Você está na página 1de 12

d e n t a l m a t e r i a l s 2 6 ( 2 0 1 0 ) e38e49

available at www.sciencedirect.com

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

Adhesion to tooth structure: A critical review of macro test methods


Roberto R. Braga , Josete B.C. Meira, Leticia C.C. Boaro, Tathy A. Xavier
University of So Paulo School of Dentistry, Dept. of Dental Materials, Av. Prof. Lineu Prestes, 2227, So Paulo, SP 05508-000, Brazil

a r t i c l e
Article history:

i n f o

a b s t r a c t
Objectives. Bond strength between adhesive systems and the tooth structure is inuenced by a large number of variables, which makes the comparison among studies virtually impossible. Also, failure often times propagates into the dental substrate or the composite, deeming the results questionable at best. In spite of the increased popularity gained by micro-tensile and micro-shear tests, in vitro evaluations using specimens with relatively large bonding

Received 19 November 2009 Accepted 19 November 2009

Keywords: Bond strength Shear Tensile Dental adhesives Finite element analysis

areas remain frequent. This review focuses on aspects related to specimen geometry and test mechanics of macro shear and tensile bond strength tests. Methods. Besides information drawn from the literature, the effect of some parameters on stress distribution at the bonded interface was assessed using nite element analysis (FEA). Results. Bond strength tends to increase with smaller bonding areas and with the use of high elastic modulus composites. Stress concentration at the bonded interface is much more severe in shear compared to tension. Among shear methods, the use of the chisel shows the highest stress concentration. Within the limits suggested by the ISO/TS 11405, crosshead speed does not seem to inuence bond strength values. Pooled data from currently available adhesives tested in either shear or tension showed 44% of adhesive failures, 31% mixed and 25% cohesive in the substrate (tooth or composite). A comparative bond strength study involving three adhesive systems revealed similarities between macro and micro counterparts regarding material ranking, whereas macro tests presented a higher incidence of cohesive failures. Signicance. Simplicity warrants macro bond strength tests an enduring popularity, in spite of their evident limitations. From a mechanical standpoint, knowing the stress distribution at the bonded interface and how it is affected by the materials and loading method used is key to explain the results. 2009 Published by Elsevier Ltd on behalf of Academy of Dental Materials. All rights reserved.

Contents
1. 2. 3. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A survey of recent bond strength studies . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Variables of inuence related to specimen design . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3.1. Bonding area . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3.2. Elastic modulus of the resin composite . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . e39 e40 e40 e40 e41

Corresponding author. Tel.: +55 11 30917840. E-mail address: rrbraga@usp.br (R.R. Braga). 0109-5641/$ see front matter 2009 Published by Elsevier Ltd on behalf of Academy of Dental Materials. All rights reserved. doi:10.1016/j.dental.2009.11.150

d e n t a l m a t e r i a l s 2 6 ( 2 0 1 0 ) e38e49

e39

4.

5. 6. 7.

Variables of inuence related to test mechanics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4.1. Type of loading . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4.2. Crosshead speed . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Incidence of cohesive failures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A comparison between macro and micro bond strength tests . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Acknowledgements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

e41 e41 e43 e43 e44 e45 e45 e45

1.

Introduction

Over the years, clinicians have relied upon laboratory evaluations to choose which adhesive systems to use in their daily practice. Though the validity of bond strength tests to predict clinical performance of dental adhesives is questionable [1,2], recent evidence shows that clinical results can, to some extent, be estimated based upon laboratory results [35]. Moreover, mechanical testing of bonded interfaces has provided some valuable information in terms of identifying substrate variables [6,7] and helping dene guidelines for application procedures [8]. Until the mid-nineties, shear and tensile bond strength tests were performed exclusively in specimens with relatively large bonded areas, usually 36 mm in diameter (approximately 728 mm2 ). However, the validity of expressing bond strength in terms of nominal (i.e., average) stress has been questioned due to the heterogeneity of the stress distribution at the bonded interface [911]. Moreover, cohesive failure of both the composite and the dental substrate is a common occurrence, precluding an accurate assessment of the interfacial bond strength [12]. The need for new methods to overcome these limitations led to the use of specimens with small bonding areas (i.e., below 2 mm2 ), in the so-called micro-tensile and micro-shear tests [1315]. In spite of the increased popularity of the micro bond strength tests and the criticism endured by the conventional tensile and shear methods, the number of articles using macro tests published in recent years remains high, meaning that a lot of the available data on dental adhesion still comes from mechanical tests performed

in specimens with large bonded areas (Fig. 1). The preference for conventional shear and tensile tests is justied because they are easy to perform, requiring minimal equipment and specimen preparation. However, though a lot of information can be found on specimen geometry and other testing variables for micro bond strength tests [1618], the same is not true for the macro tensile and shear tests. Reviews published in the past evidenced a concern with the bonding substrate and specimen storage conditions, only minimally discussing the variables of the mechanical test itself [1,12,1921]. The International Organization for Standardization (ISO) technical specication ISO/TS 11405 [22], published in 1994 and last revised in 2003, reects this tendency, describing with greater detail the characteristics and preparation of the tooth substrate for the bonding procedure, and leaving aspects such as bonding area, testing assemblies or loading conditions more vague. As a result, a wide variety of experimental protocols is found among researchers, with evident effect on the outcomes [23,24]. A systematic review with meta-analysis identied composite type, bonding area, testing mode (shear, tensile or micro-tensile) and crosshead speed as factors that signicantly inuence bond strength, along with several others related to the substrate, specimen storage conditions and thermocycling [25]. The type of device used for load application was also shown to affect the results [2629]. The purpose of this article was to review aspects related to specimen geometry and test mechanics that may inuence macro shear and tensile bond strength results. Finite element analysis (FEA) was used to assess the effect of selected variables on the stress distribution at the bonded interface.

Fig. 1 Number of articles/year published on dentin and enamel bond strength between 1982 and 2008, according to www.scopus.com. Left: articles grouped by testing method, right: articles grouped by specimen dimensions, i.e., macro or micro (publications on bond strength of orthodontic brackets to enamel were not included).

e40

d e n t a l m a t e r i a l s 2 6 ( 2 0 1 0 ) e38e49

Fig. 2 Three-dimensional models used for nite element analysis (left: shear; right: tension). Points A and B dene the diameter of the bonding area.

Specimen failure mode was discussed based on data retrieved from the recent literature. Also, a brief comparison between macro and micro bond strength tests was performed using experimental data obtained with three adhesive systems.

3. Variables of inuence related to specimen design


3.1. Bonding area

2.

A survey of recent bond strength studies

In order to verify how researchers are currently performing tensile and shear bond strength tests, 100 studies published between 2007 and 2009 (shear: 74, tensile: 26) were surveyed [30128]. Unsurprisingly, no consensus was found in any of the parameters observed. Most studies used bonding areas between 3 and 4 mm in diameter (57%), while 4% did not include this information. These numbers do not differ from those reported 12 years ago, where the mean diameter among 50 studies was 3.97 mm and 6% of the studies omitted this information [23]. Pre-formed rods were used in 31% of the tensile tests and none of the shear tests. Composite height varied between 2 and 5 mm. A description of the testing method was included in 66% of the studies. For shear loading, the knife-edge rod was used in half of the studies describing the experimental assembly utilized. All studies reported the crosshead speed, with 0.5 and 1.0 mm/min being the most frequent values (46 and 41%, respectively), also in agreement with a recent survey [24]. Specimen failure mode analysis was present in 64% of the studies, performed either under low magnication (1050) using stereomicroscopes (47%) or with the use of scanning electronic microscopy (17%). Regarding sample size, 10 specimens per group were used in 59% of the studies, while 15% used between ve and eight specimens and 26% used between 11 and 25 specimens per group. The highest coefcient of variation found in each study averaged 36 14% (minimum: 10%, maximum: 75%). This average is within the range mentioned in the ISO/TS 11405 as expected for these methods (2050%).

The choice of bonding area used in macro tensile and shear tests is often made based on the substrate area available. The ISO/TR 11405 [22] does not identify a specic value, but it does mention a clear delimitation of the bonding area as an important requirement and shows a diagram of a split mould with a 3-mm diameter hole. The relationship between bonding area and strength has received more attention with the development of micro-tensile and micro-shear tests. For specimens with rectangular bonding areas between 0.25 and 11.65 mm2 , tensile bond strength to dentin was shown to decrease as bonding area increased, following a logarithmic function [13]. A similar trend was observed in enamel, with areas between 0.5 and 3.0 mm2 [7]. Another study showed that specimens with circular cross-section between 1.1 and 3.1 mm2 (1.2 and 2.0 mm in diameter, respectively) presented an inverse linear relationship between bonding area and strength when tested either in tension or shear [14]. Such relationship between bonding area and strength is explained by fracture mechanics, initially derived from a series of experiments and mathematical deductions performed by Grifth [129], from which he concluded that the strength of a solid elastic body is governed by the presence of microscopic aws. A few decades later, Irwin [130] dened the parameters involved in crack propagation. Briey, failure of the bonded interface occurs when a crack propagates from a critical size aw found in an area subjected to high tensile stresses. The larger the bonding area, the higher is the probability of a aw of critical size being present and, consequently, the lower is the specimens bond strength. Very few studies evaluated the inuence of bonding area on macro strength tests. The shear bond strength of a two-

d e n t a l m a t e r i a l s 2 6 ( 2 0 1 0 ) e38e49

e41

step etch-and-rinse system (Single Bond, 3M ESPE) did not vary signicantly in specimens with diameters between 2 mm (3.1 mm2 , 20 MPa) and 5 mm (19.6 mm2 , 15 MPa), but it was statistically higher for specimens with 1 mm diameter (0.8 mm2 , 47 MPa) and lower for those with 6 mm diameter (28.3 mm2 , 9 MPa) [131]. Another study testing two three-step systems under tensile loading, Scotchbond Multi-Purpose (3M ESPE) and Optibond (Kerr), showed statistically higher bond strength for 2-mm diameter specimens (10.3 MPa and 15.7 MPa, respectively) compared to 4-mm diameter (7.0 MPa and 11.1 MPa, respectively) [132]. Though macro shear and tension tests show a trend for increased bond strength values with the use of small bonding areas similar to what was observed in micro-tensile specimens, the evidence in the literature is not sufcient to support a denite statement in terms of the inuence of bonding areas on strength values. Therefore, the comparison among studies using different bonding areas must consider the specimen size when interpreting the results.

Table 1 Maximum principal stress ( max ) and maximum shear stress ( max ) at the dentin/composite interface, in MPa, observed in shear and tensile loading as a function of composite elastic modulus (E, in GPa). Composite E (GPa) Shear loading
max max

Tensile loading
max max

6 9 12

159 131 114

123 114 105

18.5 17.8 17.3

7.1 6.6 6.3

3.2.

Elastic modulus of the resin composite

half of the model was represented (Fig. 2). MSC.PATRAN (MSC Software Corp., Santa Ana, CA, USA) was used for pre- and post-processing, and MSC.Marc was used as processor. In agreement with experimental data, stress concentration at the bonded interface decreased as composite modulus increased from 6 to 12 GPa, which is explained by the reduction in modulus mismatch between both materials. This effect, however, is much less pronounced for tensile loading (Table 1), as previously reported [9]. Also, the effect of composite elastic modulus on bond strength seems to be dependent upon the adhesive system used [82].

The use of stiffer composites may signicantly increase bond strength values. A recent study observed a weak but statistically signicant correlation between dentin shear bond strength and composite exural properties [116]. A similar trend was observed in an earlier study evaluating the tensile bond strength to dentin of an adhesive system associated with different composites [133]. The inuence of composite elastic modulus on stress distribution at the bonded interface was studied by nite element analysis (FEA) using three-dimensional models representing a 3-mm diameter, 2-mm high composite cylinder ( = 0.25) bonded to a dentin disk (E = 18 GPa, = 0.3) through a 50-m thick adhesive layer (E = 2 GPa, = 0.3). A load was applied to the composite either perpendicularly or parallel to the bonded interface in order to produce a nominal stress of 16 MPa. Due to the symmetry in geometry and loading conditions, only

4. Variables of inuence related to test mechanics


4.1. Type of loading

Nominal bond strength values carry an underlying assumption that stresses are uniformly distributed across the bonded interface. However, as displayed in Fig. 3, in the shear test stresses close to the loading area are much higher than the nominal shear value (16 MPa). Moreover, the choice of testing assembly has great inuence on stress distribution. The use of a knife-edge chisel causes severe stress concentration at the load application area, whereas the wire loop shows a better stress distribution at the edge of the bonding area [10]. Stress concentration with the use of the chisel may explain the small

Fig. 3 Stress distributions (maximum principal stress, max , and maximum shear stress, max ) at the dentin side of the dentin/composite interface according to the type of shear loading. Left: 0.2-mm knife-edge chisel; center: 2-mm at rod; right: wire loop. Load was applied at 0.2 mm from the bonded interface. Line AB indicates the diameter of the bonding area.

e42

d e n t a l m a t e r i a l s 2 6 ( 2 0 1 0 ) e38e49

Fig. 4 max / max across half of the diameter of the bonded interface according to the type of shear loading, applied 0.2 mm distant from the dentin/adhesive interface (left) or according to the point of load application using a 0.2-mm thick knife-edge chisel (right).

areas of composite cohesive failure close to the loading point observed experimentally [134]. Also, it may explain the statistically lower bond strengths when the chisel is compared against testing assemblies using larger contact areas between the composite and the loading device, such as the Single-Plane Shear Test Assembly (SPSTA) [131], the Ultradent notched rod and the wire loop [2729]. Another important aspect of shear tests is that closer to the interface tensile stresses are actually higher than shear, suggesting that the former is responsible for failure initiation, as previously stated [9,135,136]. For the knife-edge chisel and the wire loop methods, shear stresses start to prevail over tension at 0.3 mm from the load application area, while for the at rod tensile stresses predominate up to 1.2 mm (Fig. 4, left). Therefore, the term shear bond strength would more appropriately refer to the loading mode, rather than the nature of the stress responsible for bonding failure. The distance between the point of load application and the bonded interface in shear tests also affects stress distri-

bution. When load is applied up to 1 mm from the interface, tensile and shear stresses increase towards the bonded interface, explained by the Saint Venant principle (i.e., a generalized stress concentration in areas close to the load application point) [136]. This trend for higher stress concentration with smaller distances is supported by experimental evidence showing lower bond strength when the load was applied at the interface as opposed to a 0.5 mm distance from the dentin substrate [134]. The ratio between maximum shear and maximum principal stress decreases as load application moves away from the interface, indicative of an increase in bending moment (Fig. 4, right). When load is applied at distances beyond 1 mm from the interface (not shown), the increase in tensile stress as load application moves away from the bonded interface becomes even more evident [9,136]. In the tensile test, stresses are far more homogeneous across the interface than in shear and, therefore, maximum principal stress values are much closer to the nominal

Fig. 5 Stress distributions (maximum principal stress, max , and maximum shear stress, max ) at the dentin side of dentin/composite interfaces loaded in tension (left) or shear, using a 0.2 mm chisel applied at 0.2 mm from the interface (right). Line AB indicates the diameter of the bonding area.

d e n t a l m a t e r i a l s 2 6 ( 2 0 1 0 ) e38e49

e43

Fig. 6 Average failure mode distribution (in %) according to bonding substrate and testing mode obtained from 37 studies published between 2007 and 2009. Only data where adhesive was applied following manufacturers instructions were included. Numbers on top of each column indicate the number of publications used to calculate the averages.

Fig. 7 Bond strength averages (in MPa) of the adhesive systems according to the testing method used. Error bars correspond to 1 SD. In the same test, columns with the same letter are not statistically different (p > 0.05).

strength. However, the area subjected stress levels close to the maximum is much larger than in the shear test (Fig. 5). The height of the composite cylinder in the tensile test does not inuence stress distribution or magnitude if kept above 2 mm [9].

4.2.

Crosshead speed

Due to the viscoelastic nature of polymers and composites, it could be expected that bond strength tests would present some strain rate sensitivity. Experimental observations revealed that composite yield strength and elastic modulus increase at higher strain rates [137], possibly due to secondary molecular processes. At high strain rates, the polymer chains become stiffer and molecular mobility is reduced [138]. Determining the actual strain rate (unit: mm/mm s or s1 ) requires an extensometer and depending upon the specimen geometry it may not be feasible. Therefore, specimen loading is usually expressed in terms of crosshead speed, in mm/min. Studies evaluating the inuence of crosshead speed on macro shear and tensile bond strength are few and show contradictory results. Coincidentally, two of them used the same adhesive system and composite (Single Bond and Z100, 3M ESPE). However, bonding areas, specimen storage times and test assemblies were different. One study used the Single-Plane Shear Test Assembly (SPSTA) on specimens with 5-mm diameter bonding areas, nding no statistically significant differences among crosshead speeds between 0.5 and 10 mm/min [131]. The other study used a knife-edge steel rod to test specimens with 3-mm diameter bonding area and found statistically higher bond strengths for those loaded at 1.0 and 5.0 mm/min compared to 0.5 and 0.75 mm/min [139]. A similar scenario is observed with two studies that evaluated the effect of crosshead speed on tensile bond strength. Both used similar bonding areas (3.6 and 4.0 mm in diame-

ter) and while one did not report differences among crosshead speeds ranging from 0.5 to 5.0 mm/min [140], the other found statistically higher bond strengths for crosshead speeds of 5.0 and 10.0 mm/min compared to 0.1, 0.5 and 1.0 mm/min [141]. Such inconsistencies found for both shear and tensile tests may be explained by differences among testing assemblies and/or the brittle nature of dental adhesives and composites. The comparison of crosshead speeds among testing assemblies with different compliance levels is problematic and less meaningful than comparing load rates. Also, it has been veried that at small strains, the strain rate variation had a negligible effect on the measured stress values of amorphous polymers [142]. Nevertheless, it is important to emphasize that among the studies described, only one reported differences in bond strength within the crosshead speed range proposed in the ISO/TS 11405 (0.75 0.30 mm/min).

5.

Incidence of cohesive failures

As mentioned above, reporting bond strength in terms of nominal stress values is questionable due to the heterogeneous stress distribution and also due to the occurrence of cohesive failures both in the dental substrate and the resin composite. Dening categories for classication of failure modes of debonded specimens is a complicated task and, in some instances, the limit between mixed and cohesive failure becomes merely subjective. Fig. 6 shows the failure mode distribution observed in 37 studies recently published according to the bonding substrate and the loading mode [3134,37,3941,43,45,64,73,7680,84,8688,9599,101,102,108, 109,117,118,120,121,123125]. Overall, 44% of the specimens failed exclusively along the bonded interface, while 31% presented mixed failures and 25% presented predominantly (i.e., more than 75% of the bonding area) cohesive failure either at the composite or the dental substrate. Rather than an indication of strong bonding, cohesive failure is explained by the mechanics of the test and the brit-

e44

d e n t a l m a t e r i a l s 2 6 ( 2 0 1 0 ) e38e49

Fig. 8 Failure mode distributions (in %) observed under 1030 magnication for each adhesive system, according to the testing method. Top, left: Adper SE Plus; top, right: Adper Single Bond 2; bottom, left: Adper Scotchbond Multi-Purpose; bottom, right: pooled data.

tleness of the materials involved. In the shear test, tensile stress concentration in dentin near the crack tip causes the failure to propagate into the substrate. Versluis et al. [134] veried both experimentally and using a failure accumulation computer model a tendency for dentin failure to increase at lower crosshead speeds, thicker adhesive layers and moving the point of load application away from the bonded interface. Dentin pull-out was also associated with high bond strength values, although the correlation for individual specimens was weak. A recent study evaluating the tensile bond strength of ve resin cements to dentin reported a strong positive correlation between strength values and the area of cohesive failure in resin observed in mixed mode failures, evaluated using scanning electron microscopy [31]. Bonding area has also been associated with the incidence of cohesive failures. Specimens with rectangular cross-sectional areas larger than 7.17 mm2 built using a self-etching primer system (Clearl Liner Bond 2, Kuraray) and loaded in tension showed exclusively cohesive failures in dentin. Between 2.31 and 7.17 mm2 , both cohesive and adhesive failures were observed [13].

6. A comparison between macro and micro bond strength tests


In order to verify how macro bond strength tests compare to their micro counterparts in terms of material ranking, incidence of cohesive failures and data scattering, a three-step (Adper Scothbond Multi-Purpose), a two-step etch-and-rinse

(Adper Single Bond 2) and a self-etch system (Adper SE Plus), all from the same manufacturer (3M ESPE, St. Paul, MN, USA), were tested for bond strength to supercial bovine dentin. Except for the micro-tensile specimens, teeth were embedded in PVC cylinders using self-cure acrylic, with the dentin surface kept 2 mm above the embedding material. Dentin roughness was standardized using a 600-grit SiC paper. For macro shear and tensile tests (n = 10), a 3-mm diameter area was delimited with adhesive tape. After adhesive application following manufacturers directions, a 3-mm height truncated cone was built using a microhybrid composite (LLis, FGM Produtos Odontolgicos, Joinville, Brazil) with the smaller base (3-mm diameter) contacting the adhesive layer. Micro-shear specimens (n = 5) were built by inserting the composite into segments of Tygon tubing (Saint-Gobain Performance Plastics, Akron, OH, USA), four per tooth, with internal diameter of 0.76 and 0.4 mm in height, and photo-activating it in contact with the adhesive-coated dentin. For the micro-tensile specimens (n = 5), teeth crowns were sectioned perpendicularly to the exposed dentin surface and the resulting dentin area received the adhesive application. Such modication in dentin tubule orientation was necessary to increase the dentin thickness available for specimen sectioning. A 4-mm high composite block was built onto the dentin surface. All specimens were stored in distilled water at 37 C for 24 h prior to testing. For the micro-tensile test, stick-shaped specimens 0.81.0 mm2 (ve per tooth) were cut using a diamond wafering blade immediately prior to testing. For macro- and microshear testing, a 200-m knife-edge chisel placed in contact with the dentin surface was used to debond the composite

d e n t a l m a t e r i a l s 2 6 ( 2 0 1 0 ) e38e49

e45

truncated cones/cylinders. Tensile test used a clamp that contacted three-quarters of the truncated cone circumference. Articulated joints were used to assure that the bonded interface was perpendicular to the loading axis. For micro-tensile testing, Geraldelis jigs were used [143]. All tests were carried out at a crosshead speed of 0.5 mm/min. Specimen failure mode was assessed under a stereomicroscope at 1030 magnication. Results were submitted to one-way ANOVA/Tukey test at a pre-set global signicance level of 5%. Bond strength results are displayed in Fig. 7. As discussed above, the reduction in bonding area corresponded to an increase in bond strength values. Macro tests displayed a similar range of values, between 5.6 and 11.5 MPa. Both shear tests ranked the adhesive systems similarly, while for the tensile tests there was an inversion between the two systems with the highest bond strengths. Coefcients of variation ranged between 28 and 36% for shear, 21 and 40% for micro-shear, 32 and 38% for tension and 25 and 64% for the micro-tensile test. The higher scattering displayed by the self-etch system in both micro tests may be explained by the association of lower bond strength with a more technique-sensitive specimen preparation. Failure mode distribution is shown in Fig. 8. Only the adhesive system that achieved the lowest bond strength values in all testing modes did not present cohesive failures. For the other two systems, cohesive failures were more frequent with the macro compared to the micro bond strength tests. Pooled data revealed the incidence of cohesive failures of 45% for shear, 28% for tension, 13% for micro-shear and 12% for micro-tensile test. It must be emphasized, though, that under higher magnication, the incidence of mixed and cohesive failures may increase for all testing modes.

mens loaded in shear, compared to tension. Among the shear methods, the use of the chisel as a loading device causes the most severe stress concentration, which is also supported by experimental ndings showing lower bond strengths compared to other shear loading methods, such as the wire loop or the at rod. Within the limits suggested in the ISO/TR 11405, crosshead speed seems to have little inuence on bond strength results. Finally, in view of the many aspects affecting the results of macro bond strength tests, in order to allow for a more judicious comparison among studies researchers must provide a thorough description of the specimen design and test conguration.

Acknowledgements
Authors would like to express their gratitude to FGM Produtos Odontolgicos and 3M ESPE for kindly donating the materials used in the experimental section of this review.

references

7.

Summary

The need for tests capable of accurately assessing interfacial bond strength is clear. With that in mind, some would argue that the fracture mechanics approach is the optimal way to achieve controlled crack propagation at the bonded interface to assess adhesion [144,145]. But this method is more complex and time consuming than others for measuring bond strength to the dental substrate. Thus, in spite of their inherent shortcomings, macro bond strength tests will continue to be used for evaluating the adhesion of dental materials to tooth structure due to their simplicity. This review discussed aspects inuencing stress distribution that may impact dentin and enamel bond strength results and failure modes of macro shear and tensile bond strength tests. Some of the information is likely applicable to micro bond strength tests as well. In terms of specimen design, the effect of the elastic modulus of the second substrate, typically resin composite, on test results seems consistent among experimental studies, as well as with FEA data, i.e., a higher modulus mismatch between substrates increases the stress concentration at the interface resulting in lower bond strengths. The inuence of bonding area, on the other hand, remains undened, though at least a trend for increasing bond strength values with the use of smaller bonding areas does exist. Stress concentration is much more severe in speci-

[1] Finger WJ. Dentin bonding agents. Relevance of in vitro investigations. Am J Dent 1988;1:1848 [Special issue]. [2] Sudsangiam S, van Noort R. Do dentin bond strength tests serve a useful purpose? J Adhes Dent 1999;1:5767. [3] Hebling J, Castro FL, Costa CA. Adhesive performance of dentin bonding agents applied in vivo and in vitro. Effect of intrapulpal pressure and dentin depth. J Biomed Mater Res B: Appl Biomater 2007;83:295303. [4] Frankenberger R, Kramer N, Lohbauer U, Nikolaenko SA, Reich SM. Marginal integrity: is the clinical performance of bonded restorations predictable in vitro? J Adhes Dent 2007;9(Suppl. 1):10716. [5] Peumans M, Kanumilli P, De Munck J, Van Landuyt K, Lambrechts P, Van Meerbeek B. Clinical effectiveness of contemporary adhesives: a systematic review of current clinical trials. Dent Mater 2005;21:86481. [6] Shono Y, Ogawa T, Terashita M, Carvalho RM, Pashley EL, Pashley DH. Regional measurement of resindentin bonding as an array. J Dent Res 1999;78:699705. [7] Shono Y, Terashita M, Pashley EL, Brewer PD, Pashley DH. Effects of cross-sectional area on resinenamel tensile bond strength. Dent Mater 1997;13:2906. [8] Hashimoto M, Tay F, Svizero NR, De Gee AJ, Feilzer AJ, Sano H, et al. The effect of common errors os sealing ability of total-etch adhesives. Dent Mater 2006;22:5608. [9] Van Noort R, Noroozi S, Howard IC, Cardew G. A critique of bond strength measurements. J Dent 1989;17:617. [10] DeHoff PH, Anusavice KJ, Wang Z. Three-dimensional nite element analysis of the shear bond test. Dent Mater 1995;11:12631. [11] Van Noort R, Cardew GE, Howard IC, Noroozi S. The effect of local interfacial geometry on the measurement of the tensile bond strength to dentin. J Dent Res 1991;70:889 93. [12] Pashley DH, Sano H, Ciucchi B, Yoshiyama M, Carvalho RM. Adhesion testing of dentin bonding agents: a review. Dent Mater 1995;11:11725. [13] Sano H, Shono T, Sonoda H, Takatsu T, Ciucchi B, Carvalho R, et al. Relationship between surface area for adhesion and tensile bond strength evaluation of a micro-tensile bond test. Dent Mater 1994;10:23640.

e46

d e n t a l m a t e r i a l s 2 6 ( 2 0 1 0 ) e38e49

[14] Phrukkanon S, Burrow MF, Tyas MJ. Effect of cross-sectional surface area on bond strengths between resin and dentin. Dent Mater 1998;14:1208. [15] McDonough WG, Antonucci JM, He J, Shimada Y, Chiang MY, Schumacher GE, et al. A microshear test to measure bond strengths of dentinpolymer interfaces. Biomaterials 2002;23:36038. [16] Poitevin A, De Munck J, Van Landuyt K, Coutinho E, Peumans M, Lambrechts P, et al. Critical analysis of the inuence of different parameters on the microtensile bond strength of adhesives to dentin. J Adhes Dent 2008;10: 716. [17] Soares CJ, Soares PV, Santos-Filho PC, Armstrong SR. Microtensile specimen attachment and shape nite element analysis. J Dent Res 2008;87:8993. [18] Betamar N, Cardew G, Van Noort R. Inuence of specimen designs on the microtensile bond strength to dentin. J Adhes Dent 2007;9:15968. [19] Retief DH. Standardizing laboratory adhesion tests. Am J Dent 1991;4:2316. [20] Oilo G. Bond strength testing what does it mean? Int Dent J 1993;43:4928. [21] Watanabe I, Nakabayashi N. Measurement methods for adhesion to dentine: the current status in Japan. J Dent 1994;22:6772. [22] Technical specication ISO/TS 11405. Dental materials testing of adhesion to tooth structure. Switzerland; 2003. [23] al-Salehi SK, Burke FJ. Methods used in dentin bonding tests: an analysis of 50 investigations on bond strength. Quintessence Int 1997;28:71723. [24] Burke FJ, Hussain A, Nolan L, Fleming GJ. Methods used in dentine bonding tests: an analysis of 102 investigations on bond strength. Eur J Prosthodont Restor Dent 2008;16:15865. [25] Leloup G, DHoore W, Bouter D, Degrange M, Vreven J. Meta-analytical review of factors involved in dentin adherence. J Dent Res 2001;80:160514. [26] Oilo G, Olsson S. Tensile bond strength of dentin adhesives: a comparison of materials and methods. Dent Mater 1990;6:13844. [27] Dickens SH, Milos MF. Relationship of dentin shear bond strengths to different laboratory test designs. Am J Dent 2002;15:18592. [28] Pecora N, Yaman P, Dennison J, Herrero A. Comparison of shear bond strength relative to two testing devices. J Prosthet Dent 2002;88:5115. [29] Sinhoreti MA, Consani S, De Goes MF, Sobrinho LC, Knowles JC. Inuence of loading types on the shear strength of the dentinresin interface bonding. J Mater Sci: Mater Med 2001;12:3944. [30] Aizawa K, Kameyama A, Kato J, Oda Y, Hirai Y. Inuence of free-hand vs uniform irradiation on tensile bond strength in Er:YAG-lased dentin. J Adhes Dent 2008;10:2959. [31] Al-Assaf K, Chakmakchi M, Palaghias G, Karanika-Kouma A, Eliades G. Interfacial characteristics of adhesive luting resins and composites with dentine. Dent Mater 2007;23:82939. [32] Ando S, Watanabe T, Tsubota K, Yoshida T, Irokawa A, Takamizawa T, et al. Effect of adhesive application methods on bond strength to bovine enamel. J Oral Sci 2008;50:1816. [33] Ariyoshi M, Nikaido T, Okada A, Foxton RM, Tagami J. Dentin bond strengths of three adhesive/composite core systems using different curing units. Dent Mater J 2008;27:18794. [34] Asaka Y, Amano S, Rikuta A, Kurokawa H, Miyazaki M, Platt JA, et al. Inuence of thermal cycling on dentin bond strengths of single-step self-etch adhesive systems. Oper Dent 2007;32:738.

[35] Ayad MF, Fahmy NZ, Rosenstiel SF. Effect of surface treatment on roughness and bond strength of a heat-pressed ceramic. J Prosthet Dent 2008;99:12330. [36] Barbosa CM, Sasaki RT, Florio FM, Basting RT. Inuence of time on bond strength after bleaching with 35% hydrogen peroxide. J Contemp Dent Pract 2008;9:818. [37] Barkmeier WW, Erickson RL, Kimmes NS, Latta MA, Wilwerding TM. Effect of enamel etching time on roughness and bond strength. Oper Dent 2009;34:21722. [38] Benetti AR, Asmussen E, Peutzfeldt A. Inuence of curing rate of resin composite on the bond strength to dentin. Oper Dent 2007;32:1448. [39] Borges MA, Matos IC, Dias KR. Inuence of two self-etching primer systems on enamel adhesion. Braz Dent J 2007;18:1138. [40] Borsatto MC, Corona SA, de Araujo FP, de Souza-Gabriel AE, Pecora JD, Palma-Dibb RG. Effect of Er:YAG laser on tensile bond strength of sealants in primary teeth. J Dent Child (Chic) 2007;74:1048. [41] Brulat N, Rocca JP, Leforestier E, Fiorucci G, Nammour S, Bertrand MF. Shear bond strength of self-etching adhesive systems to Er:YAG-laser-prepared dentin. Lasers Med Sci 2009;24:537. [42] Bulucu B, Ozsezer E. Inuence of light-curing units on dentin bond strength after bleaching. J Adhes Dent 2007;9:1837. [43] Cardoso MV, Moretto SG, de Carvalho RC, Russo EM. Inuence of intrapulpal pressure simulation on the bond strength of adhesive systems to dentin. Braz Oral Res 2008;22:1705. [44] Carrieri TC, de Freitas PM, Navarro RS, Eduardo Cde P, Mori M. Adhesion of composite luting cement to Er:YAG-laser-treated dentin. Lasers Med Sci 2007;22: 16570. [45] Cekic-Nagas I, Ergun G, Tezvergil A, Vallittu PK, Lassila LV. Effect of ber-reinforced composite at the interface on bonding of resin core system to dentin. Dent Mater J 2008;27:73643. [46] Chaiyabutr Y, McGowan S, Phillips KM, Kois JC, Giordano RA. The effect of hydrouoric acid surface treatment and bond strength of a zirconia veneering ceramic. J Prosthet Dent 2008;100:194202. [47] Czarnecka B, Deregowska-Nosowicz P, Limanowska-Shaw H, Nicholson JW. Shear bond strengths of glass-ionomer cements to sound and to prepared carious dentine. J Mater Sci: Mater Med 2007;18:8459. [48] DArcangelo C, Vanini L. Effect of three surface treatments on the adhesive properties of indirect composite restorations. J Adhes Dent 2007;9:31926. [49] da Costa CC, Oshima HM, Costa Filho LC. Evaluation of shear bond strength and interfacial micromorphology of direct restorations in primary and permanent teeth an in vitro study. Gen Dent 2008;56:8593 [quiz 9485, 111112]. [50] Dantas DC, Ribeiro AI, Lima LH, de Lima MG, Guenes GM, Braz AK, et al. Inuence of water storage time on the bond strength of etch-and-rinse and self-etching adhesive systems. Braz Dent J 2008;19:21923. [51] Di Nicolo R, Shintome LK, Myaki SI, Nagayassu MP. Bond strength of resin modied glass ionomer cement to primary dentin after cutting with different bur types and dentin conditioning. J Appl Oral Sci 2007;15:45964. [52] El-Araby AM, Talic YF. The effect of thermocycling on the adhesion of self-etching adhesives on dental enamel and dentin. J Contemp Dent Pract 2007;8:1724. [53] Endo T, Osada T, Finger WJ, Hoffmann M, Kanehira M, Komatsu M. Effect of oxygen inhibition of self-etching adhesives on enameldentin polymer bond. J Adhes Dent 2007;9:338.

d e n t a l m a t e r i a l s 2 6 ( 2 0 1 0 ) e38e49

e47

[54] Erhardt MC, Shinohara MS, Bedran-Russo AK, Amaral CM, Pimenta LA. Effect of long-term water storage on etch-and-rinse and self-etching resindentin bond strengths. Gen Dent 2008;56:3727 [quiz 378379, 400]. [55] Erickson RL, De Gee AJ, Feilzer AJ. Effect of pre-etching enamel on fatigue of self-etch adhesive bonds. Dent Mater 2008;24:11723. [56] Erkut S, Kucukesmen HC, Eminkahyagil N, Imirzalioglu P, Karabulut E. Inuence of previous provisional cementation on the bond strength between two denitive resin-based luting and dentin bonding agents and human dentin. Oper Dent 2007;32:8493. [57] Esteves-Oliveira M, Zezell DM, Apel C, Turbino ML, Aranha AC, Eduardo Cde P, et al. Bond strength of self-etching primer to bur cut, Er, Cr:YSGG, and Er:YAG lased dental surfaces. Photomed Laser Surg 2007;25:37380. [58] Fawzy AS, Amer MA, El-Askary FS. Sodium hypochlorite as dentin pretreatment for etch-and-rinse single-bottle and two-step self-etching adhesives: atomic force microscope and tensile bond strength evaluation. J Adhes Dent 2008;10:13544. [59] Fuchigami K, Ikemura K, Ichizawa K. Novel, multi-purpose, PMMA-type adhesive resin with newly synthesized microcapsule of radical polymerization initiators. Dent Mater J 2008;27:3548. [60] Furukawa M, Shigetani Y, Finger WJ, Hoffmann M, Kanehira M, Endo T, et al. All-in-one self-etch model adhesives: HEMA-free and without phase separation. J Dent 2008;36:4028. [61] Furuse AY, Peutzfeldt A, Asmussen E. Effect of evaporation of solvents from one-step, self-etching adhesives. J Adhes Dent 2008;10:359. [62] Gernhardt CR, Bekes K, Hahn P, Schaller HG. Inuence of pressure application before light-curing on the bond strength of adhesive systems to dentin. Braz Dent J 2008;19:627. [63] Gogos C, Stavrianos C, Kolokouris I, Economides N, Papadoyannis I. Shear bond strength of two resin cements to human root dentin using three dentin bonding agents. Oper Dent 2007;32:316. [64] Gokce B, Comlekoglu ME, Ozpinar B, Turkun M, Kaya AD. Effect of antioxidant treatment on bond strength of a luting resin to bleached enamel. J Dent 2008;36:7805. [65] Gokce K, Aykor A, Ersoy M, Ozel E, Soyman M. Effect of phosphoric acid etching and self-etching primer application methods on dentinal shear bond strength. J Adhes Dent 2008;10:3459. [66] Gomes-Silva JM, Torres CP, Contente MM, Oliveira MA, Palma-Dibb RG, Borsatto MC. Bond strength of a pit-and-ssure sealant associated to etch-and-rinse and self-etching adhesive systems to saliva-contaminated enamel: individual vs. simultaneous light curing. Braz Dent J 2008;19:3417. [67] Goncalves M, Corona SA, Palma-Dibb RG, Pecora JD. Inuence of pulse repetition rate of Er:YAG laser and dentin depth on tensile bond strength of dentinresin interface. J Biomed Mater Res A 2008;86:47782. [68] Gurgan S, Kiremitci A, Cakir FY, Gorucu J, Alpaslan T, Yazici E, et al. Shear bond strength of composite bonded to erbium:yttriumaluminum-garnet laser-prepared dentin. Photomed Laser Surg 2008;26:495500. [69] Gurgan S, Kiremitci A, Cakir FY, Yazici E, Gorucu J, Gutknecht N. Shear bond strength of composite bonded to erbium:yttriumaluminum-garnet laser-prepared dentin. Lasers Med Sci 2009;24:11722. [70] Habekost Lde V, Camacho GB, Demarco FF, Powers JM. Tensile bond strength and exural modulus of resin cements inuence on the fracture resistance of teeth restored with ceramic inlays. Oper Dent 2007;32:48895.

[71] Holderegger C, Sailer I, Schuhmacher C, Schlapfer R, Hammerle C, Fischer J. Shear bond strength of resin cements to human dentin. Dent Mater 2008;24:94450. [72] Huh JB, Kim JH, Chung MK, Lee HY, Choi YG, Shim JS. The effect of several dentin desensitizers on shear bond strength of adhesive resin luting cement using self-etching primer. J Dent 2008;36:102532. [73] Ikeda M, Tsubota K, Takamizawa T, Yoshida T, Miyazaki M, Platt JA. Bonding durability of single-step adhesives to previously acid-etched dentin. Oper Dent 2008;33:7029. [74] Ikemura K, Tay FR, Nishiyama N, Pashley DH, Endo T. Multi-purpose bonding performance of newly synthesized phosphonic acid monomers. Dent Mater J 2007;26: 10515. [75] Ishii T, Ohara N, Oshima A, Koizumi H, Nakazawa M, Masuno T, et al. Bond strength to bovine dentin of a composite core build-up material combined with four different bonding agents. J Oral Sci 2008;50:32933. [76] Kameyama A, Aizawa K, Kato J, Hirai Y. Tensile bond strength of single-step self-etch adhesives to Er:YAG laser-irradiated dentin. Photomed Laser Surg 2009. [77] Kameyama A, Kato J, Aizawa K, Suemori T, Nakazawa Y, Ogata T, et al. Tensile bond strength of one-step self-etch adhesives to Er:YAG laser-irradiated and non-irradiated enamel. Dent Mater J 2008;27:38691. [78] Kaya AD, Turkun M, Arici M. Reversal of compromised bonding in bleached enamel using antioxidant gel. Oper Dent 2008;33:4417. [79] Korkmaz Y, Attar N. Dentin bond strength of composites with self-etching adhesives using LED curing lights. J Contemp Dent Pract 2007;8:3442. [80] Korkmaz Y, Baseren M. Effect of antibacterial varnishes applied to root dentin on shear bond strength of tooth-colored restorative materials. Oper Dent 2008;33:6571. [81] Krifka S, Borzsonyi A, Koch A, Hiller KA, Schmalz G, Friedl KH. Bond strength of adhesive systems to dentin and enamel human vs. bovine primary teeth in vitro. Dent Mater 2008;24:88894. [82] Kurokawa R, Finger WJ, Hoffmann M, Endo T, Kanehira M, Komatsu M, et al. Interactions of self-etch adhesives with resin composites. J Dent 2007;35:9239. [83] Kusunoki M, Itoh K, Utsumi Y, Hisamitsu H. Priming effects of triethylene glycol and triethylene glycol monomethacrylate on dentin bonding. Dent Mater J 2007;26:47480. [84] Lee BS, Lin PY, Chen MH, Hsieh TT, Lin CP, Lai JY, et al. Tensile bond strength of Er, Cr:YSGG laser-irradiated human dentin and analysis of dentinresin interface. Dent Mater 2007;23:5708. [85] Lee JJ, Nettey-Marbell A, Cook Jr A, Pimenta LA, Leonard R, Ritter AV. Using extracted teeth for research: the effect of storage medium and sterilization on dentin bond strengths. J Am Dent Assoc 2007;138:1599603. [86] Leevailoj C, Ua-wutthikrerk P, Poolthong S. Shear bond strength of dual-cured and self-cured resin composites to dentin using different bonding agents and techniques. Oper Dent 2007;32:14959. [87] Lepri TP, Souza-Gabriel AE, Atoui JA, Palma-Dibb RG, Pecora JD, Milori Corona SA. Shear bond strength of a sealant to contaminated-enamel surface: inuence of erbium:yttriumaluminum-garnet laser pretreatment. J Esthet Restor Dent 2008;20:38692 [discussion 393384]. [88] Luhrs AK, Guhr S, Schilke R, Borchers L, Geurtsen W, Gunay H. Shear bond strength of self-etch adhesives to enamel with additional phosphoric acid etching. Oper Dent 2008;33:15562. [89] Mahmoud SH, Abdel kader Sobh M, Zaher AR, Ghazy MH, Abdelaziz KM. Bonding of resin composite to tooth

e48

d e n t a l m a t e r i a l s 2 6 ( 2 0 1 0 ) e38e49

[90]

[91]

[92]

[93]

[94]

[95]

[96]

[97]

[98] [99]

[100]

[101]

[102]

[103]

[104]

[105]

[106]

[107]

structure of uremic patients receiving hemodialysis: shear bond strength and acid-etch patterns. J Adhes Dent 2008;10:3358. Masri M, Pilo R, Brosh T. The inuence of convergence angle and dentin micromorphology on shear bond strength of adhesive resin luting cement. J Adhes Dent 2008;10:27784. Metz MJ, Cochran MA, Matis BA, Gonzalez C, Platt JA, Pund MR. Clinical evaluation of 15% carbamide peroxide on the surface microhardness and shear bond strength of human enamel. Oper Dent 2007;32:42736. Mitra SB, Lee CY, Bui HT, Tantbirojn D, Rusin RP. Long-term adhesion and mechanism of bonding of a paste-liquid resin-modied glass-ionomer. Dent Mater 2009;25:45966. Moshaverinia A, Ansari S, Moshaverinia M, Roohpour N, Darr JA, Rehman I. Effects of incorporation of hydroxyapatite and uoroapatite nanobioceramics into conventional glass ionomer cements (GIC). Acta Biomater 2008;4:43240. Muraguchi K, Shigenobu S, Suzuki S, Tanaka T. Improvement of bonding to bleached bovine tooth surfaces by ascorbic acid treatment. Dent Mater J 2007;26: 87581. Nam KY, Kim JB, Jang BC, Kwon TY, Kim KH. Effects of dentin bonding agents on bonding durability of a owable composite to dentin. Dent Mater J 2007;26:22431. Omae M, Inoue M, Itota T, Finger WJ, Tanaka K, Yamamoto K, et al. Effect of a desensitizing agent containing glutaraldehyde and HEMA on bond strength to Er:YAG laser-irradiated dentine. J Dent 2007;35:398402. Oto T, Yasuda G, Tsubota K, Kurokawa H, Miyazaki M, Platt JA. Inuence of power density on polymerization behavior and bond strengths of dual-cured resin direct core foundation systems. Oper Dent 2009;34:1929. Paradella TC, Fava M. Bond strength of adhesive systems to human tooth enamel. Braz Oral Res 2007;21:49. Pires-de-Souza Fde C, Marco FF, Casemiro LA, Panzeri H. Desensitizing bioactive agents improves bond strength of indirect resin-cemented restorations: preliminary results. J Appl Oral Sci 2007;15:1206. Piwowarczyk A, Bender R, Ottl P, Lauer HC. Long-term bond between dual-polymerizing cementing agents and human hard dental tissue. Dent Mater 2007;23:2117. Ritter AV, Ghaname E, Leonard RH. The inuence of dental unit waterline cleaners on composite-to-dentin bond strengths. J Am Dent Assoc 2007;138:98591 [quiz; 10221023]. Ritter AV, Ghaname E, Pimenta LA. Dentin and enamel bond strengths of dual-cure composite luting agents used with dual-cure dental adhesives. J Dent 2009;37:5964. Sarac D, Bulucu B, Sarac YS, Kulunk S. The effect of dentin-cleaning agents on resin cement bond strength to dentin. J Am Dent Assoc 2008;139:7518. Sasaki LH, Lobo PD, Moriyama Y, Watanabe IS, Villaverde AB, Tanaka CS, et al. Tensile bond strength and SEM analysis of enamel etched with Er:YAG laser and phosphoric acid: a comparative study in vitro. Braz Dent J 2008;19:5761. Sassi JF, dos Reis Batista A, Ciccone-Nogueira JC, Corona SAM, Palma-Dibb RG. Inuence of light-curing unit systems on shear bond strength and marginal microlekage of composite resin restorations. Mater Res 2008;11:69 73. Schmidlin PR, Siebenmann J, Kocher P, Seemann R, Attin T, Bindl A. Effects of de- and remineralization of dentin on bond strengths yielded by one-, three-, and four-step adhesives. J Adhes Dent 2008;10:11926. Schulz H, Schimmoeller B, Pratsinis SE, Salz U, Bock T. Radiopaque dental adhesives: dispersion of ame-made

[108]

[109]

[110]

[111]

[112]

[113]

[114]

[115]

[116]

[117]

[118]

[119]

[120]

[121]

[122]

[123]

[124]

[125]

Ta2 O5 /SiO2 nanoparticles in methacrylic matrices. J Dent 2008;36:57987. Shinkai K, Suzuki S, Katoh Y. Effect of light intensity for adhesives on shear bond strength to dentin. Dent Mater J 2008;27:6605. Silva PC, Goncalves M, Nascimento TN, Centola AL. Effect of air abrasion on tensile bond strength of a single-bottle adhesive/indirect composite system to enamel. Braz Dent J 2007;18:458. Soares CJ, Branco CA, Soares PBF, Fonseca RB, Carlo HL, Fernandes Neto AJ. Effect of blood contamination during adhesive restorative procedures on dentinresin cement shear bond strength. Braz J Oral Sci 2007;6:13205. Soderholm KJ, Soares F, Argumosa M, Loveland C, Bimstein E, Guelmann M. Shear bond strength of one etch-and-rinse and ve self-etching dental adhesives when used by six operators. Acta Odontol Scand 2008;66:2439. Souza-Zaroni WC, Seixas LC, Ciccone-Nogueira JC, Chimello DT, Palma-Dibb RG. Tensile bond strength of different adhesive systems to enamel and dentin. Braz Dent J 2007;18:1248. Sugizaki J, Morigami M, Uno S, Yamada T. Clinical evaluation and interfacial morphology observation of Xeno III self-etching resin bonding and restorative system. Dent Mater J 2007;26:6027. Susin AH, Vasconcellos WA, Saad JR, Oliveira Junior OB. Tensile bond strength of self-etching versus total-etching adhesive systems under different dentinal substrate conditions. Braz Oral Res 2007;21:816. Taira Y, Soeno K, Atsuta M. Microperoxidase primer promotes adhesion of butylborane-polymerized resin to dentin. J Biomed Mater Res B: Appl Biomater 2007;81:1115. Thomsen KB, Peutzfeldt A. Resin composites: strength of the bond to dentin versus mechanical properties. Clin Oral Invest 2007;11:459. Tjandrawinata R, Irie M, Suzuki K. Twenty-four hour exural and shear bond strengths of owable light-cured composites: a comparison analysis using Weibull statistics. Dent Mater J 2007;26:58997. Toman M, Cal E, Turkun M, Ertugrul F. Bond strength of glassceramics on the uorosed enamel surfaces. J Dent 2008;36:2816. Toman M, Toksavul S, Akin A. Bond strength of all-ceramics to tooth structure: using new luting systems. J Adhes Dent 2008;10:3738. Torres CP, Chinelatti MA, Gomes-Silva JM, Borsatto MC, Palma-Dibb RG. Tensile bond strength to primary dentin after different etching times. J Dent Child (Chic) 2007;74:1137. Torres CP, Gomes-Silva JM, Borsatto MC, Barroso JM, Pecora JD, Palma-Dibb RG. Shear bond strength of self-etching and total-etch adhesive systems to Er:YAG laser-irradiated primary dentin. J Dent Child (Chic) 2009;76: 6773. Torres CRG, Pinto LQ, Leonel AG, Pucci CR, Borges AB. Interaction between total-etch and self-etch adhesives and conventional and self-adhesive resin cements. Braz J Oral Sci 2007;6:137682. Tseng WY, Chen MH, Lu HH, Lin CW, Hsieh TT, Chen CH, et al. Tensile bond strength of Er, Cr:YSGG laser-irradiated human dentin to composite inlays with two resin cements. Dent Mater J 2007;26:74655. Unlu N, Cobankara FK, Ozer F. Effect of elapsed time following bleaching on the shear bond strength of composite resin to enamel. J Biomed Mater Res B: Appl Biomater 2008;84:3638. Watanabe T, Tsubota K, Takamizawa T, Kurokawa H, Rikuta A, Ando S, et al. Effect of prior acid etching on bonding

d e n t a l m a t e r i a l s 2 6 ( 2 0 1 0 ) e38e49

e49

[126]

[127]

[128]

[129] [130] [131]

[132]

[133]

[134] [135]

durability of single-step adhesives. Oper Dent 2008;33:42633. Yazici AR, Celik C, Ozgunaltay G, Dayangac B. Bond strength of different adhesive systems to dental hard tissues. Oper Dent 2007;32:16672. Yazici AR, Karaman E, Ertan A, Ozgunaltay G, Dayangac B. Effect of different pretreatment methods on dentin bond strength of a one-step self-etch adhesive. J Contemp Dent Pract 2009;10:418. Yesilyurt C, Bulucu B, Sezen O, Bulut G, Celik D. Bond strengths of two conventional glass-ionomer cements to irradiated and non-irradiated dentin. Dent Mater J 2008;27:695701. Grifth AA. The phenomena of ow and rupture in solids. Philos Trans Roy Soc 1921;221:16398. Irwin GR. Analysis of stresses and strains near the end of a crack traversing a plate. J Appl Mech 1957;24:3614. Watanabe LG, Marshall GW, Marshall SJ. Variables inuence on shear bond strength testing to dentin. In: Advanced Adhesive Dentistry 3rd International Kuraray Symposium. 1999. p. 7590. Bianchi J, Bond strength of composite resins to dentin. Masters thesis. So Paulo: University of So Paulo; 1994. p. 67. Hasegawa T, Itoh K, Koike T, Yukitani W, Hisamitsu H, Wakumoto S, et al. Effect of mechanical properties of resin composites on the efcacy of the dentin bonding system. Oper Dent 1999;24:32330. Versluis A, Tantbirojn D, Douglas WH. Why do shear bond tests pull out dentin? J Dent Res 1997;76:1298307. Rasmussen ST. Analysis of dental shear bond strength tests, shear or tensile? Int J Adhes Adhes 1996;16:14754.

[136] Placido E, Meira JB, Lima RG, Muench A, de Souza RM, Ballester RY. Shear versus micro-shear bond strength test: a nite element stress analysis. Dent Mater 2007;23:108692. [137] Thiruppukuzhi SV, Sun CT. Models for the strain-rate-dependent behavior of polymer composites. Compos Sci Technol 2001;61:112. [138] Guo Y, Li Y. Quasi-static/dynamic response of SiO2 -epoxy nanocomposites. Mater Sci Eng A 2007;458:3305. [139] Hara AT, Pimenta LA, Rodrigues Jr AL. Inuence of cross-head speed on resindentin shear bond strength. Dent Mater 2001;17:1659. [140] Takemori T, Chigira H, Itoh K, Hisamitsu H, Wakumoto S. Factors affecting tensile bond strength of composite to dentin. Dent Mater 1993;9:1368. [141] Oshida Y, Miyazaki M. Dentin bonding system. Part II: effect of crosshead speed. Bio-Med Mater Eng 1996;6:87100. [142] Richeton J, Ahzi S, Vecchio KS, Jiang FC, Adharapurapu RR. Inuence of temperature and strain rate on the mechanical behavior of three amorphous polymers: characterization and modeling of the compressive yield stress. Int J Solids Struct 2006;43:231835. [143] Perdigao J, Geraldeli S, Carmo AR, Dutra HR. In vivo inuence of residual moisture on microtensile bond strengths of one-bottle adhesives. J Esthet Restor Dent 2002;14:318. [144] Tantbirojn D, Cheng YS, Versluis A, Hodges JS, Douglas WH. Nominal shear or fracture mechanics in the assessment of compositedentin adhesion? J Dent Res 2000;79:418. [145] Ruse ND, Troczynski T, MacEntee MI, Feduik D. Novel fracture toughness test using a notchless triangular prism (NTP) specimen. J Biomed Mater Res 1996;31:45763.