Effect of Surface Conditioning Modalities on the

Repair Bond Strength of Resin Composite to the

Zirconia Core / Veneering Ceramic Complex
Mutlu zcana / Luiz Felipe Valandrob / Sarina Maciel Braga Pereirac / Regina Amaralc /
Marco Antonio Bottinod / Gurel Pekkane

Purpose: This study evaluated the effect of different surface conditioning protocols on the repair strength of
resin composite to the zirconia core / veneering ceramic complex, simulating the clinical chipping phenomenon.
Materials and Methods: Forty disk-shaped zirconia core (Lava Zirconia, 3M ESPE) (diameter: 3 mm) specimens
were veneered circumferentially with a feldspathic veneering ceramic (VM7, Vita Zahnfabrik) (thickness: 2 mm)
using a split metal mold. They were then embedded in autopolymerizing acrylic with the bonding surfaces exposed. Specimens were randomly assigned to one of the following surface conditioning protocols (n = 10 per
group): group 1, veneer: 4% hydrofluoric acid (HF) (Porcelain Etch) + core: aluminum trioxide (50-m Al2O3) +
core+veneer: silane (ESPE-Sil); group 2: core: Al2O3 (50 m) + veneer: HF + core+veneer: silane; group 3: veneer: HF+core: 30 m aluminum trioxide particles coated with silica (30 m SiO2)+core+veneer: silane; group
4: core: 30 m SiO2+veneer: HF+core+veneer: silane. Core and veneer ceramic were conditioned individually
but no attempt was made to avoid cross contamination of conditioning, simulating the clinical intraoral repair
situation. Adhesive resin (VisioBond) was applied to both the core and the veneer ceramic, and resin composite
(Quadrant Posterior) was bonded onto both substrates using polyethylene molds and photopolymerized. After
thermocycling (6000 cycles, 5C55C), the specimens were subjected to shear bond testing using a universal
testing machine (1 mm/min). Failure modes were identified using an optical microscope, and scanning electron
microscope images were obtained. Bond strength data (MPa) were analyzed statistically using the non-parametric
Kruskal-Wallis test followed by the Wilcoxon rank-sum test and the Bonferroni Holm correction (_ = 0.05).
Results: Group 3 demonstrated significantly higher values (MPa) (8.6 2.7) than those of the other groups
(3.2 3.1, 3.2 3, and 3.1 3.5 for groups 1, 2, and 4, respectively) (p < 0.001). All groups showed exclusively adhesive failure between the repair resin and the core zirconia. The incidence of cohesive failure in the
ceramic was highest in group 3 (8 out of 10) compared to the other groups (0/10, 2/10, and 2/10, in groups
1, 2, and 4, respectively). SEM images showed that air abrasion on the zirconia core only also impinged on the
veneering ceramic where the etching pattern was affected.
Conclusion: Etching the veneer ceramic with HF gel and silica coating of the zirconia core followed by silanization
of both substrates could be advised for the repair of the zirconia core / veneering ceramic complex.
Keywords: adhesion, all-ceramics, bond strength, chipping, composite resin, repair, surface conditioning, zirconia.
J Adhes Dent 2013; 15: 207210.
doi: 10.3290/j.jad.a29717

Professor, University of Zurich, Dental Materials Unit, Center for Dental and
Oral Medicine, Clinic for Fixed and Removable Prosthodontics and Dental
Materials Science, Zurich, Switzerland. Designed the study, analyzed data,
wrote manuscript, discussed results and commented on manuscript at all
stages.

Associate Professor, Department of Restorative Dentistry, Division of Prosthodontics, Federal University of Santa Maria, Santa Maria, Brazil. Performed
the experiments, discussed results and commented on manuscript at all
stages.

Research Fellow, Department of Dental Materials and Prosthodontics, So

Paulo State University at So Jose dos Campos, Brazil. Performed the experiments, discussed results and commented on manuscript at all stages.

Vol 15, No 3, 2013

Submitted for publication: 27.12.12; accepted for publication: 19.03.13

Professor, Department of Dental Materials and Prosthodontics, So Paulo

State University at So Jose dos Campos, Brazil. Proofread manuscript, discussed results and commented on manuscript at all stages.

Associate Professor, Department of Prosthodontics, Faculty of Dentistry,

Dumlupinar University, Kutahya, Turkey. Performed the experiments, discussed results and commented on manuscript at all stages.

Correspondence: Prof. Dr. med. dent. Mutlu zcan, University of Zrich, Dental Materials Unit, Center for Dental and Oral Medicine, Clinic for Fixed and
Removable Prosthodontics and Dental Materials Science, Plattenstrasse 11,
CH-8032, Zrich, Switzerland. Tel: +41-44-63-45600, Fax: +41-44-63-44305.
e-mail: mutluozcan@hotmail.com

207

zcan et al

he clinical indication of fixed dental prostheses

(FDPs) made of a zirconia framework veneered with
a glassy matrix ceramic has increased over the last decade due to the improved implementation of CAD/CAM
procedures in dentistry. However, almost all clinical
studies to date have reported chipping of veneering ceramic at varying rates regardless of the type of veneering ceramic used.13 Undertaking repair actions in cases
of chipping, using surface conditioning methods and
adhesion promoters, may prolong the survival of such
failed FDPs, depending on the size of the defect.11
Etching with hydrofluoric acid gel followed by silanization is a well-established conditioning method to promote
adhesion of resin-based materials to feldspathic, leucite,
and lithium disilicate ceramics.1,3 In contrast, densely
sintered all-ceramics such as zirconia and alumina are
resistant to acid etching. Etching such ceramics does
not promote significant topographical changes that would
achieve proper micromechanical bonding of resin materials.14 In order to optimize adhesion, air-borne particle
abrasion of acid resistant ceramics with either aluminum
oxide (Al2O3) or tribochemical silica coating methods followed by silanization are suggested.12 Silane coupling
agents improve wettability and promote covalent bonding,
enhancing the chemical adhesion between the ceramics and resin composite.8 Thus, in a chipping scenario
of a zirconia FDP veneered with glass ceramic, different
conditioning methods are indicated for the two different
ceramic substrates. It can be anticipated that especially
when the zirconia framework is exposed, achieving durable repair may be more challenging. Furthermore, surface
conditioning methods employed for each ceramic type
may cross contaminate one another. The question then
arises as to what the best clinical conditioning strategy
for repairing the zirconia core/veneering ceramic complex
may be. A recent review of the intraoral repair of veneering
porcelain chipping of FDPs7 indicated a limited number of
studies dealing with silicate/oxide/metal alloy combined
surfaces.2,4,5,9,10 According to this review and the authors best knowledge, there is one study on the fatigue
resistance of repaired zirconia crowns2 and none on the
repair bond strength of resin materials on the zirconia /
veneer ceramic complex to date.
The objectives of this study were thus to determine the
most effective surface conditioning protocol for the repair
strength of a resin composite to the zirconia core / veneering ceramic complex and to identify the failure modes. The
null hypothesis tested was that different surface conditioning methods would not affect the repair bond strength.

MATERIALS AND METHODS

Disk-shaped zirconia (Lava Zirconia, 3M ESPE; Seefeld,
Germany) (: 3 mm) specimens were veneered circumferentially (thickness: 2 mm) with a feldspathic ceramic
(VM7, Vita Zahnfabrik; Bad Sckingen, Germany) using
a split metal mold. The mold allowed the zirconia core
ceramic disk to be positioned exactly in the middle of
the mold, leaving circular space around the core for the
208

veneering ceramic that was applied in two stages due

to the shrinkage after firing. Procedures for firing were
performed according to the veneering ceramic manufacturers instructions.
The specimens were then embedded in autopolymerizing acrylic with the bonding surfaces exposed. All specimens were wet ground down to 1200-grit silicon carbide
paper (SiC) (Struers; Willich, Germany) for 5 min. The
specimens were ultrasonically cleaned in distilled water
for 10 min, dried, and randomly assigned to one of the
following surface conditioning protocols (N = 40, n = 10
per group).
Group 1: First, the veneering ceramic was etched with
4% hydrofluoric acid (HF) (Porcelain Etch, Ultradent Products; South Jordan, UT, USA) for 90 s, rinsed with air-water spray, and dried. Then, the zirconia core was air-borne
particle abraded using an intraoral air-abrasion device
(Microetcher, Danville Engineering; San Ramon, CA, USA)
with 50-m Al2O3 (Korox, Bego; Bremen, Germany) perpendicular to the surface from a distance of approximately
10 mm for 20 s in circling motions at 2.8 bar. After air
abrasion, the remnants of the sand particles were gently
air blown for 20 s.
Group 2: First, the zirconia core was air abraded; then
the veneering ceramic was HF etched as described in
group 1. The nozzle of the air-abrasion device was aimed
at the zirconia core material. During this process, the
veneering ceramic was not protected.
Group 3: First, the veneering ceramic was HF etched;
then the zirconia core was air abraded as described in
group 1. In this group, instead of ordinary alumina particles, 30-m alumina particles coated with silica (SiO2)
were used (CoJet Sand, 3M ESPE).
Group 4: First, the zirconia core and then the veneering
ceramic was conditioned as described in group 3.
Core and veneering ceramic were conditioned individually, but no attempt was made to avoid cross contamination of either conditioning method. This simulates the
clinical intraoral situation.
All specimens received one coat of silane coupling
agent (ESPE-Sil, 3M ESPE) which was left to sit for 5 min
to allow the condensation reaction of the silane. Subsequently, one coat of adhesive resin (VisioBond, 3M
ESPE) was applied to both the core and the veneer with a
microbrush, air thinned, and photopolymerized (800 mW/
cm2) for 40 s using a photopolymerization unit (Demetron
LC, SDS Kerr; Orange, CA, USA). Resin composite (Quadrant Posterior, Cavex Holland BV; Haarlem, Netherlands)
was then bonded onto both substrates using polyethylene
molds (inner diameter: 4.9 mm; height: 3 mm) and photopolymerized from the top for 40 s.
The specimens were then thermocycled for 6000 cycles (5C55C, dwell time 30 s, transfer time 5 s).6
Spontaneous debondings during thermocycling were assigned a value of 0 MPa.
Specimens were mounted in the jig of the universal
testing machine (Zwick ROELL Z2.5 MA 18-1-3/7; Ulm,
Germany) and a blade applied the shear force to the
bonded interface at a crosshead speed of 1 mm/min
until failure.
The Journal of Adhesive Dentistry

zcan et al

Failure modes were identified using an optical microscope (Stemi 2000-C, Carl Zeiss; Gttingen, Germany)
at 100X magnification. SEM (JSM-5500, JEOL; Tokyo,
Japan) images (75X) were obtained of representative failure types. Failure types were categorized as follows: a) adhesive failure between the repair composite and/or core
zirconia or veneering ceramic (ADHES); b) cohesive failure
of the repair composite covering core zirconia and/or veneering ceramic only (COHES-com); c) cohesive failure of
core zirconia and/or veneering ceramic only (COHES-cer);
cohesive failure of the veneering ceramic and repair composite (MIX).
The data were not normally distributed according to
the Kolmogorov-Smirnov test (_ = 0.05). Accordingly,
non-parametric analysis (Kruskal-Wallis test) was carried
out to determine the significant differences between the
groups. Multiple pairwise comparisons of the groups were
made using the Wilcoxon rank-sum test for independent
samples. Significance levels were adjusted using the Bonferroni Holm correction for multiple testing.

Repair Bond Strength (MPa)

12
10
8
6
4
2
0
Group 1A

Group 2A

Group 3B

Group 4A

Fig 1 Means and standard deviations of the repair bond

strength (MPa) of resin composite to the zirconia core / veneering ceramic core complex after 4 surface conditioning protocols. Same superscript letters indicate statistical similarity.

RESULTS

DISCUSSION

The surface conditioning protocol significantly affected

the results (p < 0.05). Spontaneous debondings occurred in groups 1 (5), 2 (4), and 4 (4). Group 3 demonstrated significantly higher values (MPa) (8.6 2.7)
than those of other groups (3.2 3.1, 3.2 3,
and 3.1 3.5 for groups 1, 2, and 4, respectively)
(p < 0.001) (Fig 1). Groups 1, 2, and 4 did not show significant differences (p > 0.05).
All groups showed exclusively adhesive failure between
the repair resin and the core zirconia. The incidence of
cohesive failure in the ceramic was the highest in group 3
(8 out of 10) compared to the other groups (0/10, 2/10,
2/10, in groups 1, 2, and 4, respectively) (Table 1, Fig 2).
SEM images showed microporosities of veneering ceramic after HF etching due to glassy matrix dissolution
(Fig 3a), but after silica coating of the zirconia core, the
veneering ceramic also received silica, and the topography was affected compared to etching only (Fig 3b).

Since hydrofluoric acid etching of the veneering ceramic

and silica coating of the zirconia core (group 3) presented significantly higher repair bond strength values
that those of the other groups, the null hypotheses was
rejected. Only this group had no spontaneous debondings. Similarly, the lack of adhesive failures in the
veneering ceramic and a higher incidence of cohesive
veneering ceramic failures indicates more reliable results with this protocol. Hydrolytic degradation of Al-O-Si
compared to Si-O-Si has been previously reported. 12
This can explain the spontaneous debondings during
thermocycling (ie, automatic adhesive failures) experienced in the alumina-treated groups combined with HF
treatment (groups 1 and 2). SEM findings also revealed
that the favorable etching pattern was influenced when
the sequence of veneer and core conditioning was
changed so that silica coating was applied after etching
the veneer. However, it must be noted that polishing the

Table 1 Distribution of the frequencies of failure types for experimental groups (n = 10)
Type of failure*
Zirconia core
Group

Veneering ceramic

ADHES

COHES-com

COHES-cer

MIX

ADHES

COHES-com

COHES-cer

MIX

10

10

10

10

ADHES: adhesive failure between the repair composite and/or core zirconia or veneering ceramic; COHES-com: cohesive failure of the repair composite covering core zirconia and/or veneering ceramic only; COHES-cer: cohesive failure of core zirconia and/or veneering ceramic only; MIX: cohesive failure of the
veneering ceramic and repair composite.

Vol 15, No 3, 2013

209

zcan et al

V
V

C
C
C

Fig 2 Representative images of a) adhesive failure between

the repair composite and/or core zirconia or veneering ceramic
(ADHES). Note that there was no remnant of repair composite on either substrate. b) Cohesive failure of the veneering
ceramic and repair composite (MIX). *cohesive failure of the
composite; ) cohesive failure of the veneering ceramic. C:
zirconia core; V: veneering ceramic.

Fig 3 Typical SEM images (75X) of zirconia core (C) and

veneering ceramic (V). a) After hydrofluoric acid etching only.
Note the microporosities after glassy matrix dissolution. b)
After hydrofluoric acid etching of V and silica coating of C. Note
that the veneering ceramic also received silica, and the topography changed compared to etching only.

core / veneer complex prior to any surface conditioning

method was performed simultaneously using SiC paper
for 5 min. Although no surface roughness measurements were made on either substrate ceramic, variation in the degree of roughness in both substrates can
be anticipated. But again, this represents the typical
clinical repair situation where the surfaces of both substrates are roughened at the same time for the same
duration before a repair resin is applied onto core and
veneer ceramics. Thus, baseline roughness of one of
the substrates may be higher than the other. Whether
baseline roughness plays a role after HF etching or air
abrasion needs to be further investigated.
In this study, 6000 thermocycles were performed in
order to age the resin/ceramic interface, which is slightly
above the recommended number of cycles (5000) according to the ISO norm for testing metal-resin adhesion.6
However, a prolonged duration of aging could have more
detrimental effects on the results.
On the whole, the results cannot be considered high
for the zirconia / veneer complex. Consequently, surface
conditioning methods that yield more reliable adhesion on
zirconia core have potential for development, where reliable adhesion to the zirconia / veneer complex is desired.

REFERENCES

CONCLUSIONS

12.

Etching the veneering ceramic with hydrofluoric acid gel

for 90 s, silica coating the zirconia core, followed by silane and adhesive resin application on both substrates
resulted in the highest repair strength of the resin composite to zirconia core / veneering ceramic complex.
Cohesive failure of the veneering ceramic, indicating
reliable adhesion, was observed more frequently when
the veneering ceramic was etched before the zirconia
core was silica coated. In all groups, exclusively adhesive failures between the resin composite and zirconia
indicate the weakest link exists between these two materials.
210

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Clinical relevance: Repair of chipping of the zirconia

core / veneering ceramic complex can best be achieved
by first conditioning the veneering ceramic with hydrofluoric acid, followed by silica coating of the zirconia core
ceramic. Subsequently, silane and adhesive resin need
to be applied on both ceramic substrates.

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