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Effectiveness of indirect composite resin silanization by microtensile bond

strength test

Article  in  American Journal of Dentistry · June 2008

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Research Article
_______________________________________________________________________________________________________________________________________________________________

Effectiveness of indirect composite resin silanization evaluated

by microtensile bond strength test
MAURO ITARU HONDA, DDS, FLÁVIA MARTÃO FLÓRIO, DDS, MS, SCD & ROBERTA TARKANY BASTING, DDS, MS, SCD, PHD

ABSTRACT: Purpose: To assess the effectiveness of using silane before cementing laboratory resins, by means of
microtensile bond strength test. Methods: 40 human molars were selected, cleaned and stored in a 0.1% thymol
solution. The occlusal surfaces of these teeth were removed and flattened until dentin was exposed. Next, the laboratory
resin blocks were cemented (Adoro or Artglass) with Single Bond and Rely X adhesive cementing systems, by the same
cementing protocol, the only difference between the groups being whether or not silane was applied. The teeth to which
the blocks were cemented were prepared to obtain stick-shaped test specimens with an approximate area of 1.00 mm2 (±
0.12 mm2) for the microtensile bond strength tests. Afterwards, under x2.5 magnification, the fracture modes were
visually classified as adhesive, cohesive or mixed. Results: ANOVA (P 0.05) showed that there were significant
differences in the microtensile values between the indirect composites studied. The highest microtensile bond strength
values were found with the Artglass (58.08 MPa without silane, 49.76 MPa with silane), and lowest values with Adoro
(37.08 MPa without silane, 39.52 MPa with silane). There were no differences in the microtensile bond strength values,
with or without silane application. The fractures were considered predominantly adhesive in 68.3%, mixed in 25.8%
and cohesive in 5.9% of cases. The use of silane did not contribute significantly to increasing microtensile bond strength
during laboratory resin cementation. (Am J Dent 2008;21:153-158).

CLINICAL SIGNIFICANCE: From the point of view of initial microtensile bond strength, the use of silane in cementing
the laboratory resins (Adoro and Artglass) was not recommended, due to the increase in cost and clinical procedure time.

: Prof. Dr. Roberta Tarkany Basting, Faculty of Dentistry and São Leopoldo Mandic Dental Research Center,
Department of Restorative Dentistry – Operative, Rua José Rocha Junqueira, 13, Bairro Swift, Campinas – SP, CEP:
13045-755, Brazil. E- : rbasting@yahoo.com

Introduction
The widespread acceptance of indirect composite use is
evident from the large number of commercial brands available,
with different formulations and designations, such as glass
polymers, polycerams, ceromers or second generation poly-
mers.1 Their development seems to have followed the same
steps as the development of ceramics, with CAD-CAM type
machining systems or composite blocks, which are used for
making test specimens or restorations.2 They are materials of a
relatively lower cost than ceramics, presenting suitable esthetic
appearance and increasing reliability and durability. They may
be used as covering material in fixed partial dentures with fiber
reinforcement, showing promising results after 4 years of
clinical follow-up.3,4
Silanization is recommended for the cementation process,
particularly in ceramic restorations. However, Della Bona et al5
reported that there is still no consensus regarding cementing
composite restorations or dentures for indirect use. Probably,
this is because new materials and techniques are rapidly being
introduced, each with their own peculiarities for use, which
makes the procedures increasingly specific with each comer-
cial brand of composite.6 Moreover, the clinical guidelines for
some indirect resin systems recommend this procedure.
It is therefore necessary to have knowledge of the resin
composite cementation process for indirect use,7 particularly
with reference to the silanization procedure, even though it is
related to the repair of resin composite restorations for direct
use.8-10 The percentage of inorganic matrix in composites for
indirect use would be based on chemical bond between the
restoration and the cementing agent during silanization, since
the polymeric conversion rate is high for this type of material,
and does not allow chemical bonds to the organic matrix
afterwards.11,12 Moreover, there are extensive resinous matrix
areas at the bond surface, which could interfere in or annul the
bonding procedure.
In similar studies,13-15 the results showed no consensus
among the authors, and the methodologies used have been
questioned as far as interpretation of the results is concerned.
Microtensile tests have been indicated, because they allow a
greater incidence of adhesive fractures and better distribution of
the forces on the bond surface to be obtained,16 as well as less
variation in the results.17 Therefore, this study assessed the
effectiveness of either silanization, or non-silanization before
the cementation process of indirect resins to human dentin,
using the microtensile test to assess the bond strength.
Materials and Methods
This research was approved by the Research Ethics
Committee Protocol No.1215, in accordance with Resolution
196/1996 of the National Health Council of the Ministry of
Health, Brazil.
The factor under study in this experiment was whether or
not to apply the silane bonding agent to two commercial brands
of indirect composites, sub-divided into four levels:
- The use of silane applied before cementing ArtGlass.a
- The use of silane applied before cementing Adoro.b
- Absence of silane application before cementing ArtGlass.
- Absence of silane application before cementing Adoro.
For the experimental units, the dentin portions of 40 dental
crowns, obtained from 40 human molars, were used. Ten dental
crowns (n= 10) were randomly distributed among the levels

154 Honda et al
Fig. 1. A. Removal of occlusal enamel with diamond tip. B. Flattening of the occlusal surface with abrasive paper and later application of finishing diamond tip to
form standard smear layer. C. Cementation of laboratory resin block and starting cutting. D. Selecting the most central sticks and discarding the external ones. E.
Random selection of three sticks for testing and nine possible sticks.
under study. Each tooth provided a mean of three sticks that
were used, constituting one test specimen.
The response variable was the microtensile bond strength,
quantitatively assessed and expressed in MPa. The fracture
mode was qualitatively assessed and rated by scores after
observation under loupes.
Forty healthy maxillary and mandibular human molars
extracted for reasons not related to the research were selected.
After extraction, these teeth were stored in an aqueous 0.1%
thymol solution with pH 7.0, for a period not exceeding 5
months.
After cleaning the teeth with curettes and scalpel blades, the
occlusal faces were abraded with a 4138G diamond tip,c at high
speed with abundant cooling until the enamel was completely
removed, and the dentin exposed (Fig. 1A). Two thirds of the
most apical root portion was also removed with a high speed
diamond tip, exposing the pulp chamber.
In all the teeth the pulp chambers were filled with incre-
ments of resin composite Esthet X,d shade A2 using the Prime
& Bond NTd adhesive system following the manufacturer’s
instructions.
The occlusal surface of the teeth was planed with a
metallographic grinder (Politriz Aropol 2Ve) with aluminum
oxide abrasive paperf with decreasing grit of 220, 320, 400 and
600 used for 5 seconds for each tooth, making the dentin
surfaces uniform (Fig. 1B). To simulate surface roughness and
smear-layer formation, as is clinically obtained, a diamond tip
4138 FF was applied, making two movements back and forth in
the vestibular-lingual direction and two movements in the
mesio-facial direction, using only the weight of the high speed
American Journal of Dentistry, Vol. 21, No. 3, June, 2008
pen and absence of manual pressure.
The occlusal dentin surfaces were etched, according to the
manufacturer’s recommendation, with 37% phosphoric acid
(Scotchbond Etchantg) for 15 seconds, followed by rinsing with
water for 15 seconds. The water was removed with a light air
jet, applied in a circular manner, at a distance of 5 cm, for a
maximum period of 5 seconds to keep the tooth visually humid.
Two layers of the conventional two-step adhesive system
Adper Single Bond 2g were applied with a disposable applica-
tor,h dried for 10 seconds with an air jet and polymerized for 10
seconds with a light polymerizer (Ultraluxi).
A block-shaped pattern, measuring 5 x 5 x 3 mm thick, was
made in acrylic resin (Jet Clássicoj), using two glass slides as a
mold, with utility wax interposed to limit the distance to 3 mm.
The block was cut and finished with oxide-aluminum abrasive
disks (Sof Lexg) and its measurements gauged with a digital
caliper.k
The acrylic pattern was placed in a mold formed by a utility
wax platel with a central rectangular cut-out, and fitted to a
glass slide at the base, forming a cavity. The acrylic pattern was
centralized in this niche, in order to standardize the thickness at
3 mm, and was filled with addition silicone (Flexitime Correct
Flowb) with its own applicator, and the surface was compressed
with another glass slide. After polymerization, the excess was
cut away and the acrylic pattern removed, obtaining two
addition silicone molds that were randomly used.
The blocks of resin for indirect use, Adoro shade A3
Dentin/Body and ArtGlass shade DA3 were made in accor-
dance with the manufacturers’ instructions. Twenty blocks of
each commercial brand used were made, using the silicone
matrix with internal dimensions of 5 x 5 x 3 mm thickness,
American Journal of Dentistry, Vol. 21, No. 3, June, 2008
Indirect composite silanization 155
Table 1. Materials, shades, manufacturers, and compositions of the main
products used in this study.
Materials Shade Composition

Scotchbond Etchant --- 35% (wt) phosphoric acid gel (pH=0.6)

Adper --- Bisphenol-A-diglycidylether dimethacrylate
Single-Bond 2 (Bis-GMA), HEMA, dimethacrylates, poly-
alchenoic copolymers, ethanol and water
Adoro A3 82% (wt) silicone dioxide, dimethacrylates
Dentin body and copolymers
ArtGlass DA3 80% (wt) barium-aluminum-silicone glass,
dimethacrylates and multifunctional
methacrylates
RelyX --- 20-30% aqueous solution, 70-80% ethyl
Ceramic Primer alcohol
RelyX ARC Universal A3 Bisphenol-A-diglycidylether dimethacrylate
(Bis-GMA), triethylene glycol dimethacrylate
(TEGDMA) polymer, 65% (wt)
zirconia/sílica filler, amine, photoinitiator
system, benzoyl peroxide

inserting two layers in increments of 1.5 mm, light poly-

merizing each layer for 5 seconds with a Targis Quicka appli-
ance. Additional polymerization (macropolymerization by
continuous halogen lamp at a temperature of 98°C for 25
minutes) was performed in a Targisa power autoclave for
photothermal treatment. After the test specimens were pre-
pared, a caliper was used to measure their dimensions.
Only one of the surfaces of the blocks was selected for
cementation and it was made uniform with a metallographic
grinder (Politriz Aropol 2V) for 5 seconds with aluminum
oxide abrasive paper with a 600 grit. Mechanical surface
treatment was performed by applying 50 μm aluminum oxide
air abrasion (Bio-art micro etcher systemm) for 5 seconds, at a
distance of 1 cm, in a circular manner, at a pressure of 80 psi.
Next, 37% phosphoric acid was applied for 15 seconds,
followed by washing with water for 15 seconds and drying with
an air jet for 5 seconds.
Of the 20 blocks of each commercial brand, 10 were ran-
domly selected to receive the silane treatment (RelyX Ceramic
Primerg), this being applied for 10 seconds with the Cavibrush
disposable applicator and dried with air jets for 5 seconds. Two
layers of the adhesive Adper Single Bond 2 were applied, dried
with a brief air jet and light polymerized for 10 seconds.
The dual RelyX ARCg cement, shade Universal A3 was
applied to the composite block surface and placed on the
occlusal face, aligning it with digital pressure (Fig. 1C). The
surplus cement was gently removed with the Cavibrush
disposable applicator and light polymerized with halogen light
perpendicular to the surface for 20 seconds. Next, the sides of
each block were light polymerized at an angle of 45° for 20
seconds for each application. The light polymerizer power
(Ultralux) was checked with a radiometern after each test
specimen, presenting a minimum value of 380 mW/cm2. The
mean obtained was 420 mW/cm2. The test specimens were
stored in artificial saliva at 37°C for 6 days.
The indirect resins, adhesive system, cementing agent and
silane used in this study and their respective shades and
compositions are presented in Table 1.
Supports measuring 2.5 x 2.5 x 0.5 cm were made for
fixation to a metallographic cutter, using colorless acrylic resin
(Jet Clássico). To obtain the test specimens, a cutting machine
Fig, 2. A. Detail of central acrylic device. B. Bonding the stick to the device. C.
General scheme of the test with the base fixed to the table, with the central
device in position and the load cell adapted to the universal test machine, with
traction until rupture of the cementation.
(Isomet 1000o) was used, with a speed of 300 rpm and weight
of 150 g, with 1.2 mm thickness interval. The cuts were always
made vertically, starting from the restoration in an apical direc-
tion (Fig. 1C). Four parallel cuts were obtained in the vestibu-
lar-lingual direction and four in the mesio distal direction. The
most external slices were ignored due to the interference that
could be caused by the excess cement (Fig. 1D).
Nine possible sticks were obtained by the non-trimming
technique.18 Of these, three were randomly selected, since they
have to present a minimum dentin thickness of 2 mm to
standardize the substrate used for the tests (Fig. 1E).
For the microtensile test, a universal test machinep was
used, coupled to a load cell with a maximum capacity of 20 kgf
and adapted to a specific acrylic deviceq (Fig. 2A). The
cementation area was measured with a digital caliper.k The
cross-sectional area of the sticks was approximately 1.00 mm2
(± 0.12 mm2) and the value for each stick before testing was
adjusted at the universal testing machine to obtain significant
strength determinations.
The sticks were fixed to the device with cyanoacrylate
adhesive (Superbonder Gelr) taking care to align the cementa-tion
line with the dividing line of the appliance, and acrylic resin
monomer (Jet Clássico) was applied with the Cavibrush
disposable applicator, to hasten the gel setting reaction (Fig. 2B).
 American Journal of Dentistry, Vol. 21, No. 3, June, 2008
156 Honda et al

Table 2. Mean and standard deviation in MPa of the study groups.

Adoro
_________________________
ArtGlass
_____________________________

Mean S.D. Mean S.D.

Without silane 37.1 (Ba) 11.7 58.1 (Aa) 14.4

With silane 39.5 (Ba) 12.3 49.8 (Aa) 12.0
Means followed by different letters within parentheses (capitals in the horizontal
and lower case in the vertical) differ among them by ANOVA (P< 0.05).

Table 3. Results of the fracture type analysis in each stick, in accordance with
the different study groups.

Study groups
_____________________________________________________________________

Adoro ArtGlass
Adoro ArtGlass + silane + silane
_____________ _____________ ____________ ____________
Fracture
type n % n % n % n % P
Adhesive 19 63.3 24 80.0 19 63.3 20 66.7 3.9353
Mixed 9 30.0 4 13.3 10 33.3 8 26.7 0.69
Cohesive 2 6.7 2 6.7 1 3.3 2 6.7 Fig. 3. Fracture type classification.

greater polymeric conversion, and could result in increased

The standardized speed for the microtensile test in the test
machine was 0.5 mm/minute until failure, obtaining the
maximum value of force in kgf (Fig. 2C).
A visual analysis was made under loupes with x25
magnifications to classify the type of fracture: cohesive (when
the fracture line occurred completely in the dentin or resin
cement body); adhesive (when there was failure in the adhesive
system); or mixed (when part of the fracture line occurred in
dentin and part in resin cement) (Fig. 3).
The mean value of the three sticks was obtained,
corresponding to each tooth used, and the results obtained in
kgf were converted to MPa.
After exploratory analysis of the data, ANOVA in the two-
way factorial scheme was applied. The associations between
the fracture types and the study groups were afterwards
submitted to the Chi-square test, using the Bioestat 4.0t
statistical program. Those that presented P values (probability
of error type I)  0.05 in bicaudal distribution were considered
statistically significant associations.
Results
The general mean and standard deviation of each study
group are presented in Table 2.
The laboratory resin Adoro obtained a significantly lower
mean resistance than ArtGlass (P 0.05) with or without the
use of silane. The use of silane did not significantly increase
the microtensile strength for the indirect resins Adoro and
ArtGlass.
Data analysis with reference to fracture mode for each study
group is presented in Table 3.
There were predominantly adhesive fractures, followed by
mixed and cohesive fractures, and there was no significant
correlation between the type of fracture and resin brand, and
whether or not silane was used.
Discussion
The laboratory resins or those for indirect use generally
present polymerization methods that include continuous or
stroboscopic light polymerization, the controlled use of heat
and/or pressure or nitrogen atmosphere, with the purpose of
mechanical resistance of the composite. The high conversion of
polymers, on the other hand, diminishes the chances of
chemical bonding, mainly of the organic phase, which could
help to obtain stable and lasting cementation, although small
sites with non-reagent residual monomers always remain,
which could be potential radicals for covalent links with the
adhesive applied for cementation.20
Several types of surface treatment have been tested, in an
effort to enhance micro-mechanical and/or chemical retention,
such as aluminum oxide (50 μm) airborne particle abrasion, the
use of a diamond tip to roughen the internal surface, the use of
CoJetg (silanization by airborne particle abrasion in which the
silicone particles are deposited internally on the part to be
cemented), the use of PyrosilPenu (which is silanization with
the aid of butane gas burning),10 performing acid etching with
various types and concentrations of products.21,22
Micro-mechanical retentions are, however, fundamental and
are the main sources of bond strength. Their importance is
evidenced in laboratory studies that have shown the use of
aluminum oxide airborne particle abrasion to be more advanta-
geous, as the composite surface presents greater uniformity
after it has been applied.23-25 There is, however, concern that the
pressure of airborne particle abrasion may result in creating
surface roughness on the prosthetic part. This may cause hol-
lows not filled by the adhesive to form, and lead to diminished
bond strength, particularly when no silane was previously
applied, thus evidencing the importance of applying it.26 On the
other hand, silane may diminish the bond strength in the surface
treatment, if an adhesive is not used before applying the resin
cement, indicating the importance of using the adhesive/resin
cement combination after the silanization stage.27,28
Chemical retention is therefore an important focus of
research through the use of silanes, in an attempt to link with
the inorganic content of the composite at the one end, and
copolymerization with resin cementing material at the other
end. Because it is a bifunctional molecule, silane incorporation
is a process used in the development of resin composites,29-31
and it is present in the initial formulation of Bowen’s resin
composite,32 as well as in the bond with other substrates, such
as metals.33
American Journal of Dentistry, Vol. 21, No. 3, June, 2008
Silanization plays a recognized role, and is recommended as
a general protocol for cementing and repairing ceramic
materials, providing improved and higher bond strength
values.34 The results of silane use in laboratory composite
cementations have, however, pointed out divergences, and
although they have not shown a statistically significant
difference in microtensile strength, the results have nevertheless
been favorable.2,7,26,35,36 Another author6 has proven its superior
effect in comparison with mechanical treatment, since silane
acts by increasing the wettability of the composite and
improving adhesive strength.
In the present study, the technique of fabricating the test
specimens in the form of sticks18 and using dentin as substrate,
were chosen for the microtensile test. Although contraindicated
by Ferrari et al,37 this methodology did not appear to interfere
with the results, as occurs in the case of enamel.
No significant difference between the results of silane used
in the two resins was shown, corroborating the results of
Bouschlicher et al34 and also those found in direct or indirect
resin repairs by Gregory et al.20 Over 68% of the fractures were
considered adhesive, being in agreement with the results of
other authors that obtained a majority of adhesive fractures.13,16
The smaller area used in microtraction results in higher
microtensile strength values. Thus, values of around 37 to 58
MPa, as obtained on an average in this study, may be attributed
to the greater uniformity, with a lower number of failures at the
adhesive interface.13,18
It was observed that the laboratory resins presented statis-
tically different microtensile strength values in cementation.
The microtensile strength was significantly higher for ArtGlass,
showing that the composition of the composite and the degree
of conversion monomers may have influenced on the adhesive
procedure. Furthermore, during light activation of cementation,
light penetration through materials may be different due to the
inorganic and organic content of the two materials, resulting in
differences in the cement polymeric conversion, and conse-
quently, in the microtensile values. Therefore, in spite of the
similarity in the general composition of current polymers, the
microtensile strength values may be related to the type of
organic or inorganic content, or even a combination of them,
which interacts with the adhesive and cement. The two resins
tested are considered microparticulated resins, and according to
the manufacturer, the basic composition of Artglass consists of
80% by weight of barium-aluminum-silicone and the organic
part contains multifunctional dimethacrylates and methacryl-
ates. Adoro contains 82% by weight of silicone dioxide and the
organic part consists of dimethacrylates and copolymers. The
adhesive used (Adper Single Bond II) makes the intercom-
nection between the materials, and according to the manufac-
turer, contains Bis-GMA, HEMA, dimethacrylates, polyalche-
noic copolymers, ethanol and water. The silane (RelyX
Ceramic Primer) is pre-hydrolyzed and is based on a 20-30%
aqueous solution and 70-80% ethyl alcohol, and has the
property of creating chemical links between the organic and
inorganic parts of the polymer. This chemical link in polymer
cementations may be more related to resistance to micro-
leakage, particularly because of the dynamism of the silane
reaction and its hydrolytic resistance, than to its adhesive
strength, and therefore, not easy to measure. Factors such as
Indirect composite silanization 157
application time, drying temperature, type of solvent and pH of
the silane agent solution may also alter the values obtained.38
In spite of being difficult to understand, the interaction of
the formulations and mechanical or chemical surface treat-
ments, shows that there is specificity in the use of the various
types of polymeric materials and resin cement systems.39 The
constant search for and development of indirect polymeric
materials does not yet allow long term clinical follow-ups that
could answer important questions, such as those concerning
microleakage and adhesive strength in relation to the time of
clinical use. Faster progress in the field of research would
ideally be vital to having a better understanding of the optimal
type of cementation for every type of laboratory resin.
a. Ivoclar/Vivadent, Schaan, Liechtenstein.
b. Heraeus/Kulzer, Hanau, Germany.
c. KG Sorensen, Barueri, São Paulo, Brazil.
d. Dentsply Latin America, Petrópolis, Rio de Janeiro, Brazil.
e. Arotec, Cotia, São Paulo, Brazil.
f. Norton, São Paulo, São Paulo, Brazil.
g. 3M ESPE, St. Paul, MN, USA.
h. FGM, Joinville, Santa Catarina, Brazil.
i. Dabi Atlante, Ribeirão Preto, São Paulo, Brazil.
j. Artigos Odontológicos Clássico Ltd, São Paulo, Brazil.
k. Mitutoyo, Osaka, Japan.
l. Polidental, São Paulo, São Paulo, Brazil.
m. Bio-art, São Carlos, São Paulo, Brazil.
n. Newdent Equipamentos, Ribeirão Preto, São Paulo, Brazil.
o. Buehler, Lake Bluff, IL, USA.
p. EMIC, São José dos Pinhais, São Paulo, Brazil.
q. Erios, São Paulo, São Paulo, Brazil.
r. Loctite, Itapevi, São Paulo, Brazil.
s. Blue Equipamentos, São José do Rio Preto, São Paulo, Brazil.
t. Mamirauá Maintainable Development Institute, Belém, Pará, Brazil.
u. Sura Instruments, Jena, Germany.
Acknowledgement: To Prof. Dr. Marcelo Giannini, from the Restorative
Dentistry laboratory of the Faculty of Dentistry of Piracicaba–UNICAMP, for
guidance and use of the cutting equipment essential to the test.
Dr. Honda is a Master of Science student in Restorative Dentistry; Dr. Flório
and Dr. Basting are Professors, Dental School and Dental Research Center São
Leopoldo Mandic, Campinas, São Paulo, Brazil.
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