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Effect of Different Surface Treatments on the Bond Strength of Lithium

Disilicate Ceramic to the Zirconia Core

Article in Photomedicine and Laser Surgery · April 2016

DOI: 10.1089/pho.2015.4063

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Photomedicine and Laser Surgery
Volume 34, Number 6, 2016
ª Mary Ann Liebert, Inc.
Pp. 236–243
DOI: 10.1089/pho.2015.4063

Effect of Different Surface Treatments on the Bond

Strength of Lithium Disilicate Ceramic to the Zirconia Core

Tuba Yilmaz-Savas, DDS, PhD,1 Necla Demir, DDS, PhD,1 A. Nilgun Ozturk, DDS, PhD,1
and Hamdi Sukur Kilic, PhD2

Abstract

Objective: The aim of this study was to evaluate the effect of different surface treatments [sandblasting,
Erbium:Yttrium–Aluminium–Garnet (Er:YAG), and femtosecond lasers] on the shear bond strength (SBS) of
the CAD-on technique. Background data: Although demand for all-ceramic restorations has increased, chip-
ping remains one of the major problems for zirconia-based restorations. Materials and methods: Forty yttrium-
stabilized tetragonal zirconia polycrystalline (Y-TZP) zirconia plates (IPS e.max ZirCAD, Ivoclar Vivadent)
were cut, sintered (12.4 · 11.4 · 3 mm) and divided into four groups according to the surface treatments (n = 10):
a control group with no surface treatment (Group C), sandblasting with 50 lm Al2O3 (Group S), Er:YAG laser
irradiation (Group E), and femtosecond laser irradiation (Group F). Also, 40 cylindrical (5 mm diameter, 2 mm
height) lithium disilicate (IPS e.max CAD) veneer ceramics were cut and fused to all zirconia cores by a glass-
fusion ceramic and crystallized according to the CAD-on technique. Specimens were subjected to shear force
using a universal testing machine. The load was applied at a crosshead speed of 0.5 mm/min until failure. Mean
SBS (MPa) were analyzed with one way ANOVA ( p < 0.05). The failed specimens were examined under a
stereomicroscope at ·20 to classify the mode of failure. Results: The highest SBS was observed in Group F
(36 – 3.31 MPa), followed by Group S (33.03 – 5.05 MPa), and Group C (32.52 – 10.15 MPa). The lowest SBS
was observed in Group E (31.02 – 4.96 MPa), but no significant differences were found between the control and
surface treated groups ( p = 0.377). All the specimens showed a mixed type of failure. Conclusions: Femto-
second laser application increased the bond strength between zirconia-veneer specimens. However, the novel
CAD-on technique with no surface treatment also showed high bonding strength. Thus, this technique could
prevent ceramic chipping without additional surface treatments.

Introduction technology.7,8 This technique involves designing and milling

both zirconia core and high-strength veneering ceramic

Z irconia ceramics, including yttrium-stabilized te-

tragonal zirconia polycrystalline (Y-TZP), have become
an alternative to metals as a core material for veneered anterior
and posterior fixed dental prosthesis (FDP) because of their
biocompatibility, white color, inherent strength, transforma-
tion toughening, and relative translucency.1–4 Because of the
white color, a veneering material must be used to achieve
adequate aesthetics for zirconia cores.4 There are well-known
techniques for veneering zirconia cores such as the traditional
layering technique and the overpressing technique.5,6 In ad-
dition to these veneering techniques, a new veneering method
has been introduced with a generic term CAD-on, which
combines the advantages of zirconia ceramics and computer-
aided design/computer-aided manufacturing (CAD/CAM)
through CAD/CAM. After the milling process, the zirconia
core and its corresponding veneer ceramic fuse each other by
a glass-fusion ceramic, and are subjected to crystallization/
fusion process according to manufacturer’s intructions.7,8
However, delamination (complete debonding of the veneer
ceramics) and/or chipping (superficial cohesive fractures) of
the veneering ceramic were reported by the majority of the
studies as the most frequent complications affecting zirconia-
based restorations.9,10 Sailer et al.11 reported the veneer ce-
ramic failure rate to be 25% in a 3-year follow-up randomized
controlled clinical trial. Chipping of the veneering ceramic
can be attributed to several factors such as thermal mismatch
between the core and veneering ceramics,12 an adequate
cooling rate,13,14 uniform veneer thickness,15 framework

1
Faculty of Dentistry, Department of Prosthodontics, Selcuk University, Konya, Turkey.
2
Faculty of Science, Department of Physics, Selcuk University, Konya, Turkey.

236
BOND STRENGTH OF ZIRCONIA WITH SURFACE TREATMENTS
design,16 veneering techniques, and strength of the veneer
ceramic.17,18 The definitive reason for veneer chipping is still
unclear; however, a durable bonding at the core–veneer in-
terface seems necessary to reduce ceramic chipping for
zirconia-based restorations.18,19
To achieve an adequate and stable interfacial bonding
between the core–veneer interfaces, various surface condi-
tioning methods are used nowadays. These methods are
grinding,20 sandblasting with aluminum oxide (Al2O3),21,22
tribochemical silica coating,23,24 hydrofluoric (HF)-acid
etching,25,26 and laser irradiation.1,27,28
Sandblasting can increase the surface roughness, provides
micromechanical undercuts, cleans the zirconia surface, and
increases the surface energy and wettability, which can
improve the adhesion of the zirconia ceramics.29,30
Laser irradiation is a promising technique for the surface
treatment of Y-TZP ceramic.31 The Erbium:Yttrium–
Aluminium–Garnet (Er:YAG) laser is used in clinical den-
tistry applications, especially for the ablation of the dental
hard tissues.32–34 It is also used for surface conditioning for
dental materials,35–37 to increase surface roughness for ob-
taining adequate bonding strength.38
Femtosecond technology is an innovative laser technol-
ogy that can be used for multiple applications with its ul-
trashort light pulses.39 It has been used in a broad range of
applications, from waveguide fabrication to cell ablation,40
and has been tested as an alternative tool for orthodontics
and dental surgery during the last decade.41 Delgado-Ruiz
et al.2 reported that surface roughness of zirconia could
increase by using femtosecond laser microstructuring. They
also concluded that zirconia did not exhibit phase transfor-
mation, resulting in a surface that retains its characteristics
permanently. A recent study also showed that femtosecond
laser application is an effective method for roughening
surfaces of zirconia ceramics and increasing the bond
strength between zirconia and resin cement.27
There is lack of information about surface treatment of
zirconia ceramics by femtosecond laser and its bonding
strength with veneering ceramic. In the literature, there are
only a few studies about bond strength of zirconia core and
lithium disilicate ceramic in the CAD-on technique, and no
surface treatments were used in that studies.16,42 Also, there
is no study about the bond strength of the CAD-on technique
with which the zirconia core surfaces were treated with
sandblasting, Er:YAG, and femtosecond lasers. Therefore,
the aim of this study was to compare and evaluate the effects
of sandblasting, Er:YAG, and femtosecond lasers on shear
bond strength (SBS) between the zirconia core and ve-
neering ceramic by using the CAD-on technique. The null
hypothesis is that the application of different surface treat-
ments to the zirconia core does not affect the bond strength
between the zirconia core and the veneer ceramic.
Materials and Methods
Forty zirconia specimens (11.4 mm · 12.4 mm · 3 mm)
were cut from presintered zirconia blocks (IPS e.max Zir-
CAD, Ivoclar Vivadent) by using a slow-speed diamond saw
(Isomet, Buehler Ltd, Lake Bluff, IL) under water cooling
and sintered according to the manufacturer’s instructions.
All sintered zirconia specimens were wet-polished with 600
grit silicon carbide paper. The surfaces were cleaned with
237
ethanol and air dried. The zirconia cores were then cleaned
ultrasonically with distilled water for 10 min and air dried
before surface treatments. The specimens were randomly
divided into four experimental groups (n = 10 each).
Surface treatments
Group C (control). No surface treatment was applied to
the zirconia ceramic surfaces, and thus this group served as
a control.
Group S (sandblasting). The bonding area of the zirco-
nia ceramics were abraded with 50 lm Al2O3 particles with
a sandblasting machine (Korox; Bego, Bremen, Germany) at
a pressure of 3 bar from a distance of *10 mm for 10 sec.
Group E (Er-YAG laser irradiation). To irradiate the
zirconia ceramic surfaces, an Er:YAG laser (Fotona, At
Fidelis, Ljubljana, Slovenia) was used. A noncontact, 90
degree angled handpiece (HP R02-C, Fotona) was used
perpendicular to the zirconia ceramic surface with a working
distance of 1 mm, and the bonding area was scanned for
20 sec under cooling by using an air-water spray. Er:YAG
irradiation parameters were: 75 ls pulse duration with
300 mJ pulse energy, 6 W power setting, 20 Hz pulses/sec,
and 10.60 J/cm2 energy density.
Group F (Femtosecond laser irradiation). Femtosecond
laser pulses from an amplifier (Integra-C-3.5; Quantronix,
NY) were applied to the bonding area of the zirconia ce-
ramic surfaces with random pattern type, and the laser was
passed through the same line 10 times. The femtosecond
laser parameters were as follows: The wavelength of the
laser beam was 800 nm, 730 mW/pulse, and pulses at 90 fs
with 30 mm/sec scanning speed with a 1 kHz repetition rate
for 496 sec, and energy density was 57 J/cm2 with 25% re-
petitive pulse overlap. The laser marker system (Q-Mark,
Quantronix, NY) used to deliver the laser beam to the zir-
conia surface had a back focal length of 11 cm, which was
controlled by software, and which could scan the work plane
at various scanning speeds.
Preparation of veneering ceramics
Disk-shaped specimens (5 mm diameter and 2 mm height)
were cut using using a slow-speed diamond saw (Isomet
1000) under water cooling from the lithium disilicate CAD/
CAM blocks (IPS e.max CAD, Ivoclar Vivadent, Schaan,
Liechtenstein). All the veneer ceramics were then cleaned
ultrasonically in distilled water for 10 min and air dried. A
thixotropic glass-fusion ceramic (IPS e.max CAD Crystall/
Connect; Ivoclar Vivadent) was placed on the table of the
vibrating device (Ivomiks, Ivoclar Vivadent) and vibrated
for 10 sec according to the manufacturer’s instructions. A
small amount of liquescent glass-fusion ceramic was applied
to the middle of zirconia surface, fused with veneer ceramic,
and then vibrated using Ivomiks to ensure homogeneous
distribution of the fusion ceramic (Fig. 1). All the core-
veneer specimens were then submitted to the crystallization/
fusion process according to the manufacturer’s instructions.
238 YILMAZ-SAVAS ET AL.

Table 1. Mean Shear Bond Strengths

and Standard Deviations of the Groups (MPa)
Standard
Group Surface treatment n Mean deviation
C No treatment 10 32.52a 10.15
S Sandblasting 10 33.03a 5.05
with 50 lm Al2O3
particles
E Er:YAG laser 10 31.02a 4.96
irradiation
F Femtosecond 10 36a 3.31
laser irradiation
Same letters indicates that there is no difference between the
groups (p > 0.05).

adhesive (failure between the core and veneer ceramic),

FIG. 1. Fusion of the lithium disilicate veneer ceramic
and zirconia core by Ivomiks (Ivoclar Vivadent, Schaan,
Liechtenstein).
cohesive (failure within the veneer ceramic), or mixed
(combination of adhesive and cohesive failure modes). In
addition, one specimen from each group of all materials was
sputter-coated with gold and analyzed using a scanning
electron microscope (SEM) (SEM-Zeiss LS-10 England).
Statistical analysis

SBS test
Specimens were placed in a custom-made apparatus and
then a shear force was applied to the veneer-zirconia
bonding area by using a universal testing machine (TSTM
02500; Elista Ltd. Sti, Istanbul, Turkey) at a crosshead
speed of 0.5 mm/min until fracture (Fig. 2). SBS was cal-
culated according to the formula:
Shear bond strength (MPa) ¼ Load (N)=Area (mm2 )
Microscopic evaluation
The fractured surface of each zirconia was examined
under a stereomicroscope (Olympus SZ 40, SZ-PT, Japan)
at 20· magnification. The failure modes were classified as
The data were analyzed by one way ANOVA and Tukey
honest significant difference (HSD) multiple comparison
tests with a software program (SPSS Statistics 22, IBM,
Chicago, IL) ( p < 0.05).
Results
The mean SBS values and standard deviations (MPa) of the
four surface treatment groups are presented in (Table 1). The
highest mean SBS was observed in Group F (36 – 3.31 MPa),
followed by Group S (33.03 – 5.05 MPa). The lowest mean
SBS was observed in Group E (31.02 – 4.96 MPa), and Group
C (32.52 – 10.15 MPa), which served as control, showed
higher bond strength than Group E. However, there was no
significant difference between the test groups according to
one way ANOVA (Table 2) ( p = 0.337, p > 0.05). The sta-
tistical power of the performed test at a = 0.05 was 0.263.
Stereomicroscopic analysis showed that all of the speci-
mens showed a mixed type of failure in all groups. In all the
specimens, the fracture started at the core–veneer interface
and proceeded into the veneering ceramic that was observ-
able in the SEM images after fractures (Fig. 3A–D). Glass-
fusion and veneering ceramics remaining on the zirconia
surface were clearly visible in all the SEM images.
Figure 3D shows the traces of the femtosecond laser clearly.
These traces were filled with the glass-fusion ceramic.

Table 2. Results of the One-Way ANOVA

Sum of Mean
squares df square F p
Between groups 130.527 3 43.509 1.062 0.377
Within groups 1474.306 36 40.953
Total 1604.833 39
FIG. 2. Shear bond strength test with a custom-made ap-
paratus. The differences were significant at the p < 0.05 level.
BOND STRENGTH OF ZIRCONIA WITH SURFACE TREATMENTS
FIG. 3. Scanning electron microscopic (SEM) images of fractured specimens from each group after the shear bond
strength (SBS) testing. (A) Control. (B) Sandblasting with 50 lm Al2O3. (C) Er:YAG laser irradiation. (D) Femtosecond
laser irradiation.
Figure 3C shows that Er:YAG laser had scratched the sur-
face of zirconia. Sandblasting with Al2O3 has caused many
surface irregularities, as shown in the Fig. 3B.
Discussion
The primary requirement for a successful zirconia-based
restoration is the development of an adequate and stable
bond between the veneer ceramic and the zirconia core.
This study was evaluated the bond strength of the lithium
disilicate veneer ceramics to the zirconia cores, treated by
different surface conditioning methods (sandblasting, Er:
YAG laser, and femtosecond laser) and demonstrated that
there are no significant differences in the shear bond
strength between the groups ( p > 0.05). Therefore, the re-
sults of this study accept the null hypothesis.
According to the International Standards Organization
(ISO 9693), a minimum bond strength for metal-ceramic
restorations should be 25 MPa.43 There are various studies
about bond strength between zirconia cores and veneering
ceramics;16,17,37,44–49 however, there is no consensus about a
minimum required bond strength for bilayered all-ceramic
239
materials.44 Aboushelib et al.50 pointed out that the core–
veneer interface is the weakest part of the all-ceramic res-
torations and plays a significant role in the success of these
kinds of restorations.
Delamination or chipping of veneering ceramic in zirconia-
based restorations is described as the most frequent failure
reason,46,48,49 and the reasons were reported as multifacto-
rial.44 Several factors may affect the core–veneer interface,
such as thickness of the veneer ceramic, coefficient of thermal
expansion (CTE) mismatch and lack of thermal conduc-
tivity,13 veneer application techniques,16,51 framework de-
sign,16,51 cooling rate,14,49 wetting property of the veneer
ceramic,47 and surface roughness of the zirconia.30,48,52
The bonding strength between core and veneering ce-
ramic is affected by the type of zirconia core material,53
hence one type of zirconia core was used in this study to
eliminate the effect of the core material itself.
To achieve a relevant core–veneer bonding, several sur-
face treatments could be applied on the zirconia ceramic
surfaces. In dentistry, sandblasting with Al2O3 particles is a
well-known surface treatment technique to the ceramic and
zirconia surfaces. This procedure is used for obtaining a
240
rougher surface, to increase the bonding area either to the
inner surface of the restoration or between the core–veneer
surfaces.23,52 There are several studies about the effect of
sandblasting on the zirconia surface. Most of the studies
evaluated the bond strength between the surface-treated
zirconia core and resin cements. However, the results are
controversial. Some studies revealed that the sandblasting
is a useful surface treatment technique to improve the bond
strength between the zirconia and the veneer ceramic.48
Aboushelib et al.54 reported that sandblasting the white
zirconia surface with 50 lm Al2O3 increased the bond
strength between the zirconia core and the veneer ceramic.
On the other hand, some studies reported that sandblasting
of the Y-TZP surface does not necessarily enhance the bond
strength of the veneer ceramic to the zirconia core.45,50,52
Guess et al.44 concluded that sandblasting with Al2O3
(110 lm, 2.4 bar) had no significant effect on the bond
strength between the core and the veneering ceramic. El-
saka55 also concluded that the surface treatments of different
zirconia cores with sandblasting did not significantly im-
prove the adhesion between zirconia and veneering ceramic.
In this study, the sandblasted group did not enhance the
bond strength between the lithium disilicate veneer ceramic
and the zirconia core, because the differences are not sig-
nificant ( p > 0.05). However, according to previous studies,
the sandblasting procedure might be useful before sinter-
ing,56 and when small particles are preferred.57
When using the sandblasting procedure, it is necessary to
consider that the procedure might induce phase changes on
the zirconia surface that could change the crystal structure
from tetragonal to monoclinic.20,52,58 If the monoclinic
phase level increases on the zirconia surface, it may lead to
micro-cracks in the glass phase of the veneer ceramic at the
inter-grain level, and this may reduce the bond strength.50,59
To eliminate these phase changes, using sandblasting prior
to the sintering process56 or heat treatment was suggested.29
The monoclinic phase on the zirconia surface that was
generated during sandblasting would be turned back into the
tetragonal phase with heat treatment.29 If sandblasting is
used after the sintering process, the heat treatment could be
a veneering procedure or re-glazing after clinical adjust-
ments.60 Although phase changes or differences according
to heat treatment are not the subjects of this study, the ve-
neering process that was used in this study might reduce the
monoclinic phase ratio, and relatively small particles were
used (50 lm), as the one study recommended using 50 l
Al2O3 particles to lower phase transformation on the zir-
conia surface.60 Additionally, optimum sandblasting appli-
cation time to the zirconia surface is not clear. Sato et al.21
indicated that the thickness of the transformed layer over the
zirconia surface mainly depended upon the kind of the
sandblasting particles, not the sandblasting application time.
Therefore, 10 sec application time was chosen in this study,
which many of the studies in the literature preferred.52,61–63
The use of laser irradiation for surface roughening is an
alternative and innovative method64 and it might be a po-
tential new means of surface treatment for enhancing the
zirconia–veneer ceramic interfacial bonding and integra-
tion.28
There are various studies about laser surface treatments
on the zirconia surface; however, most of them investigated
zirconia–resin bonding strength. There are little data on the
YILMAZ-SAVAS ET AL.
effect of the laser surface treatment on the zirconia–veneer
ceramic bonding strength. Kirmali et al.37 investigated the
effects of different pre-sintering treatments on the bond
strength between the zirconia (sandblasting, Er,Cr:YSGG
laser irradiation 1–6 W) and veneer ceramic that was fab-
ricated with layering technique, and they found smaller
shear bonding strengths (13–20.54 MPa) than in this present
study. They found the highest bond strength in the laser
group, which was treated with 6 W energy, and recommended
using higher energy densities for the laser irradiation to in-
crease the bond strength between the zirconia core and the
veneering ceramic. The same energy density was used in
this study, and the bonding strength is much higher; how-
ever, the Er:YAG laser treated group showed the lowest
bond strength in this study, but the mean bond strengths of
the groups were similar. Demir et al.35 reported that Er:-
YAG laser irradiation at different intensities to sintered
zirconia surface increased the surface roughness; however,
they stated that sandblasting is the most effective surface
treatment method. Similar results were also reported by
Subasi and Inan,3 who pointed out that sandblasting and
Er:YAG surface treatments can be used for roughening
zirconia surface; however, sandblasting is a more effective
method for improving zirconia–resin bonding.
It is noteworthy that laser irradiation may cause surface
alterations on the zirconia surface. Noda et al.65 irradiated the
zirconia surface with Nd:YAG laser, and they showed that
cracks and melting points also had a blackening effect over
the zirconia surface. In addition, they pointed out that the
elemental composition of zirconia was changed by the laser
application. They concluded that Nd:YAG laser should not be
used over the tetragonal zirconia. Cavalcanti et al.36 used Er:
YAG laser over the zirconia, and reported that higher Er:
YAG laser pulse energy settings (400 and 600 mJ) caused
excessive material deterioration such as cracking. The same
Er:YAG laser pulse energy (300 mJ) was chosen in the study
by Kara et al.,27 and the authors revealed that the Er:YAG
laser caused melted and erosive areas without any crack
formation. Unlike the study by Noda et al.,65 no cracks or
black melting points were observed in either the Er:YAG or
the femtosecond laser-irradiated groups in the present study.
A recent study declared that the femtosecond laser pulses
provide promising advantages compared with conventional
abrasive surface structuring methods for zirconia ceramic.66
Delgado-Ruiz et al.2 irradiated the zirconia implant surfaces
with femtosecond laser and reported that it reduced the pres-
ence of residual elements. Additionally, they showed that the
zirconia surface characteristics did not change after the treat-
ment and did not exhibit phase transformation. Another study
also investigated the effect of different surface treatments
(femtosecond, Nd:YAG, and Er:YAG) on zirconia and the
bonding strength between the resin and the cement. The au-
thors reported that the femtosecond-treated group showed
significantly higher resin bond strength than the Nd:YAG- and
Er:YAG-treated groups.27 Unlike the study by Kara et al.,27
the femtosecond laser-treated group did not show statistically
different bond strength compared with the other groups in this
study. However, this finding is similar with another study,
which investigated the bonding strength between the surface
treated (sandblasting, 9.6% hydrofluoric acid gel, Nd:YAG
laser, and femtosecond laser), feldspathic porcelain, and metal
brackets. They showed that the femtosecond-treated group
BOND STRENGTH OF ZIRCONIA WITH SURFACE TREATMENTS
showed higher bond strength values than the other test groups;
however, there were no significant differences between the
hydrofluoric acid applied and sandblasted groups.22 It also
needs to be highlighted that a new veneering technique called
CAD-on was used in this study. Nevertheless, there is little
information in the literature about the bond strengths of this
technique. Also, there are no data to compare these findings,
because the studies in the literature about the CAD-on tech-
nique did not use any surface treatments to the zirconia core.
All the failure types were a mixed type in this study, and no
adhesive or cohesive failures were observed. Mixed type fail-
ures are clinically preferred to adhesive failures because this
type of failure usually shows the adequate interfacial bonding
and is associated with high bond strength values.67 It is note-
worthy that the absence of the cohesive failure in the veneer
ceramic indicated that the laser treatment did not induce the
internal weakening of the veneer ceramic in this study, which
was similarly reported by Gomes et al.68 SEM image shows
regular pits, which were created by the femtosecond laser
beam, and these pits were filled with glass-fusion ceramic
(Fig. 3D), which might act as the micromechanical retentive
understructures that increased the adhesion between the lithium
disilicate ceramic and the zirconia.28 These pits could not be
observed in the Er:YAG laser-treated group (Fig. 3C), and the
eroded zirconia surface could lead to lowering of the bonding
strength compared with the utreated group in this study.
One limitation of this study is that the small number of
specimens limits the interpretation of the results, because a
higher number of specimens might have produced significant
differences with a smaller standard deviation. Surface rough-
ness measurements and crystallographic analyses are the other
limitations of this study. Also, geometric shapes of the spec-
imens did not represent the anatomic forms of the restorations;
however, the geometric shape is required for the measurement
of the SBS. Further studies should focus on an increased
number of specimens per group when evaluating the bond
strength of the surface-treated zirconia cores using the CAD-
on technique in in vitro and in vivo conditions.
Conclusions
Within the limitations of this present study, the following
conclusions were drawn.
1. Surface treatment is not necessary if the CAD-on
technique is to be used.
2. Femtosecond laser irradiation formed regular pits on
the zirconia surface that could provide micro-
mechanical adhesion, unlike Er:YAG laser irradiation,
which created scratches on the zirconia surface ac-
cording to the SEM images.
Author Disclosure Statement
No competing financial interests exist.
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Address correspondence to:
Tuba Yılmaz Savas
Faculty of Dentistry
Department of Prosthodontics
Alaaddin Keykubat Campus
Selcuk University
Selcuklu, Konya
Turkey, 42080
E-mail: tuba-yilmaz@windowslive.com