Vous êtes sur la page 1sur 9

d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 13231331

available at www.sciencedirect.com

journal homepage: www.intl.elsevierhealth.com/journals/dema

Microtensile bond strength of a resin cement to feldpathic ceramic after different etching and silanization regimens in dry and aged conditions
b, Aline Scalone Brentel a , Mutlu Ozcan , Luiz Felipe Valandro a,c , Lilian Guimaraes a a a Alarc a , Regina Amaral , Marco Antonio Bottino Paulo State University, Department of Dental Materials and Prosthodontics, Sao Jos Sao e dos Campos, Brazil University Medical Center Groningen, University of Groningen, Department of Dentistry and Dental Hygiene, Clinical Dental Biomaterials, Antonius Deusinglaan 1, 9713 AV Groningen, The Netherlands c Federal University of Santa Maria, Department of Restorative and Prosthetic Dentistry, Santa Maria, Brazil
b a

a r t i c l e
Article history:

i n f o

a b s t r a c t
Objectives. This study evaluated the durability of bond strength between resin cement and a feldspathic ceramic submitted to different etching regimens with and without silane coupling agent application. Methods. Thirty-two blocks (6.4 mm 6.4 mm 4.8 mm) were fabricated using a microparticulate feldspathic ceramic (Vita VM7), ultrasonically cleaned with water for 5 min and

Received 19 July 2006 Accepted 16 November 2006

Keywords: Acidulated phosphate uoride Etching Hydrouoric acid Microtensile bond strength Feldspathic ceramic Silane coupling agent

randomly divided into four groups, according to the type of etching agent and silanization method: method 1, etching with 10% hydrouoric (HF) acid gel for 1 min + silanization; method 2, HF only; method 3, etching with 1.23% acidulated phosphate uoride (APF) for 5 min + silanization; method 4, APF only. Conditioned blocks were positioned in their individual silicone molds and resin cement (Panavia F) was applied on the treated surfaces. Specimens were stored in distilled water (37 C) for 24 h prior to sectioning. After sectioning the ceramic-cement blocks in x- and y-axis with a bonded area of approximately 0.6 mm2 , the microsticks of each block were randomly divided into two storage conditions: Dry, immediate testing; TC, thermal cycling (12,000 times) + water storage for 150 d, yielding to eight experimental groups. Microtensile bond strength tests were performed in universal testing machine (cross-head speed: 1 mm/min) and failure types were noted. Data obtained (MPa) were analyzed with three-way ANOVA and Tukeys test ( = 0.05). Results. Signicant inuence of the use of silane (p < 0.0001), storage conditions (p = 0.0013) and surface treatment were observed (p = 0.0014). The highest bond strengths were achieved in both dry and thermocycled conditions when the ceramics were etched with HF acid gel and silanized (17.4 5.8 and 17.4 4.8 MPa, respectively). Silanization after HF acid gel and APF treatment increased the results dramatically (14.5 4.217.4 4.8 MPa) compared to non-silanized groups (2.6 0.88.9 3.1 MPa) where the failure type was exclusively (100%) adhesive between the cement and the ceramic. Signicance. Silanization of the feldspathic ceramic surface after APF or HF acid etching increased the microtensile bond strength results signicantly, with the latter providing higher results. Long-term thermocycling and water storage did not decrease the results in silanized groups. 2006 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Corresponding author. Tel.: +31 50 363 8528; fax: +31 50 363 2696. E-mail addresses: mutluozcan@hotmail.com, M.Ozcan@med.rug.nl (M. Ozcan). 0109-5641/$ see front matter 2006 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved. doi:10.1016/j.dental.2006.11.011


d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 13231331



Minimal invasive approach utilizing adhesive technologies in dentistry allowed for preservation of tooth tissues to a great extend. Ceramic or resin composite indirect restorations need to be cemented adhesively. Clinical performance of metal-free xed-partial-dentures (FPD) made out of feldspathic ceramic, either in the forms of inlays, onlays or laminate veneers, substantially relies on the adhesion of the resin cements to these restorative materials and tooth tissues [1,2]. For the adhesive cementation procedures, enamel and dentin surfaces [3] as well as the ceramic surface [4] should be etched and adhesive systems should be employed. Acid-sensitive, glass-based ceramics (feldspathic, leucite and lithium disilicate ceramics) undergo surface degradation by hydrouoric (HF) acid gel yielding to a topographic pattern that favors micromechanical bonding. Also, due to its bifunctional characteristics, application of silane coupling agent on the etched ceramic surface may increase the chemical bonding between the ceramic and resin materials [57]. This process promotes the cement wettability on the ceramic surface [4,8], enhancing the contact with resin cements. Moreover, silane coupling agents couples the silica oxides present in ceramics to the organic matrix of resin cements by means of siloxane bonds [9,10]. Even though in the dental literature often the use of 510% HF acid gel has been recommended, some investigators used 1.23% acidulated phosphate uoride (APF) [11,12] that is weaker than HF acid gel. The hazardous and extreme caustic effects to soft tissues and the danger for clinical use of HF acid gels are well known due to its rapid vaporization and the danger of inhalation. For this reason, some studies questioned whether 1.23% APF gel might serve as a safe and effective substitute for etching ceramic surfaces to bond resin composite because of the reduced risk it presents [13]. HF acid gel is often indicated to be applied between 20 s and 1 min whereas APF gel for a longer period (25 min), where the latter is also used for topical uoride application. Some studies demonstrated that the bond strength of resin composites to silanized ceramics after being etched with APF was comparable to that of HF acid etching [1416]. However, the results were derived from shear tests. Although shear test measurements have been reported as the most prevalant in the literature [17], some researchers prefer modied tensile tests to eliminate the occurrence of non-uniform interfacial stresses [18,19] since the force distribution at the interface in shear testing may cause cohesive failure in the substrate which may lead to misleading information. Rapid increase in the amount of water absorbed by the composite materials causes hydrolysis and degradation of the silane. Water storage and thermocycling were described as detrimental for the silane-ceramic bond [20]. Reuter and Brose [21] reported that silanized interfaces appear to be unstable in humid conditions and the silane bond was found to deteriorate in moisture. Since the resins are permeable to water, the bond between silane and resin composite was expected to deteriorate by hydrolysis over time. However, in vitro studies either lack the aging conditions or employ short term water storage and/or thermocycling (see review by Ozcan et al.) [22].

Thus, the objectives of this study were to evaluate the microtensile bond strength between resin cement and a feldspathic ceramic submitted to different etching regimens, namely 10% HF acid gel and 1.23% APF gel with and without silanization and to observe the failure types. The studied hypotheses were that etching with HF acid gel would provide higher bond strength than APF, silanization would increase the bond strength and long-term thermocycling would reduce the bond strength values.


Material and methods

Ceramic blocks

An acetate template measuring 8 mm 8 mm 6 mm was machined. The ceramic blocks (Vita VM7 Dentin 5M2, Vita Zah nfabrik, Bad Sackingen, Germany; Batch # 7404) were prepared following the manufacturers instructions. The ceramic bulk was inserted and packed into the template. The blocks were sintered in a furnace (Vacumat, Vita) using the specic program indicated by the manufacturer. After sintering shrinkage of the ceramic of nearly 20%, the blocks measured approximately 6.4 mm 6.4 mm 4.8 mm. The cementation surface (6.4 mm 6.4 mm) was planed and polished in a machine using silicone carbide papers in sequence (600, 800 and 1200 grit) under cooling (3M, St. Paul, USA). Impressions were made from each ceramic block with addition silicone putty (Elite HD, Zhermack, Badia Polesine, Italy; Batch # 19915) in order to achieve 3 mm distance between the upper portion of the mold and the surface of the block. Thereafter, the cement was injected into this space.


Surface treatment methods

Prior to etching and silanization, all blocks were ultrasonically cleaned (Vitasonic, Vita Zanhfabrik, Germany) for 5 min using distilled water. Thirty-two ceramic blocks were randomly divided into four groups, according to the type of etching agent (HF acid gel or APF) with and without silanization. Eight blocks were designed for each etching method: Method 1: Ceramic surfaces were etched with 10% HF acid gel (Dentsply Petropolis, Brazil; Batch # 235100) for 1 min, rinsed with airwater spray and dried. The ceramics were cleaned ultrasonically in distilled water for 4 min. Then silane coupling agent was applied (Porcelain Primer, Bisco, Schaumburg, IL; Batch # 04000110696) with a clean brush one layer. Method 2: Same procedures were followed as described in method 1 without silanization. Method 3: In this group, ceramic surfaces were etched with 1.23% APF (Odahcam, Dentsply, Petropolis, Brazil; Batch # 592) for 5 min, rinsed with airwater spray and dried. The ceramics were cleaned ultrasonically in distilled water for 4 min. Then silane coupling agent was applied (Porcelain Primer) with a clean brush one layer. Method 4: Same procedures were followed as described in method 3 without silanization.

d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 13231331


Fig. 1 (a) Resin cement applied on ceramic block and attached to the metal base. (b) Production of non-trimmed of bar specimens.

Additional ceramic specimens (1 specimen/group) were prepared and submitted to the two types of etching procedures corresponding to the experimental groups. These non-silanized specimens were analyzed by scanning electron microscope (SEM) (ZEISS EVO50, Zeiss, Jena, Germany) in order to observe the topographic patterns achieved by the treatment methods described.


Application of cement

Each treated ceramic block was placed in its silicone mold. The resin cement (Panavia F, Kuraray, Okayama, Japan; Batch # 00022E) was mixed following the manufacturers instructions and injected into the mold on the treated surface of the ceramic block, using a centrix syringe (DFL, Rio de Janeiro, Brazil). The cement in the mold was light polymerized (XL 3000, 3M ESPE, MN, USA; light output: 500 mW/cm2 ) for 40 s at the sides of the specimen. Oxygen inhibiting gel (Oxyguard II, Kuraray, Okayama, Japan; Batch # 00482A) was applied on the free surfaces. After 10 min, the ceramic block-resin cement assembly was removed from the mold and the cement was once again submitted to light polymerization from ve aspects of the block (upper and lateral) for 40 s per side [23]. The blocks were rinsed with water and stored in distilled water at 37 C for 24 h until preparation of the specimens (sp).


Specimen preparation for the microtensile test

Ceramic-cement blocks were sectioned using a diamond disc Paulo, Brazil, no. 34570) at low-speed, under (Microdont, Sao

water cooling, in a sectioning machine [24]. Initially, the cemented blocks were xated with cyanoacrylate adhesive Paulo, Brazil) on a gel (Super Bonder Gel, Loctite Ltd., Sao metallic base that was attached to the sectioning machine. The blocks were positioned as perpendicular as possible in relation to the diamond disc of the machine. The rst section measuring approximately 1 mm was discarded in case of the possibility of excess or absence of cement at the interface that might alter the results. Thereafter, two sections measuring 0.8 0.1 mm in thickness were achieved. Each section was rotated in 90 and once again xated to the metallic base. The rst section was discarded (1 0.1 mm) because of the aforementioned reasons. Subsequently, three to four other sections were achieved, also measuring 0.8 0.1 mm in thickness. This process was followed for the other two sections and thus only the central specimens were used for the experiments. The beam specimens had non-machined (non-trimmed) adhesive zone with a bonded area measuring approximately 0.6 mm2 and 10 mm length (Fig. 1a and b). The sps obtained from each ceramic block were randomly divided into two testing conditions. In dry conditions (dry), the specimens were submitted to microtensile test immediately after sectioning. In aged conditions (TC), specimens were thermocycled (12,000 cycles; 555 C, dwelling Paulo, Brazil) time: 30 s, transfer time: 2 s) (Nova Etica, Sao and stored in distilled water at 37 C for 150 d and then submitted to testing. Thus, eight groups were planned, considering the surface treatment (four levels) and storage condition (two levels) factors yielding to 48 sp in each (n = 48) (Table 1).

Table 1 Experimental groups, considering the etching agents, silanization and storage conditions (HF: hydrouoric acid gel, APF: acidulated phosphate uoride) Type of etching agent Silanization
With HF Without

Dry TC Dry TC Dry TC Dry TC

Gr1 Gr2 Gr3 Gr4 Gr5 Gr6 Gr7 Gr8

Number planned sp
48 48 48 48 48 48 48 48

With APF Without


d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 13231331


Microtensile bond strength test

Each specimen was xated with cyanoacrylate gel (Super Bon Paulo, Brazil), keeping the adhesive der Gel, Loctite Ltd, Sao zone free, to the rods of a device adapted for this test. The specimens were positioned parallel to the long axis of the device in order to reduce the bending stresses. The device was xated in the universal testing machine (EMIC DL-1000, EMIC, Jose dos Pinhais, Brazil), as parallel as possible in relation Sao to application of the tensile load, and testing was performed at a cross speed of 1 mm min1 . The bond strength was calculated according to the formula R = F/A, where R is the strength (MPa), F is the load required for rupture of the specimen (N) and A is the interface area of the specimen (mm2 ), measured with a digital caliper before the test.

Fig. 2 Means and standard deviations of the microtensile bond strength data for dry and thermocycled conditions with and without silanization. For abbreviations see Table 1.


Failure type analysis

Three-way ANOVA revealed signicant inuence of the etching protocol (p = 0.0014), silanization (p < 0.0001) and storage conditions (p = 0.0013). Interaction between factors was also signicant (p = 0.010). Table 3 presents the post hoc Tukey test results for multiple comparisons ( = 0.05) with means and standard deviations obtained from each experimental group. The highest bond strengths were achieved in both dry and thermocycled conditions when the ceramics were etched with HF acid gel and silanized (17.4 5.8 and 17.4 4.8 MPa, respectively). Non-silanized groups presented lower results for both HF acid gel (4.5 1.2 MPa) and APF treated groups (2.6 0.8 MPa) than with silanization (17.4 4.8 and 14.6 4.5 MPa, respectively) after thermocycling and water storage. After 12,000 thermal cycles, no signicant decrease was observed in both HF and AFP treated groups (p < 0.05) compared to the groups tested dry. On the other hand, thermocycling and long-term water storage decreased the results signicantly in non-silanized groups (p < 0.0001) (Fig. 3a and b).

All sps submitted to the microtensile test were analyzed under light microscope (MP 320, Carl Zeiss, Jena, Germany) at 1005000 magnication and some sps were selected for analysis under scanning electron microscope (SEM) at 1000 and 2000 magnication for observation of the types of failures, between ceramic and cement (ADHES); cohesive failure in the cement (COHES-cem); cohesive failure in the ceramic (COHES-cer); cohesive failure in the cement and ceramic (MIX).


Statistical analysis

Statistical analysis was performed using the software Statistix 8.0 for Windows (Analytical Software Inc., Tallahassee, FL, USA). Bond strength data (MPa) were submitted to three-way analysis of variance and Tukeys test ( = 0.05). The chi-square test was used in order to analyze the percentage of sps failed before testing in all groups ( = 0.05). P values less than 0.05 are considered to be statistically signicant in all tests. Multiple comparisons were made by repeated measures tests at a signicance level of 0.05.


Statistical analysis of pre-test failures


Microtensile bond strength results
Table 4 presents the number and percentages (%) of sps lost either during thermocycling or specimen cutting prior to microtensile bond strength test in eight experimental groups. The percentage of sps failed before testing in all groups was statistically analyzed by the chi-square test ( = 0.05).

Means and standard deviations are demonstrated in Table 2 and presented in Fig. 2.

Table 2 Results of three-way ANOVA Source

Silane Storage Surface treatment Silane storage Silane surface treatment Storage surface treatment Silane storage surface treatment Error Total

1 1 1 1 1 1 1 246 253

3933.09 204.07 199.22 217.04 12.98 0.07 0.64 4723.02

3933.09 204.07 199.22 217.04 12.98 0.07 0.64 19.20

204.86 10.63 10.38 11.30 0.68 0.00 0.03

<0.0001 0.0013 0.0014 0.0009 0.4118 0.9532 0.8552

d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 13231331


Table 3 Means and standard deviations of the bond strength data (MPa) of the studied groups Type of etching agent Silane
With HF Without

Dry TC Dry TC Dry TC Dry TC

Bond strength (MPa)*

Gr1: 17.4 5.8 a Gr2: 17.4 4.8 a Gr3: 8.9 3.1 c Gr4: 4.5 1.2 d Gr5: 14.5 4.2 b Gr6: 14.6 4.5 b Gr7: 7.5 2.2 cd Gr8: 2.6 0.8 d

With APF Without

The same letters indicate no signicant differences (Tukeys test, = 0.05).

Table 4 Number (No) of specimens (sp) produced, and percentage (%) of pre-test failures (PTF) during cutting and thermocycling (TC) and total number of sps prior to microtensile bond strength test (MTBS) Groups
Gr1 Gr2 Gr3 Gr4 Gr5 Gr6 Gr7 Gr8

No. of sps
48 48 48 48 48 48 48 48

No. and % of PTF during cutting

0 (0) 0 (0) 25 (52) 27 (56) 0 (0) 0 (0) 32 (67) 30 (62 .5)

No. and % of spontaneous PTF during TC

0 (0) 0 (0) 0 (0) 4 (0.1) 0 (0) 0 (0) 0 (0) 12 (25)

Total no. and % of PTF prior to MTBS

0 (0) 0 (0) 25 (52) 31 (56 .1) 0 (0) 0 (0) 32 (67) 42 (87 .5)

No. and % of tested sp in MTBS

48 (100) 48 (100) 23 (48) 17 (43 .9) 48 (100) 48 (100) 16 (33) 6 (12 .5)

Table 5 Number of tested specimens (sp) per group and incidence of failure types in percentage (%) after the microtensile test Groups Total no. of tested sp and % ADHES
Gr1 Gr2 Gr3 Gr4 Gr5 Gr6 Gr7 Gr8

Type of failurea MIX

35 (73) 33 (69) 0 (0) 0 (0) 37 (77) 36 (75) 0 (0) 0 (0)

0 (0) 0 (0) 0 (0) 0 (0) 0 (0) 0 (0) 0 (0) 0 (0)

7 (14.5) 6 (12.5) 0 (0) 0 (0) 4 (8.3) 2 (4.2) 0 (0) 0 (0)

48 (100) 48 (100) 23 (100) 17 (100) 48 (100) 48 (100) 16 (100) 6 (100)

6 (12 .5) 9 (18 .5) 23 (100) 17 (100) 7 (14 .7) 10 (20 .8) 16 (100) 6 (100)

Failure between ceramic and cement (ADHES); cohesive failure of cement and ceramic (MIX); cohesive failure of the cement (COHES-cem); cohesive failure of ceramic (COHES-cer).

Signicantly more pre-test failures were experienced during cutting procedure in both non-silanized HF acid and APF treated groups (5267%) when compared with silanized groups (0%) (p = 0.214 for HF and p < 0.001 for APF). During thermocycling, again non-silanized groups presented more pre-test failures (0.125%) compared to silanized groups (0%) (p < 0.001). Both HF and APF treated groups did not present pre-test failures during cutting or thermocycling when they were silanized after etching.


Topographic analysis and failure types

micromechanical retention compared to APF, corroborating the higher bond strength results obtained from HF gel treated groups. Light microscopy analysis demonstrated that groups that received no silanization showed exclusively ADHES type of failures (100%) for both etch materials. After thermocycling, in silanized groups, mainly MIX type of failures were observed in HF and APF treated groups (6975%, respectively). Regardless of the etching agent type employed and storage conditions, ADHES type of failures ranged between 12.5% and 20.8% and COHES-cer failures between 4.2% and 14.5% (Table 5).

Surface topography of the feldspathic ceramic treated with 10% HF acid gel for 1 min followed by ultrasonic cleaning presented more intensive degradation of the ceramic than with 1.23% APF applied for 5 min (APF) (Fig. 4a and b). This indicates that HF acid provided a more favorable topographic pattern for



The results of this study showed that the microtensile bond strength results were increased by silanization of the ceramic


d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 13231331

Fig. 3 (a) Means of microtensile bond strength data taking the three factors studied into account. (b) Means of microtensile bond strength data regardless of the acid agent considering the storage conditions and silanization.

surface after APF or HF acid etching, with the latter providing higher bond strengths. Thermocycling for 12,000 times and water storage for 150 d reduced the bond strengths dramatically when the ceramics were not silanized. Therefore two hypotheses set for this study were conrmed (1 and 2) and the third one was partially conrmed (3). Acid-sensitive ceramics (silica-based) present surface degradation when exposed to some acids. HF acid and APF attack the glassy phase of these ceramics (SiO2 ), expose silica oxides yielding topographic changes for increased micromechanical retention and for chemical bonding with

the silane coupling agent and resin cement. Some studies have demonstrated that HF acid provides high bond strength to resin materials [58,11,19]. Regardless of the silanization and storage condition factors, HF acid gel application on the feldspathic ceramic tested provided statistically higher bond strength values than those of APF as reported in previous studies [7,11]. The HF acid gel is a more aggressive etching agent to the ceramic surface than APF. Thus, application of HF acid gel generates more adequate micromorphological surface topography for micromechanical retention of the resin cement that is reected by the higher bond strength values obtained from HF acid treated groups. While a micro-rough surface is desirable, aggressive etching conditions may result in strong and deep degradation of the ceramic and thereby weaken the ceramic surface material. In a fractography analysis of sps submitted to tensile bond testing [24], it was observed that fracture was initiated by formation of a crack in the crystalline phase that was probably weakened by the etching process. This factor may danger the clinical performance of feldspathic ceramics treated with HF acid gel. In clinical practice the optimum bond strength of resin composites to ceramic is not known. In a previous study [25], no signicant difference was found between the tensile bond strengths of specimens etched with 9.6% HF acid or 4% APF. However, the groups etched with 4% APF, showed a wider statistical spread than HF acid treated group. This suggested that HF acid etching might well produce more reliable and consistent results but this was not conrmed, as the sample size was too small. In this study, although the results from HF acid treated groups were signicantly higher than those of APF treated groups, considering the fact that APF is a less hazardous compound, it could still be considered to perform well when ceramics are silamized. Further studies should be conducted to establish an etching protocol to favor the micromechanical retention without weakening the etched ceramic material [26]. Besides providing a more favorable micromorphology for micromechanical retention compared to APF, HF acid significantly reduces the surface contact angle compared to APF, increasing the surface free energy and wettability of the cement [4,27]. However, despite the higher bond strength provided by HF acid gel compared to APF, regardless of the other two factors tested in this study, the difference between the two acid treated groups and silanized groups was small, yet sig-

Fig. 4 Representative SEM micrographs of the feldspathic ceramic surface treated with (a) 10% HF for 1 min and (b) 1.23% APF for 5 min (original magnication 2000). Note the more aggressive etched pattern with deeper microporosities (a) compared to APF treated surface (b).

d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 13231331


nicant. When both etching procedures were combined with silanization, the bond strength results were stable after longterm water storage period and thermal cycling. This nding clearly reveals the importance of chemical adhesion obtained from silane coupling agent. Silanes with general chemical formula X-(CH2 ) Si-(OR) are able to provide chemical bonding with organic surfaces such as resin materials and polymers and inorganic surfaces, such as silica-based ceramics [28]. MPS silanes (3-methacryloxypropyltrimethoxysilane in ethanol) present molecules that react with water, forming silanol groups (SiOH) from the methacryloxy groups (SiOCH3 ). Silanol groups react to form a siloxane network (SiOSiO) with the silica oxide present in material. Silica oxide is present in feldspathic ceramics or oxides articially deposited on acid-resistant ceramics serve as a good basis for the silane coupling agents to react [6,9,29]. The monomeric ends of silane then reacts with methacrylate groups of the resin material. Thus, the bonding process between ceramic surface and resin cement occurs through the chemical process between silica oxides and silane bonding agent. In the present study, application of silane was fundamental in order to achieve durable adhesion of the resin cement, after both types of etching agents. These results conrm previous studies [5,8,11,19]. On the other hand, pre-test failures were more frequently experienced during cutting procedure and thermocycling in both non-silanized HF acid and APF treated groups (5267%) when compared with silanized groups (0%). This reinforces the high and stable bond strength achieved with both surface treatments. The high number of pre-test failures and the exclusive adhesive failure between the resin cement and the ceramic reects the low and instable adhesion achieved after etching with HF and APF without silanization. Since no pre-test failures were experienced in silane treated groups, complimentary to the mictotensile bond strength results, this nding conrms the importance of chemical bonding generated by silane application. Similarly, while some studies showed enhanced bond strength with the application of silane to the etched ceramic surface, others reported signicant variations in bond strengths between brands of silanes [10]. Thus, besides the bond strength values, qualitative analysis of the fracture surface should also be presented in in vitro studies. Fractographic analysis of the fractured surface of sp would reduce the risk of misinterpretation of bond strength results. It should also be noted that evaluation of bond strength of ceramics utilizing microtensile test was only applicable when the bond strength values were higher than approximately 5 MPa that allowed for sectioning the specimens. Interestingly however, both HF and APF treated, silanized groups did not present pre-test failures during cutting the specimens or thermocycling. Chemical bonding procedure is particularly more important for lowfused monophase feldspathic ceramics (e.g. Duceram LFC, Ducera) [11,24]. These ceramics are highly glassy materials and their clinical application in the form of extensive onlay or resin-bonded FPDs, where mechanical retention is less, is largely dependent on chemical adhesion of resin cement to such ceramics [12]. Water storage and thermocycling were also described detrimental for the silane-ceramic bond in order to simulate the

aging conditions intraorally [22]. However, silanized interfaces appear to be unstable in humid conditions. One interesting nding in this study was that although the number of cycles was higher than the previous studies [24,30,31], after thermocyling and long-term water storage, no signicant decrease in bond strength was observed. It could be attributed to the variations between the testing methodologies. The present study delivered data from microtensile bond test. Laboratory tests for the assessment of bond strength, such as tensile and shear tests are based on load application on specimens until there is catastrophic failure. Thus, in order to measure the actual bond strength between the adhesive and the substrate, regardless of the type of test, the bonding interface is the area most submitted to stress. The bonded surface area is usually the place from which catastrophic failure initiates, crossing the extension of the bonding area [24]. According to some studies, evaluating the stress distribution at the interface, shear test is considered to be unable to apply stress precisely at the bonding interface, which generates non-uniform stress at the interface, thus applying more stress on the substrate and introducing errors in bond strength between adhesive and adherent [25,32,33]. This is explained by the fact that stresses are concentrated at restricted areas outside the interface, yielding higher potential of cohesive failure in the base material from this critical point of stress concentration. Bar specimens with adhesive surface area of 0.6 mm2 were used in this study. Previous studies have revealed that this shape of sp generates uniform stress distribution at the bonding interface, especially when the bonded area is smaller than 1 mm2 [34,35]. Therefore no signicant decrease after thermocycling could be due to the small adhesive interface area and thereby less hydrolytic degredation of the silane coupling agent and the resin cement or lower lm thickness of the cement and eventually higher polymerization. In this aspect, geometrical conguration of specimens (Cfactor = number of bonded surfaces/number of free surfaces) is an important factor. It has been demonstrated that the C-factor signicantly interferes with the shrinkage stress of composites [36] that is increased when the C-factor is higher. In this study, the C-factor may be considered as 0.2 (one bonded surface, ve free surfaces) that enhances composite ow and reduces shrinkage stress thereby the negative effect on the bond strength. On the other hand, in clinical applications such as inlays and onlays, the cement is conned within the cavity thus increasing the C-factor and shrinkage stress that may affect the bond strength [37,38]. Therefore in that respect, not only the bond strength values but also failure types and pre-test failures should be taken into consideration during interpreting the bond strength performance of adhesives to glass ceramics. The concentration and recommended etching times vary among the various etchants and the ceramic types. The highest shear bond strength was achieved when ceramic surface was etched for 120 s with 10% HF acid gel [39,40]. Wolf et al. [41] on the other hand, reported the highest composite-ceramic bond with 150 and 300 s etching when a silane coupling agent was used. Additional etching time resulted in a reduction of the bond strength. The content of leucite crystals in conventional feldspathic porcelain varies from 20 to 30%. It also varies between enamel and dentin porcelain. The size of the


d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 13231331

leucite crystals in feldspathic porcelain ranges from approximately 520 m and etching duration affects the results [42]. In all these studies however, different brands of ceramics and storage regimens were used. Since HF reacts with silica in feldspathic porcelain to form hexa-uorosilicates, the glassy matrix and crystalline phase propotion in a ceramic composite play a major role for adequate etching protocol. Furthermore, since long term aging conditions were often not employed in these studies, they could neither be compared with each other nor with this present study. Future studies should concentrate on the individual etching time for the specic glassmatrix ceramic and preferably in simulated aged conditions. Although no clinical incidence report exists in the dental literature regarding to the hazardous consequences of HF acid gel, caution should be exercised during handling this material. However, considering the microscopical changes observed in SEM microphotographs after APF application, this acid agent should also be cautiously handled when ouridation is performed in patients with ceramic restorations.



1. Silanization of the feldspathic ceramic surface after APF or HF acid etching increased the microtensile bond strength results signicantly, with the latter providing higher results. 2. Thermocycling for 12,000 times followed by 150 d water storage reduced the bond strength of resin cement to feldspathic ceramic tested dramatically when the ceramics were not silanized but storage conditions did not decrease the results in silanized groups. 3. Both HF and APF treated, silanized groups did not present pre-test failures during cutting the specimens or thermocycling.

We would like to acknowledge Prof. Dr. Durval Rodrigues Jr. Paulo University, Lorena Chemical Engineering School, (Sao Lorena, Brazil) for his assistance with SEM evaluations.


[1] Hayashi M, Tsuchitani Y, Kawamura Y, Miura M, Takeshige F, Ebisu S. Eight-year clinical evaluation of red ceramic inlays. Oper Dent 2000;25:47381. [2] Fradeani M, Redemagni M. An 11-year clinical evaluation of leucite-reinforced glass-ceramic crowns: a retrospective study. Quintessence Int 2002;33:50310. [3] Nakabayashi N, Pashley DH. Hybridization of dental hard Paulo: Quintessence; 2000. p. 127. tissues. Sao [4] Phoenix S, Shen C. Characterization of treated porcelain surfaces via dynamic contact angle analysis. Int J Prosthodont 1995;8:18794. [5] Aida M, Hayakawa T, Mizukawa K. Adhesion of composite to porcelain with various surface conditions. J Prosthet Dent 1995;73:46470. [6] Ozcan M, Vallittu PK. Effect of surface conditioning methods on the bond strength of luting cement to ceramics. Dent Mater 2003;19:72531.

[7] Della Bona A, Shen C, Anusavice KJ. Work of adhesion of resin on treated lithia disilicate-based ceramic. Dent Mater 2004;20:33844. [8] Lu R, Harcourt JK, Tyas MJ, Alexander B. An investigation of the composite resin/porcelain interface. Aust Dent J 1992;37:129. [9] Soderholm KJM, Shang SW. Molecular orientation of silane at the surface of colloidal silica. J Dent Res 1993;72:10504. [10] Matinlinna JP, Lassila LVJ, Ozcan M, Yli-Urpo A, Vallittu PK. An introduction to silanes and their clinical applications in dentistry. Int J Prosthodont 2004;17:15564. [11] Ozcan M. Evaluation of alternative intraoral repair techniques for fractured ceramic-fused-to-metal restorations. J Oral Rehabil 2003;30:194203. [12] Della Bona A, Anusavice KJ, Shen C. Microtensile strength of composite bonded to hot-pressed ceramics. J Adhes Dent 2000;2:30513. [13] Ozcan M, Akkaya A. New approach to bonding all-ceramic adhesive xed partial dentures: a clinical report. J Prosthet Dent 2002;88:2524. [14] Sposetti V, Shen C, Levin A. The effect of topical uoride application on porcelain restorations. J Prosthet Dent 1986;55:67782. [15] Wunderich RC, Yaman P. In vitro effect of topical uoride on dental porcelain. J Prosthet Dent 1986;55:3858. [16] Abbasi J, Bertolotti RL, Lacy AM, Wtanabe LG. Bond strengths of porcelain repair monomers. J Dent Res 1988;67:223. [17] van Noort, Noroozi S, Howard IJ, Cardew G. A critique of bond strength measurements. J Dent 1989;17:617. [18] Cardoso PE, Sadek FT, Goracci C, Ferrari M. Adhesion testing with the microtensile method: effects of dental substrate and adhesive system on bond strength measurements. J Adhes Dent 2002;4:2917. [19] El Zohairy AA, De Gee AJ, Mohsen MM, Feilzer AJ. Microtensile bond strength testing of luting cements to prefabricated CAD/CAM ceramic and composite blocks. Dent Mater 2003;19:57583. [20] Roulet JF. Degradation of dental polymers. Basel, Germany: Karger; 1987. p. 60. [21] Reuter JE, Brose MO. Failures in full crown retained dental bridges. Br Dent J 1984;157:613. . A brief history and current [22] Ozcan M, Pfeiffer P, Nergiz I status of metal/ceramic surface conditioning concepts for resin bonding in dentistry. Quintessence Int 1998;29:71324. [23] Foxton RM, Pereira PNR, Nakajima M, Tagami J, Miura H. Durability of the dual-cure resin cement/ceramic bond with different curing strategies. J Adhes Dent 2002;4:4959. [24] Andreatta Filho OD, Galhano G, Bottino MA, Camargo FP, Valandro LF, Nishioka RS. Evaluation of the bond strength between an aluminous ceramic and a resin cement: effect of thermo-cycling. Braz Dent Sci 2003;6:329. [25] Della Bona A, Anusavice KJ, Hood JAA. Effect of ceramic surface treatment on tensile bond strength to a resin cement. Int J Prosthodont 2002;15:24853. [26] Della Bona A, Van Noort R. Shear vs. tensile bond strength of resin composite bonded to ceramic. J Dent Res 1995;74:15916. [27] Addison O, Marquis PM, Fleming GJ. The impact of hydrouoric acid surface treatments on the performance of a procelain laminate restorative material. Dent Mater 2006;16:[Epub ahead of print]. [28] Jardel V, Degrange M, Picard B, Derrien G. Correlation of topography to bond strength of etched ceramic. Int J Prosthodont 1999;12:5964. [29] Diaz-Arnold AM, Aquilino SA. An evaluation of the bond strengths of four organosilane materials in response to thermal stress. J Prosthet Dent 1989;62:25760. [30] Plueddemann EP. Adhesion through silane coupling agents. J Adhesion 1970;2:184201.

d e n t a l m a t e r i a l s 2 3 ( 2 0 0 7 ) 13231331


[31] Cochran M, Carlson T, Moore B, Richmond N, Brackett W. Tensile bond strengths of ve porcelain repair systems. Oper Dent 1988;13:1127. [32] Pratt RC, Burgess JO, Schwartz RS, Smith JH. Evaluation of bond strength of six porcelain repair systems. J Prosthet Dent 1989;62:113. [33] Versluis A, Tantbirojn D, Douglas WH. Why do shear bond tests pull out dentin? J Dent Res 1997;76:1298 307. [34] Sudsangiam S, Van Noort R. Do dentin bond strength tests serve a useful purpose? J Adhes Dent 1999;1:5767. [35] Phrukkanon S, Burrow MF, Tyas MJ. The inuence of cross-sectional shape and surface area on the microtensile bond test. Dent Mater 1998;14:21221. [36] Shono Y, Terashita M, Shimada J, Kozono Y, Carvalho RM, Russel CM, et al. Durability of resin-dentin bond. J Adhes Dent 1999;1:2118.

[37] Davidson CL, de Gee AJ, Feilzer AJ. The competition between the composite-dentin bond strength and the polymerization contraction stress. J Dent Res 1984;63:13969. [38] Carvalho RM, Pereira JC, Yoshiyama M, Pashley DH. A review of polymerization contraction: the inuence of stress development versus stress relief. Oper Dent 1997;21:1724. [39] Stangel I, Nathanson D, Hsu CS. Shear strength of the composite bond to etched porcelain. J Dent Res 1987;66:14605. [40] Chen JH, Matsumura H, Atsuta M. Effect of different etching periods on the bond strength of a composite resin to a machinable porcelain. J Dent 1998;26:538. [41] Wolf DM, Powers JM, OKeefe KL. Bond strength of composite to etched and sandblasted porcelain. Am J Dent 1993;6:1558. [42] Barghi N, Fischer DE, Vatani L. Effects of porcelain leucite content, types of etchants, and etching time on porcelain-composite bond. Esthet Restor Dent 2006;18:4753.