Dental Materials (2006) 22, 283–290

www.intl.elsevierhealth.com/journals/dema

Microtensile bond strength of a resin cement to

glass infiltrated zirconia-reinforced ceramic:
The effect of surface conditioning
Regina Amarala, Mutlu Özcanc,*, Marco Antonio Bottinoa,
Luiz Felipe Valandrob
a
São Paulo State University, Department of Dental Materials and Prosthodontics,
São José dos Campos, Brazil
b
Federal University of Santa Maria, Department of Restorative Dentistry, Santa Maria, Brazil
c
Faculty of Medical Sciences, Department of Dentistry and Dental Hygiene,
Antonius Deusinglaan, University of Groningen, Groningen, The Netherlands

Received 6 January 2005; accepted 7 April 2005

KEYWORDS Summary Objectives. This study evaluated the effect of three surface condition-
Bond strength; ing methods on the microtensile bond strength of resin cement to a glass-infiltrated
Microtensile test; zirconia-reinforced alumina-based core ceramic.
Silane coupling agent; Methods. Thirty blocks (5!5!4 mm) of In-Ceram Zirconia ceramics (In-Ceram
Silica coating; Zirconia-INC-ZR, VITA) were fabricated according to the manufacturer’s instructions
Surface conditioning and duplicated in resin composite. The specimens were polished and assigned to one
methods; of the following three treatment conditions (nZ10): (1) Airborne particle abrasion
Zirconia ceramics with 110 mm Al2O3 particles C silanization, (2) Silica coating with 110 mm SiOx
particles (Rocatec Pre and Plus, 3M ESPE) C silanization, (3) Silica coating with
30 mm SiOx particles (CoJet, 3M ESPE) C silanization. The ceramic-composite blocks
were cemented with the resin cement (Panavia F) and stored at 37 8C in distilled
water for 7 days prior to bond tests. The blocks were cut under coolant water to
produce bar specimens with a bonding area of approximately 0.6 mm2. The bond
strength tests were performed in a universal testing machine (cross-head speed:
1 mm/min). The mean bond strengths of the specimens of each block were
statistically analyzed using ANOVA and Tukey’s test (a%0.05).
Results. Silica coating with silanization either using 110 mm SiOx or 30 mm SiOx
particles increased the bond strength of the resin cement (24.6G2.7 MPa and 26.7G
2.4 MPa, respectively) to the zirconia-based ceramic significantly compared to that
of airborne particle abrasion with 110-mm Al2O3 (20.5G3.8 MPa) (ANOVA, P!0.05).

* Corresponding author. Tel.:C31 50 363 8528; fax: C31 50 363 2696.

E-mail address: mutluozcan@hotmail.com (M. Özcan).

0109-5641/$ - see front matter Q 2005 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.dental.2005.04.021
284
Significance. Conditioning the INC-ZR ceramic surfaces with silica coating and
silanization using either chairside or laboratory devices provided higher bond
strengths of the resin cement than with airborne particle abrasion using 110 mm
Al2O3.
Q 2005 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.
Introduction
Etching the inner surfaces of ceramics with glassy
matrix using hydrofluoric acid followed by the
application of a silane coupling agent is an efficient
conditioning method for bonding resin composite
[1–6]. However neither etching with this agent nor
adding silane resulted in an adequate resin bond to
some new high-strength ceramics [7,8]. Particularly
high-alumina [9–12] or zirconia-reinforced ceramics
[13,14] cannot be roughened by hydrofluoric acid
etching since such ceramics do not contain a silicon
dioxide (silica) phase. Similarly, cement adhesion
to glass-infiltrated zirconia–alumina ceramic
(In-Ceram Zirconia-INC-ZR) is also not favorable
since this ceramic presents the same character-
istics due to its high crystal content (aluminum
oxide: G67 wt%; zirconium oxide: G13 wt%) and
limited vitreous phase (lanthanum aluminum sili-
cate: G20 wt%) [15]. For this reason, special
conditioning systems are indicated for these types
of ceramics [16].
Previous investigations revealed that most clini-
cal failures have initiated from the cementation or
internal surfaces. Failure rates due to high-strength
ceramic fractures have been reported to range
between 2.3 and 8% [17–19]. Therefore, the
integrity of the luting cement to ceramic surfaces
plays a major role in the longevity of the restoration
and the failures originated from cementation
surfaces identified the need for a reliable con-
ditioning method to strengthen this critical area.
Modern surface conditioning methods require
airborne particle abrasion of the surface before
bonding in order to achieve high bond strength. One
such system is silica coating. In this technique,
the surfaces are air-abraded with aluminum oxide
particles modified with silisic acid [20,21]. The
blasting pressure results in the embedding of silica
particles on the ceramic surface, rendering the
silica-modified surface chemically more reactive to
the resin through silane coupling agents. Silane
molecules, after being hydrolized to silanol, can
form polysiloxane network or hyroxyl groups cover
the silica surface. Monomeric ends of the silane
molecules react with the methacrylate groups of
the adhesive resins by free radical polymerization
R. Amaral et al.
process. When a ceramic exhibits chemical states of
silicon and oxygen, then siloxane bond will be
achieved as these represent the binding sites for the
coupling agent to the ceramic surface. Since silane
coupling agents do not bond well to alumina, the
bond strengths of resin composite to such ceramics
could be affected [10].
Air-particle abrasion is a prerequisite for achiev-
ing sufficient bond strength between the resins and
high-strength ceramics that are reinforced either
with alumina or zirconia [22]. The air abrasion
systems rely on air-particle abrasion with different
particle sizes ranging from 30 to 250 mm [16,23].
The abrasive process removes loose contaminated
layers and the roughened surface provides some
degree of mechanical interlocking or ‘keying’ with
the adhesive. It can be argued that the increased
roughness also forms a larger surface area for the
bond. While these mechanisms explain some of the
general characteristics of adhesion to roughened
surfaces, it may also introduce physico-chemical
changes that affect surface energy and wettability.
Such conditioning systems could be applied either
at the laboratory or chairside, using large or small
size particles. However, there is limited knowledge
as to whether micromechanical retention using
large or small particle size increase resin bond to
high-strength ceramics of different microstructures
and chemical compositions.
A high and reliable resin bond to alumina and
zirconia ceramics was also achieved with airborne
particle abrasion and by using a phosphate mono-
mer (MDP) containing resin composite luting
cement. Although there are some studies on bond
strength of resin cements to the zirconium-based
ceramics [24–26], to the authors’ knowledge, no
study has investigated the bond strength of
phosphate-monomer based resin cement to zirco-
nium-reinforced ceramics in combination with
conditioning methods that rely on chairside con-
ditioning systems.
The aim of this study, therefore, was to evaluate
the effect of three surface conditioning methods
based on airborne particle abrasion, employing
three types of sand particles, on the microtensile
bond strength of the resin cement to a glass-
infiltrated zirconia-reinforced ceramic.
Bond strength of a resin cement to zirconia ceramic 285

Material and methods
Thirty blocks (5!5!4 mm) of zirconia-reinforced
alumina-based ceramics [In-Ceram Zirconia-INC-ZR
(VITA Zahnfabrik, Bad Sackingen, Germany)] were
fabricated according to the manufacturer’s
instructions. Ceramic surfaces were ground finished
up to 1200-grit silicon carbide abrasive (3M, St.
Paul, USA) in a polishing machine (Labpol 8–12,
Extec, USA) and cleaned for 10 min in an ultrasonic
bath (Quantrex 90, L&R Ultrasonics, Kearny, NJ,
USA) containing ethylacetate and air-dried. Each
ceramic block was duplicated in composite resin
(W3D-Master, Wilcos, Petrópolis, RJ, Brazil) using a
mold made out of silicon impression material
(Express, 3M/ESPE, St. Paul, USA). Composite
resin layers were incrementally condensed into
the mold to fill up the mold and each layer was light
polymerized for 40 s (XL 3000-3M/ESPE, St. Paul,
USA; light output: 500 mW/cm2). One composite
resin block was fabricated for each ceramic block.
Surface conditioning methods
Table 1 summarizes the three surface conditioning
methods, silane, ceramic and cement used for the
experiments. The ceramic blocks (10 blocks per
conditioning) were assigned to one of the three
following treatment conditions:
Chairside Gritblasting (CGB): In this group, air-
borne particle abrasion was performed using
110 mm grain sized Al2O3 particles using an intraoral
air abrasion device (Micro–Etcher, Danville Inc.,
San Ramon, CA, USA) at a pressure of 2.8 bars from
a distance of approx. 10 mm, for 20 s in circling
movements.
Laboratory Silica Coating (LSC): Silica coating
process was conducted using a laboratory type of
air abrasion device (Rocatector Delta device, 3M
ESPE) in which the specimens were first conditioned
by air-abrasion with 110 mm grain sized Al2O3
particles at a pressure of 2.8 bars with Rocatec
Pre abrasive. Then the specimens were air-abraded
with Rocatec Plus abrasive, which was 110 mm grain
sized SiOx, at 2.8 bars under the same conditions
with CGB.
Chairside Silica Coating (CSC): Silica coating
process was achieved using an intraoral air abrasion
device (Micro–Etcher, Danville Inc., San Ramon, CA,
USA) filled with CoJetw-Sand (30 mm SiOx particles)
(3M-ESPE, Minnesota, USA) under the same con-
ditions with CGB.
Following all three surface conditioning
methods, the remnants of sand particles were
gently air blown, silane coupling agent (ESPEw-Sil,
3M ESPE AG, Seefeld, Germany) was applied and
waited for its evaporation for 5 min.
Topographic analyses of conditioned
ceramic surface
Additional ceramic specimens were conditioned
using the three surface conditioning methods in
order to observe the topographic surface changes
under the Scanning Electron Microscope (SEM)
(JEOL-JSM-T330A, Jeol Ltd, Tokyo, Japan).

Table 1 Characteristics of surface conditioning methods, silane, ceramic and cement used for the experiments
with codes and manufacturing company names.
Conditioning principles, Abbreviation Characteristics Manufacturer
silane, ceramic, cement
Chairside Gritblasting CGB 110 mm Al2O3, (2.8 bars, 10 mm, 20 s) Korox, Bego, Bremen,
Germany
Laboratory Silica Coating LSC Rocatec Pre (110 mm Al2O3)C Roca- 3M ESPE AG, Seefeld,
Germany tec Plus (110 mm SiOx) (both at 2.8
bars, 10 mm, 20 s)
Chairside Silica Coating CSC CoJetw-Sand (30 mm SiOx) (2.8 bars, 3M-ESPE, Minnesota, USA
10 mm, 20 s)
Silane coupling agent 3-methacryloxyprophyltrimethoxy 3M ESPE AG, Seefeld,
Germany silane in ethanol (ESPEw-Sil) (5 min)
Ceramic
In-Ceram Zirconia INC-ZR Glass-infiltrated zirconia Vita Zahnfabrik, Bad
Saeckingen, Germany
Cement
Panavia F Filler (78%),10-Methacryloyloxyde- Kuraray, Okayama, Japan
cyldihydrogenphosphate (MDP),
dimethacrylates, chemical and
photoinitiators
286 R. Amaral et al.

Bonding procedure and specimen

preparation

Each conditioned ceramic block was bonded to a

composite block under the load of 750 g using a
resin cement system (Panavia F, Kuraray CO.,
Okayama, Japan). The excess resin cement was
removed by means of a brush. The resin cement was
then light polymerized (XL 3000) for 40 s from each
direction. Oxyguard was applied on the cement
layer for 10 min. The blocks were washed with air-
water spray and stored in distilled water at 37 8C for
7 days prior to bond tests.
The blocks were then bonded with cyanoacrylate
glue (Super Bonder Gel, Loctite Ltd, São Paulo,
Brazil) to a metal base that was coupled to a cutting
machine. Slices were obtained using a slow-speed
diamond wheel saw (KG Sorensen, Barueri, Brazil)
under cooling. The peripheral slices were disre-
garded in case the results could be influenced by
Figure 1 (a) Cutting procedure to obtain slices of
either the excess or insufficient amount of resin
cemented ceramic and composite blocks with ca 0.8 mm
cement at the interface. Three slices (0.8G0.1 mm thickness (3 slices per block); (b) The slices rotated 908
in thickness) were obtained per block initially. The and bonded onto the metal base again for further cutting
slices were rotated 908 and bonded onto the metal procedures (0.8 mm-thickness) in order to obtain non-
base again. The peripheral bar specimens were also trimmed bar specimens with ca 8 mm in length and
disregarded for the same reasons described above. 0.6 mm2 adhesive surface area.
Other 3 sectioning were carried out. (Fig. 1(a)-(b)).
Twelve non-trimmed bar specimens (with
approximately 8 mm in length and 0.6G0.1 mm2 order to determine the significant differences
adhesive surface area) were obtained per block between surface conditioning methods. P values
(Fig. 2(a)-(c)). less than 0.05 are considered to be statistically
significant in all tests.
Microtensile bond strength test

The bar specimens were glued parallel to the long

axis of an adapted caliper using cyanoacrylate
glue. This apparatus was coupled to the universal
testing machine (EMIC DL-1000, EMIC, São José
dos Pinhais, Brazil) and the specimens were
loaded in tension to failure at a crosshead speed
of 1 mm minK1.
Bond strength values were calculated using the
formula, sZL/A, where ‘L’ is the load at failure
(Kgf) and ‘A’ is the adhesive area (mm2) measured
using a digital caliper (Mitutoyo, Tokyo, Japan)
prior to the tests.
Statistical analysis
Statistical analysis was performed using Statistics
8.0 for Windows (Analytical Software Inc, Talla-
hassee, FL, USA). The means of the specimens of
each blocks were obtained and these values
(nZ10) were analyzed by 1-way analysis of
variance (ANOVA) and Tukey’s test (aZ05) in
Results
The results of the microtensile bond strength tests
for three surface conditioning methods are pre-
sented in Table 2.
Silica coating with silanization either with
110 mm SiOx particles or 30 mm SiOx revealed
significantly higher bond strengths of the resin
cement (24.6G2.6 MPa and 26.7G2.4 MPa,
respectively) to the INC-ZR ceramic compared to
that of airborne particle abrasion with 110-mm
Al2O3 (20.5G3.8 MPa) (ANOVA, PZ0.0004). There
were no significant differences between both silica
coating groups (PO0.05)
SEM analysis at !2000 magnification, comp-
lementary to the bond strength tests, revealed
that all three types of sand particles penetrated the
substrate surfaces and the ceramic surfaces were
covered with abundant sand particles even after air
blowing (Fig. 3(a)–(c)).
Bond strength of a resin cement to zirconia ceramic
(a)
Resin
composite
not tested
tested
Figure 2 (a) Protocol of specimen choice according to cutting procedure (tested-and non-tested regions); (b) Bar
specimens with ca 8 mm in length and 0.6G0.1 mm2 bonded surface area; (c) Bonded zone (*) between the ceramic and
composite block at the bar specimen.
Discussion
In this study, roughening the zirconia-reinforced
ceramic surfaces with air particle abrasion and
applying silane prior to cementation provided high
bond strengths and silica coating followed by
silanization evidently enhanced the bond between
the luting cement and the ceramic surfaces. The
silica layer left by silica coating on the ceramic
surface provides a basis for silane to react. In the
ceramic-resin bond, silane functions as a coupling
agent, which adsorbs onto and alters the surface of
the ceramic, thereby facilitating chemical inter-
action [11,23].
When alumina or zirconia ceramics are glass
infiltrated, they are melted together at high
temperatures to form a ceramic composite. The
chemical components of the ceramics (traces such
as Li2O, Na2O, K2O, CaO, MgO) are then bonded to
each other by strong covalent bonds with hydroxyl
groups at the surface of the ceramic material [27].
When the surface is air abraded, this would
generate more hydroxyl groups on the surface and
also enhance the micro-mechanical retention.
Furthermore, the methoxy groups of silane would
react with water to form silanol groups that in turn,
will react with the surface hydroxyl groups to form
siloxane network. Amphoteric alumina in the
ceramic matrix could form chemical adhesion,
covalent bridges, through its surface hydroxyl
groups with hydrolyzed silanol groups of the silane:
–Al–O–Si–[10].
In principle, the presence of the glassy phase in
ceramics favors better siloxane bonds. The silanol
groups could then react further to form a siloxane
(–Si–O–Si–O–) network with the silica on the surface.
The In-Ceram ceramic system tested in this study,
In-Ceram Zirconia (INC-ZR), is glass infiltrated. Most
probably the glass infiltration facilitated better
287
(b) (c)
Resin *
Cement
Ceramic
*Adhesive zone
silane bonding and therefore increased bond
strength values were obtained for this ceramic.
These findings are in compliance with the study of
Özcan and Vallittu [10], even though a different
experimental set up was used where a bis-GMA
based resin cement and shear bond test were
employed.
Material selection and clinical recommendations
on resin bonding are based on mechanical labora-
tory tests that show great variability in materials
and methods. One of the most common testing-
method is the shear bond test. However the specific
fracture pattern in shear testing may cause
cohesive failure in the substrate that may lead to
erraneous interpretation of the data while in
microtensile tests, stress distribution was reported
to be more homogeneous [28–31]. Although, for this
reason, microtensile test was employed in this
study, similar ceramic-cement performance was
observed in dry conditions in the study of Özcan and
Vallittu [10].
Some studies, on the other hand, have evaluated
ceramics with different microstructures, reporting
Table 2 Microtensile bond strength (MPa) of the
resin luting cement, and statistical differences con-
sidering the surface conditioning factor after (a)
Airborne particle abrasion with 110 mm Al2O3 particles,
(b) Silica coating with 110 mm Al2O3 and 110-mm SiOx
particles, (c) Silica coating with 30 mm SiOx particles.
Groups s* (MPa) (SD)
1-INC ZIRC-CGB 20.5a (3.8)
2-INC ZIRC-LSC 24.6b (2.7)
3-INC ZIRC-CSC 26.7b (2,4)
For abbreviations, see Table 1. Different superscripted
letters indicate significant differences between the cer-
amic-surface conditioning combinations (P!0.05). SD, stan-
dard deviation.
288
Figure 3 (a) Typical SEM micrographs (!2000) of conditioned ceramic surfaces for a-Airborne particle abrasion with
110 mm Al2O3 particles, (b) Silica coating with 110 mm SiOx particles, c-Silica coating with 30 mm SiOx particles. Note that
after all three conditioning methods, ceramic surfaces were covered with abundant sand particles.
that high-strength ceramics are compact materials
making them difficult to gritblast [13,22]. Interest-
ingly, the results of this study indicate that the
silica coating system with small particle size of
30 mm SiOx particles as well as large particle size of
110 mm SiOx produced statistically higher mean
bond strength values than with chairside grit
blasting using 110-mm grain sized Al2O3 particles.
One can expect higher surface roughness created
using bigger particle size thereby higher micro-
mechanical retention but this was not achieved in
this study. One reason for this could be associated
with the phenomenon of less wettability and
contact angle [13,32] between the silane coupling
agent and the deep grooves on the ceramic surfaces
occurred after grit blasting. However this
assumption could not be verified for the application
of 110 mm SiOx. The reason for this can be
explained on the grounds that particle deposition
mechanisms differ depending on the substrate
characteristics, particle composition, size
distribution, quantity and morphology. Although
SEM images demonstrated comparable views with
agglomerates of sand particles, it is difficult to
deduce whether the sand is in contact with the
alumina or the glass phase of the ceramic tested
in this study. Nevertheless, the results of this
study together with some other studies reveal
good adhesion of silica particles in the vitreous
phases of the glass-infiltrated zirconia ceramics
R. Amaral et al.
[33–36]. In a previous study, a significant increase
of silica on the surface of the In-Ceram ceramic
(15.8–19.7 wt%) was detected after blasting with
Rocatec-Plus (SiOx) when compared with the
samples blasted only with Rocatec-Pre (Al2O3
particles) suggesting better bond strength between
the In-Ceram ceramic and the resin cements due to
the increase of silica content and the interaction
with the silane agent. Our ongoing studies involve
Energy Dispersive X-ray Spectroscopy (EDS) analysis
to gain more insight on the interaction between
these three sand particles and the ceramic
composites [37].
The other reason for lower results obtained after
110 mm grain sized Al2O3 particle deposition could
be due to the weak bond between Al–Si–O as
reported earlier elsewhere [10].
Although satisfactory bond strength values of
resin cement to high-strength ceramics are yet to
be determined for clinically successful
performance, the bond values obtained for the
ceramic tested in this study could be considered
sufficient with both conditioning methods. In
clinical applications however, when air abrasion
will be contemplated by chairside, clinicians
should also consider the possible material loss
[9] especially at the margins of the restorations
that may lead to ditching when bigger grain size
particles are used during airborne particle
abrasion.
Bond strength of a resin cement to zirconia ceramic
Bonding of ceramic to tooth substance is based
on the adhesion of luting cement and its bonding
resin to the ceramic substrate together with the
adhesion of luting cement to enamel and dentine.
Future studies should also concentrate on the
involvement of the tooth tissues in the test
complex.
The cement–ceramic adhesion is susceptible to
chemical, thermal and mechanical influences under
intraoral conditions. One limitation of this study
could be the lack of thermocycling although there
are controversial reports on the effect of thermo-
cycling in the literature [16].
Some earlier studies reported high and stable
bond strength to the zirconia reinforced ceramic
after airborne particle abrasion using Al2 O 3
particles in combination with phosphate monomer
based resin cement [24–26]. Comparing the results
of these studies with this present study, it can be
suggested that the silica coating and silanization
may allow a better bond strength to the zirconium
with this resin cement.
The general outcome of this study suggests
that relatively recent surface conditioning tech-
niques based on the combination of micromecha-
nical and chemical conditioning should be
considered for improved adhesion of resin
cements to glass-infiltrated zirconia ceramics.
More importantly, these methods seem to offset
the importance of the varieties of the substrates
and therefore could be applicable to a wide
range of high-strength ceramics [31]. The equip-
ments to apply these techniques were sophisti-
cated and expensive during the last two decades
but they are recently simplified and brought to
the chairside. By employing chairside devices for
airborne particle abrasion, contamination during
delivery of the restoration from the laboratory to
chairside could also be avoided. As long as the
available conditioning methods will not be
optimized, the development in the high-strength
ceramic field is expected to continue experien-
cing failures.
Conclusions
Silica coating either with 110 mm SiOx particles or
30 mm SiOx followed by silanization increased the
bond strength of the phosphate monomer-based
resin cement to glass infiltrated zirconia-
reinforced ceramic when compared with airborne
particle abrasion using 110 mm Al2 O 3 and
silanization.
289
Acknowledgements
We express our appreciation to the Wilcos Ltd in
Brazil (Petrópolis/RJ, Brazil) and VITA Zahnfabrik
(Bad Säckingen, Germany) for providing some of
the materials used in this study. We also thank
Prof. Dr. Ivan Balducci, School of Dentistry, São
Paulo State University at São José dos Campos,
Brazil, for his assistance with statistical analysis.
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