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Microleakage of ceramic inlays luted

with different resin cements and dentin


adhesives
Bulent Uludag, DDS, PhD,a Ozge Ozturk, DDS, PhD,b and
A. Nilgun Ozturk, DDS, PhDc
Faculty of Dentistry, University of Ankara, Ankara, Turkey; Faculty
of Dentistry, University of Selcuk, Konya, Turkey
Statement of problem. Despite recent advances in adhesive dentistry, resin cement/dentin adhesive combinations
are not able to prevent microleakage in ceramic inlays. Marginal quality of tooth-colored restorations in large Class II
cavities is satisfactory in enamel margins, but microleakage in dentin margins remains a concern.

Purpose. The purpose of this study was to evaluate the microleakage of all-ceramic inlays luted with 2 dual-polymeriz-
ing resin cements or 1 autopolymerizing resin cement in combination with different dentin adhesives.

Material and methods. One hundred and twenty extracted human mandibular third molars were used in this study.
Teeth were prepared to receive Class II MOD inlays with enamel gingival margins on 1 proximal surface and dentin
gingival margins on the other surface. One hundred and twenty prepared teeth were divided into 3 groups of 40; 1
group for each resin cement: RelyX ARC, Variolink II, or Panavia 21. Each of the 3 groups were further divided into 4
dentin adhesive groups; Single Bond, ExciTE DSC, ED Primer, or Admira Bond. Each of the resin cements were used in
combination with the 4 dentin adhesives, and IPS Empress ceramic inlays were placed with 12 different cement/adhe-
sive combinations. After 1000 thermal cycles in a 5°-55°C water bath with a dwell time of 30 seconds, all specimens
were subjected to cyclic axial mechanical loading. Then the restored teeth were stored in 0.5% basic fuchsin solution
for 24 hours. The extent of dye penetration along the margins was measured with a stereomicroscope at x40 magnifi-
cation. The data were evaluated statistically using repeated-measures ANOVA and Duncan tests (α=.05).

Results. Microleakage at dentin margins was greater than that at enamel margins (P<.05) for all groups. Variolink II
and RelyX ARC resin cements showed significantly lower microleakage results than Panavia 21 with all dentin adhe-
sives in enamel margins. For dentin margins, Variolink II/Admira Bond combination showed the lowest microleakage
value in dentin (P<.05).

Conclusions. The overall microleakage at the enamel margins was significantly less than at the dentin margins (P<.05).
Panavia 21 showed higher microleakage values than Variolink II and RelyX ARC in enamel margins. (J Prosthet Dent
2009;102:235-241)

Clinical Implications
The results of this study suggest that there are no significant dif-
ferences in microleakage at dentin margins between dual-polym-
erizing resin cements and autopolymerizing resin cements with
the different cement/adhesive combinations evaluated.

Efficient adhesion between cav- nificant cause of pulpal inflamma- Microleakage at the enamel-resto-
ity walls and restorative materials is tion, pulp necrosis,3-7 and secondary ration interface has been minimized
important for long-lasting restora- caries4-8 in restored teeth. The signs since the introduction of acid etch-
tions.1,2 Microleakage of cariogenic of microleakage include immediate ing by Buonocore in 1955,12 but seal-
bacteria along the cavity walls of postoperative sensitivity, chronic sen- ing dentin margins remains a chal-
restorations is reported to be a sig- sitivity, and marginal discoloration.9-11 lenge.2,7,13,14

a
Professor, Department of Prosthodontics, University of Ankara, Faculty of Dentistry.
b
Private practice, Istanbul, Turkey.
c
Associate Professor, Department of Prosthodontics, University of Selcuk, Faculty of Dentistry.
Uludug et al
236 Volume 102 Issue 4
Composite resin restorative ma- between the tooth structure and the stored in 0.5% thymol (Merck KGaA,
terials undergo significant volumetric restoration.38 Darmstadt, Germany) at room tem-
shrinkage when polymerized. It has There are 2 types of tooth sur- perature from the day of extraction.
been suggested that this property re- face treatments. The total-etch tech- The teeth were cleaned using scalers
sults in poor margin quality in com- nique involves conditioning enamel and rotating brushes to completely
posite resin restorations.1 Different and dentin with phosphoric acid in remove soft tissue remnants. Teeth
composite resin restorative systems a single step. To avoid overetching were embedded up to 2 mm apical to
and techniques have been developed, the dentin, the phosphoric acid gel is the cemento-enamel junction in auto-
and direct composite resin placement usually applied first to the enamel polymerizing resin (Palavit G; Heraeus
is one of these techniques.15 However, margins and then to the dentin sur- Kulzer GmbH, Wehrheim, Germany).
clinicians have difficulty establish- face.39 Self-etching adhesives, how- The teeth were prepared for Class
ing proper anatomic form, proximal ever, contain acidic monomers which II MOD inlays. All preparations were
contour, and contact in large, direct are copolymerized with adhesive made according to the following cri-
placement composite resin restora- monomers after surface condition- teria using inlay diamond rotary cut-
tions. Indirect inlay systems have been ing.39-41 An intrinsic problem of self- ting instruments (Inlay Prep Kit 4261;
developed to overcome this limitation etching systems is the acid-base re- Komet Dental, London, UK): 10 de-
of direct placement restorations.16 action of the acidic monomers with grees of axial wall convergence; flat
One of the advantages attrib- the amines used in the initiator sys- floor; 3-mm depth and 4-mm width
uted to the ceramic inlay technique tems,39,42,43 such as the camphorqui- of the isthmus; 1 proximal box lim-
is a thermal expansion coefficient of none/amine system in light-polymer- ited to enamel (1 mm coronal to the
the ceramic which is similar to that izing adhesives. cemento-enamel junction), and the
of the tooth hard substance, as well Many techniques involving dyes other extending 1 mm apical to the
as the reduced volume of shrinking have been used to assess microleak- cemento-enamel junction. Impres-
composite resin (limited to the luting age both in vivo and in vitro. Dye pen- sions were then made with polyether
resins), both of which are known to etration is a technique to determine impression material (Impregum F;
have positive effects on marginal ad- the loss of adhesion. Other methods, 3M ESPE, Seefeld, Germany) of all
aptation.17-20 such as the silver nitrate staining tech- specimens, and refractory dies were
Clinical success with ceramic in- nique, or penetration of radioactive prepared (Cergo Fit; Dentsply Degu-
lays/onlays has been assisted by the substances, are not commonly used Dent GmbH, Hanau, Germany).
development of a reliable bond be- because they are time-consuming To fabricate the IPS Empress in-
tween composite resin and dental tis- and the handling of these materials lays, restoration patterns were waxed
sues.21,22 Generally, an adhesive resin is difficult.44 Digital image analysis (Yeti Dentalprodukte GmbH, Engen,
cement is recommended for luting allows quantitative measurement of Germany), sprued, and invested
ceramic inlays,23 particularly because the length of dye penetration. This with refractory material (AlphaDie
of the excellent esthetic and mechani- method can assess the condition and MF; Schütz-Dental GmbH, Rosbach,
cal properties (flexural strength, com- amount of microleakage of restora- Germany). The paper ring and sprue
pressive strength) of adhesive resin tions more accurately than the tradi- former were removed after 1 hour.
cements.20,24,25 Light-polymerized, du- tional scoring system that made mi- The molds were then transferred to
al-polymerized, and autopolymerized croleakage studies more subjective.45 a burn-out furnace (Vulcan 3-550,
luting composite resins have all been The purpose of this study was to Dentsply Ceramco, York, Pa), heated
used with ceramic inlays.26-28 Etched evaluate the microleakage of all-ce- from room temperature to 250°C at
enamel12 provides an ideal surface ramic inlays luted with 2 dual-polym- a rate of 5°C/min, held at 250°C for
for reliable bonding performance us- erizing resin cements and 1 autopoly- 30 minutes, then further heated from
ing adhesive resins.29,30 Success with merizing resin cement in combination 250° to 850°C at a rate of 5°C/min,
bonding to dentin, however, has been with different dentin adhesives. The and finally held at 850°C for 60 min-
less reliable due to the unique char- null hypothesis was that the adhesive/ utes. After completion of the heating
acteristics of the dentin substrates, cement combinations have no effect cycles, the investment ring was imme-
including high organic content, tubu- on microleakage. diately removed from the heating fur-
lar structure variations, and the pres- nace, and the cold ingot was placed in
ence of outward fluid movement.31-37 MATERIAL AND METHODS the investment ring. The investment
In an attempt to improve the bond ring with the ingot and the alumina
between dentin and composite resin, One hundred and twenty extract- plunger were transferred to the 700°C
a number of dentin adhesives have ed caries- and restoration-free hu- preheated pressing furnace (EP 600;
been introduced. These react to form man mandibular third molars were Ivoclar Vivadent, Schaan, Lichten-
chemical or micromechanical bonds used in this study. The teeth were stein). For the IPS Empress ceramics,
The Journal of Prosthetic Dentistry Uludug et al
October 2009 237
the furnace was heated from 700° to etched with 9.6% hydrofluoric acid the cavity surface, gently air dried for
1180°C. The ingot was subjected to (Porcelain Etch Gel; Pulpdent Corp, 5 seconds, and polymerized for 10
a plunger pressure of 5 bar, as recom- Watertown, Mass) for 2 minutes. For seconds with the light-polymerizing
mended by the manufacturer. After Panavia 21 resin cement, a layer of a unit (Hilux 200 Light Curing Unit;
pressing, the ceramic inlays were di- silane coupling agent mixture (Clearfil Benlioglu Dental, Ankara, Turkey).
vested, finished with diamond rotary Porcelain Bond Activator and Clearfil RelyX ARC was mixed for 10 sec-
cutting instruments (ND.0136.006; SE Bond Primer; Kuraray Co Ltd, Osa- onds and applied to both prepared
Komet Gebr Brasseler GmbH, Lemgo, ka, Japan) was applied to the ceramic teeth and the bonding surface of the
Germany), and glazed. bonding (intaglio) surfaces for 5 sec- ceramic restorations. A static load (1
One hundred and twenty prepared onds, then air dried. For Variolink II kg) was used to stabilize the inlays
teeth were divided into 3 groups of and RelyX ARC, a layer of silane cou- during the bonding procedure. Ex-
40, 1 group for each of 3 resin ce- pling agent (Silane Bond Enhancer; cessive cement was removed with an
ments: RelyX ARC, Variolink II, and Pulpdent Corp) was applied to the ce- explorer, and the cement was polym-
Panavia 21. Each of the 3 groups was ramic bonding surfaces for 1 minute, erized for 40 seconds with the light-
further divided into 4 dentin adhesive then air dried. polymerizing unit at 350 mW/cm2
groups: Single Bond, ExciTE DSC, ED For the RelyX/Single Bond group, with a light tip-to-specimen distance
Primer, and Admira Bond. Each of the 35% phosphoric acid gel (Scotchbond of 2 mm.
resin cements was used in combina- Etchant; 3M EPSE, St. Paul, Minn) For the RelyX/ExciTE DSC group,
tion with the 4 dentin adhesives. The was applied to the enamel surface for 35% phosphoric acid gel (Scotch-
resin cements and dentin adhesives 30 seconds and the dentin surface for bond Etchant; 3M ESPE) was applied
used in this study are described in 15 seconds, water rinsed for 10 sec- to the enamel surface for 30 seconds
Table I. onds, and then gently air dried for 5 and the dentin surface for 15 sec-
All of the ceramic inlays were seconds. Single Bond was applied to onds, water rinsed for 10 seconds,

Table I. Resin cements and dentin adhesives used in this study


Resin Batch
Cement Manufacturer Number Composition

RelyX ARC 3M ESPE, St. Paul, Minn 20050524 Bis-GMA, TEGDMA, silica-zirconia glass

Variolink II Ivoclar Vivadent, G13371 Bis-GMA, UDMA, TEGDMA silicon dioxide,


Schaan, Liechtenstein autopolymerizing initiators, light-polymerizing
initiators, stabilizer, pigments

Panavia 21 Kuraray Co Ltd, 41235 Bis-GMA, MDP, quartz, benzoyl peroxide, initiators,
Osaka, Japan phosphate, monomer, amine, sulfine, stabilizer

Dentin Batch
Adhesive Manufacturer Number Composition

Single Bond 3M ESPE 7MH Bis-GMA, polyalkenoic acid co-polymer, dimethacrylate,


HEMA, photoinitiators, ethanol, water

ExciTE DSC Ivoclar Vivadent G11590 HEMA, dimethacrylate, phosphonic acid acrylate,
silicon dioxide, initiators, stabilizer, alcohol

ED Primer Kuraray Co Ltd 41154 HEMA, 5-MASA, MDP, water, catalyst

Admira Bond VOCO GmbH, 779921 Ormocer (organically modifed ceramic), bis-GMA,
Cuxhaven, Germany HEMA, organic acid, acetone

Bis-GMA: bisphenol-A glycidyl dimethacrylate; TEGDMA: tetraethyleneglycol dimethacrylate; UDMA: urethane dimethacrylate;
MDP: 10-methacryloyloxy-decyl dihydrogen phosphate; HEMA: 2-hydroxyethyl methacrylate; 5-MASA: methacryloyl-5-aminosalicylic acid

Uludug et al
238 Volume 102 Issue 4
and gently air dried for 5 seconds. 5°and 55°C using a dwell time of scope (Carl Zeiss AG, Oberkochen,
ExciTE DSC was applied to the cavity 30 seconds. All specimens were sub- Germany), and the data were trans-
surface, gently air dried for 3 seconds, jected to cyclic axial mechanical load- ferred to a personal computer. For
and polymerized for 10 seconds with ing (100,000 cycles, 1.6 Hz, constant each specimen, staining along the
the light-polymerizing unit. RelyX occlusal load of 50 N) using a 5-mm cavity walls was measured using im-
ARC was applied in the same man- steel ball. Specimens were coated with age analysis software (KS 400 Image
ner. For the RelyX/ED Primer group, nail polish (Del Laboratories, Inc, for Windows; Carl Zeiss AG) and the
ED Primer was applied to the cavity Uniondale, NY) 1 mm short of the percentage of dye penetration was
surface for 60 seconds and gently air restoration margins and immersed calculated in relation to the entire
dried. RelyX ARC was applied as pre- in 0.5% basic fuchsin dye (SPI Sup- cavity length. The differences in the
viously described. plies Division, Structure Probe, Inc, amount of dye penetration along the
For the RelyX/Admira Bond group, West Chester, Pa) for 24 hours. Fol- cavity walls were evaluated statistical-
35% phosphoric acid gel (Scotchbond lowing removal from the solution, the ly using repeated-measures analysis of
Etchant; 3M ESPE) was applied to the teeth were rinsed under tap water and variance (ANOVA) and Duncan tests
enamel surface for 30 seconds and embedded in autopolymerizing orth- (α=.05).
the dentin surface for 15 seconds, wa- odontic acrylic resin (Orthocryl EQ;
ter rinsed for 10 seconds, and gently Dentaurum, Ispringen, Germany). RESULTS
air dried for 5 seconds. Admira Bond Each tooth was vertically sectioned
was applied to the cavity surface for twice mesial-distally, through the Table II illustrates the mean per-
30 seconds, gently air dried, and po- restorations along the long axis, into centage and SD for the microleakage
lymerized for 10 seconds with the 0.5-mm-wide sections, with a water- results obtained with the 2 resin ce-
light-polymerizing unit. RelyX ARC cooled diamond disc (Mikrocut; Met- ments in combination with the 4 den-
was applied. Variolink II and Panavia kom, Bursa, Turkey). Four specimens tin adhesives. The results of repeated-
21 resin cements were used in combi- (0.5 x 10 x 15 mm) were made from measures ANOVA are summarized in
nation with the 4 dentin adhesives in each tooth. Table III and indicate that microleak-
the same manner. For each specimen, dye penetra- age values vary according to the resin
After 24 hours of storage in wa- tion along the cavity walls in dentin cements and dentin adhesives (P<.05)
ter at 37°C, all teeth were subjected and enamel on each of the 4 sec- used. There were significant differ-
to 1000 thermal cycles (Thermal Cy- tioned surfaces was digitally photo- ences in microleakage between the
cle; Nüve, Ankara, Turkey) between graphed at x40 under a stereomicro- enamel and dentin margins (P<.05).

Table II. Percent mean values and SD for microleakage (n=10)


Enamel Dentin

Variolink II RelyX ARC Panavia 21 Variolink II RelyX ARC Panavia 21

Mean SD Mean SD Mean SD Mean SD Mean SD Mean SD

ExciTE Ab Aa βb Aβ a βa Aa
β0.58 0.81 Aβ1.38 1.95 A2.69 2.77 β2.21 1.57 β2.91 2.45 A9.08 2.29
DSC

Single Ab Ab Ab Aa Aβ a Aa
β0.56 1.1 β0.23 0.32 A5.58 2.87 β3.52 2.21 β3.53 2.97 A10.93 2.50
Bond

ED Aa Ab Aβ a Aβ a Aa βa
β1.01 1.22 β0.54 0.90 A3.99 2.76 A1.90 1.98 A5.00 3.59 A5.44 2.83
Primer

Admira Aa Ab Aβ b βa Aβ a βa
β0.75 1.22 β1.39 1.59 A3.81 1.63 β0.93 1.28 A4.74 2.70 A6.66 1.73
Bond

Superscripted lowercase letters (a, b) indicate differences in cement/bonding agent combination (with respect to orientation);
right superscript characters (A, Aβ, and β) indicate differences in orientation/cement combination (with respect to bonding agent);
left subscript characters (β, Aβ, and A) indicate differences in orientation/bonding agent combination (with respect to cement).
Same characters on same sides (left or right) of values indicate no significant difference in results (P<.05).

The Journal of Prosthetic Dentistry Uludug et al


October 2009 239

Table III. Results of repeated-measures ANOVA


Sum of Mean
Source Squares Square df F P

Between Groups

Cement 928.0 464.0 2 77.9 <.001

Bonding agent 46.0 15.3 3 2.57 .050

Cement x bonding agent 132.8 22.1 6 3.72 .002

Within groups

Orientation 491.0 491.0 1 138.1 <.001

Orientation x cement 69.9 35.0 2 9.83 <.001

Orientation x bonding agent 30.1 10.0 3 2.82 .042

Orientation x cement x bonding agent 89.5 15.0 6 4.19 <.001

Microleakage at the dentin mar- strated a good seal, in contrast to the croleakage results with all dentin ad-
gins was greater than that at the dentin margins, because the smallest hesives in enamel margins. Panavia 21
enamel margins (P<.05) for all groups. degree of microleakage was observed combined with the self-etching adhe-
Variolink II and RelyX ARC resin ce- in enamel. It is also known that the sive, ED Primer, showed significantly
ments showed the lowest microleak- composition and other special char- higher microleakage values than
age results with all dentin adhesives in acteristics of luting agents, such as Variolink II and RelyX ARC in enamel
enamel margins. Panavia 21 showed the setting properties and the dentin margins. This can be explained by the
higher microleakage values than adhesives used, determine the degree 2 different enamel bonding mecha-
Variolink II and RelyX ARC. The low- of leakage.7 Universal dentin adhe- nisms of the total-etch and the self-
est microleakage value was obtained sives have been recommended for etching techniques. The slow polym-
with RelyX/Single Bond in enamel for bonding porcelain, composite resin, erization rate of Panavia 21 may allow
all resin cements (P<.05). With den- and alloy to both dentin and enamel. more water to diffuse from the vital
tin margins, there were no significant One reported benefit of these agents dentin into the hydrophilic interface
differences between RelyX ARC and is the ability to seal dentin, which re- between the Panavia 21 primer and
Variolink II combinations with Single sults in a reduction of interfacial mi- dentin, due to its more hydrophibic
Bond and ExciTE DSC dentin adhe- croleakage and pulpal sensitivity.29,30 nature.39,41 The 2 phases seem to
sives. However, the Variolink II/Ad- For all-ceramic inlays, microleakage weaken the interface.
mira Bond combination showed the is an important consideration for pre- With dentin margins, there were
lowest microleakage value in dentin serving the marginal seal due to less no significant differences between
(P<.05). Panavia 21 combined with than ideal marginal adaptation of the dual-polymerizing resin cements and
ED Primer showed the lowest micro- porcelain material.29 the autopolymerizing resin cement. In
leakage compared to the other Pana- The total-etch technique involves a recent study in which ceramic inlays
via 21/dentin adhesive combinations. conditioning enamel and dentin with cemented with a dual-polymerized or
phosphoric acid in a single step. Self- autopolymerized composite resin lut-
DISCUSSION etching adhesives, however, contain ing agent were clinically evaluated,
acidic monomers which are copo- Sjögren et al28 reported no signifi-
With regard to the influence of lymerized with adhesive monomers cant differences between the 2 luting
the adhesive/cement combinations after surface conditioning.39,40 There- agents. These findings were confirmed
on the dentin margins, the results of fore, self-etching cementation sys- by van Dijken et al,27 who investigated
this study do not support rejection tems require no rinsing step and are the use of a dual-polymerized and an
of the null hypothesis. This study is therefore generally less technique autopolymerized composite resin lut-
in agreement with other studies35-37 sensitive.40 Variolink II and RelyX ARC ing agent in restorations with exten-
in which enamel margins demon- resin cements showed the lowest mi- sive dentin/enamel-bonded ceramic
Uludug et al
240 Volume 102 Issue 4
coverage. An in vitro study of micro- 1. Microleakage at enamel mar- 16.Soares CJ, Martins LR, Fernandes Neto AJ,
Giannini M. Marginal adaptation of indi-
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margins for Variolink II/Excite and 2. The autopolymerizing resin ce- 17.Bott B, Hannig M. Optimizing class II com-
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were no significant differences be- higher microleakage values than Vari- 7.
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Noteworthy Abstracts of the Current Literature


Marginal and internal fits of fixed dental prostheses zirconia retainers

Beuer F, Aggstaller H, Edelhoff D, Gernet W, Sorensen J.


Dent Mater 2009;25:94-102. Epub 2008 Jul 11.

Objectives: CAM (computer-aided manufacturing) and CAD (computer-aided design)/CAM systems facilitate the use
of zirconia substructure materials for all-ceramic fixed partial dentures. This in vitro study compared the precision of
fit of frameworks milled from semi-sintered zirconia blocks that were designed and machined with two CAD/CAM and
one CAM system.

Methods: Three-unit posterior fixed dental prostheses (FDP) (n=10) were fabricated for standardized dies by: a mill-
ing center CAD/CAM system (Etkon), a laboratory CAD/CAM system (Cerec InLab), and a laboratory CAM system
(Cercon). After adaptation by a dental technician, the FDP were cemented on definitive dies, embedded and sec-
tioned. The marginal and internal fits were measured under an optical microscope at 50x magnification. A one-way
analysis of variance (ANOVA) was used to compare data (α=0.05).

Results: The mean (S.D.) for the marginal fit and internal fit adaptation were: 29.1 μm (14.0) and 62.7 μm (18.9)
for the milling center system, 56.6 μm (19.6) and 73.5 μm (20.6) for the laboratory CAD/CAM system, and 81.4 μm
(20.3) and 119.2 μm (37.5) for the laboratory CAM system. One-way ANOVA showed significant differences between
systems for marginal fit (P<0.001) and internal fit (P<0.001).

Significance: All systems showed marginal gaps below 120 μm and were therefore considered clinically acceptable.
The CAD/CAM systems were more precise than the CAM system.

Reprinted with permission of the Academy of Dental Materials.

Uludug et al

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