations posite restorations. These techniques use

flowable and microhybrid resin-based com-
posites that are polymerized with a progres-
sive curing technique to restore dentin, as
SIMONE DELIPERI, D.D.S.; DAVID N. BARDWELL,
D.M.D., M.S. well as a microhybrid composite polymeri-
zed with a pulse-curing technique to restore
enamel. Combined with an oblique, succes-

A
malgam was the material of choice worldwide
for Class I and Class II restorations for more
than a century.1 Its high strength, good wear
resistance, technique insensitivity, low cost
and adaptability for restoring small, medium
and large lesions were responsible for this success.1-6 A
declining acceptance of amalgam among
To minimize clinicians and patients, however, began
in the early 1980s due to some inherent
the stress from
problems. For example, amalgam’s corro-
polymerization sion and difficulty bonding to tooth struc-
shrinkage, ture, along with the necessity to remove
efforts have sound tooth structure for retention, are
been directed problematic. Also at issue for some
7,8
sive cusp buildup method, these techniques
can minimize polymerization shrinkage
greatly.
Conclusions. Selection and appropriate
use of materials, better placement tech-
niques and control polymerization
shrinkage may result in more predictable
and esthetic Class II resin-based composite
restorations.
Clinical Implications. By using the
techniques discussed by the authors, clini-
cians can reduce enamel microcracks and
substantially improve the adaptation of
resin-based composite to deep dentin. As a
consequence, marginal discoloration, recur-

rent caries and postoperative sensitivity

toward people are its lack of esthetics and fears
about potential mercury toxicity.1,5-9 The
improving
need for amalgam alternatives has been
placement a topic in the dental literature for several
techniques, years.
material and Resin-based composites were advo-
composite cated as a possible solution to this
formulation, problem because they were mercury-free
and thermally nonconductive, and they
and curing
matched the shade of natural teeth and
methods. bonded to tooth structure readily with
the use of adhesive systems. Histori-
cally, dentists who used resin-based composites to
restore posterior teeth experienced poor wear resistance,
can be reduced, and longevity of these resto-
rations potentially can be improved.
difficulties in achieving good proximal
contact and contour, polymerization
shrinkage and poor dentin marginal
adaptation.10-14 To avoid these shortcom-
ings, indirect resin-based composite and
ceramic inlays were introduced,15
spurning intensive research on resin-
based composites.
In the past 10 years, a dramatic

JADA, Vol. 133, October 2002 1387

Copyright ©2002 American Dental Association. All rights reserved.
COSMETIC & RESTORATIVE CARE
improvement in newer-generation bonding agents
and resin-based composite formulations has
occurred. The improved performance of resin-
based composites and the increasing demand for
esthetics are encouraging more clinicians to
select resin-based composites for posterior resto-
rations.16-19 Although wear resistance of contem-
porary resin-based composites has improved sig-
nificantly19-22 and good proximal contact and
contour can be achieved,23-25 polymerization
shrinkage remains the biggest challenge in direct
resin-based composite restorations.26-29
METHODS AND MATERIALS
Polymerization shrinkage is responsible for the
formation of a gap between resin-based com-
posite and the cavity wall. This gap may vary
from 1.67 to 5.68 percent of the total volume of
the restoration,30 and it may be filled with oral
fluids. Oral fluids contain bacteria, which may be
responsible for postoperative sensitivity and
recurrent caries.31 When resin-based composites
are cured, they shrink, and a residual polymeri-
zation stress is generated, which may be
responsible for bonding failure. Stress from po-
lymerization shrinkage is influenced by restora-
tive technique, modulus of resin elasticity, po-
lymerization rate, and cavity configuration or
“C-factor.” The C-factor is the ratio between
bonded and unbonded surfaces32; an increase in
this ratio results in increased polymerization
stress. Three-dimensional cavity preparations
(Class I) have the highest (most unfavorable)
C-factor because only outer unbonded surfaces
absorb stress. To minimize the stress from po-
lymerization shrinkage, efforts have been
directed toward improving placement techniques,
material and composite formulation, and curing
methods.
Placement techniques and issues. The
incremental technique. This technique is based
on polymerizing with resin-based composite
layers less than 2-millimeters thick33,34 and can
help achieve good marginal quality, prevent dis-
tortion of the cavity wall (thus securing adhesion
to dentin) and ensure complete polymerization of
the resin-based composite. Following are vari-
ances related to differing stratifications:
dHorizontal technique.28,34,35 This technique is
an occlusogingival layering generally used for
small restorations; this technique increases the
C-factor.
dThree-site technique.36,37 This is a layering
1388 JADA, Vol. 133, October 2002
Copyright ©2002 American Dental Association. All rights reserved.
technique that is associated with the use of a
clear matrix and reflective wedges. It attempts to
guide the polymerization vectors toward the gin-
gival margin.
dOblique technique. In this technique, wedge-
shaped composite increments are placed to fur-
ther prevent distortion of cavity walls and reduce
the C-factor. This technique may be associated
with polymerization first through the cavity
walls and then from the occlusal surface to direct
vectors of polymerization toward the adhesive
surface (indirect polymerization technique).28,38
dSuccessive cusp buildup technique.39-41 In this
technique, the first composite increment is
applied to a single dentin surface without con-
tacting the opposing cavity walls, and the resto-
ration is built up by placing a series of wedge-
shaped composite increments to minimize the
C-factor in 3-D cavity preparations. Each cusp
then is built up separately.
Direct shrinkage. A chemically cured resin-
based composite is used on the gingival floor in
an attempt to direct the vectors of polymerization
toward the warmer cavity walls. This should help
to reduce the gap at the cervical margin.23,42,43
Bulk technique. The bulk technique is recom-
mended by some authors to reduce stress at the
cavosurface margins.34,44 Some manufacturers
recommend using this technique with packable
composites even though this is not supported by
a recent study.45 Rueggeberg and colleagues46
showed that the depth of cure does not exceed
more than 2 mm when curing resin-based com-
posites with modern light-curing units.
Resin-based composite materials. In the
past 20 years, resin-based composites have been
improved by reducing particle size, increasing
filler quantity, improving adhesion between filler
and organic matrix, and using low-molecular-
weight monomers to improve handling and po-
lymerization.8,47-51 By experimenting with particle
size, shape and volume, manufacturers have
introduced resin-based composites with differing
physical and handling properties (Table 1).
Microfill, hybrid, microhybrid, packable and flow-
able composites now are available to be used for
varying clinical situations (Table 2).
Microfills. Microfills are 35 to 50 percent filled
by volume and have an average particle size
ranging from 0.04 to 0.1 micrometer. They have
low modulus of elasticity and high polishability;
however, they exhibit low fracture toughness and
increased marginal breakdown.
 COSMETIC & RESTORATIVE CARE

TABLE 1

RESIN-BASED COMPOSITES CLASSIFICATION AND PHYSICAL

PROPERTIES.
COMPOSITE AVERAGE PARTICLE FILLER PERCENTAGE PHYSICAL PROPERTIES†
TYPE SIZE (MICROMETERS) (VOLUME %)*
Wear Fracture Polishability
Resistance Toughness

Microfill 0.04-0.1 35-50 E F E

Hybrid 1-3 70-77 F↔G‡ E G

Microhybrid 0.4-0.8 56-66 E E G

Packable 0.7-20 48-65 P↔G‡ P↔E‡ P

Flowable 0.04-1 44-54 P P F↔G‡

* Sources: Kugel,47 Wakefield and Kofford50 and Leinfelder and colleagues.53

† E: Excellent; G: good; F: fair; P: poor.
‡ Varying among the same type of resin-based composite.

Hybrids. Hybrids TABLE 2

are 70 to 77 percent
filled by volume and
an average particle
size ranging from 1 to
3 µm. They do not
maintain a high polish
but do have improved
physical properties
when compared with
CLINICAL INDICATIONS OF RESIN-BASED COMPOSITES.
COMPOSITE TYPE CLINICAL INDICATIONS
Microfill Enamel replacement in Class III, IV and V restorations
Minimal correction of tooth form and localized
discoloration
Hybrid Posterior resin-based composite restoration
Class V restoration
Dentin build-up in Class III and IV restoration

microfills. Microhybrid Posterior and anterior direct composite restoration

Microhybrids. Micro- Veneer
Correction of tooth form and discoloration
hybrids are 56 to 66
percent filled by Packable Posterior resin-based composite restoration

volume and have an Flowable Pit and fissure restoration

average particle size Liner in Class I, II and V restoration (dentin)

ranging from 0.4 to 0.8

µm. They have particle
sizes small enough to polish to a shine similar to the physical properties of packable composites are
microfills but large enough to be highly filled, not superior to conventional hybrids.52-54
thus achieving higher strength. The results are Flowables. Flowable composites are 44 to 54
resin-based composites with good physical percent filled by volume and have an average par-
properties, high polishability and improved wear ticle size ranging from 0.04 to 1 µm. Their
resistance. decreased viscosity is achieved by reducing the
Packables. Packable composites are 48 to 65 filler volume so they are less rigid, yet they are
percent filled by volume and have an average prone to more polymerization shrinkage and wear
particle size ranging from 0.7 to 20 µm. Their than conventional composites.47,55-57 Flowable com-
improved handling properties are obtained by posites have been said to improve marginal adap-
adding a higher percentage of irregular or porous tation of posterior composites by acting as an
filler, fibrous filler and resin matrix. They are elastic, stress-absorbing layer of subsequently
indicated for stress-bearing areas and allow easier applied resin-based composite increments.58-61
establishment of physiological contact points in Dentin-enamel adhesive systems. Since the
Class II restorations. Research has shown that introduction of the enamel-etching technique by

JADA, Vol. 133, October 2002 1389

Copyright ©2002 American Dental Association. All rights reserved.
COSMETIC & RESTORATIVE CARE
Buonocore62 in 1955, bonding to enamel has been
considered a reliable procedure. Bonding to
dentin, which was introduced more recently and
has improved over the years, has become com-
monplace; early dentin-enamel adhesive systems,
or DAS, bond strength to dentin ranged from 1 to
10 megapascals,63 while contemporary DAS can
achieve values of around 22 Mpa.64
Two procedures widely used in bonding to
tooth structure are the total-etch technique and
the self-etching technique (primers and adhe-
sives). The former is considered the gold
standard for bonding and is achieved by etching
enamel and dentin with 30 to 40 percent phos-
phoric acid. Bonding and mechanical retention
are ensured by the penetration of resin into the
microporosities of etched enamel and by the for-
mation of a hybrid layer and resin tags as a con-
sequence of resin penetration on demineralized
peritubular, intertubular and intratubular
dentin.65-72 Self-etching primers and adhesives are
a simplification of enamel-dentin bonding pro-
cedures with demineralization, priming and resin
concentrated into one material. This is an
attempt on the part of manufacturers to give den-
tists a DAS that is easy to manipulate, saves
time and is less technique-sensitive. In most
cases, long-term clinical evaluations are needed
for validation.70-76
Curing methods. In 1984, Davidson and col-
leagues30 stressed the importance of having com-
posite flow in the direction of the cavity walls to
allow for maximum internal adaptation during
the early setting phase of composite. Two studies
demonstrated that the relief of polymerization
stress through composite flow is reached with the
use of low-light energy; conversely, they recorded
higher polymerization shrinkage with higher
light energy.77,78 Miyazaki and colleagues77
demonstrated that composite exhibited improved
physical properties when cured at a low intensity
and with slow polymerization vs. higher intensity
and faster polymerization. Since then, studies
have reported improved marginal adaptation and
physical properties of resin-based composite
using this technique, aptly named “soft-start”
polymerization.79-90
Plasma arc, argon laser curing lights used to
polymerize resin-based composites decrease expo-
sure time and increase depth of cure when com-
pared with conventional curing lights.91
Increased resin brittleness and polymerization
shrinkage, poor physical properties and the
1390 JADA, Vol. 133, October 2002
Copyright ©2002 American Dental Association. All rights reserved.
degree of polymerization, however, make this
light source’s effectiveness questionable.92-95 Blue
light-emitting diode curing lights are being
studied and may present another option for
resin-based composite polymerization.96,97
DISCUSSION
Most composite placement techniques introduced
in the past 20 years were based on the concept
that resin-based composite shrinks toward the
light and employed this theory to attempt to
favorably direct the vectors of polymerization.
Versluis and colleagues98 demonstrated that the
direction of polymerization contraction is more
influenced by the quality of the adhesion and the
C-factor, than by the position of the light source.
Losche99 pointed out that the optimal results
obtained by using some of these placement tech-
niques (three-site and indirect polymerization)
are related to a reduction in light transmission
rather than the direction of the polymerization
vectors. The inability of reflective wedges to
ensure the polymerization of composites100 and
the difficulties in obtaining a good proximal con-
tact101 have contributed to clear wedges’ loss of
popularity. Furthermore, the introduction of new
light-curing methods has contributed to the
decline in use of the three-site technique. Simi-
larly, the results of the directed shrinkage tech-
nique are, at best, controversial.57,102-104
On the other hand, the successive cusp buildup
technique25,39-41 has not received a lot of attention
in the literature, but it is an interesting concept
that, when used appropriately, can minimize the
development of stress at the tooth-resin interface.
This technique is performed by strategically
placing successive layers of wedge-shaped com-
posite to decrease the C-factor ratio. Wedge-
shaped composite increments are 1- to 1.5-mm,
triangular apico-occlusal layers of uncured com-
posite that are condensed and sculpted directly in
the preparation using a composite instrument
(Figure 1 and Figure 2). Liebenberg 25,39,40 stressed
that the first layer must be very thin and applied
to a single dentinal surface without contacting
opposing cavity walls. The cavity is completely
filled with wedge-shaped composite increments,
and each cusp then is built up separately.
Development of new techniques. We use a
placement technique similar to that described by
Liebenberg39 but with some modifications. We
use a pulse-curing technique to polymerize com-
posite at the enamel cavosurface margins and a
 COSMETIC & RESTORATIVE CARE

progressive curing technique to polymerize com-

posite dentin increments; when also using the
selective composite technique, we select different
composite materials to restore dentin (flowables
and microhybrids) and enamel (microhybrids). We
found that the technique we use can help reduce
enamel microcracks and improve the adaptation
of the composite to deep dentin while achieving
high esthetics and function.
It is our goal to continue to improve the prog-
nosis of posterior resin-based composite restora-
tions in an era in which dentists are not afraid to
use resin-based composites in the posterior
regions. On the other hand, the ADA’s recommen-
dations18 for posterior resin-based composite res-
torations are being stretched in clinical practice
because patients may not be able to afford the
ideal indirect restoration in situations involving Figure 1. Schematic representation of wedge-shaped com-
posite increments (1-6) used to build up the enamel prox-
large posterior restorations.25 imal surface. F: Facial aspect. L: Lingual aspect.
Pulse curing to reduce enamel microcracks. It is
universally accepted that the marginal seal gen-
erally can be preserved around enamel cavosur-
face margins with contemporary adhesive sys-
tems.68,70,105 It is difficult to ensure perfect
marginal adaptation either at gingival or occlusal
enamel cavosurface margins. Enamel is a highly
mineralized tissue and has a modulus of elasticity
higher than that of dentin, resulting in a lower
flexibility and decreased ability in relief of
shrinkage stress. When bonding composites to
enamel, two unfavorable events may happen:
poor marginal adaptation and seal occur due to
incorrect application of bonding adhesive, and the
bonding interface remains intact but microcracks
develop just outside the cavosurface margins due
to the stress of polymerization shrinkage.82-84,106-11
This latter phenomenon is particularly common
in high–C-factor restorations (unfavorable ratio
of bonded and unbonded surfaces in the restora-
Figure 2. Schematic representation of the flowable com-
tion)32 and may be increased by use of high- posite increment (1) and wedge-shaped increments (2-7)
modulus composites as they may transmit more used to build up dentin; two increments (8 and 9) are
used to build up enamel using the successive cusp
polymerization shrinkage forces to the tooth. buildup technique. F: Facial aspect. L: Lingual aspect.
Microcracks represent a way for microleakage to
occur, and the use of a composite sealer may
delay this phenomenon only partly. cally. The pulse technique initially uses low-
To reduce microcracks, clinicians can control intensity curing for a short period to provide
the rate of polymerization, alter placement tech- sufficient network formation on the top composite
nique and choose composite that have the appro- surface while delaying the gel point in the
priate modulus of elasticity. The reduction of the depth underneath until final high-intensity
C-factor throughout the application of a microhy- polymerization is started. It then uses a conven-
brid composite to a single-bonded surface and the tional mode for the building of dentinal composite
pulse polymerization of each enamel composite increments with a specific energy density for each
increment may help reduce microcracks drasti- composite.82-84

JADA, Vol. 133, October 2002 1391

Copyright ©2002 American Dental Association. All rights reserved.
COSMETIC & RESTORATIVE CARE
TABLE 3
RECOMMENDED PHOTOCURING INTENSITIES AND TIMES FOR ENAMEL
AND DENTIN BUILDUP.
BUILDUP COMPOSITE SHADE
LOCATION (PRODUCT NAME)*
Proximal Enamel Pearl Smoke Pearl
Neutral/Pearl Frost
(Vitalescence)
Dentin A2 (flowable,
PermaFlo) A3.5-A3-
A2-A1 (Vitalescence)
Occlusal Enamel Pearl Smoke/Pearl
Neutral/Pearl Frost
Trans Smoke/Trans
Mist/Trans Frost
(Vitalescence)
* Vitalescence and PermaFlo are manufactured by Ultradent Products Inc., South Jordan, Utah.
† mW/cm2: Milliwatts per square centimeter.
‡ Intensity at first polymerization (intensity after waiting period).
§ Photocuring time at first polymerization (time after waiting period).
A classical soft-start polymerization also may
be used, but the advantages of this alternate
curing mode have not been thoroughly investi-
gated. Mehl and colleagues80 and Ernst and col-
leagues88 found that the variable curing method
can improve marginal integrity with different
composites when cured with a soft-start polym-
erization, while Friedl and colleagues112 and
Bouschlicher and colleagues113 did not find any
improvement using the same soft-start polymeri-
zation method. This result may be explained by
the varied amount and concentration of photoini-
tiators. Certain resin-based composites may
require shorter exposure time to get the same
degree of conversion while maintaining the same
intensity. As a matter of fact, the gel point is
anticipated even with a soft-start polymerization.
Yoshikawa and colleagues110 recently demon-
strated composite improved marginal adaptation
using a soft-start polymerization; however,
enamel microcracks still were present and
unaffected.
The pulse polymerization technique is based on
the same principle as soft-start polymerization,
but it is applied with a different modality, which
may be less technique-sensitive to composites’
chemical variation.114 Pulse polymerization should
be used not only in the enamel occlusal cavosur-
face margins, but also at the cervical enamel
margin to reduce microcracks at this critical area.
To correctly apply this pulse-curing technique,
clinicians should use a light-curing unit with pro-
1392 JADA, Vol. 133, October 2002
Copyright ©2002 American Dental Association. All rights reserved.
POLYMERIZATION INTENSITY TIME (SECONDS)§
TECHNIQUE (MW/CM2†)‡
Pulse 200 (300) 3 (40)
Progressive (300) (40)
curing
Pulse 200 (600) 3 (10 [occlusal],
10 [facial], 10
[palatal])
grammable time and intensity (VIP Light, Bisco
Inc., Schaumburg, Ill.; Spectrum 800,
Dentsply/Caulk, Milford, Del.).
Enamel buildup: proximal surface. In Class II
restorations, the enamel proximal surface is built
up first through the application of different
wedge-shaped composite increments using an
oblique layering technique while being careful to
avoid having a single composite increment be in
contact with opposing cavity walls. Each com-
posite increment is pulse-cured with a low-
intensity light for a short duration (depending on
the type of composite and depth of the prepara-
tion) followed by a waiting time of three minutes
to allow for strain relief. During this three-minute
waiting time, a thin layer of flowable composite is
applied to a single surface in the dentin pulp floor
and axial wall of the preparation to reduce the
C-factor and help avoid cusp deflection due to
stress from polymerization (Figure 2). At this
point, the resin-based composite restoration’s
proximal surface and the flowable composite are
cured together at once at a higher intensity using
a progressive curing technique (Table 3). Final
polymerization of the composite restoration’s
proximal surface and the flowable composite is
completed at higher intensity (Table 3). If more
than one tooth is to be restored at one appoint-
ment, another restoration can be started during
the three-minute waiting time following the pro-
cedure described previously.
Progressive curing technique. To completely fill

the dentin, wedge-shaped composite increments
are placed using the stratified layering technique
in which a higher chroma is placed in the middle
of the preparation and a lower chroma is placed
close to the cuspal walls41,115 (Figure 2). Each com-
posite dentin increment is cured using a progres-
sive curing technique (40 seconds at 300 milli-
watts per square centimeter instead of a
conventional continuous irradiation mode of 20
seconds at 600 mW/cm2) (Table 3). Lower light
intensity and longer curing time have resulted in
an improvement in marginal adaptation while
maintaining the excellent physical properties of
the composite.77,78
Enamel buildup: occlusal surface. The restora-
tion is completed when the final composite incre-
ments are layered onto the enamel cavosurface
margins. Each cusp is built up separately without
contacting the opposing ones and is pulse-cured
separately (three seconds at 200 mW/cm2). Sec-
ondary anatomy is created before a final
polymerization at a higher intensity is applied (30
seconds at 600 mW/cm2) (Table 3). This technique
allows the dentist to create anatomically correct
morphology by using the outlying cavosurface
margins as a guide for composite sculpturing.
Occlusion adjustment usually is minimal or not
necessary, which saves the dentist time and pre-
serves the wear of posterior composites.116,117
Selective composite technique. A goal of the
selective composite technique is to use different
combinations of composite materials to restore
enamel and dentin. Enamel is a highly mineral-
ized tissue and contains 92 percent inorganic
hydroxyapatite by volume. Dentin is only 45 per-
cent inorganic and is arranged in an organic
matrix that consists primarily of collagen. It is
crossed by dentinal tubules running from the
dentinoenamel junction to the pulp. Variations in
tubule size, as well as direction and number of
tubules, are responsible for regional variations in
dentin structure. Bonding resin-based composite
to the dentinal surfaces is considerably more com-
plex and less reliable than bonding resin-based
composite to acid-etched enamel.118,119 It also has
been demonstrated that when bonding to deep
dentin, a decrease in bond strength may occur.120-124
This may explain the adhesive failure at the
dentin-composite restoration interface even
though high-bond strength and tight composite to
acid-etched enamel seal are achieved. As a conse-
quence, composite can be deformed under occlusal
load and thermal stress.125
Copyright ©2002 American Dental Association. All rights reserved.
COSMETIC & RESTORATIVE CARE
Since enamel and dentin are different sub-
strates, they should be restored with different
resin-based composite materials. Cervical and
occlusal enamel are restored using a microhybrid
resin-based composite that has a wear pattern
and modulus of elasticity closer to that of enamel
than other resin-based composites. Dentin has a
modulus of elasticity lower than enamel and the
use of an intermediate elastic layer may be indi-
cated.126-128 The combination of a filled adhesive
and a flowable composite may help create an elas-
ticity gradient between the dentin and the micro-
hybrid composite; thus, the flowable composite
may improve the effectiveness of the dentin
bonding agent in counteracting the polymeriza-
tion stress at the restoration-dentin interface.
Hannig and Friedrichs125 and Belli and
colleagues111 reported successfully using flowable
composite when it was placed in dentin exclu-
sively; however, its use for both enamel and
dentin has been questioned and has yielded
ambiguous results.57,90
The following case report provides a sequence
of clinical procedures we used when placing direct
Class II restoration following our technique.
CASE REPORT
An 18-year-old woman complained of increased
tooth sensitivity on her maxillary right first
molar (Figure 3). Clinical and radiographic analy-
ses revealed caries in the mesial surface
extending to the dentin. To restore the tooth, we
selected a microhybrid composite (Vitalescence,
Ultradent Products Inc., South Jordan, Utah)
that had a large variety of enamel shades that
mimic tooth structure. Different microhybrid com-
posites (Esthet-X, Dentsply/Caulk; Point 4, Kerr,
Orange, Calif.; Amelogen, Ultradent Products
Inc.) that are based on the natural layering tech-
nique129,130 also could have been used. All four of
these composite systems provide a variety of
shades that mimic dentin and enamel surfaces of
young, adult and geriatric patients.
After local anesthesia was achieved in the
patient, we placed a rubber dam. As the partially
erupted second molar would not ensure pre-
dictable stability, we positioned the dental dam
clamp on tooth no. 3. We removed the caries using
a no. 330 carbide bur (759, Ultradent Products
Inc.) and rounded sharp angles with a no. 4 bur
and a no. 6 bur (767 and 768, Ultradent Products
Inc., respectively). The cavity preparation was
completed when we placed a gingival butt joint
JADA, Vol. 133, October 2002 1393
COSMETIC & RESTORATIVE CARE
Figure 3. Preoperative occlusal view of tooth no. 3.
Figure 5. A matrix was placed to protect adjacent tooth
structure during cavity preparation and etching. Then
etching was performed using 35 percent phosphoric acid.
with no bevel on the axial or occlusal surface
using a 330 carbide bur (Figure 4). Adjacent tooth
structure was protected during preparation with a
matrix (InterGuard, Ultradent Products Inc.)
(Figure 5).
We disinfected the preparation using a 2 per-
cent chlorhexidine antibacterial solution (Con-
sepsis, Ultradent Products Inc.), acid-etched
enamel and dentin for 15 seconds with 35 percent
phosphoric acid (Ultra-Etch, Ultradent Products
Inc.), removed the etchant and water sprayed the
preparation for 30 seconds being careful to main-
tain a moist surface. We placed a fifth-generation,
40 percent filled ethanol-based adhesive system
(PQ1, Ultradent Products Inc.) in the preparation,
gently air-thinned it until the milky appearance
disappeared (Figure 6) and light-cured it for 20
seconds using a curing light.
We placed a sectional matrix (Composi-Tight,
Garrison Dental Solution, Spring Lake, Mich.), a
plastic wedge (Flexi Wedge, Garrison Dental Solu-
1394 JADA, Vol. 133, October 2002
Copyright ©2002 American Dental Association. All rights reserved.
Figure 4. Tooth no. 3 after a rubber dam was placed,
caries was removed and the cavity preparation was com-
pleted with a gingival butt joint and no bevel either on
the axial or occlusal surface.
tion) and a G-ring to reconstruct the mesial sur-
face (Figure 7). We burnished the matrix against
the adjacent tooth and built up the enamel
proximal surface using the Pearl Neutral, or PN,
enamel shade of the microhybrid composite in an
oblique fashion without contacting opposing cavity
walls (Figure 8). We pulse-cured each layer for
three seconds at 200 mW/cm2. We then removed
the sectional matrix, plastic wedge and G-ring;
placed a thin layer of the A2 shade of the flowable
composite (PermaFlo, Ultradent Products Inc.) in
the deepest portion of dentin, applying it to a
single surface (Figure 9); and light-cured flowable
and microhybrid composites for 40 seconds at 300
mW/cm2. We completely filled the dentin using a
combination of A3.5, A3 and A2 dentin shades of
the microhybrid composite throughout by
applying wedge-shaped composite increments
using the stratified layering technique (Figure 10)
and the progressive cure technique.
We completed the restoration by applying PN
microhybrid composite to the enamel cavosurface
margins. We built up each occlusal surface sepa-
rately without having it contact the opposite cusp
and pulse-cured them at 600 mW/cm2 separately
for three seconds (Figure 11, page 1396) before a
final polymerization at a higher intensity (30 sec-
onds at 600 mW/cm2). We removed the dental
dam, checked the occlusion and polished the
restoration using the Finale (Ultradent Products
Inc.) polishing system. We etched the restoration’s
cavosurface margins with 35 percent phosphoric
acid and sealed them with a composite sealer
(PermaSeal, Ultradent Products Inc.) (Figure 12,
page 1396).
 COSMETIC & RESTORATIVE CARE

Figure 6. Enamel’s and dentin’s glossy appearances after Figure 7. A sectional matrix, plastic wedge and G-ring
application of a fifth-generation, 40 percent filled placed to reconstruct the proximal surface.
ethanol-based adhesive system.

Figure 8. Tooth no. 3 after the enamel proximal surface
was built up using the Pearl Neutral enamel shade of the
microhybrid composite (Vitalescence, Ultradent Products
Inc., South Jordan, Utah).
Figure 9. Tooth no. 3 after the sectional matrix, plastic
wedge and G-ring were removed and the A2 shade of the
flowable composite (PermaFlo, Ultradent Products Inc.,
South Jordan, Utah) was applied to a single dentin
surface.

A B
Figure 10. A and B. Tooth no. 3 after wedge-shaped composite increments of A3.5, A3 and A2 shades of the microhy-
brid composite (PermaFlo, Ultradent Products Inc., South Jordan, Utah) were used to reconstruct dentin.

JADA, Vol. 133, October 2002 1395

Copyright ©2002 American Dental Association. All rights reserved.
COSMETIC & RESTORATIVE CARE
Figure 11. Tooth no. 3 after Pearl Neutral enamel shade
of the microhybrid composite (Vitalescence, Ultradent
Products Inc., South Jordan, Utah) was used to build up
the occlusal surface according to the successive cusp
buildup technique.
CONCLUSION
Research is under way to develop resin-based
composite materials with novel monomers, new
photoinitiators and improved particle systems to
reduce polymerization stresses. In this article, we
outlined principles for the judicious selection and
use of modern dental materials, careful control of
polymerization shrinkage, and effective place-
ment techniques that can be used to create more
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 d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 1542–1548

available at www.sciencedirect.com

journal homepage: www.intl.elsevierhealth.com/journals/dema

Dentin regional bond strength of self-etch and

total-etch adhesive systems

Jatyr P. Proença a , Mário Polido b , Estrella Osorio a , Maria Carolina G. Erhardt a ,

Fátima S. Aguilera a , Franklin Garcı́a-Godoy c , Raquel Osorio a , Manuel Toledano a,∗
a Department of Dental Materials, School of Dentistry, University of Granada, Campus Cartuja s\n, 18071 Granada, Spain
b Department of Dental Materials, Instituto Superior de Ciências da Saúde-Sul, Monte da Caparica, Portugal
c Clinical Research Center, College of Dental Medicine, Nova Southeastern University, Fort Lauderdale, FL, USA

a r t i c l e i n f o a b s t r a c t

Article history: Objectives. To evaluate the microtensile bond strength (MTBS) of self-etch (with or without
Received 21 March 2006 H3 PO4 -etching) and total-etch bonding systems bonded to different regions of dentin.
Received in revised form Methods. Long flat dentin cavity preparations extending from top-crown to root-apex within
11 January 2007 the same tooth were performed and bonded: using two-step (Clearfil SE Bond/SEB, Resul-
Accepted 6 February 2007 cin Aqua Prime/RES) and one-step (Etch & Prime 3.0/EP, One-Up Bond F/OUB, Prompt
L-Pop/PLP, Solist/SOL and Futurabond/FUT) self-etch adhesives; these same adhesives were
also applied following H3 PO4 -etching of dentin and finally two more groups were bonded
Keywords: with total-etch adhesives (Single Bond/SB and Prime & Bond NT/PBNT). Build-ups of resin
Self-etch composite were constructed incrementally to ensure sufficient bulk for the MTBS test and
Total-etch the different regions of dentin were identified by painting with different colours on the top
Bond strength of the resin composite. Specimens were sliced into beams and tested in tension. ANOVA
Dentin regions and multiple comparisons tests were used (p < 0.05).
Adhesion Results. Regardless of the tested dentin region, SEB attained the highest MTBS to smear layer-
covered surfaces (i.e., coronal dentin: 42.7 MPa), while H3 PO4 -etching of dentin hampered
bonds (i.e., coronal dentin: 27.7 MPa). When bonding with PBNT, SB, RES, EP, PLP, SOL and
FUT, MTBS was similar for different dentin regions. H3 PO4 -etching of dentin did not alter
the attained MTBS.
Significance. SEB yielded the highest MTBS to all regions of dentin. When bonding to parallel-
cut dentin, previous H3 PO4 -etching of dentin did not increase MTBS and differences in bond
strength among dentin regions were absent.
© 2007 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

1. Introduction Efficacy of current adhesive systems is regularly evaluated by

Bonding to dentin has been referred to be a less reliable
and predictable technique when compared to enamel bond-
ing [1,2]. Dentin is a hydrated complex composite material
composed of a collagen-based organic matrix with hydrox-
yapatite reinforcement, varying with anatomical location [3].
their ability to bond to coronal dentin, nevertheless, develop-
ments in periodontology significantly increased the demand
for restoration of root dentin defects [4]. In these clini-
cally relevant substrates, the structural anisotropy found due
to physiological and pathological alterations imply that the
nature of the dentin substrate presented for bonding also vary,

Corresponding author. Tel.: +34 958243788; fax: +34 958240908.

∗

E-mail address: toledano@ugr.es (M. Toledano).

0109-5641/$ – see front matter © 2007 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.dental.2007.02.001
 d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 1542–1548
and discrepancies in bond strengths might be encountered
[3].
A number of new adhesive systems have been developed in
an attempt to obtain a reliable bonding to dentin. Two differ-
ent approaches are the most frequently used. The total-etch
technique relies on the removal of the smear layer and expo-
sure of the collagen matrix by acid etching [5], followed by the
application of a self-priming agent that combines the primer
and the adhesive resin into one solution [6]. Further incom-
plete expansion of collagen may impair resin infiltration and
compromise bonding with these systems [7,8]. The second
approach is the use of self-etching primers, in which the acid
and the primer are combined in one solution to form an acidic
monomer [9] and a final bonding step is later applied. Current
trends in adhesive technology are directed towards the one-
step self-etch systems, which have the bonding mechanism
based upon the simultaneous etching, priming and bonding
to the smear-covered dental tissue using one single solution
[10,11]. Reducing the steps of the adhesive procedure shortens
the application time, and leads to a lower technique sensitivity
[12]. When using all these self-etching systems less discrep-
ancy is expected between the depth of demineralisation and
depth of resin infiltration [9,13]. However, the benefit of sav-
ing time may be achieved at the expense of compromising
the quality of resin–dentin bonds [2,14,15], as these adhesives
contain highly hydrophilic and acid monomers that make
hybrid layers more permeable and sensitive to water sorption
from the underlying dentin [16,17]. The self-etching adhesives
vary in their acidity by virtue of the composition and con-
centration of polymerizable acids and acidic resin monomers
[18,19].
Previous studies suggested that bonding of self-etching
adhesive systems to cervical and root dentin may be improved
by modifications to protocols that are normally employed to
coronal dentin [20,21,22], which include the removal of surface
hypermineralized layer by pre-treatment with stronger acids
the mineralized components of the smear layer that are effi-
cient buffers, making the pH of acidic monomers too high to
demineralize the underlying dentin [23]. Although self-etching
adhesives etch and prime the dentin surface simultaneously,
previous etching should be considered as it produces a wet-
table surface due to the removal of the smear layer [1,2],
helping for the infiltration of the resin monomers through the
demineralized interfibrillar spaces [18,20].
The aim of this study was to determine the microtensile
bond strength of two- and one-step self-etch bonding agents
– previously treated or not with 36% phosphoric acid – com-
pared to total-etch systems, when bonded to different dentin
regions (coronal, cervical and root dentin). The null hypothe-
sis to be tested was that there was no significant difference in
bond strengths of the different adhesive approaches (with or
without prior application of phosphoric acid when using self-
etching systems) and systems (self-etching versus total-etch
adhesives) when applied to coronal, cervical or root dentin.
2. Materials and methods
Ninety-six caries-free extracted human third molars stored at
4 ◦ C in 0.5% chloramine T for up to 1 month following extrac-
1543
tion were selected. Outer enamel and dentin were removed
from both the mesial and distal tooth surfaces by means of
180-grit silicon carbide papers. A long flat cut was performed
into middle dentin extending from the occlusal-crown to the
apex of the root within the same tooth [4], exposing three
different dentin regions: cuspal or coronal, cervical (near the
dentin–enamel junction) and root region, that was approxi-
mately 3 mm below the dentin–enamel junction.
Composition, manufacturers, and application protocol of
the tested adhesives are displayed in Table 1. The total-etch
bonding agents were applied according to manufacturers’
directions. The self-etch systems were applied following man-
ufacturers’ instructions or after previous 36% H3 PO4 -etching
(Dentsply/DeTrey, Konstanz, Germany—lot # 041210) of dentin.
Dentin was etched for 15 s and rinsed for 10 s. The pH of the
bonding agents was assessed using pH indicator strips (Merck
KgaA, Darmstadt, Germany).
Resin build-ups, each 6 mm in height, were constructed
incrementally (2 mm) with Tetric Ceram (Ivoclar Vivadent,
Schäan, Liechtenstein—lot # H09718) light-cured hybrid com-
posite resin. Each layer of the composite was separately
light-activated for 40 s with a Translux EC halogen light-curing
unit (Kerr Demetron, Danbury, CT, USA). Light intensity output
was monitored with a Curing Radiometer (Danville Engineer-
ing Co., Danville, CA, USA) to be at least 600 mW/cm2 . The
different regions of dentin were identified (coronal, cervical
and root thirds) and painted with different colours on the top
of the composite.
After storage in distilled water at 37 ◦ C for 24 h, teeth were
longitudinally sectioned in a buccal-lingual direction from its
central part, yielding two halves, each one containing the
resin-bonded dentin surfaces. Specimens were then vertically
sectioned into serial slabs, and further into beams with cross-
sectional areas of 1 mm2 , following the method described by
Shono et al. [21]. Six molars were performed per group, and
each molar gathered 3–4 beams from each dentin region, hav-
ing been obtained 20–24 beams per group and dentin region.
All beams were attached to a modified Bencor Multi-T
testing apparatus (Instron Inc., Canton, MA, USA) with a
cyanoacrylate adhesive (Zapit/Dental Ventures of America
Inc., Corona, CA, USA) and stressed to failure in tension using
a universal testing machine (Instron Inc., Canton, MA, USA) at
a crosshead speed of 0.5 mm/min. The fractured beams were
carefully removed from the apparatus and the cross-sectional
area at the site of failure was measured to the nearest 0.01 mm
with a pair of digital calipers (Sylvae Ultra-Call/Fowler Inc.,
Newton, MA, USA). Fractured specimens were examined with
a stereomicroscope (Olympus/DeTrey, Konstanz, Germany) at
40× magnification to determine the mode of failure (adhesive,
cohesive or mixed).
Bond strength data were analyzed with ANOVA and Stu-
dent Newman Keuls multiple comparisons tests. Statistical
significance was set in advance at the 0.05 probability level.
3. Results
The pH values of the primers of each adhesive system are
shown in Table 1. Mean MTBS values obtained in each group
are described in Table 2. Mean bond strength was affected by
 1544
Table 1 – Information about tested adhesive systems
Adhesive Components Principle ingredients Mode/steps of application

Clearfil SE Bond (SEB) – Kuraray Co. Ltd., Osaka, Japan – lot # 41158 (pH 1.9)
Primer 10-MDP; HEMA; hydrophilic dimethacrylate; dl-camphorquinone; Apply primer for 20$$ . Mild air stream. Apply bond.
N,N-diethanol-p-touidine; water Gentle air stream. Light cure for 10$$
Two-step self-etch
Bond 10-MDP; bis-GMA; HEMA; hydrophobic dimethacrylate;
di-camphorquinone; N,N-diethanol-p-toluidine; silanated colloidal
silica.
Resulcin AquaPrime + monobond (RES) – Merz Dental, Lütjenburg, Germany – lot # 99490191 (pH 1)
AquaPrime 2-Methacryloyloxyethyl-dihydrogen-phosphate Mix AquaPrime with water (1:1). Scrub into dentin
Monobond Bis-GMA, TEGDMA, polymethacryl-oligomaleic acid surface for 30$$ . Gently air dry. Apply monobond. Air
blow gently. Light cure for 20$$
One-up bond F (OUB) – Tokuyama Europe GmbH, Dusseldorf, Germany – lot # 513 (pH 1.3)
Mix bonding A and B (1:1). Apply mixed material for

Agent A Phosphoric monomer, MAC-10, multifunctional methacrylic
monomer, co-initiator
Agent B Monofunctional monomers, water, fluoroaluminosilicate microfiller,
dye-sensitizer, borate derivative catalyst
Etch & prime 3.0 (EP) – Degussa AG, Hanau, Germany – lot # 019920 (pH 0.76)
One-step self-etch Universal HEMA, water, ethanol, stabilizer
Catalyst HEMA, initiators, stabilizers,
tetra-methacryloyloxyethylpyrophosphate
Prompt L-Pop (PLP) – 3M ESPE, St. Paul, MN, USA – lot # 41926 (pH 0.7)
Red blister Bis-GMA, methacrylated phosphoric esters, CQ, stabilizers
Yellow blister Water, zinc-fluoride complex, stabilizers
Solist (SOL) – DMG GmbH, Hamburg, Germany – lot # 99450003 (pH 1.8)
HEMA, TEGDMA, acetone, catalyst/stabilizer, elastomers
Futurabond (FUT) – Voco GmbH, Cuxhaven, Germany – lot # 01148E1 (pH 1)
Bis-GMA, diurethanedimethacrylate, hydroxyethylmethacrylate, BHT,
acetone, organic acids
d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 1542–1548
90$$ . Gently air stream. Light cure for 20$$
Mix Universal and Catalyst. Apply for 30$$ . Air blow
gently. Light cure for 10$$ . Repeat previously
mentioned steps
Pack activating. Scrub first coat 15$$ . Gently air dry.
Light-cure 10$$ . Second coat application (scrubbing)
15$$ . Gently air dry. Light-cure 10$$
Apply adhesive for 30$$ . Air blow gently. Light cure for 10$$ . Apply a
second coat for 5$$ . Air blow gently. Light cure for 10$$
Apply adhesive (scrubbing) for 30$$ . Air blow gently. Light cure for 20$$ .
Apply adhesive. Air blow gently. Leave second coat uncured

Total-etch Prime & Bond NT (PBNT) – Dentsply/DeTrey, Konstanz, Germany – lot # 0403000422 (pH 2.4)
PENTA, UDMA resin, Resin R5-62-1, T-resin, D-resin, nanofiller,
initiators, stabilizer, cetylamine hydrofluoride, acetone
Single Bond (SB) – 3M ESPE, St. Paul, MN, USA – lot # 040314 (pH 4.3)
HEMA, water, ethanol, amines, bis-GMA, methacrylate-functional,
copolymer of polyacrylic and polyitaconic acids, dimethacrlates
H3 PO4 etch for 15$$ . Rinse with water spray for 15$$ . Leave a moist
surface with a soft blow of air. Saturate the surface with ample
amounts of the adhesive, reapply if necessary. Leave the surface
undisturbed for 20$$ . Air blow gently for 5$$ . Light cure for 10$$
H3 PO4 conditioning for 15$$ . Rinse with water spray for 10$$ , leaving
tooth moist. Apply two consecutive coats of the adhesive with a fully
saturated brush tip. Dry gently 5$$ . Light cure 10$$

10-MDP: 10-methacryloxydecyl dihydrogen phosphate; HEMA: 2-hydroxyethyl methacrylate; bis-GMA: bis-phenol A diglycidylmethacrylate; TEGDMA: triethylene glycol-dimethacrylate; MAC-10:
methacryloyloxyalkyl acid phosphate; CQ: camphoroquinone; BHT: butylated hydroxy toluene; PENTA: penta-acrylate ester; UDMA: urethane dimethacrylate.
 d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 1542–1548 1545

the adhesive system (F = 8.648; p < 0.001), dentin pre-treatment

(F = 11.968; p < 0.001), and dentin region (F = 6.715; p < 0.001).

20.5 (7.7) Ab
22.8 (6.3) Ab
18.0 (3.4) Ab
Interactions between variables were significant (p < 0.001). The

PBNT
power of the multiple ANOVA was about 70%.
The two-step system SEB exhibited the highest MTBS when

–
–
–
Total-etch bonded to untreated dentin, while former prior H3 PO4 etching
decreased bond strengths, irrespective of the dentin region.
Resin–dentin bonds obtained for RES, EP, PLP, SOL and FUT

28.0 (10.2) Abc

23.5 (4.4) Ab were similar for all dentin regions and were not affected by

23.2 (5.9) Ab
acid-etching of dentin. Following H3 PO4 conditioning, MTBS
SB

to coronal dentin increased for OUB. MTBS with the total-etch

bonding agents presented similar bonding effectiveness to the

Within the same column, identical upper case letters indicate no differences (p < 0.05). For each row, matching lower case letters indicate no differences (p < 0.05).
–
–
– different dentin substrates.
Table 3 summarizes the failure modes percentage of
22.6 (11.5) Ab

17.2 (10.6) Aa

21.5 (10.5) Aa

the debonded specimens in the tested groups. Most of the

17.1 (7.0) Ab

16.8 (2.7) Aa
15.6 (4.6) Ac

observed modes of failure were adhesive. Major rates of

FUT

mixed failures were noticed for SEB groups, normally associ-

ated with higher bond strengths. Pure cohesive failures were
Table 2 – Mean microtensile bond strength (MPa) and standard deviation (S.D.) obtained for each tested group (n = 20 ± 4)

rarely detected. Root dentin showed half of the lower rate

of mixed failures when compared with the rest of dentin
22.4 (10.2) Aa
22.0 (9.9) Abc

18.2 (7.3) Abc

locations, after following the manufacturers’s directions. The

22.5 (9.7) Ab

22.1 (6.5) Ab

24.4 (5.6) Aa

percentage of mixed failures decreased after using prior H3 PO4

SOL

conditioning.
One-step self-etch

4. Discussion
25.0 (12.2) Abc

24.9 (9.4) Aab

25.4 (18.9) Ab

22.9 (11.0) Ab

21.9 (11.5) Aa
25.0 (9.8) Aa

There is a growing demand of treating cervical lesions, root

PLP

caries and root sensitivity [4,22,23]. Therefore, this study eval-

uated the effect of regional dentin variations on the MTBS of
two- and one-step self-etch bonding agents, pre-treated or not
23.6 (11.1) Bb

16.3 (10.1) Bb
23.3 (8.0) Bbc

with 36% phosphoric acid, compared to total-etch systems.

31.5 (7.5) Aa
19.7 (5.9) Ba
20.2 (6.6) Ba

The two-step self-etching system SEB exhibited the highest

OUB

MTBS when applied following manufacturer’s instructions, if

compared to the rest of the tested adhesives, irrespective of
the bonding approach (i.e., total-etch or self-etch). The supe-
rior performance of this system may be related to: (1) the
21.8 (9.0) Abc

synergy of an unsaturated methacrylate phosphate ester (10-

23.0 (9.6) Ab

14.3 (5.7) Ab

18.7 (6.8) Aa
15.4 (6.4) Aa
12.9 (1.0) Ac

MDP) as the acidic monomer in combination with HEMA [19],

EP

which is believed to improve the wetting of the tooth surface

and chelate to calcium ions of dentin [2,24]; (2) a higher expo-
sure of the peritubular dentin, which is highly mineralized
[3], bonding the specimens parallel to the tubules. This bet-
24.7 (10.3) Aa
24.1 (8.6) Abc

21.9 (9.6) Abc

18.1 (6.8) Ab

21.2 (9.4) Ab

25.7 (9.5) Aa

ter hybridization might also have been reflected in the relative

Two-step self-etch

RES

lower percentage of adhesive failures obtained after the MTBS

testing (Table 3).
H3 PO4 -conditioning produced a significantly decrease in
SEB dentin bond strength. Chelating interactions between 10-
42.7 (10.7) Aa
42.6 (13.9) Aa
40.6 (16.2) Aa
27.7 (8.7) Bab
21.2 (10.4) Ba
20.8 (8.3) Ba

MDP and dentin are reduced after phosphoric acid etching,

as hydroxyapatite crystallites availability might have further
SEB

decreased, diminishing SEB bond strength to dentin [25,26,27].

RES (two-step self-etching) yielded significantly lower
MTBS, regardless of the dentin substrate. The incorporation of
phosphoric acid ester monomers on its formulation confers an
Dentin/treatment

aggressive characteristic (pH 1) to this bonding agent, enabling

Cervical + H3 PO4
Coronal + H3 PO4

a stronger etching action on smear layers [11] and opening

Root + H3 PO4

of dentinal tubules that will produce an upward movement

Cervical
Coronal

of fluids from the underlying dentin toward the surface [18].

Root

A wet bonding technique is recommended by the manufac-

turer, so the water exudation from hydrated dentin [11,18] will
1546 d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 1542–1548

interfere with proper infiltration and coupling [28] of the sub-

0
4
0
sequent application of a hydrophobic rich resin (Bis-GMA and

PBNT
TEGDMA are the main components—Table 1), accounting for

49
46
40
M

–
–
–
the poor bonding performance of this adhesive.
PLP (pH 0.7), EP (pH 0.76), SOL (pH 1.8) and FUT (pH 1)

51
50
60
were neither affected by the dentin substrate nor by phospho-
ric acid etching, only OUB (pH 1.3) presented higher MTBS to

C
H3 PO4 -treated coronal dentin. Such results raise the finding

0
7
0
that within a certain range, differences in pH values may not
51
48
52
M
be the only important parameter to justify differences in bond
SB

–
–
–
strength efficiency [29]. The higher bond strengths obtained
with self-etch adhesives may also depend on other factors
A

49
45
48
[13,29], such as the dissociation constant (pKa ) [29], the chemi-
cal structure of the adhesive components (which may be more
C

0
0
0
0
0
0
or less chelating) [19], the solubility of the formed salts [24] and
FUT

its application time [6].

46
35
45
49
39
49
M

When bonding with self-etching adhesives to uncut

enamel, many manufacturers are recommending the use of
54
65
55
51
61
51
A

phosphoric acid, based upon the attained results with the

above mentioned adhesive systems, the accidental etching of
C

0
0
0
0
0
0

dentin during the adhesive procedure will not affect dentin

SOL

bond strength.
46
45
43
38
47
50
M

Moreover, it is important to stress that when one-step

self-etch agents are used, some problems arise: (1) a water
54
55
57
62
53
50
A
Adhesive system

flow-off from the bonded dentin results in a dilution of the

concentration of the adhesive monomers [13,30,31], lower-
C

0
0
0
0
0
1

ing their inward rates of diffusion; (2) the combination of

Table 3 – Distribution (as percentage) of failure modes: A: adhesive, M: mixed, and C: cohesive

PLP

48
46
48
45
44
40
M

acids, hydrophilic and hydrophobic monomers into a single

solution may compromise the function of each one of these
52
54
52
55
56
59
A

components [32,33]; (3) a differential infiltration gradient is

established as a consequence of phase separation within the
C

0
0
0
4
0
0

adhesive, and due to differences in molecular weight or affin-

ity to dentin of the infiltrating compounds of the adhesive
OUB

46
51
36
50
42
42
M

system [30,34]; (4) a relatively high concentration of solvent

is required to keep these adhesives blended in solution, and
54
49
64
46
58
58
A

air-drying is not able to accomplish significant solvent evapo-

ration [35]. The retention of water/HEMA solvents within the
C

0
2
0
0
0
0

hybrid layer hampers polymerization [36], which conducts to

reduced mechanical properties and lower bonding effective-
47
48
33
31
43
35
M
EP

ness [35,36].
Particular shortcomings related to the specific composition
53
50
67
69
57
65
A

of each one-step self-etch system may also be considered to

explain the poor bonding effectiveness obtained with these
C

0
0
0
0
0
1

adhesives. PLP and EP are solutions consisting of methacry-

late phosphoric acid mono- and di-esters, and are though to
RES

39
49
43
43
48
46
M

induce a continuous demineralization of the adjacent dentin

structures in the tubules, destabilizing the collagen [14,30]. In
61
51
57
57
52
53
A

the case of SOL, a precipitation of dissolved Ca+ salts within

the adhesive layer and the incorporation of polyetherurethane
C

5
6
8
0
0
0

(an elastomeric component with a high-molecular weight,

highly hydrophilic and hygroscopic) on its formulation may
SEB

80
64
80
65
60
59
M

have induced an osmotic water flux from deep dentin that has
also limited its bonding efficacy [33]. FUT consists of organic
15
30
12
35
40
41
A

acids combined with hydrophobic monomers and HEMA, all

dissolved in acetone. However, FUT does not contain water
Cervical + H3 PO4
Coronal + H3 PO4

on its composition, which is required to dissociate the weak

Root + H3 PO4

acids into ionized forms [11,31]. It can be assumed that its

Cervical
Coronal

acidic monomers may not be properly dissociated, resulting in

Root

lower bond strengths [31]. Its performance may also be compli-

cated by the manufacturer’s requirement of leaving the second
 d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 1542–1548
adhesive coat uncured prior to the placement of the composite
resin. So, this subsequent non-polymerized coat that also con-
tains acidic and hydrophilic monomers may facilitate osmotic
water transport from the blisters through the upper part of the
adhesive layer [15,16].
The one-step self-etch and the total-etch self-priming
adhesives share a common characteristic, in that the polymer-
ized adhesive layers are straight coupled to resin composites
without coverage of a further hydrophobic resin layer
[15,16,33]. In the present study SB and PBNT attained simi-
lar bond strength values to all dentin substrates, and it could
not be observed MTBS differences between any total-etch or
one-step self-etch bonding agent evaluated.
Previous studies on coronal dentin with the same method-
ology showed similar MTBS results for total-etch (SB) and
two-step self-etch adhesives (SEB) [30,37]. So, encountered dif-
ferences in the present study may be related to variations at
the selected dentin substrate for adhesion [22]. Bonding to
parallel-cut dentin implies that the numbers of resin tags,
which have been postulated to contribute to bond strength
in the order of 25% [38] are reduced, so a decrease in bond
strengths in the case of the total-etch bonding system is
expected [39]. Phrukkanon et al. [21] and Yoshiyama et al.
[4] demonstrated that bond strength of total-etch adhesives
may be affected by the different locations of dentin, while a
self-etch system produces consistent bonding irrespective of
dentin location or tubule orientation. The higher MTBS val-
ues attained by SEB might also be related to the exposition of
a larger mineralized surface area ready for bonding with the
10-MDP molecule, thus creating a stronger chemical bond [24].
These differences in results are important, as clinically, lon-
gitudinal sections of dentinal tubules are frequently exposed
on cavity walls preparations [39].
The results of this study require the rejection of the null
hypothesis that there are not differences in dentin bond
strength of self-etch (two- and one-step) or total-etch adhesive
systems to different regions of dentin. Although the obtained
results from this in vitro study may not be directly extrapo-
lated to the clinical situation, they provide useful information
concerning the performance of simplified self- and total-
etch adhesives to different regions of dentin. Even so, further
investigations are required to determine the long-term perfor-
mance of these adhesives on the different sites of dentin.
5. Conclusions
For all dentin regions, the highest bond strength was obtained
when the two-step self-etching adhesive system (SEB) was
applied. When bonding to parallel-cut dentin, previous H3 PO4 -
etching does not increase bond strength and differences do
not exist when comparing attained MTBS by one-step or total-
etch bonding systems to the different dentin regions.
Acknowledgement
This research project was supported by grants CICYT/FEDER
MAT2004-06872-C03-02 and RED CYTED VIII. J.
1547
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http://intl.elsevierhealth.com/journals/dema

Effects of saliva contamination on resin –resin

bond strength
Sigurdur O. Eirikssona,*, Patricia N.R. Pereirab, Edward J. Swift Jr.b,
Harald O. Heymannb, Asgeir Sigurdssonc

a
Institute of Dental Research, Faculty of Odontology, University of Iceland, Reykjavik, Iceland
b
Department of Operative Dentistry, University of North Carolina at Chapel Hill, Chapel Hill, NC, USA
c
Department of Endodontics, University of North Carolina at Chapel Hill, Chapel Hill, NC, USA

KEYWORDS
Resin composite;
Saliva contamination;
Adhesion;
Dental materials;
Dentin bonding agent
Summary Objective. The purpose of this study is to evaluate the effects of saliva
contamination on microtensile bond strength (mTBS) between resin interfaces and to
determine which decontamination methods best re-established the original resin –
resin bond strength.
Materials and methods. Ninety-six light-cured resin composite cylinders of Z-250,
Renew, Clearfil APX, and Pertac II were randomly divided into six groups. For each
material, one group of specimens was not contaminated, serving as the control. For
the other specimens, the top surface of each block was treated with saliva that was
slowly dried (Treatment 1); dried forcefully (Treatment 2); slowly dried, rinsed, and
dried (Treatment 3); slowly dried, rinsed, dried, and bonded with Single Bond, One-
Step, Clearfil SE Bond, or Prompt L-Pop (Treatment 4); or slowly dried, but not rinsed,
and bonded using the same adhesives (Treatment 5). Two 2-mm increments of resin
composite were applied and light-cured. After 24 h, the assemblies were trimmed for
microtensile bond testing and were loaded to failure at 1 mm/min. Data were analyzed
using two-way and one-way ANOVA and Fisher’s PLSD ðp , 0:05Þ:
Results. Control values ranged from 45.1 MPa for Pertac II to 71.5 MPa for APX.
Treatment 1 caused significant reduction in resin –resin bond strength for all materials
tested but for two of the materials in treatment 2. Pertac II was the only material that
did not show a statistical difference from control group for treatment 3. Treatment 4
re-established the control values for Z-250 and Renew and treatment 5 was the only
one to show no statistical difference for all materials tested. SEM observation revealed
a smooth surface in treatment 1, but treatment 3 showed a few craters. Treatment 4
and 5 showed a mixture of cohesive failure in the composite and adhesive.
Significance. The most reliable method for decontaminating saliva from resin
surfaces involves the application of adhesives.
Q 2003 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Introduction

The increasing popularity of dental composites has

*Corresponding author. Dental School, University of Iceland,
Vatnsmyrarvegur 16, Reykjavik 101, Iceland. Tel.: þ354-525-
4850/ þ 354-897-2050; fax: þ 354-525-4874.
E-mail address: bbj@simnet.is
drawn attention to the importance of moisture and
contamination control, because composites do not
‘forgive’ contamination or produce a better seal

0109-5641/$ - 30.00 þ 0.00 Q 2003 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/S0109-5641(03)00066-6
38
with time as amalgam restorations do. The diffi-
culty of achieving moisture control is a common
problem encountered in restorative dentistry,
especially when rubber dam isolation is impossible.
In addition, clinicians are encouraged to place resin
composite restorations in increments to ensure
complete polymerization of large restorations for
optimal physical properties1 and bonding to the
surrounding tooth structure. 2 Gap formation
between bonded restoration and tooth walls can
be caused from the stresses of polymerization
shrinkage.3,4
Although the incremental filling technique is
desirable, the longer time required for placement
and polymerization of increments also can make
contamination control more difficult. A few studies
have been done on adhesives involving contami-
nation of enamel5 – 12 and dentin5 – 8,13 surfaces;
however, there is a lack of information on the
effect of contamination between the surfaces of
resin increments.
Many ‘one-bottle’ dental adhesives have become
available in the past few years. They combine the
primer and adhesive components of multi-step
bonding systems in a single solution.14 Solvents
such as acetone or ethanol in the one-bottle
adhesives remove residual moisture and enhance
resin wetting of the substrate.5,14,15 Two-step self-
etching primer systems, which combine the etchant
and primer in one-bottle, and the adhesive in a
separate bottle- as well as ‘All-in-One’ self-etching
adhesives that combine etchant, primer, and
adhesive in a single solution - have become
available recently. There is a need to evaluate the
role of these various new dentin bonding systems in
Table 1 Composition of the bonding agents.
Adhesives Composition
Single Bond Bis-GMA, HEMA, dimethacrylates,
polyalkenoic copolymer, ethanol,
water, photoinitiator
One-Step Bis-GMA, BPDM, HEMA, acetone
Clearfil SE Bond MDP, HEMA, hydrophilic dimeth-
primer arylate, n,n Diethanol-p-Toluidine,
camphoroquinone (CQ), water
Clearfil SE Bond MDP, Bis-GMA, HEMA, hydrophobic
adhesive aliphatic dimethacrylate,
n,n Diethanol-p-Toluidine,
silanated colloidal silica CQ
Prompt L-Pop Water, methacrylated phosphoric
acid esters, fluoride complex w/
zinc, parabenes
Abbreviations: Bis-GMA: bisphenol-A-glycidylmethacrylate; HEMA: hydroxyethyl methacrylate; BPDM: bisphenyl dimethacrylate;
MDP: 10-methacryloyloxy methacrylate.
a
Bonding procedures as executed in treatments 4 and 5: (a) apply primer, (b) mild air flow, (c) apply adhesive (d) light cured.
S.O. Eiriksson et al.
decontaminating resin increments that were con-
taminated with saliva during placement of compo-
site restorations.
The purpose of this study is to evaluate the
effects of saliva contamination on microtensile
bond strength (mTBS) between resin interfaces
and to determine the best decontamination method
to re-establish the original resin – resin bond
strength. The hypothesis tested was that saliva
contamination would reduce resin – resin microten-
sile bond strength, but that some adhesives could
reverse this effect.
Materials and methods
Four commercially available resin composites and
bonding agents were used. The bonding agents,
compositions, batch numbers and manufacturers
are listed in Table 1. An ethanol-based adhesive,
Single Bond (SB), and an acetone-based adhesive,
One Step (OS) were used as the one-bottle
adhesives. Clearfil SE Bond (SE) was used as the
two-step self-etching primer system, and Prompt L-
Pop (LP) was the all-in-one self-etching adhesive
used. Each bonding agent was used with its
respective hybrid resin composite from the same
manufacturer. SB was used with zirconia silica-
filled Z-250, OS with barium glass-filled Renew, SE
with barium glass-filled Clearfil APX and LP with
quartz-filled Pertac II (Table 2). The bonding agents
were applied and cured according to the manufac-
turers’ instructions (Table 1). A transparent vinyl
cylinder 4 mm high £ 10 mm wide was filled with
resin composite. The excess was removed with
Batch no. Bonding Manufacturer
instructiona
9CL c(2x),b,d(10s) 3M ESPE, St Paul, MN
9900010095 c(2x),b,d(10s) BISCO Inc., Schaumburg, IL
61119 a,b Kuraray Co., Ltd, Tokyo,
Japan
61119 c,b,d(10s) Kuraray Co., Ltd, Tokyo,
Japan
61414 c(15s),b,d(10s) 3M ESPE, St Paul, MN
Effects of saliva contamination on resin– resin bond strength
Table 2 Composition of the resin composites.
Resin composites Composition
Z-250 Bis-GMA, UDMA, Bis-EMA
Renew Bis-GMA, Triethyleneglycol, BPDM
Clearfil APX Bis-GMA, TEGDMA, CQ
Pertac II No data
Abbreviations: BisGMA: bis-phenol-A-diglycidyl methacrylate; UDMA: urethane dimethacrylate; bis-EMA: bisphenol A polyetheylene
glycol diether dimethacrylate; BPDM: biphenol dimethacrylate; TEGDMA: triethylene glycol dimethacrylate; MDP: 10-
methacryloyloxy methacrylate.
a spatula in order to produce a relatively flat
surface, and the composite was light-cured from
the top and bottom surfaces of the cylinder for 60 s
each to ensure complete polymerization of the
composite, using a visible light-curing unit (Optilux
501, Demetron/Kerr, Danbury, CT, USA). The
intensity of the light was maintained at 690 mW/
cm2. The oxygen-inhibited layer was retained in
order to replicate the clinical circumstances of
incremental filling technique.
The composite cylinders were randomly divided
into six groups according to the different surface
contamination/treatments. Four cylinders were
fabricated per treatment for each material, for a
total of 96 composite cylinders. Saliva was col-
lected from a single individual, at the site and at
the same time that the specimens were made.
Fresh saliva is considered an acceptable material to
be used in saliva contamination testing.13,16 The
specimens were treated as follows:
Control group. The control group was not
contaminated with saliva nor treated with bonding
agent; rather, two layers of composite were added
to the original cured composite.
Treatment 1. Saliva was applied to the speci-
mens with a microbrush (Kerr Corporation, Orange,
CA) and dried carefully with oil-free compressed air
for 20 s from a distance of 10 cm. Care was taken to
maintain a layer of dry saliva on top of the samples.
Treatment 2. Saliva was applied with a micro-
brush and was immediately blown off with a strong
stream of air from a distance of 1 cm for 20 s.
Treatment 3. Saliva was applied and dried as
previously described in Treatment 1. A copious
amount of water was then used to rinse off the
contamination for 20 s followed by air-drying
for 20 s.
Treatment 4. Saliva application and rinsing were
done as in Treatment 3, except that a bonding agent
was applied to the surface and was light-cured as
recommended by its manufacturer (Table 1).
Treatment 5. Saliva application was performed
as in Treatment 1; however, instead of rinsing,
a bonding agent was applied directly on
39
Filler (%vol.) Batch no. Manufacturer
Zirconia-silica (60%) 0EH 3M ESPE, St Paul, MN
Barium– glass (59%) 0000007094 BISCO Inc., Schaumburg, IL
Barium– glass (70%) 00551A Kuraray Co., Ltd, Tokyo, Japan
Quartz-filled 012, 014 3M ESPE, St Paul, MN
the contaminated surface and was light-cured as
recommended.
After surface treatment, the periphery of the
specimen was marked with permanent ink to ensure
that the interface could be detected when cutting
the samples. Each treated surface was ‘restored’
with two 2-mm increments of resin composite, with
each being light-cured using the Optilux 501 for
40 s. The bonded assemblies were stored for 24 h in
distilled water at 37 8C.
The specimens were sectioned using a diamond
saw (Isomet, Buehler Ltd, Lake Bluff, IL, USA) into
0.7 mm thick slabs. Each slab was trimmed into an
hourglass shape using a fine diamond on a water-
irrigated high-speed handpiece to a cross sectional
area of 1.0 mm2 ^ 0.2 mm2.17 The thickness and
width of the bonded area of each specimen were
measured using a digital micrometer. Each cylinder
was cut into three specimens, for a total of 288
specimens (12 per material per treatment). The
specimens were glued with cyanoacrylate (Zapit,
DVA, Corona, CA, USA) to a Bencor Multi-T testing
apparatus (Danville Engineering, Danville, CA)
mounted in an Instron universal testing machine
(model 4411, Instron Corporation, Canton, MA,
USA). Specimens were loaded to failure at a
crosshead speed of 1 mm/min. The microtensile
bond strength was calculated by dividing the
maximum load at fracture by the cross-sectional
surface area of the bonded surface. If a spon-
taneous interfacial debonding occurred while the
specimens were being mounted or sectioned, the
bond strength was recorded as 0 MPa. The data
were analyzed using two-way and one-way ANOVA
and Fisher’s PLSD ðp , 0:05Þ:
After debonding, the specimens were fixed in 10%
neutral buffered formalin for at least 8 h18 for
decontaminating the specimens. To evaluate the
fracture pattern, three representative specimens
from each treatment were chosen randomly and
observed by two of the investigators. Both debonded
sides of the fractured specimens were trimmed,
placed on stubs, desiccated in ambient conditions,
gold sputter-coated (5100 sputter-coater, Polaron
40 S.O. Eiriksson et al.

Figure 1 Results of microtensile bond strength test for different restorative materials MPa (Bar ¼ SD). Means with the
same superscript are not statistically different within each composite/adhesive treatment (Fisher’s PLSD, p . 0:05).

Equipment Ltd, Watford, England), and examined
with a JSM 6300 scanning electron microscope (SEM,
JEOL USA Inc., Peabody, MA, USA). The debonded
sides were evaluated for mode of fracture and
difference in texture from control treatments.
Results
Microtensile bond strengths are summarized in
Fig. 1. Two-way ANOVA showed that the factors
‘surface treatments’ and ‘materials’ and their
interaction were significant ðp , 0:0001Þ: Fisher’s
PLSD revealed no statistical difference between
treatment 5 and the control group ðp ¼ 0:1355Þ but
all other treatments had significantly lower micro-
tensile bond strengths than the control ðp , 0:05Þ:
One-way ANOVA and Fisher’s PLSD test revealed
that slowly drying the saliva on top of the specimens
(treatment 1) resulted in significant reductions in
resin – resin bond strengths for all materials ðp ,
0:0001Þ; ranging from 16.4% (Z-250) to 43.4% (APX)
of the control values. Drying saliva forcefully on
the surfaces (treatment 2) resulted a significant
decrease in bond strength for Z-250 ðp , 0:0001Þ
and APX ðp ¼ 0:0012Þ; however, bond strengths
were not significantly different from the control
treatments for either Renew ðp ¼ 0:8408Þ or Pertac
II ðp ¼ 0:7592Þ: Rinsing saliva off with water (treat-
ment 3) produced a significant difference from the
control for Z-250 ðp ¼ 0:0058Þ; Renew ðp ¼ 0:0146Þ
and APX ðp ¼ 0:0122Þ; but not for Pertac II ðp ¼
0:2461Þ:
For Z-250 and Renew, adding their respective
bonding agents (treatment 4) re-established bond
strengths to nearly the control level (p ¼ 0:5997
and p ¼ 0:5965; respectively). However, bond
strengths remained significantly lower than the
controls for both APX ðp ¼ 0:004Þ and Pertac II ðp ,
0:0001Þ: The application of bonding agent on top of
slowly dried saliva (treatment 5) re-established
bond strengths to values similar to the control
values for all materials tested ðp , 0:05Þ:
Scanning electron microscopic observation
revealed a smooth surface on the specimens in
treatment 1 when compared to the other treat-
ments (Figs. 2 and 3). Treatment 3 specimens had

Figure 2 (a) and (b) are representative SEM photographs of fractured specimen without contamination (Control
group) £ 2000. (a) Z-250. (b) APX.
Effects of saliva contamination on resin– resin bond strength 41

Figure 3 SEM of fractured specimens, contaminated with saliva that was dried slowly on the surface, showing smooth
surfaces on the composites (Treatment 1) £ 2000. (a) Z250. (b) APX.

a few craters or blisters indicating water, air, or
saliva might still have been trapped in the compo-
site buildup (Fig. 4). A mixture of cohesive failure in
composite and adhesive in both base and first
increment was observed under the SEM for treat-
ments 4 and 5.
Discussion
Saliva is mostly water 99.4% with 0.6% solids. The
solid is composed of macromolecules like proteins,
glycoprotein sugars and amylase, inorganic par-
ticles like calcium, sodium and chloride and organic
particles like urea, amino acids, fatty acids and free
glucose. In this study, salivary contamination
caused significant decreases in bond strength
between resin increments, which is in agreement
with results published by Hitmi et al.13 In their
study, salivary contamination was achieved after
polymerization of the bonding agent on dentin prior
to application of composite.
Scanning electron microscopic observation of
saliva-contaminated resins revealed a smooth sur-
face on the specimens, (Figs. 2 and 3), which
probably resulted in reduced bond strengths due to
lack of interaction of the increment with the
contaminated surface. Drying the saliva quickly
resulted in significantly higher bond strengths than
drying the saliva slowly, and this may be attributed
to saliva film thickness. The water evaporates
leaving a film of glycoprotein sugars on the
surfaces. Although quick drying improved the bond
strengths of two materials, this procedure may not
be a completely reliable method for decontaminat-
ing the surface because Z-250 only showed re-
establishment of 40% of control values, and APX
showed 75%.
Rinsing saliva with water before adding new
layers of composite raised the resin – resin bond
strength to 77 – 80% of control values for Z250,
Renew and APX and to the control values for Pertac
II. SEM observation of treatment 3 showed a few
craters or blisters indicating water, air or saliva
might still have been trapped in the composite
buildup (3). The bond strength data, along with the
SEM photographs (Fig. 5), suggest that once saliva
contacts the composite, salivary pellicle deposits
on the composite and lowers the bond strength of
the next layer, even if the saliva is there for only a
short time (treatment 2) or is rinsed away with
water (treatment 3), indicating that this approach

Figure 4 (a) and (b) are representative SEM photographs of fractured specimen which were contaminated with saliva,
dried and rinsed with water.(Treatment 3) £ 2000. (a) Z-250 shows porosities indicating moisture or air trapped on the
composite. (b) APX. Porosities were observed on the surface.
42
Figure 5 (a) and (b) are representative SEM photographs of fractured specimens that were contaminated with saliva,
dried and rinsed with water, dried again and bonding agent applied showing mixture of cohesive failure in composite and
adhesive in both the base and the first applied increment (Treatment 4) £ 2000. (a) Z-250/S B. (b) APX/SE.
is not a predictable method for decontaminating
the surfaces.
The addition of a bonding agent in treatment 4
increased the bond strength of Z-250 and Renew to
similar levels as their controls. Z-250, Renew and
APX all had bond strengths approaching 60 MPa. A
mixture of cohesive failure in composite and
adhesive in both the base and the first applied
increment was observed under the SEM.
In 1985, Lloyd and Dhuru19 made repairs to a day-
old composite and found that inclusion of Scotch-
bond (3M) bonding agent raised the fracture
toughness of P10 (3M) specimens kept in saliva for
1 h back to values obtained for immediately
repaired non-contaminated specimen. Shahdad
and Kennedy20 reported that surface abrasion
significantly improved the bond strength and that
the use of bonding agents further enhanced bond
strength but not significantly. They also reported
that the use of the bonding agent alone improved
the bond strength significantly ðp , 0:001Þ: Fritz
et al.8 tested an experimental adhesive resin
containing UDMA, HEMA and 4-META dissolved in
acetone on saliva-contaminated enamel and dentin
surfaces. They applied the saliva after curing the
surfaces, rinsed it off and applied resin composite
with or without primer. They found no difference
between these treatments and a statistical signifi-
cant difference from control treatment for dentin.
This is in disagreement with our results for treat-
ment 4 and shows that more research is necessary in
this area to determine the effect on all the different
surfaces of the cavity preparation.
Interestingly, application of a bonding agent on
the dried saliva-contaminated surface gave the
most reliable results in all treatments. This was
especially noted with the self-etching primer/ad-
hesive. The single-bottle adhesives contain solvents
such as ethanol (SB) and acetone (OS) that seem
able to denature the glycoprotein sugars and
remove the saliva contamination from the surface
S.O. Eiriksson et al.
to create bond strength similar to the rinsed
surfaces in treatment 4. A similar phenomenon
was observed with the self-etching primer (SE),
which contains derivatives of ethanol. Surprisingly,
Prompt L-Pop re-established only 53% of bond
strength of the control values for Pertac II in
treatment 4 but 100% in treatment 5 (Fig. 1).
These results may have been caused by moisture
trapped on the composite surface interfering with
the bonding ability or by failure of the bonding
agent to form a uniform surface coating. It has been
reported that Prompt L-Pop might not be success-
fully polymerized in thin layers,21 which could
account for the relatively low results when com-
pared to the other treatments/materials.
Additional coats of the adhesive system might
solve this problem.22,23 The solvent in Prompt
L-Pop is water and the difference between treat-
ments 4 and 5 may also be explained by the non-
volatile nature of this solvent compared to the
other dentin bonding agents. More careful drying is
necessary to ensure complete removal of the water
solvent. El-Kalla and Garcia-Godoy5 tested the
effect of saliva on etched enamel and dentin on
bond strengths using three adhesives containing
acetone and one containing water as a solvent. The
water-based bonding agent was the only one
significantly different from its control treatment
when tested on enamel but showed a non-signifi-
cant difference when tested on dentin.
Webster et al.9 found that if the saliva contami-
nation occurred after a primer had been placed and
cured on enamel, reapplication of primer after
drying the saliva provided a good bond to the
underlying primer layer. Rosa et al.6 spread saliva
on acid-etched enamel without air-thinning or
rinsing it off with water. In their study they used
Single Bond, Prime&Bond NT, which is acetone-
based, and the Bis-GMA/HEMA bonding resin from
the Scotchbond Multi-Purpose system. Application
of saliva lowered the bond strength statistically only
Effects of saliva contamination on resin– resin bond strength
for Scotchbond Multi-Purpose, which was explained
by a high percentage of organic solvents in SB and
Prime&Bond NT, but no such solvents are in
Scotchbond Multi-Purpose. The adsorbed moisture
of saliva may be rapidly displaced if the solvent is
sufficiently hydrophilic.24 Xie et al.7 also showed
decreased bond strength when he applied the
adhesive from Scotchbond Multi-Purpose after con-
taminating etched enamel with artificial saliva. Re-
etching restored the bond strengths. In a similar
study by Rosa et al.6 the same adhesives were tested
on the effect of saliva contamination on dentin and
found no statistically significant difference within
each adhesive. In that case they also used the primer
from Scotchbond Multi-Purpose, which contains
HEMA,25 water, and polyalkenoic acid26 which
facilitates bonding to wet dentin.25,26 Hitt and
Feigal10 and Feigal et al.11,12 have reported that
the bonding agents containing hydrophilic mono-
mers can counteract the adverse effect of saliva on
the bond strength of sealants to etched enamel. This
result is consistent with our finding that priming
the saliva-contaminated resin composite yielded the
highest mean bond strengths and may be related to
the fact that the resin was light-cured before the
contamination occurred. Also, its hydrophobic
nature might prevent the saliva from diluting or
penetrating its surface. Peshke et al.27 tested the
influence of incorrectly performed steps during the
application of the water-based dentin adhesive
system OptiBond FL on the marginal quality of
Class V restorations in vitro and found that saliva
contamination prior to application of the primer
solution did not affect the margin quality
significantly.
To simulate in vivo manipulation of composite
surfaces prior to re-bonding, the resin composite
cylinders were fabricated with a composite spatula,
thus making it impossible to reproduce perfectly flat
composite surfaces for tensile testing. Although
ideally the specimens should exhibit flat surfaces to
avoid complex stresses during testing, the technique
adopted for this study was chosen because it more
closely paralleled the clinical situation. The oxygen
inhibited layer is viscous and contains unreacted
acrylate groups which improve adhesion between
the substrate and the second layer by the formation
of covalent bonds.28,29 This unreacted layer may,
however, induce brittleness because of inadequate
links due to a local decrease in photo initiator
concentration.30,31 Truffier-Boutry32 reports higher
shear bond strength from the oxygen-inhibition on
the surface layer of the substrate compared to
surfaces without oxygen-inhibition. The method-
ology used in this study maintained the oxygen-
inhibited layer in a way similar to incremental filling
43
technique. Since the surface area tested in the mTBS
test is much less than the conventional tensile and
shear bond strength tests, possible irregularities
created with the spatula compared to the trimmed
specimens that have been polished with 600-grit
discs may not play as much difference as they would
have in the conventional tests.
Conclusions
Saliva contamination significantly reduced bond
strengths between resin composite surfaces regard-
less of the materials evaluated. Blowing the saliva
off quickly or rinsing with water did not restore
bond strengths to normal levels for some of the
materials tested. SEM examination suggested that
water, air or saliva might remain trapped between
resin layers. Within the limitations of this study, it
can be concluded that the application of a
dentin/enamel adhesive is necessary whenever
saliva contamination exists on composite incre-
ments to ensure better interfacial bonding. Rinsing
the saliva from the surfaces might not be necessary
to promote good resin – resin adhesion.
Acknowledgements
Based on a portion of a thesis submitted to the
graduate faculty, University of North Carolina, in
partial fulfillment of the requirements for the MS
degree.
This study was funded by Bisco Inc, Schaumburg,
IL. The authors thank Bisco Inc., 3M Dental Products
Division, Kuraray Co. Ltd, and 3M ESPE for providing
the materials for this study. The authors have no
financial interest in Bisco, Inc.
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