Dental Materials Journal 2011; 30(3): 392–397

Influence of silane heat treatment on bond strength of resin cement to a

feldspathic ceramic
Rodrigo Furtado de CARVALHO1, Maria Elizabeth Marques Nogueira MARTINS2,
José Renato Cavalcanti de QUEIROZ2, Fabíola Pessoa Pereira LEITE2 and Mutlu ÖZCAN3
1
Federal University of Juiz de Fora, Faculty of Dentistry, Rua Jose Lourenco Kelme, Campus University, Bairro São Pedro 36036-900, Juiz de Fora,
MG, Brazil
2
Federal University of Juiz de Fora, Faculty of Dentistry, Department of Restorative Dentistry, Rua Jose Lourenco Kelme, Campus University, Bairro
São Pedro 36036-900, Juiz de Fora, MG, Brazil
3
University of Zürich, Dental Materials Unit, Center for Dental and Oral Medicine, Clinic for Fixed and Removable Prosthodontics and Dental Materials
Science, Plattenstrasse 11, CH-8032 Zürich, Switzerland
Corresponding author,  Rodrigo Furtado de CARVALHO;  E-mail:  rf-carvalho@hotmail.com


This study evaluated the influence of heat treatment (HT) of the silane on the microtensile bond strength of resin cement to a
feldspathic ceramic. Ceramic (VITA VM7) and composite blocks (N=32) were divided into four groups (n=6 for bond test, n=2 for SEM)
at random and subject to following sequence of conditioning: G1: HF 9.6%+Silane+Panavia F2.0, G2: HF 9.6%+Silane+HT+Panavia
F2.0, G3: Silane+HT+Panavia F2.0, and G4: Silane+Panavia F2.0. HT was performed in an oven (100°C, 2 minutes). G1 (17.6±2.3
MPa) and G2 (19±3.2 MPa) showed significantly higher mean bond strength than those of G3 (9.1±2.8 MPa) and G4 (10.9±1.8 MPa).
SEM analysis showed exclusively mixed failures. Silane HT did not increase the bond strength.

Keywords: Adhesion, Cementation, Ceramics, Microtensile strength, Thermal treatment



Silane coupling agents promote bonding between

INTRODUCTION
Ceramics are often the materials of choice for aesthetic
restorations in dentistry due to their high resistance
to abrasion, compression, chemical stability,
biocompatibility, favorable aesthetic features,
translucence and fluorescence1).
Among several types of ceramics, feldspathic ceramic
is commonly used in the fabrication of indirect
restorations such as laminates, inlays, onlays or overlays.
Feldspathic ceramics are composed of two minerals:
quartz and feldspath. The feldspath is linked to some
metallic oxides forming the glass phase while the quartz
comprises a crystalline phase1).
The effectiveness of partial ceramic restorations is
linked to adequate cementation procedures that are
dependent on some factors such as composition of
ceramic materials, surface conditioning methods and
cement agents2,3). The surface conditioning of ceramics
vary between ceramic types depending on their chemical
composition4). The feldspathic ceramics are classified as
acid sensitive materials that suffer from surface
degradation by hydrofluoric acid gel (HF). HF application
creates a topography favoring micro-mechanical
retention5-8) due to selective dissolution of glass matrix
that is identified as retentive micro-pores, fissures and
grooves on the conditioned ceramic surface4,8-11).
The cementation process of a prosthetic restoration
is the final step of operative treatment after a series of
procedures. For adhesive cementation of glassy matrix
ceramics, after etching with HF, it is recommended to
use silane coupling agent, a monomer with reactive
organic radicals and hydro-soluble monovalent group12,13).
inorganic phase of ceramic and organic phase of bonding
agent applied on the ceramic surface by siloxane
bond12,13). In addition, silane increases the surface energy
of ceramic substrates and improves cement damping.
These events consequently promote microscopic
interactions between both parts.
Silane performance could be improved by heat
treatment procedure. Heat treatment of silane results in
the elimination of alcohol, water and other by-products
of the ceramic surface14-16). In addition, heat treatment
helps to complete the condensation reaction between
silicate and silane providing formation of covalent bonds
between the silane-ceramic interface, which in turn
becomes more effective and stable14-16). Therefore, it could
be anticipated that this stable silane reaction may
eliminate the use of hazardous HF acid gel during the
cementation phase.
Resin cements exhibit low solubility in the oral
environment, and adhere effectively to different
substrates when compared to other luting agents17).
Resin cements that are suitable for glass ceramics are
usually composed of bis-phenol glycidyl methacrylate
(bis-GMA) or urethane dimethacrylate (UEDMA) matrix
in combination with other monomers with lower
molecular weight such as triethyleneglycol
dimethacrylate (TEGDMA). An annexation of hydrophilic
functional groups, HEMA and 4-META, changes the
organic composition of resin cements enabling adhesion
to dental tissues. Such materials are basically composites
with adequate viscosity for cementation that may be
chemically, photo or dual polymerized. The resin cement
Panavia F2.0 (Kuraray, Japan) contains phosphate

Received Aug 25, 2010: Accepted Feb 23, 2011

doi:10.4012/dmj.2010-137 JOI JST.JSTAGE/dmj/2010-137
 Dent Mater J 2011; 30(3): 392–397 393

monomer in its composition being capable of adhering to
oxides and at the same time providing adequate adhesion
between the cement and the restorative material.
The choice of standardized tests focusing on adhesive
joint strength is essential to evaluate the bond strength
of different materials18). Among different testing
methods, the conventional tensile test yields to
non-uniform force distribution at the adhesive area.
Also, in tensile bond tests the exact parallel alignment of
the test specimens is difficult19). While the pull-out test
creates the concentration of tension in the substrate
having no effect in the adhesive area13,20), microtensile
test allows the distribution of tension in the adhesive
area18,21-25).
The aim of this present study was to evaluate the
influence of heat treatment of silane coupling agent on
the microtensile bond strength of phosphate monomer
based resin cement to feldspathic ceramic.
MATERIALS AND METHODS
Ceramic specimen preparation
The brands, manufacturers, chemical compositions and
batch numbers of the materials used in this study are
listed in Table 1.
Initially, a standard acrylic resin with dimensions of
6 mm×8 mm×8 mm was made. From this acrylic, ceramic
blocks were obtained measuring the same size for all
groups. The pattern of acrylic resin was molded with a
dense mass of the heavy part of polysiloxane (Elite HD,
Zhermach, Badia Polesine, Italy). The powder (VITA
VM7 Dentin 5M2) and modeling liquid (Modeling for
Liquid Vita VM7, VITA Zahnfabrik, Bad Säckingen,
Germany) were mixed according to the manufacturer’s
instructions. The ceramic slurry was placed in small
portions using a spatula, condensed inside the silicon
impression and vibrated manually until completing the
entire space of this impression. The excess fluid was
removed with soft absorbent paper. Then, the ceramic
block was removed from the tray. Finally, 32 blocks of
ceramic were obtained from a single impression. The
blocks were sintered on the refractory base in the furnace
(Vacumat, VITA Zahnfabrik) following the firing cycles
recommended by the manufacturer. Considering that
the contraction after sintering of ceramics is around
20%, post-sintering blocks had approximate dimensions
of 4.8 mm×6.4 mm×6.4 mm. The internal surfaces of
each block have undergone a radiographic evaluation in
order to observe possible faults within the body. In case
of such defects, the specimens were excluded from the
study and new ones were made. Subsequently, the
ceramic excess was removed with diamond discs at low
speed. The bond surface was ground finished using
silicone carbide abrasives of 600, 800, 1000, 1200 grit in
sequence under water. Then the specimens were
ultrasonically cleaned in distilled water for 5 minutes.
Impressions were made from each ceramic block.
After the impression material (Elite HD) was set, ceramic
blocks were removed from the mold. Microhybrid resin
composite (W3D MASTER, Wilcos of Brazil Ind., RJ,
Brazil) was placed in increments of 2 mm. Each increment
was photo polymerized for 40 seconds (Ultraled,
Ultradent®, UT, USA) until the mold was filled, resulting
in a block of composite (4.8 mm×6.4 mm×6.4 mm) for
each ceramic block. As a result, the bonding surface of
the composite resin blocks had the same area as the
surfaces of ceramic blocks. The ceramic blocks were
again ultrasonically cleaned as described above.

Table 1 The brands, manufacturers, chemical compositions and batch numbers of the materials used in this study.
Brands Manufacturer Chemical composition Batch number
W3D MASTER Wilcos of Brazil, Rio Methacrylate-based monomers 23.7 w%, silica, 002051
de Jeneiro, Brazil silicate glass and fluoride containing fillers 75.6 w%,
polymerization catalysts 0.6 w%, inorganic pigments
0.1 w%

Vita VM7 Vita Zahnfabrik, Bad Silicaoxide, aluminiumoxide, lanthanumoxide, 11040

Säckingen, Germany magnesium oxide, zincoxide, potassiumoxide,
inorganic pigments

Porcelain Dentsply, Petrópolis, 9.6% Hydrofluoric acid 11040

Conditioner RJ, Brazil

Clearfil Ceramic Kuraray Medical Inc., 3-Methacryloxypropyl trimethoxy silane, MDP, 61182
Primer Tokyo, Japan ethanol

Panavia F2.0 Kuraray Medical Inc., Silanated barium glass, silanated silica, surface 61187
Tokyo, Japan treated sodium fluoride, bis-phenol polyethoxy
dimetacrylate, MDP, hydrophobic dimethacrylate,
hydrophilic dimethacrylate, benzoyl peroxide,
sodium aromatic sulfinate, N,N-diethanol
p-toluidine, photo-initiator
394 Dent Mater J 2011; 30(3): 392–397
Adhesion protocol
The ceramic blocks were then randomly divided into four
groups (n=6) and conditioned as follows:
In Groups 1 and 2, the ceramic blocks were
conditioned with HF acid gel (Porcelain Conditioner,
Dentsply, Rio de Jeneiro, Brazil) for 20 seconds, rinsed
with water spray for 60 seconds, and ultrasonically
cleaned in distilled water for 4 minutes. They were then
dried with air spray for 30 seconds. In Group 1, silane
was applied on the bonding surface of each ceramic block
(Clearfil Ceramic Primer, Kuraray Medical Inc.,
Okayama, Japan) and dried completely with air spray.
In Group 2, after silane application, heat treatment
was achieved in a furnace (EDG, Sao Paulo, Brazil) at
100°C for 2 minutes.
In Group 3 and 4, on the ceramic surfaces no HF
etching but only silanization was performed. In Group 3
silane layer was heat-treated but in Group 4 no heat
treatment was applied.
Subsequently, resin cement (Panavia F2.0, Kuraray
Medical Inc., Tokyo, Japan) was adhered onto the
conditioned ceramic surface, according to the
manufacturers instructions. The ceramic and the
composite block were aligned perpendicular. After the
cement was placed on the conditioned surface, vertical
load of 750 g was applied for 10 minutes. The excess of
cement was removed, margins of the blocks were photo-
polymerized for 40 seconds at each site (Ultra LED,
Ultradent, UT) and an oxygen inhibiting gel was applied
at the margins. The ceramic-cement-resin assembly was
then washed with air-water spray and kept in distilled
water at 37°C for seven days prior to specimen
preparation for microtensile bond strength test.
Microtensile bond strength test
Initially, the ceramic-cement-composite resin assembly
was fixed with cyanoacrylate adhesive (Super Bonder
Gel, Loctite Ltd., São Paulo, Brazil) on cylindrical
metallic base of the cutting machine. The calibration of
the machine was repeated for each new specimen. Bar
specimens were obtained by cutting the assembly using
steel diamond discs (Microdont, São Paulo, Brazil) at low
speed under water-cooling. The external sections of 1
mm were eliminated due to possible excess cement. The
blocks were turned 90° and fixed again on the metallic
base. From each block, 9 transversal sections were
obtained and from those sections bar specimens with a
length of ±8 mm and adhesive area of ±1 mm² were
obtained.
Bonding area of each bar specimen was measured
Table 2 The mean (±standard deviations-SD) microtensile bond strength (MPa) values for the experimental groups.
Groups Mean (SD)
1 17.6 (2.3)a
2 19.0 (3.2) a
3   9.1 (2.8)b
4 10.9 (1.8) b
*The same superscripted letters indicate no significant differences (Tukey’s test, =0.05).
before the tests using a digital caliper (Starret Industry
Commerce Ltd., Sao Paulo, Brazil) with an accuracy of
100 µm. The bar specimens were fixed to the alignment
device with one drop of cyanoacrylate glue (Super Bonder
Gel) on the composite and one on the ceramic part of the
bar specimen. It was made sure that the adhesive
interface was free of the glue. The tensile forces were
applied at a cross-head speed of 1 mm/min until
debonding in the Universal Testing Machine (Model DL
1000, EMIC, Systems and Equipments Ltd., São José
dos Pinhais, Brazil).
After the tests, failure types were analyzed using an
optical microscope (Zeiss MC 80 DX, Jena, Germany) at
×50 magnification. Failure classification was as follows:
adhesive between the cement and ceramic (adhesive
zone), cohesive in the ceramic or cohesive in the resin
block. Specimens were further evaluated under Scanning
Electron Microscopy (SEM) (Jeol-JSM-T330A, Tokyo,
Japan).
Furthermore, on additional eight ceramic blocks
chemical analysis was performed using X-ray Energy
Dispersive Spectrometry (EDS) (Jeol-JSM-T330A) at low
vacuum level of 40 Pa pressure using the secondary
electron mode (20 KV of acceleration, working distance:
15 mm).
Statistical analysis
Statistical analysis was performed using SPSS 11.0
software for Windows (SPSS Inc., Chicago, IL, USA).
Bond strength data (MPa) were submitted to two-way
analysis of variance (2-way ANOVA) with the bond
strength as the dependent variable and the heat
treatment and etching as independent variables. Due to
significant differences between groups, multiple
comparisons were made using Tukey’s tests. P values
less than 0.05 were considered to be statistically
significant in all tests.
RESULTS
During cutting procedures, 0, 0, 5, 3 pre-test failures
were experienced for Groups 1, 2, 3 and 4. These were
considered as 0 MPa.
Groups 1 and 2, where the ceramic surfaces were
etched with HF gel, showed significantly higher mean
bond strength (17.6±2.3 and 19±3.2, respectively) than
those of Groups 3 and 4 where the ceramics were only
silanized (9.1±2.8, 10.9±1.8, respectively) (p<0.05) (Table
2). Heat treatment of silane did not increase the results
neither in the HF etched nor in the non-etched groups
Minimum Maximum
13.72 20.39
13.98 22.40
 6.31 12.59
 7.37 13.63
 Dent Mater J 2011; 30(3): 392–397 395

(p>0.05). ceramic based on silica (SiO2), potassium feldspath (K2O.

The failure analysis showed exclusively mixed
failures (adhesive between ceramic and cement and
cohesive in the cement) in all groups (Figs. 1a-b).
SEM image of non-heat treated silanized surfaces
showed more agglomerates than the heat-treated ones
(Figs. 2a-b).
EDS analysis presented Silica (Si), Sodium (Na),
Aluminum (Al), Potassium (K), Oxygen (O) and Carbon
(C) which characterizes the microstructure of a glass-
Al2O3. 6SiO2) or sodium (Na2O.Al2O3.6SiO2).
DISCUSSION
During the adhesive cementation process of ceramic
restorations, many factors may influence the bonding
between the restorative material and the dental tissues.
The bond strength could be measured using different
mechanical tests. Shear test is widely used, as it is an

(a) (b)

Fig. 1 Representative SEM micrographs (×500 magnification) of mixed failure types from (a) Group 1 and (b) Group 2.

(a) (b)

Fig. 2 Representative SEM micrographs (×2,000 magnification) of silanized ceramic surfaces (a) before and (b) after heat
treatment. Note that the non-heat treated silanized surfaces showed more agglomerates than the heat-treated
ones.
396 Dent Mater J 2011; 30(3): 392–397
easy method to perform. However, shear test is not
considered as an ideal mechanical test since it often
yields to cohesive failures in the substrate19). The high
incidence of cohesive failures of the substrate is related
to non-uniform stress distribution at the adhesive joint
that undergo shear stresses requiring more forces from
the substrate than the adhesive interface itself. On the
other hand, conventional tensile tests have some
limitations due to the difficulty of aligning the specimens
in the universal testing machine, which in turn
distributes the stresses uneven at the adhesive
interface25). The choice of the microtensile test in this
study was because of its reliability in testing adhesion to
dental tissues or and ceramics as opposed to the other
methods2,13). Alignment of the bar specimens are also of
importance in this test. Therefore, an alignment device
was adapted for parallel placement of the specimens
during testing.
The results of this study showed no additional effect
of silane heat treatment on the mean bond strength.
Thus, the hypothesis was rejected. These findings did
not corroborate with the studies of Hooshmand et al.14)
and Moharamzadeh et al.26). This may be explained by
the differences in the test method used. While Hooshmand
et al.14) used the conventional tensile test, in the study of
Moharamzadeh et al.26) shear test was used.
The heat treatment of silane in fact eliminates the
water, alcohol and other by-products from the ceramic
surface. In addition, it helps to complete the condensation
reaction between silica and silane promoting the
formation of a covalent bond in the silane-ceramic
interface, making it more effective and resistant3). Silane
heat treatment could be achieved in different ways. In
previous studies, hot air application at 100°C for 1
minute16), hot air application at 50°C for 15 seconds16)
and heat treatment in furnace at 100°C for 2 minutes26)
have been tried. As a result of a series of preliminary
experiments for standardization, in this study, heat
treatment was performed in the oven at 100°C for 2
minutes. The results of this study also did not corroborate
with the results of Fabianelli et al.16), where also
microtensile test was employed. Although the test
method was the same in that study, silane heat treatment
was performed with hot air at 100°C for only 1 minute.
Therefore, prolonged duration and heat application
mode seems to affect the results yielding to discrepancy
between the results of different studies. Future studies
should try to standardize the heat application on silane.
The durable bonding between ceramic and resin
cement that is achieved through surface conditioning
appeared to be an important factor in the longevity of the
restorations17). The commonly applied surface
conditioning feldspathic ceramic is HF acid etching
followed by silane application7-9). The hydrofluoric acid
reacts selectively with the silica present on the
microstructure of ceramic forming hexafluorsilica. As a
result of this reaction, the ceramic surface becomes
irregular and porous increasing the surface area and
facilitating the penetration of the bonding agent into the
microretentions of ceramic surface conditioned by acid.
In this study, the major gain in bond strength was due to
the HF etching as observed in Groups 1 and 2. In the
groups where no HF etching was performed the mean
bond strength was almost 50% less. These findings
indicate the importance of etching prior to silane
application that was clearly more important than the
silane heat treatment. On the other hand, the use of
silane has a great importance for the adhesive
cementation technique11,22). As it is considered an organic-
functional molecule, it promotes chemical adhesion
between the inorganic substratum and organic polymers.
It should also be noted that in this study an MDP
containing resin cement was used. Silane reaction may
differ with other resin cements containing methacrylate
monomers.
Besides microtensile bond strength results, the SEM
findings showed that heat treatment seemed to promote
better damping, absorption of the silane yielding to
greater contact and infiltration of the bonding agent into
the porosities of the etched ceramic.
The microtensile bond strength data must be coupled
with the failure types. Failure analysis showed
exclusively mixed failures. No cohesive failures in the
ceramic substrate were observed. Previous studies also
reported higher incidence of mixed or adhesive failures
compared to other test methods where more cohesive
failures of the substrate was observed5,26).
According to results of this study, it may be possible
to conclude that the heat treatment of silane does not
improve the bond strength of the cement, Panavia F2.0,
tested in this study.
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