Effect of Post-silanization Heat Treatments of Silanized

Feldspathic Ceramic on Adhesion to Resin Cement

Pedro Henrique Corazzaa / Samia Carolina Mota Cavalcantia / José Renato Cavalcanti
Queirozb / Marco Antonio Bottinoc / Luiz Felipe Valandrod

Purpose: To evaluate the effect of post-silanization heat treatment of a silane agent and rinsing with hot water of
silanized CAD/CAM feldspathic ceramic surfaces on the microtensile bond strength between resin cement and
the ceramic, before and after mechanical cycling.
Materials and Methods: Blocks measuring 10 x 5.7 x 3.25 mm3 were produced from feldspathic ceramic cubes
(VITA Mark II, VITA Zanhfabrik). Each ceramic block was duplicated in composite resin using a template made
of polyvinylsiloxane impression material. Afterwards, ceramic and corresponding resin composite blocks were
ultrasonically cleaned and randomly divided according to the 5 strategies used for conditioning the ceramic sur-
face (n = 10): GHF: etching with hydrofluoric acid 10% + rinsing with water at room temperature + silanization at
20°C; G20: silanization; G77: silanization + oven drying at 77°C; G20r: silanization + hot water rinsing; G77r: si-
lanization + oven drying at 77°C + hot water rinsing. The resin and ceramic blocks were cemented using a dual-
curing resin cement. Every group was divided in two subgroups: aging condition (mechanical cycling, designated
as a) or non-aging (designated as n). All the bonded assemblies were sectioned into microsticks for microtensile
bond strength (+TBS) testing. The failure mode of the tested specimens was assessed and +TBS data were sta-
tistically analyzed in two ways: first 2-way ANOVA (GHF, G20 and G77 in non-aging/aging conditions) and 3-way
ANOVA (temperature x rinsing x aging factors, excluding GHF), followed by Tukey’s test (p = 0.05).
Results: The 2-way ANOVA revealed that the +TBS was significantly affected by the surface treatment
(p < 0.001) but not by aging (p = 0.68), and Tukey’s test showed that G77-n/G77-a (18.0 MPa) > GHF-n/GHF-a
(12.2 MPa) > G20-n/G20-a (9.1 MPa). The 3-way ANOVA revealed that the +TBS was significantly affected by the
“heat treatment” and “rinsing” factors (p < 0.001), but not affected by “aging” (p = 0.36). The rinsing procedure
decreased, while oven drying increased the bond strengths. Group G77, in both non-aging and aging conditions
(18.6–17.4 MPa), had the highest bond values. Failure modes were mainly mixed for all groups.
Conclusion: Oven drying at 77°C improved the bond strength between the resin cement and feldspathic ceramic,
but hot water rinsing reduced the bond strength and should not be recommended.
Keywords: adhesion, microtensile bond strength, ceramic, heat treatment, silane.

J Adhes Dent 2013; 15: 473–479. Submitted for publication: 14.03.12; accepted for publication: 20.12.12.
doi: 10.3290/j.jad.a29592

In recent years, clinical interest in feldspathic ceramic

a Doctoral Student, Department of Prosthodontics and Dental Materials, São restorations has grown, particularly in those made by
Jose dos Campos Dental School, São Paulo State University (UNESP), São CAD/CAM systems. The bonding procedure is crucial to
José dos Campos, Brazil. Performed experiments, experimental design,
wrote manuscript.
obtain success using this type of restoration.9 For ad-
b
hesive cementation of these glassy matrix ceramics, an
Research Assistant, Department of Physics, Technological Institute of Aero-
nautics São José dos Campos, Brazil. Idea, hypothesis, experimental design, important step is the well-established method of using a
wrote and proofread manuscript. silane coupling agent to improve adhesion between the
c Professor, Department of Prosthodontics and Dental Materials, São Jose dos inorganic phase of the ceramic and the organic phase of
Campos Dental School, São Paulo State University (UNESP), São José dos the bonding agent.15 However, adequate performance
Campos, Brazil. Experimental design, contributed substantially to discussion,
proofread the manuscript. of silane is limited by water hydrolysis, which damages
d Associate Professor, Prosthodontics Unit, Faculty of Odontology, Federal Uni-
the physical bonds at the interface and weakens the
versity of Santa Maria, Santa Maria, Brazil. Experimental design, contributed adhesion.14 Consequently, this results in the mechani-
substantially to discussion, proofread manuscript. cal failure of adhesion with the bonding agent systems,
reducing the lifespan of the restoration.
Correspondence: Dr. José Renato Cavalcanti de Queiroz, Praça Marechal Edu- In order to minimize this effect, hydrofluoric acid (HF) is
ardo Gomes, 50, Vila das Acácias, São José dos Campos, SP, Brazil 12.228- applied to the ceramic surface to improve the conditions
900. Tel: +55-84-3222-1804; Fax: +55-84-3222-9975. e-mail: joserenatocq@
hotmail.com of the silane reaction with the glassy matrix. This ap-

Vol 15, No 5, 2013 473

Corazza et al

Table 1 Brand name, material type, main composition, manufacturers and batch number of the materials used in
this study

Brand name Material type Main composition Manufacturer Batch

number
VITAblocs Mark II Feldspathic Feldspathic crystalline particles (SiO2, Al2O3, Na2O, K2O) in VITA Zahnfabrik 15220
ceramic glassy matrix

W3D-Master Composite resin Methacrylate-based monomers 23.7 wt%, silica, silicate Wilcos 001/10
glass and fluoride containing fillers 75.6 wt%, polymerization
catalysts 0.6 wt%, inorganic pigments 0.1 wt%

Monobond-S Silane coupling 1% 3-methacryloxypropyl trimethoxysilane (3-MPS) ethanol/ Ivoclar Vivadent M71746
agent water-based solvent

Variolink II Resin cement Monomer matrix: bis-GMA, urethane dimethacrylate, and Ivoclar Vivadent N16895
triethylene glycol dimethacrylate. Inorganic fillers: barium
glass, ytterbium trifluoride, Ba-Al-fluorosilicate glass, and
spheroid mixed oxide

Porcelain Acid etchant 10% hydrofluoric acid Dentsply 452321D

conditioner

proach has made it possible to adhere minimally invasive etching with HF acid before silane application could be
restorations to dental tissues that do not rely on mech- eliminated. However, since the ceramic restoration re-
anical retention principles. However, the high chemical ceives bite forces during its functional life, the effect of
toxicity of HF acid etching, the possibility of producing post-silanization heat treatment and hot water rinsing of
insoluble silica-fluoride salts that can interfere in resin silanized feldspathic ceramic on the silane layer’s cap-
bond strength, and the fact that some high crystalline acity to absorb mechanical stress is important and has
content ceramics may not benefit from this process are not been previously tested.19
three important reasons for omitting HF from the bonding Accordingly, the aim of this study was to evaluate the
procedure.11 Despite these reasons, HF continues to be effect of post-silanization heat treatment and rinsing with
used in dentistry both because of its success in improv- hot water of silanized CAD/CAM feldspathic ceramic sur-
ing bonding with glassy ceramics and due to the lack of faces on the microtensile bond strength between resin
an alternative surface treatment that offers the same cement and the ceramic, before and after mechanical
quality of bonding results as this traditional conditioning cycling (aging). The hypothesis was that these alternative
approach. The literature describes that several ceramic ceramic surface treatments would have a beneficial effect
surface treatments involving acids that present fewer on the bond strength, while the mechanical cycling would
hazards have been tested without success compared to have a negative effect on adhesion.
HF etching.5,8 If the goal is to eliminate the HF etching
procedure without jeopardizing the chemical reaction at
this interface, the traditional bonding protocol must be MATERIALS AND METHODS
changed in a way that optimizes the silane effect on bond-
ing ceramic to resin. The brand names, material types, main compositions,
In dentistry, silane drying conditions and post-si- manufacturers, and batch numbers of the products used
lanization heat treatment to eliminate solvents and to in the current study are presented in Table 1.
enhance the crosslink reaction have previously been
discussed.6,11,13,17 Moreover, previous studies have Experimental Setup
shown that bathing silanized ceramic in hot water im- Based on the results of a pilot study with a conventional
proves the capacity of the interface to resist hydrolytic feldspathic ceramic treatment (hydrofluoric acid + silane
degradation under storage in water and during thermocy- + resin cement), the power and sample statistical test
cling.13 It has been proposed that hot water rinsing can was performed to determine the number of samples
eliminate physi- or chemisorbed silane molecules, reduc- “n” required for this study. Since a power of 0.83 was
ing the thickness of the layer and maintaining only the determined for n = 5, this was the sample size chosen
innermost region closest to the ceramic surface, which is for this investigation. Seven blanks (15 mm x 12 mm x
the most stable and hydrolysis-resistant region.20 After 10 mm) of feldspathic ceramic for CAD/CAM (VITA Mark
storage and thermocycling, the results of early in vitro II, VITA Zanhfabrik; Bad Säckingen, Germany) were sec-
studies11,13,17 showed that these procedures (post-si- tioned (LabCut 1010, Extec; Enfield, CT, USA) into 50
lanization heat treatment and/or hot water rinsing) were blocks of approximately 10 mm x 5.7 mm x 3.25 mm.
sufficient to promote adequate bond strength between The ceramic blocks were molded using addition sili-
glass ceramic and a polymeric matrix, suggesting that cone putty (Elite HD, Zhermack; Badia Polesine, Italy).

474 The Journal of Adhesive Dentistry

 Corazza et al

Each block was pushed into the silicone putty until Table 2 Experimental design considering the 3 fac-
3 mm remained between the upper portion of the mold tors (surface treatment in 3 levels, rinsing in 2 levels,
and the surface of the block. Thereafter, a composite resin and mechanical cycling in 2 levels)
was applied incrementally (1.5 mm thickness for each in-
crement) and light cured for 40 s (XL 3000, 3M ESPE; St Groups Surface Treatment Rinsing Mechanical
Paul, MN, USA) at a light output of 500 mW/cm2 on the cycling
upper side of the specimen. The light intensity was verified
with a radiometer throughout the experiment, so that it was GHF-n HF 10% etching + silane No
no lower than 500 mW/cm2. The cementation surfaces of GHF-a Aged
each ceramic block and resin composite block were ground
finished with 600-grit silicon carbide metallographic abra- G20-n Silane No No
sive papers (3M ESPE) under water cooling in a polishing G20-a Aged
machine (DP-10, Panambra; São Paulo, Brazil) in order to
standardize the surface. Prior to the ceramic surface treat- G20r-n Yes No
ments, all the blocks (ceramic and composite) were ultra- G20r-a Aged
sonically cleaned (VITAsonic, VITA Zanhfabrik) in isopropyl
alcohol for 5 min and dried by oil-free air spray for 15 s. G77-n Silane + Heat treat- No No
The paired blocks (ceramic and resin composite) were ment at 77°C
G77-a Aged
randomly divided into groups according to the 5 strategies
used to treat the ceramic surface (n = 10): G77r-n Yes No
y GHF: The ceramic surface was etched using 10% HF
G77r-a Aged
acid gel (Dentsply; Petropolis, Brazil) for 60 s, rinsed
with air-water spray for 30 s, and air dried. The ce-
ramics were ultrasonically cleaned in distilled water
for 5 min. A silane coupling agent was applied on the low speed under water cooling. The edge sections (mea-
cementation surface and left to react with the surface suring approximately 1 mm) were discarded due to the
for 3 min. Next, an air spray was applied for 15 s. possibility of excess or absence of cement at the inter-
y G20 and G77: A silane coupling agent was applied to face that might alter the results. Only the central speci-
the ceramic surfaces, left to react with the surface for mens were used for the experiments. Approximately
3 min and air dried for 15 s. The G20 group specimens 15 sticks were obtained from each block. The beam
were maintained at 20°C (controlled ambient tem- sticks had non-machined (non-trimmed) bonding areas,
perature) for 1 min prior to cementation. The G77 group with a bonded area measuring 1.0 ± 0.1 mm2 and ap-
specimens were placed into an oven at 77°C for 1 min. proximately 7 mm in length.
y G20r and G77r (rinsed groups): These groups were
prepared in the same way as G20 and G77, respect- Microtensile Bond Strength Test (+TBS)
ively, followed by hot water rinsing (ca 79°C) of the Each stick was fixed to the rods of a device adapted
silanized ceramic surface for 15 s and drying for 30 s for this test using cyanoacrylate gel (Super Bonder Gel,
with air spray. Loctite; São Paulo, Brazil) to maintain the adhesive
zone unattached to the device rods. The sticks were
The silane coupling agent was applied under controlled positioned parallel to the long axis of the device to re-
relative air humidity of 23%. The temperature evaluated duce the bending stresses. The device was fixed in a
was based on the ambient temperature (20°C), and the universal testing machine (EMIC DL-1000, EMIC; São
alcohol (solvent) evaporation temperature (79°C) was José dos Pinhais, Brazil) as parallel as possible to the
adjusted to the altitude of the research laboratory in application of the tensile load. Testing was performed at
São José dos Campos, Brazil (77°C). a crosshead speed of 0.5 mm/min.
The resin composite blocks were cemented (Variolink The bond strength was calculated according to the for-
II, Ivoclar Vivadent; Schaan, Liechtenstein) on the ceramic mula R = F/A, where R is the strength (MPa), F is the load
blocks under a constant pressure of 750 g for 1 min using in Newtons (N) required to fracture the specimen, and A
a cementation device, and then light cured for 40 s on is the interface area of the specimen (mm2) as measured
each side. The ceramic-resin blocks were stored in dis- with a digital caliper before testing.
tilled water at 37°C for 24 h.
The groups were divided in two subgroups (n = 5): a, Fracture Analysis
aged; and n, non-aged. The aged groups were submit- The specimens were analyzed under an optical micro-
ted to 200,000 mechanical cycles at 4 Hz and a load scope (Measuring Microscope MFA Mitutoyo; Tokyo,
of 133 N under immersion in water at 37°C (ERIOS ER- Japan) at 30X magnification, and the images were re-
11000; São Paulo, Brazil) (Table 2). corded using a digital camera (Cybershot, Model DSC
S85, Sony; Tokyo, Japan) connected to the microscope
Specimen Preparation for Bond Strength Test to characterize the ceramic surfaces and the failure
The ceramic-resin blocks were sectioned in a sectioning modes. In addition, the fractured surfaces of the sticks
machine (LabCut 1010, Extec) using a diamond disk at were gold coated in a sputtering device and analyzed

Vol 15, No 5, 2013 475

Corazza et al

Table 3 Number of sticks and blocks produced and number (N), percentage (%) of pre-test failures (PTF) during
sectioning, microstick preparation, mechanical cycling (MC), and total number of sticks prior to μTBS according to
the experimental groups

Groups Specimens N (%) of PTF during: N (%) of Total

sticks blocks cutting preparation MC PTF Sticks tested
GHF-n 70 5 0 (0%) 13 (18.57%) 0 (0%) 13 (18.57%) 57 (81.83%)

GHF-a 70 5 0 (0%) 12 (17.14%) 0 (0%) 12 (17.14%) 58 (82.86%)

G20-n 80 5 42 (52.5%) 8 (10%) 0 (0%) 50 (62.5%) 30 (37.5%)

G20-a 80 5 39 (48.75%) 3 (3.75%) 0 (0%) 42 (52.5%) 38 (47.5%)

G77-n 75 5 2 (2.67%) 13 (17.33%) 0 (0%) 15 (20%) 60 (80%)

G77-a 75 5 0 (0%) 0 (0%) 0 (0%) 0 (0%) 75 (100%)

G20r-n 70 5 33 (47.14%) 9 (12.86%) 0 (0%) 42 (60%) 28 (40%)

G20r-a 70 5 40 (57.14%) 4 (5.71%) 14 (20%) 58 (82.85%) 12 (17.15%)

G77r-n 70 5 20 (28.57%) 18 (25.71%) 0 (0%) 38 (54.29%) 32 (45.71%)

G77r-a 75 5 12 (16%) 5 (6.67%) 0 (0%) 17 (22.67%) 58 (77.33%)

Table 4 Results of 2-way ANOVA for μTBS data for rinsing. To analyze the influence of hot water rinsing as-
surface treatment (ST) and aging (*p < 0.05). sociated with the heating treatment and aging, excluding
the HF + silane groups, 3-way ANOVA was used. Both
Source DF Seq SS Adj MS F p analyses were performed using the means of the repeti-
tions (microsticks) from each block.
ST 2 403.644 201.822 29.08 0.0*

Aging 1 1.178 1.178 0.17 0.684

RESULTS
ST x aging 2 26.419 13.209 1.9 0.171

Error 24 166.658 6.940

During mechanical cycling, only one block debonded
(G20r-a). The microsticks that failed prior to and during
Total 29 597.809 block sectioning were included in the statistical analy-
ses; these were assigned the lowest value measured
within the respective group.2,22 Some microsticks failed
during +TBS test preparation and were not included in
the statistical analyses (Table 3).
The two-way ANOVA, considering the factors surface
under a scanning electron microscope (Zeiss DSM 950, treatment and aging, revealed that the +TBS was signifi-
Carl Zeiss; Jena, Germany) at 20 kV in the secondary cantly affected by the surface treatment (p < 0.001) and
electron mode for topographical observation. not affected by aging (p = 0.68) (Table 4). Tukey’s test
The failure types were classified according to the fol- revealed that: G77/G77-a (18.0 ± 1.6 MPa) > GHF/GHF-a
lowing scores: A: adhesive fracture along the interfacial (12.2 ± 2 MPa) > G20/G20-a (9.1 ± 3.9 MPa).
region between the bonding agent and ceramic; B: cohe- The second analysis (3-way ANOVA; heat treatment of
sive fracture along the luting agent; C: cohesive fracture silane x hot water rinsing x aging) revealed that the +TBS
along the ceramic; and D: mixed fracture, adhesive failure was significantly affected by the factors heat treatment and
between the resin and ceramic together with a cohesive rinsing (p < 0.001) but not by aging (p = 0.36) (Table 5).
fracture of the resin. The percentage of each type of fail- The means of μTBS (MPa) for the different heat treatments
ure was calculated for each group. of silane and rinsing factors are shown in Fig 1.
The fracture analysis of the specimens revealed ad-
Statistical Analysis hesive failure along the interfacial region between the
Two statistical tests were applied to analyze the data. resin cement and the feldspathic ceramic, cohesive
To analyze the influence of the heat treatment of silane fracture of feldspathic ceramic, and mixed failure, ie,
on the bond strength, 2-way ANOVA was performed to cohesive fracture of the resin cement combined with ad-
compare the surface treatments before and after aging hesive failure. The pattern of failure was predominantly
(yes or no), excluding the groups submitted to hot water mixed (Table 6).

476 The Journal of Adhesive Dentistry

 Corazza et al

Table 5 Results of 3-way ANOVA for μTBS data for Table 6 Means and standard deviations (SD) of μTBS
temperature of silane dry (T), hot water rinsing (R) and results (MPa) and failure modes (%) (adhesive, cohe-
aging by mechanical cycling (A) factors (*p < 0.05). sive, mixed) for different groups

Source DF Seq SS Adj MS F p Groups μTBS results Failure mode (%)

T 1 512.90 576.61 52.07 0.0* Mean SD Adhesive Cohesive Mixed
R 1 165.70 167.15 18.26 0.0* GHF-n 13.3 1.5 5.88 17.65 76.47
A 1 4.16 7.99 0.87 0.358 GHF-a 11.2 1.9 13.8 20.69 65.52
TxR 1 24.39 28.36 3.10 0.089 G20-n 8.0 3 3.45 6.9 89.7
TxA 1 0.62 2.12 0.23 0.634 G20-a 10.3 4.6 2 13.51 83.78
RxA 1 1.77 1.77 0.19 0.663 G77-n 18.6 1.1 3.28 34.43 62.3
TxRxA 1 45.11 45.11 4.93 0.034* G77-a 17.4 1.8 - 28.76 71.23
Error 32 274.61 9.15 G20r-n 7.6 2.3 38.2 5.88 55.88
Total 39 1029.28 G20r-a 6.0 2.1 28.57 - 71.43

G77r-n 10.1 4.8 9.38 21.87 68.75

G77r-a 14.1 2.7 8.2 11.48 80.33

Interval plot of mean

95% CI fot the mean
20

15
Mean

10

0
NO YES NO YES
Rinsing G20 G77
temperature

Fig 1 +TBS results (MPa) of the groups submitted to different Fig 2 Photomicrography (SEM) of a stick (G77-aging) show-
heat treatment (temperature at 20°C [G20] in blue and 77°C ing a representative mixed failure mode (interfacial zone of
[G77] in red) and additional hot water rinsing (NO x YES). ceramic side). Magnification: 70X.

DISCUSSION interface aging using mechanical cycling. Thus, the

test hypothesis was partially rejected.
Adhesion between feldspathic ceramic and resin ce- The groups with no acid etching and no oven drying at
ments has been improved by alternative surface treat- 77°C showed the lowest μTBS results and also the high-
ments with post-silanization heat treatment and hot est PTF percentage. All G20 groups had over 50% PTF.
water rinsing, even following storage and thermocy- This is a consistent finding, since the weaker the adhe-
cling, 11,13,17 by increasing the crosslinking network sion, the greater the susceptibility to failures during the
and removing physisorbed and chemisorbed regions of cutting of the blocks.
the silane layer, leaving only the reacted region near Cementation is an important step in restoration with
the ceramic surface.18,21 The findings from the current ceramics, and the bond strength between the ceramic and
study verified that only the increase in temperature to resin cement contributes to the success of restoration.
dry the silane improved bond strength, even following Several in vitro studies have evaluated the adhesion be-

Vol 15, No 5, 2013 477

Corazza et al

tween ceramic and resin.5,6,8,11,13,17 Some studies have silane layer, removing the outermost unreacted silane
indicated that the +TBS test is a more appropriate method regions.14 However, the thickness plays a role in bond
than the shear test for evaluating the bond strength of strength results.18 While an excessive amount of cou-
adhesive interfaces, since the +TBS test provides more pling agent is inefficient at providing a reliable bond,7
uniform interfacial stress distribution than does the shear it is also true that the development of a thicker silane
test.4 In order to minimize the influence of interfacial film with a stronger crosslinking network can be very
defects and eliminate non-uniform stress distribution at useful.12,18 Structures under stress need a thick silane
the adhesive interface, a tensile bond test with a reduced layer to contribute to the film’s mechanical properties
testing area was developed. Due to these considerations, and possible solvent effects of the matrix.12,18 Thus,
the +TBS was performed in this study (sticks), using the there must be an optimum thickness for the silane layer
blocks as experimental units.2,24 that effectively bonds organic and inorganic materials,
The interface studied (ceramic/resin) was bonded by supports hydrolysis degradation, and absorbs mech-
a silane coupling agent. The instability of this layer can anical stress without cracks forming within the silane
cause hydrolytic degradation at the adhesive interface.16 layer.19
Thus, bis-GMA resin cement without adhesive monomers Hooshmand et al13 verified that hot water rinsing
was used in this research. Consequently, the effect of the (80°C) following post-silanization heat treatment (50°C)
surface treatments examined was demonstrated in the improved initial bond strength and reduced adhesive fail-
+TBS results, since the quality of the bond using a silane ures. However, the results obtained here indicate that
coupling agent depends not only on the silane specifica- rinsing had a negative effect on bond strength at both
tions (solution pH, concentration, the nature of the sol- temperatures tested (20°C and 77°C). Moreover, this
vent, hydrolysis time), but also on the application protocol treatment increased the number of PTF in the aged groups
used (drying conditions, time between silane application (-a) at both temperatures; one block in G20r-a was com-
and bonding, temperature, air humidity).1 Thus, one pre- promised during mechanical cycling and the incidence of
caution taken concerned relative humidity control during adhesive failures was greater. These results suggest that
the silane application procedures. It has been previously the region (chemisorbed and physisorbed) of the silane
demonstrated that silane adhesion decreases as the rela- layer that was removed could be important to resist the
tive humidity of the air increases, probably affecting the stress created during mechanical cycling.
water desorption rate.23 In this study, silane was applied Previous studies have shown that storage for differ-
at room temperature (20°C) at 23% relative humidity, ent periods and thermocycling did not reduce the bond
and then the specimens were submitted to further heat strength when silane was dried on a polished surface
treatment either in an oven or by hot water application. without previous surface treatment (acid etching).13 The
The post-silanization heat treatment of the silane layer present results showed that mechanical cycling (200,000
at 77°C in an oven was chosen due to the boiling tem- cycles) in a wet environment was unable to reduce the
perature of the solvent used (alcohol) and the possibility bond strength for all the surface treatments tested, but
of removing unreacted silane regions by air movement was important for indicating the quality of adhesion among
or other strategies used to apply heat to the silanized the groups, such that the number of PTF for weak surface
surface.11,13,17,19 treatments increased.
The well-established etching treatment of the porce- In this study, only one silane coupling agent was
lain surface has been reported in the literature for a long used. Although 3-methacryloxypropyl trimethoxysilane is
time.20,22 However, previous in vitro studies showed that the most commonly used silane coupling agent to bond
conventional surface treatment with acid etching could feldspathic ceramic surfaces to resinous materials, this
be substituted by heat treatment of the silanized ceramic could be considered as a limitation of this study. In future
surface,11,13,17 which agrees with the present results. De- studies, the post-silanization heat treatment parameters
spite aging by mechanical cycling, post-silanization heat need to be verified for other silanes. In addition, greater
treatment in an oven at 77°C improved the +TBS with aging by harsh mechanical cycling should be performed
the lowest standard deviation and reduced the pre-test to assess the resistance to hydrolysis of the interfaces
failures (PTF) compared with other groups, even with trad- evaluated at this juncture.
itional feldspathic ceramic surface treatment (acid etch-
ing). Furthermore, these groups presented a decrease in
adhesive failures following the +TBS test. Some theories CONCLUSIONS
have been proposed to explain the effect of post-silani-
zation heat treatment on the silane layer: a) increased The heat treatment at 77°C of an applied silane agent
crosslinking network, inhibiting water diffusion through improved resin adhesion to the glassy ceramic, but hot
the silane layer;7,23 b) oligomerization with full siloxane water rinsing of the silanized surface decreased the
bond formation between the glass matrix and silane cou- bond strength and is not recommended. The mechanical
pling agent;3,15 c) evaporation of solvent and volatilization cycling regimen used here was unable to damage the
of wastes formed during silanol group hydrolization, which interfaces; thus, the parameters should be changed for
could create large internal pressure gradients.3,10 futures studies.
Concerning rinsing the silanized surface with hot wa-
ter, this procedure can reduce the thickness of the

478 The Journal of Adhesive Dentistry

 Corazza et al

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