Effect of Surface Conditioning Modalities on the

Repair Bond Strength of Resin Composite to the

Zirconia Core / Veneering Ceramic Complex
Mutlu Özcana / 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 ex-
posed. 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-μm Al2O3)  + 
core + veneer: silane (ESPE-Sil); group 2: core: Al2O3 (50 μm) + veneer: HF + core + veneer: silane; group 3: ve-
neer: HF + core: 30 μm aluminum trioxide particles coated with silica (30 μm SiO2) + core + veneer: silane; group
4: core: 30 μm 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, 5°C–55ºC), 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 exclu-
sively 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: 207–210. Submitted for publication: 27.12.12; accepted for publication: 19.03.13
doi: 10.3290/j.jad.a29717

a 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.
b Associate Professor, Department of Restorative Dentistry, Division of Prosth-
odontics, Federal University of Santa Maria, Santa Maria, Brazil. Performed
the experiments, discussed results and commented on manuscript at all
stages.
c
Research Fellow, Department of Dental Materials and Prosthodontics, São
Paulo State University at São Jose dos Campos, Brazil. Performed the experi-
ments, discussed results and commented on manuscript at all stages.
d Professor, Department of Dental Materials and Prosthodontics, São Paulo
State University at São Jose dos Campos, Brazil. Proofread manuscript, dis-
cussed results and commented on manuscript at all stages.
e Associate Professor, Department of Prosthodontics, Faculty of Dentistry,
Dumlupinar University, Kutahya, Turkey. Performed the experiments, dis-
cussed results and commented on manuscript at all stages.
Correspondence: Prof. Dr. med. dent. Mutlu Özcan, University of Zürich, Den-
tal Materials Unit, Center for Dental and Oral Medicine, Clinic for Fixed and
Removable Prosthodontics and Dental Materials Science, Plattenstrasse 11,
CH-8032, Zürich, Switzerland. Tel: +41-44-63-45600, Fax: +41-44-63-44305.
e-mail: mutluozcan@hotmail.com

Vol 15, No 3, 2013 207

Özcan et al
T he clinical indication of fixed dental prostheses
(FDPs) made of a zirconia framework veneered with
a glassy matrix ceramic has increased over the last de-
cade due to the improved implementation of CAD/CAM
procedures in dentistry. However, almost all clinical
studies to date have reported chipping of veneering ce-
ramic at varying rates regardless of the type of veneer-
ing 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 silaniza-
tion 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 materi-
als.14 In order to optimize adhesion, air-borne particle
abrasion of acid resistant ceramics with either aluminum
oxide (Al2O3) or tribochemical silica coating methods fol-
lowed by silanization are suggested.12 Silane coupling
agents improve wettability and promote covalent bonding,
enhancing the chemical adhesion between the ceram-
ics 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 dura-
ble 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 au-
thors’ 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 / veneer-
ing ceramic complex and to identify the failure modes. The
null hypothesis tested was that different surface condi-
tioning methods would not affect the repair bond strength.
MATERIALS AND METHODS
Disk-shaped zirconia (Lava Zirconia, 3M ESPE; Seefeld,
Germany) (Ø: 3 mm) specimens were veneered circum-
ferentially (thickness: 2 mm) with a feldspathic ceramic
(VM7, Vita Zahnfabrik; Bad Säckingen, 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 manufac-
turer’s instructions.
The specimens were then embedded in autopolymer-
izing acrylic with the bonding surfaces exposed. All speci-
mens 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 Prod-
ucts; South Jordan, UT, USA) for 90 s, rinsed with air-wa-
ter 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-µm Al2O3 (Korox, Bego; Bremen, Germany) per-
pendicular 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 par-
ticles, 30-µm 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 individu-
ally, but no attempt was made to avoid cross contamina-
tion 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. Sub-
sequently, 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 (Quad-
rant Posterior, Cavex Holland BV; Haarlem, Netherlands)
was then bonded onto both substrates using polyethylene
molds (inner diameter: 4.9 mm; height: 3 mm) and pho-
topolymerized from the top for 40 s.
The specimens were then thermocycled for 6000 cy-
cles (5°C–55ºC, dwell time 30 s, transfer time 5 s).6
Spontaneous debondings during thermocycling were as-
signed 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
 Özcan et al

Failure modes were identified using an optical micro-

Repair Bond Strength (MPa)
scope (Stemi 2000-C, Carl Zeiss; Göttingen, Germany) 12
at 100X magnification. SEM (JSM-5500, JEOL; Tokyo,
Japan) images (75X) were obtained of representative fail- 10
ure types. Failure types were categorized as follows: a) ad-
hesive failure between the repair composite and/or core 8
zirconia or veneering ceramic (ADHES); b) cohesive failure
of the repair composite covering core zirconia and/or ve- 6
neering ceramic only (COHES-com); c) cohesive failure of
core zirconia and/or veneering ceramic only (COHES-cer); 4
cohesive failure of the veneering ceramic and repair com-
posite (MIX). 2
The data were not normally distributed according to
the Kolmogorov-Smirnov test (! = 0.05). Accordingly, 0
non-parametric analysis (Kruskal-Wallis test) was carried Group 1A Group 2A Group 3B Group 4A
out to determine the significant differences between the
groups. Multiple pairwise comparisons of the groups were Fig 1 Means and standard deviations of the repair bond
made using the Wilcoxon rank-sum test for independent strength (MPa) of resin composite to the zirconia core / ve-
neering ceramic core complex after 4 surface conditioning pro-
samples. Significance levels were adjusted using the Bon-
tocols. Same superscript letters indicate statistical similarity.
ferroni Holm correction for multiple testing.

RESULTS DISCUSSION

The surface conditioning protocol significantly affected
the results (p < 0.05). Spontaneous debondings oc-
curred in groups 1 (5), 2 (4), and 4 (4). Group 3 dem-
onstrated 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 sig-
nificant 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 cer-
amic 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 topogra-
phy 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) pre-
sented significantly higher repair bond strength values
that those of the other groups, the null hypotheses was
rejected. Only this group had no spontaneous debond-
ings. Similarly, the lack of adhesive failures in the
veneering ceramic and a higher incidence of cohesive
veneering ceramic failures indicates more reliable re-
sults 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) experi-
enced 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 Veneering ceramic
Group ADHES COHES-com COHES-cer MIX ADHES COHES-com COHES-cer MIX

1 10 0 0 0 5 5 0 0

2 10 0 0 0 4 4 2 3

3 10 0 0 0 0 2 8 5

4 10 0 0 0 4 4 2 0

ADHES: adhesive failure between the repair composite and/or core zirconia or veneering ceramic; COHES-com: cohesive failure of the repair composite cov-
ering 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

Özcan et al
V * V
C C
a b ! a
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 compos-
ite 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.
core / veneer complex prior to any surface conditioning
method was performed simultaneously using SiC paper
for 5 min. Although no surface roughness measure-
ments were made on either substrate ceramic, varia-
tion 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 sub-
strates 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) accord-
ing 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 reli-
able adhesion to the zirconia / veneer complex is desired.
CONCLUSIONS
Etching the veneering ceramic with hydrofluoric acid gel
for 90 s, silica coating the zirconia core, followed by si-
lane and adhesive resin application on both substrates
resulted in the highest repair strength of the resin com-
posite 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 adhe-
sive failures between the resin composite and zirconia
indicate the weakest link exists between these two ma-
terials.
210
V V
C
C
b
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 topog-
raphy changed compared to etching only.
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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 hydroflu-
oric acid, followed by silica coating of the zirconia core
ceramic. Subsequently, silane and adhesive resin need
to be applied on both ceramic substrates.
The Journal of Adhesive Dentistry