Microleakage of porcelain veneer restorations bonded to enamel ...

dental materials xxx (2006) xxx–xxx 

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Microleakage of porcelain veneer restorations bonded to 

enamel and dentin with a new self-adhesive resin-based 

dental cement 

Gabriela Ibarra a,∗ , Glen H. Johnson a , Werner Geurtsen a , Marcos A. Vargas b 

a School of Dentistry, Department of Restorative Dentistry, University of Washington, Seattle, WA, USA 

b College of Dentistry, Department of Operative Dentistry, University of Iowa, Iowa City, USA 

article info 

Article history: 

Received 29 September 2005 

Received in revised form 19 

December 2005 

Accepted 10 January 2006 

Keywords: 

Self-adhesive resin cement 

Ceramic veneers 

Microleakage 

Dentin adhesion 

Enamel adhesion 

1. Introduction 

abstract 

The use of bonded ceramic restorations in dentistry has 

increased appreciably due to the development of adhesive 

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

procedure critical to long-term success. 

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 following 

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- 

ageat37 ◦ 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 slowspeed 

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 penetration 

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. 

materials that allow for more conservative restorative techniques 

as well as the ability of achieving excellent esthetic 

appearance and adequate strength [1]. Among these bonded 

ceramic restorations, ceramic veneers have gained popularity 

∗ Corresponding author at: Department of Restorative Dentistry, University of Washington, 1959 N.E. Pacific Street, Box 357456, Seattle, 

WA 98195-7456, USA. Tel.: +1 206 543 5948; fax: +1 206 543 7783. 

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

0109-5641/$ – see front matter © 2006 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved. 

doi:10.1016/j.dental.2006.01.013 

DENTAL-913; No. of Pages 8

2 dental materials xxx (2006) xxx–xxx 

as a conservative restoration, where a thin ceramic covering 

is bonded, preferentially to enamel, after minimal preparation 

on tooth structure [2,3]. 

The cementation technique, which is a time-consuming 

and technique-sensitive procedure, is key to the long-term 

success of these types of restorations. The strength and 

the durability of the bond between the porcelain, the luting 

cement and the enamel/dentin interface play an important 

role in the outcome of ceramic veneers, particularly when 

dentin is involved [3]. It is not uncommon that, particularly 

in the gingival third of a veneer preparation, dentin will be 

exposed due to the thin layer of enamel present at this site [4]. 

In this case, the cementation procedure becomes even more 

critical because high failure rates in veneers have been associated 

to large exposed dentin surfaces and the cervical margin 

has been regarded as a problematic area to achieve perfect 

marginal adaptation [3]. 

A self-adhesive, resin-based dental cement (Rely-X 

UniCem, 3M-ESPE), which advocates no pre-treatment of 

tooth surfaces, thus simplifying the cementation procedure, 

has recently been introduced. This cement has an 

organic matrix composed of multi-functional phosphoric acid 

methacrylates, which react with inorganic fillers (72 wt.%) 

that are basic in nature or with hydroxyapatite from tooth 

structure. Water that is released from the setting reaction 

is thought to play a role in its neutralization, raising the 

pH value from 1 to 6. The setting of the cement is based 

on a free radical polymerization reaction initiated by either 

photoactivation or a redox system [5,6]. 

The cement has been recommended for luting all metalbased 

and ceramic crowns, as well as partial coverage ceramic 

and indirect composite restorations, with the exception of 

veneers [5,6]. 

Good marginal adaptation of all-ceramic crowns cemented 

with Rely-X UniCem to dentin has already been documented 

[5]. Preliminary studies have shown good results when bonding 

pressed ceramic inlay restorations to dentin and enamel 

margins [7]. 

If the self-adhesive cement could be used predictably for 

the cementation of ceramic veneer restorations, it would serve 

as a user-friendly universal cement. However, more studies 

are needed before final recommendations for the clinical use 

of this cement can be made. 

The clinical success of cemented restorations has been 

evaluated by measuring marginal fit and microleakage for 

many years, in spite of the fact that there is no restoration 

or luting material able to achieve a complete marginal seal 

[8,9]. In the case of all-ceramic restorations, microleakage has 

been correlated with the loss of the integrity of the bond 

to tooth structure, and this has been associated with other 

problems 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 cemented 

restoration [12]. 

The aim of this study was to test the hypothesis that 

the application of a new self-adhesive resin cement, used 

as a luting agent, would result in good marginal integrity of 

ceramic veneers to dentin as well as enamel, without prior 

conditioning of the tooth surface or in combination with 

other adhesive systems that previously condition enamel and 

dentin. 

Altogether, the hypothesis tested was that the microleakage 

of the new self-adhesive luting cement is similar to a 

conventional resin cement when bonding a porcelain veneer 

to enamel and dentin. 

2. Materials and methods 

Thirty-six human premolars, previously stored in a 

NaN3 + NaCl solution for no more than 6 months, were 

prepared for porcelain veneer restorations. The preparations 

were made with a #834 016 bur (Brasseler, Savannah, GA 

31419, USA) to establish a 0.3 mm depth cut, and finished 

with a fine rounded tip diamond #6844 016 (Brasseler, Savannah, 

GA 31419, USA). The preparation’s margins ended as 

butt joint at the incisal edge and a chamfer that extended 

approximately 1 mm beyond the CEJ. An impression of 

each of the preparations was made with a vinyl polysiloxane 

impression material (Aquasil LV and Aquasil, Caulk, Dentsply; 

Lot 020608) using copper rings for material retention. The 

teeth were then stored in artificial saliva solution and the 

impressions were sent to a commercial laboratory (Nakanishi 

Dental Laboratory Inc., Seattle, WA). Leucite-reinforced 

pressed ceramic (Empress I) porcelain veneer restorations 

were fabricated in an A-1 shade based on the Vita shade 

guide, etched with hydrofluoric acid and silanated in the 

laboratory. 

The teeth were then divided into four treatment groups 

according to the cementation procedure (Table 1). Group 

1: restorations cemented using a conventional resin-based 

cement and its proprietary adhesive system as a control 

(Variolink II [Base Yellow 210/A3, Lot E 43489; Catalyst 

Lot E 34696] and Excite [Lot E41824], Ivoclar/Vivadent). 

Group 2: restorations cemented using self-adhesive, modifiedresin 

dental cement (Rely-X UniCem Maxicaps, 3M-ESPE; 

Lot 143650) in combination with enamel and dentin conditioning 

with phosphoric acid and a one-bottle adhesive 

system (Single Bond, 3M-ESPE). Group 3: restorations 

cemented using a self-adhesive resin-based dental cement 

(Rely-X UniCem Maxicaps, 3M-ESPE; Lot 143650) in combination 

with a self-etching adhesive system (Adper Prompt 

L-Pop, 3M-ESPE; Lot 147563) to condition enamel and dentin. 

Group 4: restorations cemented with a self-adhesive resinbased 

dental cement (Rely-X UniCem Maxicaps, 3M-ESPE; 

Lot 143650) without previous conditioning of enamel and 

dentin. 

Before cementation, all veneers were tried-in, cleaned with 

phosphoric acid and re-silanated (Rely-X Ceramic Primer; Lot 

2721) in accordance with clinical practice. 

Light-curing of the adhesives and the cement was carried 

out with a Demetron 401 light unit (Demetron/Kerr, Danbury, 

CT) as indicated in Table 1. Light output was measured 

every six samples to ensure proper resin polymerization 

(750 mW/cm 2 ). 

The specimens were stored in artificial saliva at 37 ◦ C for 

72 h and were thermocycled in 5 and 55 ◦ C water temperatures 

for 2000 cycles with 20 s dwell time at each temperature and a 

transfer time of 10 s, for a total of 60 s per cycle.

dental materials xxx (2006) xxx–xxx 3 

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

cements 

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 s 

Rinse × 30 s Rinse × 30 s Rinse × 30 s Rinse × 30 s 

Air dry Air dry Air dry Air dry 

Silanate internal 

aspect × 60 s 

Allow solvent to 

evaporate 

Apply adhesive to 

internal aspect 

Substrate preparation H3PO4: etch 

enamel × 15–30 s and 

dentin × 10–15 s 




evaporate 

Apply one coat of 

adhesive to internal 

aspect 




evaporate 

Lightly scrub one layer 

of adhesive to internal 

aspect: 15 s 

Air-thin Air-dry for 2–5 s Air-thin 

DO NOT light cure DO NOT light cure DO NOT light cure 

H3PO4: etch enamel and 

dentin × 10 s 

Rinse: 5 s at least Rinse: 30 s Adhesive: lightly scrub 

one layer on enamel 

and dentin: 15 s 

Remove excess 

water—do not over-dry 

dentin 

Adhesive: apply several 

layers 

Air-dry: 1–3 s. Avoid 

pooling 

Seating instructions Apply base cement to 

veneer and tooth 

Maintain pressure for 

several seconds and 

tack: 10–20 s 

Remove excess cement 

with brush 

Light-cure × 40 s 

2.1. Microleakage evaluation 

Blot excess water—leave 

moist surface 




evaporate 

Slightly dry surface Leave dentin and 

enamel surface 

moist/glossy 

Air-thin 

Adhesive: apply 2 coats Adhesive: apply a 

second coat without 

rubbing 

Air dry: 2–5 s Air dry 

Cure: 20 s DO NOT light cure DO NOT light cure 

Apply mixed cement to 

veneer 

Tack-cure excess 

cement × 2–4 s and 

remove 

The apices of the roots were sealed with an acrylic resin 

(Duralay Inlay Pattern Resin, Reliance) and the teeth were then 

coated with two layers of quick dry nail varnish that extended 

up to 1 mm from the margins of the ceramic veneer restorations. 

Care was taken not to over dry the enamel surrounding 

the margins while the nail varnish dried. 

The teeth were placed in 50 wt.% ammoniacal silver 

nitrate for 24 h, rinsed extensively with water, and placed in 

freshly mixed developer solution (Kodak Developer D-76, CAT 

1464817, 0251 C5 02749) under a strong light for 12 h. After 

rinsing them with water and sand blasting the porcelain surface 

carefully, a 1 mm layer of composite was bonded to the 

veneer (All Bond 2, Bisco, Lot 0200002521; Filtek Z 250 B 1 shade, 

3M-ESPE, Lot 9BB) to provide sufficient bulk for handling, and 

light-cured for 40 s. The roots were removed and the crowns 

were sectioned in a cervical–incisal direction with a diamond 

blade to obtain three slices (∼1 mm) from each tooth (Fig. 1). 

Sections were analyzed for leakage at the cervical and 

incisal margins by means of a light microscope (Nikon Eclipse 

E400, Japan) at 1×, 2× and 4×, using an image analysis com- 





remove 





remove 

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

Fig. 1 – Section of the crown showing the interface of 

enamel (E) and dentin (D) with the porcelain veneer (PV) 

and the overlying composite (C). Penetration of the 

ammoniacal silver nitrate can be observed on the dentin 

side (arrow).


puter program (Meta Vue, Universal Imaging Corp., Downingtown, 

PA). Microleakage values were obtained by measuring 

stain penetration for the total surface length, separately for 

dentin and enamel, and were expressed as a percentage of 

the 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 singlefactor 

analysis of variance model was employed to test for 

significant main effects, separately for dentin and for enamel. 

If main effects were significant (˛ = 0.05) and test for equal variance 

was not significant, the Student–Newman–Kuel’s post 

hoc test for multiple comparison of means was conducted 

to determine which means differed. When the assumption 

of equal variances was not met, the Games–Howell post hoc 

test was used to identify which means differed. All hypothesis 

testing was conducted at the 95% level of confidence. 

2.3. SEM evaluation 

After cementation, one tooth from each group was prepared 

for SEM evaluation. The teeth were stored in water for 4 weeks 

and were fixed for 72 h in 2.5% glutaraldehyde in 0.1 M Nacacodylate 

buffer. Cross-sections of an approximate thickness 

of 1 mm (Fig. 1) were obtained from the teeth using a watercooled 

slow-speed diamond saw (Buehler Isomet 1000 TM , 

Buehler Ltd., Lake Bluff, IL, USA) and each section was sequentially 

polished with 600 and 800 grit of silicon carbide paper, 6 

and 1 �m diamond slurries and 0.04 �m aluminum oxide. The 

specimens were dehydrated in an ascending series of ethanol 

and critical-point dried with HMDS, mounted on aluminum 

stubs and gold-sputter coated to prepare them for analysis 

under 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 evaluation 

of microleakage at the interface. Three sections were obtained 

from each of the 48 teeth and information was gathered from 

both sides of each section. Microleakage was observed in most 

of the specimens, especially on the dentin side, which is consistent 

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 Single 

Bond and Unicem group (SB + U), 54.7% in the Prompt and 

Unicem group (AP + U) and 28.1% in the Unicem group (U) 

(Fig. 2). ANOVA test was significant and the test for equal variances 

was not significant. The Student–Newman–Kuel’s (SNK) 

test to compare means (˛ = 0.05) revealed that on dentin: U 

had significantly less leakage than SB + U and AP + U but was 

not different than E + V and that E + V, SB + U, AP + U were not 

shown to differ. 

The microleakage values for the enamel side were 2.5% in 

the E + V group, 3.1% in SB + U group, 2.2% in the AP + U group 

Fig. 2 – Mean percent microleakage values between 

porcelain veneers and dentin. The numbers identify mean 

subsets not shown to differ at ˛ = 0.05. The vertical bars 

show the value of a single standard deviation. 

and 10.8% in the U group (Fig. 3). ANOVA test for main effects 

was again significant, as was the test for equal variances 

due to a higher standard deviation associated with enamel 

microleakage for U. For this reason, the Games–Howell test 

(˛ = 0.05) was employed to compare means. This test revealed 

that on enamel, U had leakage values that were significantly 

greater than any of the groups where an adhesive system 

was used in combination with the luting cement. In the latter 

groups, leakage was minimal and no statistically significant 

difference was found amongst them (Fig. 3). 

3.2. Scanning electron microscopy analysis 

The interface of the samples cemented with E + V, SB + U 

and AP + U showed good adaptation of the cement to the 

enamel surface. No gap formation between the cement and 

the enamel was evident in the E + V group, which is consistent 

with the microleakage values obtained for these specimens 

(Fig. 4). It appeared that the use of an adhesive resulted in 

consistently good adaptation of the cement to the enamel, 

regardless of the type of conditioning, as was demonstrated 

by similar leakage values when using phosphoric acid and the 

self-etching adhesive system (Figs. 5 and 6). 

The samples treated only with unicem (U) showed a gap 

between the cement and the enamel, which is in accordance 

with the high leakage values observed in this group 

(Figs. 7 and 8). 

Fig. 3 – Mean percent microleakage values between 

porcelain veneers and enamel. The numbers identify mean 

subsets not shown to differ at ˛ = 0.05. The vertical bars 

show the value of a single standard deviation.

Fig. 4 – Scanning electron microscopy image showing good 

adaptation at the enamel–cement interface (arrows) in a 

sample cemented with E + V. An almost imperceptible 

transition seemed to take place at the 

enamel–cement–porcelain interface, where minimal 

leakage values were observed. 



sample cemented with SB + U. An almost imperceptible 

transition seemed to take place at the 

enamel–cement–porcelain interface, where minimal 

leakage values were also observed. 




sample cemented with AP + U. Minimal leakage values 

were also observed in these set of specimens. 

Fig. 7 – Scanning electron microscopy image showing gap 

formation at the enamel–cement interface (arrows). An 

imperceptible transition seemed to take place at the 

cement–porcelain interface, where no leakage was 

observed. 

4. Discussion 

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

microleakage and the use of a 50 wt.% silver nitrate solution 

has been considered an acceptable technique for this purpose


Fig. 8 – Scanning electron microscopy image showing gap 

formation at the enamel–unicem interface (arrows). An 

imperceptible transition seemed to take place at the 

cement–porcelain interface, where no leakage was 

observed. 

[19]. A disadvantage of this tracer is that the silver nitrate 

particle is an extremely small particle that measures approximately 

0.059 nm in radius and the solution has an acidic pH 

of ∼4.2 [9,20]. Therefore, penetration of the silver particle at 

the interface is frequently observed and it has been suggested 

that it may be greater because of dissolution of remnant calcium 

phosphate salts at the adhesive interface, resulting in 

increased porosity due to a light etching effect by the mildly 

acidic solution. To avoid this potential drawback, the use of 

a 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-X 

Unicem (3M-ESPE) (U) showed improved sealing of dentin at 

the cervical margin when compared to a conventional resin 

cement for which the smear layer was removed by the use 

of phosphoric acid, although this was not statistically significant 

in this study. These findings are in accordance with Behr 

et al. [5] who found similar marginal adaptation based on dye 

penetration and SEM replica analysis, to that obtained with 

conventional cements on dentin margins. 

The use of two different adhesive systems, a one-step totaletch 

(Single Bond, 3M-ESPE) and a one-step self-etch (Rely-X 

Adper Prompt, 3M-ESPE), to condition the enamel and dentin 

prior to cementation, did not improve the sealing ability of 

(U) in dentin, when compared to the control. De Munck et 

al. [21] reported similar �TBS values when bonding to dentin 

using Rely-X Unicem without previously etching the dentin 

with H3PO4 or a conventional cement as a control. However, 

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 with 

either H3PO4 or an acidic monomer from the self-etching system, 

increased leakage was observed. Pre-etching may remove 

all of the buffer capacity of dentin, interfering with its ability 

to raise the pH of the acidic resin as it sets, thereby lowering 

its conversion (David Pashley, personal communication). 

According to Behr et al. [5], in images obtained with transmission 

electron microscopy, a lack of a hybrid layer is evident 

at the dentin interface when the self-adhesive cement is used. 

This agrees with De Munck et al. [21] who reported no evidence 

of dentin demineralization even considering the initial low pH 

of the cement (pH

using the adhesive systems was less effective than when the 

cement was used alone. 

Furthermore, it has been reported that the one-step selfetching 

adhesive system (AP) has shown better sealing when 

subsequent coats of adhesive are applied. Light-curing the 

first coat on dentin before applying the second coat, has been 

recommended to assure adequate resin polymerization [26]. 

Nevertheless, Tay et al. [25] more recently reported that dentinal 

fluid transudation is still observed after additional layers 

of simplified adhesive systems are applied, even if they are 

light-cured separately. In the present study, the one-step selfetching 

adhesive (AP) was used following the manufacturer’s 

instructions (Table 1) which now recommend application of 

two consecutive coats of adhesive without light-curing the 

first coat. Interestingly, there was no statistically significant 

difference regarding leakage when compared to the conventional 

system but there was a difference when compared to 

(U) alone. Leakage was observed, in general, between the tooth 

structure and the cement. We speculate that there was a deficient 

seal probably due to a lack of complete polymerization 

of the luting cement because of the presence of water at the 

interface. 

When the self-adhesive cement (U) was used on its own, 

the microleakage values were no different than the values 

obtained with the conventional cement. According to the 

information available on this self-adhesive cement, neutralization 

of the acidic reaction takes place as polymerization 

progresses (ESPE-information from the manufacturer). It is 

important to mention that the small amount of leakage that 

was observed in dentin may not be indicative of adequate 

long-term performance of the cement. The durability that selfetching 

adhesive systems have on cement-dentin bonds after 

some time, remains to be evaluated. 

4.2. Enamel interface 

Without any conditioning (U) showed significantly greater 

leakage at the enamel interface, which was not seen when the 

cement was used in combination with other adhesive systems 

or a conventional cement. This may suggest an insufficient 

etching ability of the cement to smear layer covered enamel, 

and therefore, the lack of development of adequate micromechanical 

retention. The use of the conventional cement as well 

as the one-bottle and the self-etching adhesive systems were 

likely to result in good micromechanical retention, since the 

former used phosphoric acid prior to the adhesive application 

and the latter was a strong self-etching adhesive (AP) which 

has been shown to adequately etch enamel [27]. These results 

are in agreement with DeMunk et al. [21], who reported lower 

�TBS to enamel that was not acid-etched previous to the use 

of Rely-X Unicem, with mostly adhesive failures in the samples, 

which is probably due to the lack of etching through 

the smear layer into the underlying enamel. In this same 

study, the �TBS values increased significantly when enamel 

was previously etched with phosphoric acid, which obviously 

resulted in the formation of adequate micromechanical 

retention. 

The role of chemical bonding of the self-adhesive cement 

with enamel may be insufficient to obtain an adequate seal 

between the cement and enamel. This is evident in the SEM 


images, where previously treated enamel by either a phosphoric 

acid conditioner or a strong self-etching adhesive system, 

show no evidence of gap formation between the cement 

and the enamel (Figs. 4–6). However, when the self-adhesive 

cement was used on its own, an evident gap can be observed 

(Figs. 7 and 8), which may be due to a combination of factors 

such as inadequate etching through the enamel smear 

layer for micromechanical retention on the enamel surface, 

and the weak cohesive strength of enamel smear layers [28] of 

the cement. 

The inadequate formation of micromechanical retention 

on enamel may be due to the high viscosity that the cement 

has after mixing and the short interaction time that it has with 

the tooth surface before light-curing takes place. The initial 

low pH (


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Microleakage of porcelain veneer restorations bonded to enamel ...

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