Ceramics International 43 (2017) 1272–1277

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Ceramics International
journal homepage: www.elsevier.com/locate/ceramint

Evaluation of shear bond strength of a novel nano-zirconia and veneering

ceramics
crossmark
a,⁎
Muhammad Hidayat Muhamad Dauda, Hsu ZennYew , Jasmina Qamaruz Zamana,
Norziha Yahayab, Andanastuti Muchtarc
a
Department of Operative Dentistry, Faculty of Dentistry, Universiti Kebangsaan Malaysia, Jalan Raja Muda Abdul Aziz, 50300 Kuala Lumpur, Malaysia
b
Department of Prosthodontic, Faculty of Dentistry, Universiti Kebangsaan Malaysia, Jalan Raja Muda Abdul Aziz, 50300 Kuala Lumpur, Malaysia
c
Department of Mechanical and Materials Engineering, Faculty of Engineering and Built Environment, Universiti Kebangsaan Malaysia, 43600 Bangi,
Selangor, Malaysia

A R T I C L E I N F O A BS T RAC T

Keywords: The core–veneer bond strength of zirconia is believed to be influenced by various factors, including zirconia
A. Slip casting types. To date, studies on bond strength between veneering porcelain and zirconia core fabricated by slip-cast
A. Milling technique are few. The aim of this study was to investigate and compare the shear bond strength (SBS) of three
D. ZrO2 core materials with two veneering porcelains. Sixty cylindrical discs (11 mm in diameter and 3 mm in thickness)
Shear bond strength
were fabricated and divided into Experimental zirconia (Zir), Cercon® (Cer) and metal (Met) core group.
Ceramkiss® (Ck) and InLine® (IL) veneering porcelains were fired to each core at a thickness of 3 mm. Before
veneering, all core materials were sandblasted with 100 µm Al2O3, and a layer of opaque liner was applied in the
first firing. The bonded samples were subjected to shear bond test following storage in distilled water (37 °C) for
24 h. Scanning electron micrograph (SEM) was used to identify the mode of bonding failure. The results were
analyzed with One-way ANOVA and Independent t-test with Tukey post-hoc test. Interaction effect analysis was
performed using two-way ANOVA. Met-IL showed the highest mean SBS value (28.9 ± 3.8 MPa), whereas Cer-
IL group obtained the lowest value (2.8 ± 0.7 MPa). The mean SBS values of Zir-Ck and Zir-IL were found to be
23.1 ± 2.4 MPa and 4.1 ± 0.9 MPa respectively. When veneered with the same veneering porcelain, both
experimental zirconia and Cercon® were comparable, whereas significant differences were observed between
metal and zirconia groups. All core materials exhibited significant differences in terms of shear bond strength
when veneered with different veneering ceramics. Cohesive failure occurred in the high SBS group, whereas
mixed cohesive-adhesive failures were seen in the other groups. The core–veneer SBS is material dependent.
The types of core and veneering materials significantly affected the SBS. Slip casted experimental zirconia and
commercial zirconia demonstrated similar bonding capabilities with the existing veneering porcelain designed
for zirconia core.

1. Introduction Despite the excellent mechanical properties of zirconia framework,

In recent years, zirconia has become widely accepted as the
restorative framework material of choice because of its excellent
mechanical properties. Zirconia is usually milled into a framework
using CAD/CAM (Computer Aided Design/Computer Assisted
Manufacturing) technology and is further layered with veneering
feldspathic porcelain to form a uniquely strong and aesthetic dental
restoration. Comparable survival rate of this restoration to metal-based
restoration has been found; approximately 85–100% of the CAD/CAM
milled zirconia prosthesis remains functional for 3–7 years [1–5].
technical complication such as veneering porcelain chipping is still
continuously reported after the zirconia-ceramic restoration is sub-
jected to loading [2,4,6–8]. A recent study has shown that almost 15%
clinical veneer chipping occurred after 7 years [4]; 32% of zirconia-
based restorations chipped compared with only 10% of metal-ceramic
restorations after 10 years [8]. The causes of clinical chipping are
multifactorial, as follows: flaws during fabrication, a low bond strength,
excessive occlusal load, and inadequate framework design [2,7,9].
Low bond strength was recorded as the main cause for veneer
chipping [9]. Coefficient of Thermal Expansion (CTE) mismatch

⁎
Corresponding author.
E-mail addresses: hidayat_daud@yahoo.co (M.H.M. Daud), hz_yew@ukm.edu.my (Y. Hsu Zenn), jasmina@ukm.edu.my (J.Q. Zaman), norzihayahaya@gmail.com (N. Yahaya),
muchtar@ukm.edu.my (A. Muchtar).

http://dx.doi.org/10.1016/j.ceramint.2016.10.076
Received 8 September 2016; Received in revised form 12 October 2016; Accepted 12 October 2016
Available online 12 October 2016
0272-8842/ © 2016 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
M.H.M. Daud et al.
[10,11], veneering porcelain thickness [12], and different types of
zirconia core and veneering ceramics, as well as different manufac-
turers [13] and poor wetting properties of zirconia core [9] played an
important role in development of residual stresses and weakening of
the bond strength at core–veneering porcelain interface. Bond strength
between zirconia and veneering porcelain was between 11 MPa [14]
and 34.3 MPa [15], as recorded in several studies for the last 10 years.
This wide range of shear values shows that zirconia-ceramic restoration
does not have any conclusive minimum bond strength and a standard
protocol for the test to be conducted in vitro. Most of the authors have
referred to the standard guideline available for metal-ceramic restora-
tions [16–19]. Many authors have tried several methods and materials
combinations to produce better core–veneer bonding. In addition, they
proposed a better formulation for zirconia manufacturing that could
achieve a satisfactory outcome and may reduce the chipping potential.
Recently, a novel nano-zirconia material has been developed by
means of controlled colloidal processing and slip cast technique [20].
This is the first time this technique has been used to fabricate 100 wt%
nano-zirconia material. This material claimed to produce denser, more
homogenous slurry with minimal porosity [20], which is difficult to
achieve during commercial zirconia fabrication. Furthermore, mechan-
ical properties of nano-zirconia fabricated by both slip cast and
commercial dry-press techniques have shown comparable findings
[20–23].
Therefore, there is a great potential for this novel zirconia to be
used as an alternative to the currently available dental zirconia and to
subsequently reduce the clinical failure. However, a limited study
specifically examined the core–veneer bond strength of zirconia
fabricated by colloidal process and slip cast technique. The evidence
to compare the core–veneer bond strength produced by this technique
and other manufacturing methods are also lacking. Thus, the aims of
this study were to investigate the bond strength of slip casted
experimental nano-zirconia with different commercially available ve-
neering ceramics by shear bond test and to observe the mode of
bonding failure.
2. Experimental procedure
2.1. Materials
The study utilized 3 core systems (Metal, Cercon and Experimental
zirconia) and 2 veneering materials (InLine and Ceramkiss) with six
core–veneer combinations (Fig. 1) where 10 samples fabricated for
each combination group. Samples included in the study were free from
macroscopic cutting defects after the sintering process, and the desired
geometry was achieved (11 mm diameter and 3 mm thickness).
Deformed or fractured samples during manufacturing or sintering
process with poor attachment to lateral arms of the jig at universal
testing machine were excluded from the study.
2.2. Core preparation
The experimental zirconia was fabricated via colloidal process and
slip-cast technique. Powder at 40 g (50 nm) was ultrasonically mixed
with 45 ml distilled water to form an aqueous solution. Two molar of
nitric acid (HNO3) were added in the mixture to get a more stable pH.
Then, 100 ml (0.5 wt%) polyethyleneimine (PEI) were pipetted in the
mixture to disperse the agglomerated zirconia particles and stirred
under magnetic vibrator (IKA Color Squid Magnetic®) for 45 min. The
homogenous aqueous solution was poured into 12 teflon molds
(15 mm diameter and 4 mm thickness) and left in situ for 24 h. The
samples were eventually sintered at 1400 °C for 2 h to obtain the final
geometry [20].
Commercial zirconia discs were prepared by milling 20 Cercon®
blocks in CAD/CAM machine (Cercon Brain®). Afterward, all samples
were sintered at 1350 °C for 1.5 h to obtain a standardized geometry of
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Ceramics International 43 (2017) 1272–1277
samples. Metal-ceramic combination was used as a control group. The
lost wax technique was used to fabricate the metal cores. Wax patterns
(20 discs) corresponding to final geometry of samples were fabricated
and sprued onto cylindrical holder. De-waxing process was carried out,
and the created channel was filled with semiprecious noble metal alloy
(Lodestar, Ivoclar Vivadent) during casting. Afterward, the sprued
metal was de-invested, ground, and polished with diamond coated
polishing burs [18,24,25].
All samples were sandblasted with 110 µm aluminium oxide
particles at 4 bars and at 10 mm distance from nozzle to the core
surface at a perpendicular position and immediately steam-cleaned to
create adequate surface roughness [26–28].
2.3. Veneering process
Prior to veneering the porcelain, a thin layer of veneering opaque
was painted on the bonding core surface area and sintered. Then,
powder and liquid of the veneering ceramics (InLine® and Ceramkiss®)
were mixed using a ratio recommended by the manufacturer to form a
slurry mixture. The mixture was then manually packed onto a core
surface by using a metal split mold. The air bubbles and water particles
were removed by blotting with a clean thin cloth.
The core–veneer assemblies were placed in a furnace (Programat
P500, Vivadent®) and fired at specific temperature and condition under
respective Ceramkiss® or InLine® programmes [29,30]. Double firing
was carried out to compensate the shrinkage to obtain the required
3 mm by 3 mm veneer geometry [24,25]. Slow cooling was applied [31]
and all samples were steam-cleaned. Samples were further cleaned
with distilled water ultrasonically for 30 min and stored in water at
37 °C for 24 h [24,25].
2.4. Determination of shear strength value
The test was conducted by using Universal Testing Machine (UTM;
Shimadzu®, Japan) with a 5 kN load cell. Ortho-polymerized acrylic
resin was fabricated to hold the samples to the UTM. Shearing process
was carried out at crosshead speed of 0.5 mm per min until all samples
debonded (Fig. 2). The bond strengths was calculated [load (N)/area
(mm2)] and recorded as megapascals (MPa) [27,32]. Representative
debonded samples from every group were subjected to scanning
electron microscope (SEM) (Fei Quanta 200). After being sputter-
coated with gold-platter for 30 s, the samples were observed at ×50
magnification at the center of the debonded area to observe the mode
of bonding failure (adhesive, cohesive, and mixed adhesive/cohesive)
[33].
Previous studies [14,25] were carried out with 10–15 samples. This
study was designed to have 90% statistical power based on the results
from preliminary test with sample size of 10 per core–veneer assem-
blies. Independent t-test was used to analyze the comparison within
core groups and one-way ANOVA with Tukey's post-hoc test were used
to compare within the veneering porcelain groups. The interaction
effects between cores, veneers and core–veneer combinations were
determined by two-way ANOVA analysis. The level of significance for
all statistical testing was pre-determined at a p-value of 0.05 or less.
3. Results and discussion
3.1. Comparison of SBS of slip casted experimental nano-zirconia,
commercial nano-zirconia (cercon®) and metal to ceramkiss® and
inline® veneering ceramics
Results of this study appeared to be normally distributed based on
statistical Shapiro-Wilk test and Kurtosis value for all tested groups
that fall between −2 and +2.
The mean SBS values for six core–veneer assemblies are presented
in Table 1. Zir-Ck was comparable to Cer-Ck but slightly lower than
M.H.M. Daud et al. Ceramics International 43 (2017) 1272–1277

Fig. 1. Flow chart of sample preparations.

recommended minimal value for metal-ceramic restoration (25 MPa)

[16]. However, ‘adequate bond strength’ for all-ceramic restorations
has yet to be determined. The highest mean SBS value recorded for
Met-IL, whereas Cer-IL group obtained the lowest value. Both Zir-IL
and Met-Ck groups performed poorly with SBS value of less than
10 MPa.
Cercon® and Ceramkiss® (Cer-Ck) produced mean SBS value (18.6
± 2.5 MPa) in the same range (20.2 ± 5.1 MPa to 27.2 ± 3.4 MPa) as
other studies with the same test design and surface conditions [34,35].
However, Guess et al. [14] reported half of the value acquired in this
Fig. 2. Mounted shear blade and sample on Universal Testing Machine (Shimadzu®). study probably because of the use of the Schmitz-Schulmeyer test
method with larger rectangular specimens. On the contrary,
Table 1 Aboushelib et al. [36] obtained approximately twofold higher value
Mean shear bond and standard error in megapascal (MPa) unit in different core–veneer than the value presented in this study. The use of stronger pressed-on
systems.
veneering ceramics and different test design (microtensile bond
Core–veneer combinations Mean Bond Strength (SE) strength test) may have accounted for this result.
Based on two-way ANOVA analysis, significant differences were
Zir-IL 4.1 (0.91) noted within each core and veneering porcelain groups as presented in
Zir-Ck 23.1 (2.43)
Table 2. Further Tukey's post-hoc test revealed that metal and Cercon®
Cer-IL 2.8 (0.67)
Cer-Ck 18.6 (2.54) core groups contributed to the significant difference of SBS value when
Met-IL 28.9 (3.75) being veneered with either porcelain materials. Similarly, significant
Met-Ck 7.2 (2.3) difference within the veneering porcelain groups was also noted where
the differences were observed between metal and zirconia (experi-
SE: Standard error
mental and Cercon) groups. There were no significant differences
between the experimental zirconia and Cercon® groups when either
veneering porcelain was used. Significant interaction or strong rela-

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Table 2 Table 4
Interaction effects within and between core–veneer systems. Co-efficient of thermal expansion (CTE) of core and veneer materials.

Tested Material Sig. Material CTE (10−6/C)

Core Metal *0.01a Core The experimental zirconia N/A

Cercon® Cercon® 9.5
Experimental zirconia Metal 13.8

Veneer InLine® *0.03a Veneering porcelain Ceramkiss® 9.2

Ceramkiss® InLine® 12.4
b
Core*Veneer *P < 0.001

Two-way ANOVA analysis considered adequate [14,25]. The use of a framework material with a
*a as indication of statistical significant difference with a p value of less than 0.05
slightly higher CTE creates positive CTE mismatch, thereby resulting in
*b as indication of statistical significant difference with a p value of less than 0.001
desirable residual compressive stress in the weaker veneering porcelain
and enhancing the overall strength of the assemblies [17]. The slight
Table 3
Pairwise comparison of SBS between and within core–veneer assembly group.
positive CTE mismatch found between Cercon® and Ceramkiss® (Cer-
Ck) as well as between metal and InLine® (Met-IL) (Table 4) may have
Core– Bond Strength Between Bond Strength p value been the reason for the superior bond strength reported in these
veneer Value (MPa) Group Value (MPa) groups.
* In contrast, the CTE of Cercon® is lower than InLine®, resulting in
Met-IL 28.9 Zir-IL 4.1 < 0.008
Cer-IL 2.8 *
< 0.008 negative CTE mismatch. The lowest SBS values achieved by Cer-IL
Met-Ck 7.2 *
< 0.008 combinations in the current study may be attributed to this negative
CTE variance. This result is consistent with observation made by
Zir-Ck 23.1 Cer-Ck 18.6 0.22
Aboushelib et al. [17] in which delamination of the veneer and
Met-IL 28.9 0.21
Zir-IL 4.1 *
< 0.008
formation of microcracks was observed when CTE of the veneering
porcelain is higher than that of the zirconia framework. The vast CTE
Cer-Ck 18.6 Met-IL 28.9 0.35 discrepancy between metal and Ceramkiss® (Met-Ck; more than
4.6×10−6/°C) may contribute to the inferior SBS of the group.
*
Zir-IL 4.1 < 0.008
*
Cer-IL 2.8 < 0.008
However, CTE for experimental zirconia has yet to be determined.
Met-Ck 7.2 Zir-Ck 23.1 *
< 0.008 It may be assumed that the value approximates that of Cercon® based
Cer-Ck 18.6 *
0.003 on the SBS obtained with Ceramkiss®. Further microstructural analyses
of the interface between the experimental zirconia and veneering
Zir-IL 4.1 Cer-IL 2.8 0.24
porcelain are required to better establish the role of stresses induced
Met-Ck 7.2 0.23
from the thermal expansion.
Cer-IL 2.8 Met-Ck 7.2 0.08
*
Zir-Ck 23.1 < 0.008 3.2. Determination of mode of bonding failure

Independent t-test analysis.

* The mode of bonding failure for the superior groups with SBS value
Indication for statistical significant difference with a p value of less than 0.00833
after Bonferroni correction.
tionship between cores and veneering ceramics was also observed.
On top of that, all core materials showed significant differences in
the SBS when veneered with different veneering ceramics with a p
value of less than 0.008 after Bonferroni correction (Table 3). For both
experimental zirconia and Cercon®, the use of Ceramkiss® as veneering
porcelain resulted in significantly higher SBS values than when these
cores were veneered with InLine®. When veneered to the same
veneering porcelain (either Ceramkiss® or InLine®), no significant
difference was found in the SBS between the experimental zirconia
and Cercon®. However, significant differences between zirconia and
metal groups were found if identical veneering ceramic was used (Met-
IL, Zir-IL, and Cer-IL).
Overall, no significant difference was found among the superior
core–veneer groups with bond strength of more than 18 MPa (Zir-Ck,
Cer-Ck and Met-IL). Similar findings were also found amongst the
inferior core–veneer groups with less than 8 MPa (Zir-IL, Cer-IL, and
Met-Ck). Nevertheless, when comparing the superior and inferior
core–veneer groups, significant differences were documented (Table 3).
Statistical interaction analysis in this study confirmed that the
core–veneer bond strength was material dependent. Many authors
identified co-efficiency of thermal expansion (CTE) as one of the
properties affecting the bond strength [14,37–39]. The general con-
sensus agreed that CTE of the framework material should closely match
the layering porcelain [14,17,35,40]. A CTE mismatch of approxi-
mately 0.5 to 1.0×10−6/°C between core and veneering porcelain is
of more than 18 MPa were found to be cohesive failure as majority area
of core surfaces were covered by veneers after shear bond test
[Fig. 3(a), (c), and (e)]. Meanwhile, mixed cohesive-adhesive failure
was observed on inferior groups with SBS value of less than 8 MPa
[Fig. 3(b), (d), and (f)].
Under magnification of ×50, only Zir-Ck and Met-Ck groups
[Fig. 3(a) and (f)] presented with generalized residual veneers at the
periphery of shearing zone. By contrast, in all other groups, the
remaining veneers appear to be thicker and are confined to a localized
area [Fig. 3(b), (c), (d), and (e)]. All zirconia groups [Fig. 3(a), (b), (c),
and (d)] exhibited surface irregularities to a certain degree. Surface
roughness including grooves and trace lines [41] were more evident in
both Cercon® groups. The irregularities on the surfaces of experimental
zirconia and Cercon® may be created during grinding and milling
process, respectively. Metal groups demonstrated a more homogenous
characteristic [Fig. 3(e) and (f)].
4. Conclusions
Within the limitations of this study, experimental zirconia displayed
comparable results to that of a commercially available zirconia
(Cercon®) when veneered with the same veneering porcelain. Based
on the SBS results, it can be concluded that zirconia fabricated by
means of slip casting or compaction technique possesses similar
bonding capabilities with veneering porcelain. The core–veneer bond
strength appears to be material-dependent. If veneering porcelain
specific to the core material is used, no significant difference in the
SBS was found between the experimental zirconia, Cercon® and metal.

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Fig. 3. SEM images analysis of core–veneer assembly groups.
The result of this study also reflects the important role of CTE in both
core–veneer materials. The clinical implication of these outcomes is
that the selection of veneering porcelain specific to the core and vice-
versa is crucial in determining core–veneer bond strength.
Combinations of core and veneer with superior SBS displayed cohesive
failures in the veneering porcelain, whereas mixed cohesive and
adhesive failures occur in inferior SBS assemblies.
Acknowledgments
The authors acknowledge the Universiti Kebangsaan Malaysia
(UKM) and Pusat Pengurusan Penyelidikan & Instrumentasi (CRIM)
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Ceramics International 43 (2017) 1272–1277
for their sponsorship under the Geran Galakan Penyelidik Muda
(GGPM-2014-051).
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