d e n t a l m a t e r i a l s x x x ( 2 0 0 6 ) xxx–xxx

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Microleakage of porcelain veneer restorations bonded toenamel and dentin with a new self-adhesive resin-baseddental cement

Gabriela Ibarraa,∗, Glen H. Johnsona, Werner Geurtsena, Marcos A. Vargasb

a School of Dentistry, Department of Restorative Dentistry, University of Washington, Seattle, WA, USAb College of Dentistry, Department of Operative Dentistry, University of Iowa, Iowa City, USA

a r t i c l e i n f o

Article history:

Received 29 September 2005

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a b s t r a c t

Cementation technique of bonded ceramic restorations is a time-consuming and technique-

sensitive procedure critical to long-term success.

1

Ti

W

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eceived in revised form 19

ecember 2005

ccepted 10 January 2006

eywords:

elf-adhesive resin cement

eramic veneers

icroleakage

entin adhesion

namel adhesion

Objective. Evaluate the performance of a self-adhesive, modified-resin dental cement (Rely-

X UniCem, 3M-ESPE) for the cementation of ceramic veneer restorations without previous

conditioning of the tooth surface, and in combination with a one-bottle adhesive and a

self-etching adhesive.

Methods. Thirty-six premolars received a veneer preparation that extended into dentin.

Leucite-reinforced pressed glass ceramic (Empress 1) veneers were cemented follow-

ing manufacturers’ instructions, according to the following treatment groups (n = 9): (1)

Variolink–Excite Ivoclar–Vivadent (V + E control), (2) Unicem + Single Bond 3M-ESPE (U + SB),

(3) Unicem + Adper Prompt L-Pop 3M-ESPE (U + AP), (4) Unicem 3M-ESPE (U). After 24 h stor-

age at 37 ◦C, teeth were thermocycled (2000 cycles) at 5 and 55 ◦C, immersed in ammoniacal

silver nitrate for 24 h, placed in a developer solution overnight and sectioned using a slow-

speed saw. Three 1 mm longitudinal sections were obtained from each tooth and evaluated

for leakage with a microscope (1× to 4×). Imaging software was used to measure stain pen-

etration along the dentin and enamel surfaces.

Results. ANOVA with SNK (˛ = 0.05) revealed that on dentin, U had significantly less leakage

than U + SB and U + AP, but no different than V + E; on enamel U had leakage values that were

significantly greater than the groups with adhesives.

Significance. The self-adhesive cement U gave low leakage on dentin that was comparable

to the cement that employed an adhesive for sealing dentin, whereas this cement benefits

from use of an adhesive when cementing to enamel.

© 2006 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

. Introduction

he use of bonded ceramic restorations in dentistry hasncreased appreciably due to the development of adhesive

∗ Corresponding author at: Department of Restorative Dentistry, University of Washington, 1959 N.E. Pacific Street, Box 357456, Seattle,A 98195-7456, USA. Tel.: +1 206 543 5948; fax: +1 206 543 7783.

E-mail address: gibarra@u.washington.edu (G. Ibarra).

materials that allow for more conservative restorative tech-niques as well as the ability of achieving excellent estheticappearance and adequate strength [1]. Among these bondedceramic restorations, ceramic veneers have gained popularity

109-5641/$ – see front matter © 2006 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.oi:10.1016/j.dental.2006.01.013

DENTAL-913; No. of Pages 8

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as a conservative restoration, where a thin ceramic coveringis bonded, preferentially to enamel, after minimal preparationon tooth structure [2,3].

The cementation technique, which is a time-consumingand technique-sensitive procedure, is key to the long-termsuccess of these types of restorations. The strength andthe durability of the bond between the porcelain, the lutingcement and the enamel/dentin interface play an importantrole in the outcome of ceramic veneers, particularly whendentin is involved [3]. It is not uncommon that, particularlyin the gingival third of a veneer preparation, dentin will beexposed due to the thin layer of enamel present at this site [4].In this case, the cementation procedure becomes even morecritical because high failure rates in veneers have been associ-ated to large exposed dentin surfaces and the cervical marginhas been regarded as a problematic area to achieve perfectmarginal adaptation [3].

A self-adhesive, resin-based dental cement (Rely-XUniCem, 3M-ESPE), which advocates no pre-treatment oftooth surfaces, thus simplifying the cementation proce-dure, has recently been introduced. This cement has anorganic matrix composed of multi-functional phosphoric acidmethacrylates, which react with inorganic fillers (72 wt.%)that are basic in nature or with hydroxyapatite from toothstructure. Water that is released from the setting reactionis thought to play a role in its neutralization, raising thepH value from 1 to 6. The setting of the cement is based

other adhesive systems that previously condition enamel anddentin.

Altogether, the hypothesis tested was that the microleak-age of the new self-adhesive luting cement is similar to aconventional resin cement when bonding a porcelain veneerto enamel and dentin.

2. Materials and methods

Thirty-six human premolars, previously stored in aNaN3 + NaCl solution for no more than 6 months, wereprepared for porcelain veneer restorations. The preparationswere made with a #834 016 bur (Brasseler, Savannah, GA31419, USA) to establish a 0.3 mm depth cut, and finishedwith a fine rounded tip diamond #6844 016 (Brasseler, Savan-nah, GA 31419, USA). The preparation’s margins ended asbutt joint at the incisal edge and a chamfer that extendedapproximately 1 mm beyond the CEJ. An impression ofeach of the preparations was made with a vinyl polysiloxaneimpression material (Aquasil LV and Aquasil, Caulk, Dentsply;Lot 020608) using copper rings for material retention. Theteeth were then stored in artificial saliva solution and theimpressions were sent to a commercial laboratory (Nakan-ishi Dental Laboratory Inc., Seattle, WA). Leucite-reinforcedpressed ceramic (Empress I) porcelain veneer restorationswere fabricated in an A-1 shade based on the Vita shade

on a free radical polymerization reaction initiated by eitherphotoactivation or a redox system [5,6].

The cement has been recommended for luting all metal-based and ceramic crowns, as well as partial coverage ceramicand indirect composite restorations, with the exception ofveneers [5,6].

Good marginal adaptation of all-ceramic crowns cementedwith Rely-X UniCem to dentin has already been documented[5]. Preliminary studies have shown good results when bond-ing pressed ceramic inlay restorations to dentin and enamelmargins [7].

If the self-adhesive cement could be used predictably forthe cementation of ceramic veneer restorations, it would serveas a user-friendly universal cement. However, more studiesare needed before final recommendations for the clinical useof this cement can be made.

The clinical success of cemented restorations has beenevaluated by measuring marginal fit and microleakage formany years, in spite of the fact that there is no restorationor luting material able to achieve a complete marginal seal[8,9]. In the case of all-ceramic restorations, microleakage hasbeen correlated with the loss of the integrity of the bondto tooth structure, and this has been associated with otherproblems such as secondary caries, post-operative sensitivity,pulpal inflammation, staining and plaque accumulation [9–11]due to the clinically undetectable passage of bacteria, fluids,molecules or ions between tooth structure and the cementedrestoration [12].

The aim of this study was to test the hypothesis thatthe application of a new self-adhesive resin cement, usedas a luting agent, would result in good marginal integrity ofceramic veneers to dentin as well as enamel, without priorconditioning of the tooth surface or in combination with

guide, etched with hydrofluoric acid and silanated in thelaboratory.

The teeth were then divided into four treatment groupsaccording to the cementation procedure (Table 1). Group1: restorations cemented using a conventional resin-basedcement and its proprietary adhesive system as a con-trol (Variolink II [Base Yellow 210/A3, Lot E 43489; Cata-lyst Lot E 34696] and Excite [Lot E41824], Ivoclar/Vivadent).Group 2: restorations cemented using self-adhesive, modified-resin dental cement (Rely-X UniCem Maxicaps, 3M-ESPE;Lot 143650) in combination with enamel and dentin con-ditioning with phosphoric acid and a one-bottle adhe-sive system (Single Bond, 3M-ESPE). Group 3: restorationscemented using a self-adhesive resin-based dental cement(Rely-X UniCem Maxicaps, 3M-ESPE; Lot 143650) in combi-nation with a self-etching adhesive system (Adper PromptL-Pop, 3M-ESPE; Lot 147563) to condition enamel and dentin.Group 4: restorations cemented with a self-adhesive resin-based dental cement (Rely-X UniCem Maxicaps, 3M-ESPE;Lot 143650) without previous conditioning of enamel anddentin.

Before cementation, all veneers were tried-in, cleaned withphosphoric acid and re-silanated (Rely-X Ceramic Primer; Lot2721) in accordance with clinical practice.

Light-curing of the adhesives and the cement was carriedout with a Demetron 401 light unit (Demetron/Kerr, Dan-bury, CT) as indicated in Table 1. Light output was mea-sured every six samples to ensure proper resin polymerization(750 mW/cm2).

The specimens were stored in artificial saliva at 37 ◦C for72 h and were thermocycled in 5 and 55 ◦C water temperaturesfor 2000 cycles with 20 s dwell time at each temperature and atransfer time of 10 s, for a total of 60 s per cycle.

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Table 1 – Application technique for seating ceramic veneer restorations with different adhesive systems and lutingcements

Treatment Materials

Excite/Variolink Single bond/Unicem Prompt L-pop/Unicem Unicem

Veneer preparation Etch with H3PO4 × 60 s Etch with H3PO4 × 60 s Etch with H3PO4 × 60 s Etch with H3PO4 × 60 sRinse × 30 s Rinse × 30 s Rinse × 30 s Rinse × 30 sAir dry Air dry Air dry Air drySilanate internalaspect × 60 s

Silanate internalaspect × 60 s

Silanate internalaspect × 60 s

Silanate internalaspect × 60 s

Allow solvent toevaporate

Allow solvent toevaporate

Allow solvent toevaporate

Allow solvent toevaporate

Apply adhesive tointernal aspect

Apply one coat ofadhesive to internalaspect

Lightly scrub one layerof adhesive to internalaspect: 15 s

Air-thin Air-dry for 2–5 s Air-thinDO NOT light cure DO NOT light cure DO NOT light cure

Substrate preparation H3PO4: etchenamel × 15–30 s anddentin × 10–15 s

H3PO4: etch enamel anddentin × 10 s

Slightly dry surface Leave dentin andenamel surfacemoist/glossy

Rinse: 5 s at least Rinse: 30 s Adhesive: lightly scrubone layer on enameland dentin: 15 s

Remove excesswater—do not over-drydentin

Blot excess water—leavemoist surface

Air-thin

Adhesive: apply severallayers

Adhesive: apply 2 coats Adhesive: apply asecond coat withoutrubbing

Air-dry: 1–3 s. Avoidpooling

Air dry: 2–5 s Air dry

Cure: 20 s DO NOT light cure DO NOT light cureSeating instructions Apply base cement to

veneer and toothApply mixed cement toveneer

Apply mixed cement toveneer

Apply mixed cement toveneer

Maintain pressure forseveral seconds andtack: 10–20 s

Tack-cure excesscement × 2–4 s andremove

Tack-cure excesscement × 2–4 s andremove

Tack-cure excesscement × 2–4 s andremove

Remove excess cementwith brush

Light-cure × 40 s Light-cure × 40 s Light-cure × 40 s

Light-cure × 40 s

2.1. Microleakage evaluation

The apices of the roots were sealed with an acrylic resin(Duralay Inlay Pattern Resin, Reliance) and the teeth were thencoated with two layers of quick dry nail varnish that extendedup to 1 mm from the margins of the ceramic veneer restora-tions. Care was taken not to over dry the enamel surroundingthe margins while the nail varnish dried.

The teeth were placed in 50 wt.% ammoniacal silvernitrate for 24 h, rinsed extensively with water, and placed infreshly mixed developer solution (Kodak Developer D-76, CAT1464817, 0251 C5 02749) under a strong light for 12 h. Afterrinsing them with water and sand blasting the porcelain sur-face carefully, a 1 mm layer of composite was bonded to theveneer (All Bond 2, Bisco, Lot 0200002521; Filtek Z 250 B 1 shade,3M-ESPE, Lot 9BB) to provide sufficient bulk for handling, andlight-cured for 40 s. The roots were removed and the crownswere sectioned in a cervical–incisal direction with a diamondblade to obtain three slices (∼1 mm) from each tooth (Fig. 1).

Sections were analyzed for leakage at the cervical andincisal margins by means of a light microscope (Nikon EclipseE400, Japan) at 1×, 2× and 4×, using an image analysis com-

Fig. 1 – Section of the crown showing the interface ofenamel (E) and dentin (D) with the porcelain veneer (PV)and the overlying composite (C). Penetration of theammoniacal silver nitrate can be observed on the dentinside (arrow).

4 d e n t a l m a t e r i a l s x x x ( 2 0 0 6 ) xxx–xxx

puter program (Meta Vue, Universal Imaging Corp., Downing-town, PA). Microleakage values were obtained by measuringstain penetration for the total surface length, separately fordentin and enamel, and were expressed as a percentage ofthe total length of the veneer preparation.

2.2. Statistical analysis

Since there were four different cement-bonding combinations(i.e., treatments) and samples were independent, a single-factor analysis of variance model was employed to test forsignificant main effects, separately for dentin and for enamel.If main effects were significant (˛ = 0.05) and test for equal vari-ance was not significant, the Student–Newman–Kuel’s posthoc test for multiple comparison of means was conductedto determine which means differed. When the assumptionof equal variances was not met, the Games–Howell post hoctest was used to identify which means differed. All hypothesistesting was conducted at the 95% level of confidence.

2.3. SEM evaluation

After cementation, one tooth from each group was preparedfor SEM evaluation. The teeth were stored in water for 4 weeksand were fixed for 72 h in 2.5% glutaraldehyde in 0.1 M Na-cacodylate buffer. Cross-sections of an approximate thicknessof 1 mm (Fig. 1) were obtained from the teeth using a water-

Fig. 2 – Mean percent microleakage values betweenporcelain veneers and dentin. The numbers identify meansubsets not shown to differ at ˛ = 0.05. The vertical barsshow the value of a single standard deviation.

and 10.8% in the U group (Fig. 3). ANOVA test for main effectswas again significant, as was the test for equal variancesdue to a higher standard deviation associated with enamelmicroleakage for U. For this reason, the Games–Howell test(˛ = 0.05) was employed to compare means. This test revealedthat on enamel, U had leakage values that were significantlygreater than any of the groups where an adhesive systemwas used in combination with the luting cement. In the lattergroups, leakage was minimal and no statistically significantdifference was found amongst them (Fig. 3).

3.2. Scanning electron microscopy analysis

The interface of the samples cemented with E + V, SB + Uand AP + U showed good adaptation of the cement to theenamel surface. No gap formation between the cement andthe enamel was evident in the E + V group, which is consistentwith the microleakage values obtained for these specimens(Fig. 4). It appeared that the use of an adhesive resulted inconsistently good adaptation of the cement to the enamel,regardless of the type of conditioning, as was demonstratedby similar leakage values when using phosphoric acid and theself-etching adhesive system (Figs. 5 and 6).

The samples treated only with unicem (U) showed a gapbetween the cement and the enamel, which is in accor-dance with the high leakage values observed in this group(Figs. 7 and 8).

cooled slow-speed diamond saw (Buehler Isomet 1000TM,Buehler Ltd., Lake Bluff, IL, USA) and each section was sequen-tially polished with 600 and 800 grit of silicon carbide paper, 6and 1 �m diamond slurries and 0.04 �m aluminum oxide. Thespecimens were dehydrated in an ascending series of ethanoland critical-point dried with HMDS, mounted on aluminumstubs and gold-sputter coated to prepare them for analysisunder a field-emission scanning electron microscope (FE-SEM,Hitachi S-4000).

3. Results

3.1. Microleakage analysis

A total of 144 specimen sections were available for evaluationof microleakage at the interface. Three sections were obtainedfrom each of the 48 teeth and information was gathered fromboth sides of each section. Microleakage was observed in mostof the specimens, especially on the dentin side, which is con-sistent with existing evidence [13–18].

Mean microleakage values for the dentin side were 44.1%in the Variolink and Excite group (E + V), 55.5% in the SingleBond and Unicem group (SB + U), 54.7% in the Prompt andUnicem group (AP + U) and 28.1% in the Unicem group (U)(Fig. 2). ANOVA test was significant and the test for equal vari-ances was not significant. The Student–Newman–Kuel’s (SNK)test to compare means (˛ = 0.05) revealed that on dentin: Uhad significantly less leakage than SB + U and AP + U but wasnot different than E + V and that E + V, SB + U, AP + U were notshown to differ.

The microleakage values for the enamel side were 2.5% inthe E + V group, 3.1% in SB + U group, 2.2% in the AP + U group

Fig. 3 – Mean percent microleakage values betweenporcelain veneers and enamel. The numbers identify meansubsets not shown to differ at ˛ = 0.05. The vertical barsshow the value of a single standard deviation.

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Fig. 4 – Scanning electron microscopy image showing goodadaptation at the enamel–cement interface (arrows) in asample cemented with E + V. An almost imperceptibletransition seemed to take place at theenamel–cement–porcelain interface, where minimalleakage values were observed.

Fig. 5 – Scanning electron microscopy image showing goodadaptation at the enamel–cement interface (arrows) in asample cemented with SB + U. An almost imperceptibletel

Fig. 6 – Scanning electron microscopy image showing goodadaptation at the enamel–cement interface (arrows) in asample cemented with AP + U. Minimal leakage valueswere also observed in these set of specimens.

Fig. 7 – Scanning electron microscopy image showing gapformation at the enamel–cement interface (arrows). Animperceptible transition seemed to take place at thecement–porcelain interface, where no leakage wasobserved.

4. Discussion

The use of dyes is one of the oldest techniques to measure

ransition seemed to take place at the namel–cement–porcelain interface, where minimaleakage values were also observed.

microleakage and the use of a 50 wt.% silver nitrate solutionhas been considered an acceptable technique for this purpose

6 d e n t a l m a t e r i a l s x x x ( 2 0 0 6 ) xxx–xxx

Fig. 8 – Scanning electron microscopy image showing gapformation at the enamel–unicem interface (arrows). Animperceptible transition seemed to take place at thecement–porcelain interface, where no leakage wasobserved.

[19]. A disadvantage of this tracer is that the silver nitrateparticle is an extremely small particle that measures approx-imately 0.059 nm in radius and the solution has an acidic pHof ∼4.2 [9,20]. Therefore, penetration of the silver particle atthe interface is frequently observed and it has been suggestedthat it may be greater because of dissolution of remnant cal-cium phosphate salts at the adhesive interface, resulting inincreased porosity due to a light etching effect by the mildlyacidic solution. To avoid this potential drawback, the use ofa buffered solution of ammoniacal silver nitrate with a pH of∼9.5, has been reported [20] and was used in the current study.

4.1. Dentin interface

Without any conditioning, the self-etching cement Rely-XUnicem (3M-ESPE) (U) showed improved sealing of dentin atthe cervical margin when compared to a conventional resincement for which the smear layer was removed by the useof phosphoric acid, although this was not statistically signifi-cant in this study. These findings are in accordance with Behret al. [5] who found similar marginal adaptation based on dyepenetration and SEM replica analysis, to that obtained withconventional cements on dentin margins.

The use of two different adhesive systems, a one-step total-etch (Single Bond, 3M-ESPE) and a one-step self-etch (Rely-XAdper Prompt, 3M-ESPE), to condition the enamel and dentinprior to cementation, did not improve the sealing ability of

when the dentin was etched prior to cementation with Rely-X Unicem, the �TBS values significantly decreased. Similarly,in the present study, when the dentin was pre-treated witheither H3PO4 or an acidic monomer from the self-etching sys-tem, increased leakage was observed. Pre-etching may removeall of the buffer capacity of dentin, interfering with its abilityto raise the pH of the acidic resin as it sets, thereby loweringits conversion (David Pashley, personal communication).

According to Behr et al. [5], in images obtained with trans-mission electron microscopy, a lack of a hybrid layer is evidentat the dentin interface when the self-adhesive cement is used.This agrees with De Munck et al. [21] who reported no evidenceof dentin demineralization even considering the initial low pHof the cement (pH <2, according to the manufacturer). Thisresult in the absence of a hybrid layer which, although thinner,is present when self-etching adhesive systems are used [22].Indeed, if the acid resin cement does not penetrate throughthe smear layer, the strength of the bond may be limited tothe strength of the smear layer.

In this study, the cement was never used alone after etch-ing dentin, but in combination with either a simplified total-etch single-bottle adhesive or a one-step self-etching adhe-sive, which coated the pre-treated dentin with a resin layer. Inboth cases, there were increased leakage values over thoseseen when the self-adhesive cement was used alone. It isknown that the previously reported incompatibility of sim-plified adhesives, especially single-step self-etch adhesives,

(U) in dentin, when compared to the control. De Munck etal. [21] reported similar �TBS values when bonding to dentinusing Rely-X Unicem without previously etching the dentinwith H3PO4 or a conventional cement as a control. However,

and dual/auto-cured luting cements may be due, in part, toadverse acid–base reactions between the acidic monomersand the basic tertiary amines that are commonly used as cata-lysts in these systems [23]. The tertiary amines are consumedas they come in contact with the acidic resin monomersdue to the absence of an additional adhesive resin layer,which decreases their capacity to generate free radicals forthe polymerization reaction. To solve this problem, alterna-tive redox catalyst systems have been introduced, such asthe commonly used sodium salt of aryl sulphinic acid [24].Many single-bottle adhesive systems have an additional bot-tle of an activator solution that contains such a salt. Theone-step self-etch adhesives are even more susceptible tothis adverse chemical reaction because they are inherentlymore acidic due to a higher content of acidic resin monomers[24].

On the other hand, the one-bottle or simplified adhesives,either total-etch or self-etch, behave as permeable mem-branes due to the absence of a more hydrophobic resin coat,such as is used in conventional systems [25]. Transudationof dentinal fluid across these simplified adhesives has beenobserved, and it has been speculated that this may interferewith the proper polymerization of the luting resin cement byinducing emulsion polymerization of the coupling hydropho-bic resin cements [23,25]. It has also been reported that theslow-setting of the dual/auto-cured luting cements may allowsufficient movement of dentinal fluid to cause microblistersat the resin–composite interface, which may result in subse-quent failure of the bond because these blisters will eventuallyact as stress raisers [25]. As a result of these mechanisms, alack of a hermetic seal at the tooth structure–adhesive inter-face will probably occur. In the current study, the seal at thecervical margin of the cemented veneer restorations when

d e n t a l m a t e r i a l s x x x ( 2 0 0 6 ) xxx–xxx 7

using the adhesive systems was less effective than when thecement was used alone.

Furthermore, it has been reported that the one-step self-etching adhesive system (AP) has shown better sealing whensubsequent coats of adhesive are applied. Light-curing thefirst coat on dentin before applying the second coat, has beenrecommended to assure adequate resin polymerization [26].Nevertheless, Tay et al. [25] more recently reported that denti-nal fluid transudation is still observed after additional layersof simplified adhesive systems are applied, even if they arelight-cured separately. In the present study, the one-step self-etching adhesive (AP) was used following the manufacturer’sinstructions (Table 1) which now recommend application oftwo consecutive coats of adhesive without light-curing thefirst coat. Interestingly, there was no statistically significantdifference regarding leakage when compared to the conven-tional system but there was a difference when compared to(U) alone. Leakage was observed, in general, between the toothstructure and the cement. We speculate that there was a defi-cient seal probably due to a lack of complete polymerizationof the luting cement because of the presence of water at theinterface.

When the self-adhesive cement (U) was used on its own,the microleakage values were no different than the valuesobtained with the conventional cement. According to theinformation available on this self-adhesive cement, neutral-ization of the acidic reaction takes place as polymerizationpiwles

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images, where previously treated enamel by either a phos-phoric acid conditioner or a strong self-etching adhesive sys-tem, show no evidence of gap formation between the cementand the enamel (Figs. 4–6). However, when the self-adhesivecement was used on its own, an evident gap can be observed(Figs. 7 and 8), which may be due to a combination of fac-tors such as inadequate etching through the enamel smearlayer for micromechanical retention on the enamel surface,and the weak cohesive strength of enamel smear layers [28] ofthe cement.

The inadequate formation of micromechanical retentionon enamel may be due to the high viscosity that the cementhas after mixing and the short interaction time that it has withthe tooth surface before light-curing takes place. The initiallow pH (<2) may not be sufficient to etch the enamel if etchingtime is not adequate, and if neutralization reactions take placerapidly.

Another explanation for the presence of gaps at theenamel interface could be lack of adequate pressure duringthe cementation procedure. De Munk [21] has reported animproved adaptation of the cement to the substrate when itis applied under pressure due to its thixotropic characteris-tics. In this study, however, the veneers were cemented underpressure that simulated that applied in the clinical setting, andalthough gap formation was not seen at the dentin interface,it was still evident at the enamel interface.

r

rogresses (ESPE-information from the manufacturer). It ismportant to mention that the small amount of leakage thatas observed in dentin may not be indicative of adequate

ong-term performance of the cement. The durability that self-tching adhesive systems have on cement-dentin bonds afterome time, remains to be evaluated.

.2. Enamel interface

ithout any conditioning (U) showed significantly greatereakage at the enamel interface, which was not seen when theement was used in combination with other adhesive systemsr a conventional cement. This may suggest an insufficienttching ability of the cement to smear layer covered enamel,nd therefore, the lack of development of adequate microme-hanical retention. The use of the conventional cement as wells the one-bottle and the self-etching adhesive systems wereikely to result in good micromechanical retention, since theormer used phosphoric acid prior to the adhesive applicationnd the latter was a strong self-etching adhesive (AP) whichas been shown to adequately etch enamel [27]. These resultsre in agreement with DeMunk et al. [21], who reported lowerTBS to enamel that was not acid-etched previous to the usef Rely-X Unicem, with mostly adhesive failures in the sam-les, which is probably due to the lack of etching throughhe smear layer into the underlying enamel. In this sametudy, the �TBS values increased significantly when enamelas previously etched with phosphoric acid, which obvi-usly resulted in the formation of adequate micromechanicaletention.

The role of chemical bonding of the self-adhesive cementith enamel may be insufficient to obtain an adequate sealetween the cement and enamel. This is evident in the SEM

5. Conclusions

The seal of the self-adhesive, resin-based cement is compa-rable to cements that employ adhesives for sealing dentin,whereas this cement appears to benefit from the use of a con-ventional conditioner, such as phosphoric acid, or a strongself-etching adhesive system when cementing to enamel.

Due to the excessive enamel microleakage observed inthis study when the self-adhesive cement was used alone,the authors would not recommend its use for cementationof ceramic veneers. The hypothesis tested was rejected forenamel substrates.

The lack of adequate performance of this self-etchingadhesive cement on enamel suggests the need to moreextensively investigate the adhesion mechanism of the self-adhesive cement, surface characterization of the substrateand evaluation of its long-term clinical performance.

Acknowledgements

“This investigation was supported in part by 3M-ESPE”.The authors would like to express their gratitude to OHSU

for the thermocycling of the samples and to Dr. David Pashleyfor his valuable contribution.

e f e r e n c e s

[1] Rosenstiel SF, Land MF, Crispin BJ. Dental luting agents: areview of the current literature. J Prosthet Dent1998;80(3):280–301.

8 d e n t a l m a t e r i a l s x x x ( 2 0 0 6 ) xxx–xxx

[2] Peumans M, Van Meerbeek B, Yoshida Y, Lambrechts P,Vanherle G. Porcelain veneers bonded to tooth structure:an ultramorphological FE-SEM examination of theadhesive interface. Dent Mater 1999;15:105–19.

[3] Peumans M, Van Meerbeek B, Lambrechts P, Vanherle G.Porcelain veneers: a review of the literature. J Dent2000;28:163–77.

[4] Ferrari M, Patroni S, Balleri P. Measurement of enamelthickness in relation to reduction for etched laminateveneers. Int J Periodontics Restorative Dent1992;12(5):407–13.

[5] Behr M, Rosentritt M, Regnet T, Lang R, Handel G.Marginal adaptation in dentin of a self-adhesive universalresin cement compared with well-tried systems. DentMater 2004;20:191–7.

[6] Technical data sheet, 3M-ESPE.[7] Rosentritt M, Behr M, Lang R, Handel G. Influence of

cement type on the marginal adaptation of all ceramicMOD inlays. Dent Mater 2004;20:463–9.

[8] Gladys S, Van Meerbeek B, Lambrechts P, Vanherle G.Microleakage of adhesive restorative materials. Am JDentistry 2001;14(3):170–6.

[9] Alani AH, Toh CG. Detection of microleakage arounddental restorations: a review. Oper Dent 1997;22(4):173–85.

[10] Hekimoglu C, Anil N, Yalcin E. A microleakage study ofceramic laminate veneers by autoradiography: effect ofincisal edge preparation. J Oral Rehabil 2004;31:265–70.

[11] Cox CF, Felton D, Bergenholtz G. Histopathologicalresponse of infected cavities treated with Gluma andScotchbond dentin bonding agents. Am J Dent

[16] Retief DH. Do adhesives prevent microleakage? Int Dent J1994;44:19–26.

[17] Sim C, Neo J, Kiam Chua EK, Tan BY. The effect of dentinbonding agents on the microleakage of porcelain veneers.Dent Mater 1994;10(4):278–81.

[18] Tay FR, Gwinnett AJ, Pang KM, Wei SHV. Variability inmicroleakage observed in a total-etch wet-bondingtechnique under different handling conditions. J Dent Res1995;74:1168–78.

[19] Hammesfahr PD, Huang CT, Shaffer SE. Microleakage andbond strength of resin restorations with various bondingagents. Dent Mater 1987;3:194–9.

[20] Tay FR, Pashley DH. Water treeing—a potential mechanismfor degradation of dentin adhesives. Am J Dent2003;16(1):6–12.

[21] De Munk J, Vargas MA, Van Landuyt K, Hikita K,Lambrechts P, Van Meerbeek B. Bonding of anauto-adhesive luting material to enamel and dentin. DentMater 2004;20:963–71.

[22] Tay FR, Sano H, Carvalho R, Pashley EL, Pashley DH. Anultrastructural study of the influence of acidity ofself-etching primers and smear layer thickness on bondingto intact dentin. J Adhes Dent 2000;2(2):83–98.

[23] Tay FR, Pashley DH, Suh BI, Carvalho RM, Itthagarun A.Single-step adhesives are permeable membranes. J Dent2002;30:371–82.

[24] Tay FR, Pashley DH, Peters MC. Adhesive permeabilityaffects composite coupling to dentin treated with aself-etch adhesive. Oper Dent 2003;28(5):610–21.

[25] Tay FR, Frankenberger R, Krejci I, Bouillaguet S, PashleyDH, Carvalho RM, Lai CNS. Single-bottle adhesives behave

1988;1:189–94.[12] Kidd EAM. Microleakage: a review. J Dent 1976;4:199–206.[13] Kanka J. Microleakage of five dentin bonding systems.

Dent Mater 1989;5:415–6.[14] Lacy AM, Wada C, Du W, Watanabe L. In vitro

microleakage at the gingival margin of porcelain and resinveneers. J Prosthet Dent 1991;67(1):7–10.

[15] Zaimoglu A, Karaagaclioglu L, Uctasli S. Influence ofporcelain materials and composite luting resin onmicroleakage of porcelain veneers. J Oral Rehabil1992;19:319.

as permeable membranes after polymerization. I. In vivoevidence. J Dent 2004;32(8):611–21.

[26] Pashley EL, Agee KA, Pashley DH, Tay FR. Effects of oneversus two applications of an unfilled, all-in-one adhesiveon dentin bonding. J Dent 2002;30:83–90.

[27] Pashley DH, Tay FR. Aggressiveness of contemporaryself-etching adhesives. Part II: etching effects on ungroundenamel. Dent Mater 2001;17:430–44.

[28] Tao L, Pashley DH, Boyd L. Effect of different types ofsmear layers on dentin and enamel shear bond strengths.Dent Mater 1988;4:208–16.