|Year : 2016 | Volume
| Issue : 2 | Page : 109-117
Effect of different desensitizing adhesive systems on the shear bond strength of composite resin to dentin surface
Ahlam Abd El-Galil Nassar, Hussien Y El-Sayed, Wedad M Etman
Conservative Dentistry Department, Faculty of Dentistry, Tanta University, Tanta, Egypt
|Date of Submission||06-Apr-2016|
|Date of Acceptance||07-Apr-2016|
|Date of Web Publication||23-Aug-2016|
Ahlam Abd El-Galil Nassar
Conservative Dentistry Department, Faculty of Dentistry, Tanta University, Algharbia, Tanta Elgeish Street, Tanta
Source of Support: None, Conflict of Interest: None
The aim of this study was to evaluate the effect of different desensitizing agents, oxalate desensitizer and I-Bond, on the shear bond strength of composite resin to dentin surface.
Materials and methods
Occlusal surfaces of 80 sound human molars extracted were trimmed to expose a flat dentin surface. Each prepared sample was inserted in a metallic mold, which was designed with a Teflon mold having a hole (4 mm diameter ×3 mm height) for filling the restorative material. The samples were divided into four groups (20 each): group I (the control group), in which Adper Single Bond 2 and composite were applied; group II, in which oxalate desensitizer (D/Sense Crystal) was applied followed by Adper Single Bond 2 and composite; group III, in which oxalate desensitizer was applied, followed by re-etching and application of Adper Single Bond 2 and composite; and group IV, in which I-Bond and composite were used. All samples were thermocycled for 500 cycles (5–55°C). The samples in each group were subdivided into two subgroups (10 each) (A and B) according to storage time (24 h or 6 months, respectively). Shear bond strength of eight samples from each subgroup was measured. Debonded surfaces were examined under a stereomicroscope at magnification ×40 to determine the mode of failure. The remaining two samples were prepared to be examined under scanning electron microscope to reveal the resin penetration.
Group I (the control group) recorded the highest shear bond strength values (11.838 ± 3.141 and 6.842 ± 3.912, respectively) in the two subgroups, followed by group IV (6.695 ± 3.164 and 6.217 ± 3.276, respectively) and group III (7.707 ± 3.845 and 3.681 ± 1.743, respectively), whereas the lowest values were found in group II (6.347 ± 3.208 and 3.240 ± 1.804, respectively). The incidence of adhesive mode of failure was higher in all tested groups, followed by mixed mode. Scanning electron microscope results confirmed the obtained statistical analysis of collected data.
Both desensitizing agents and storage time had a negative significant effect on the shear bond strength of composite restoration to dentin surface.
Keywords: desensitizing agents, shear bond strength, water storage
|How to cite this article:|
Nassar AA, El-Sayed HY, Etman WM. Effect of different desensitizing adhesive systems on the shear bond strength of composite resin to dentin surface. Tanta Dent J 2016;13:109-17
|How to cite this URL:|
Nassar AA, El-Sayed HY, Etman WM. Effect of different desensitizing adhesive systems on the shear bond strength of composite resin to dentin surface. Tanta Dent J [serial online] 2016 [cited 2017 Dec 16];13:109-17. Available from: http://www.tmj.eg.net/text.asp?2016/13/2/109/188913
| Introduction|| |
Resin composite restoration has been used clinically over the past few years due to increased esthetic demands by patients and good adhesion demands by clinicians through application of adhesives ,.
Some problems during adhesive application were recorded. One of these is overetching and overdrying the dentin, which might cause bonding difficulties or complications due to the intrinsic wetness of vital deep dentin after removal of the smear layer ,. Another problem is the increased permeability associated with the simplified version of the etch-and-rinse adhesive systems. In addition, incomplete sealing due to continuous transudation of dentinal fluid through open dentinal tubules before polymerization of the adhesive may result in entrapment of water-filled blisters along the adhesive interface ,. Compression of these blisters during mastication may cause rapid fluid movement within the dentinal tubules that activates the intradental nerve fibers, which results in postoperative sensitivity . This was the most widely accepted theory of the mechanism of dentin hypersensitivity, which is called the hydrodynamic theory . Among the potential risk factors for dentin hypersensitivity are excessive consumption of dietary acids, toothbrush abrasion, chemical erosion, exposed dentin, and eating disorders .
Treatment of dentin hypersensitivity using the concept of dentin desensitization tends to concentrate on tubule-occluding approaches, and hence both dentin permeability and sensitivity are reduced ,. This has been performed with various precipitates or by covering the exposed dentin with an impermeable layer to prevent the osmotic gradient changes that create the painful stimuli . In addition, desensitization of teeth after cavity preparation has been described in an attempt to avoid postoperative sensitivity .
Some desensitizing agents act by precipitation of crystalline salts in dentinal tubules ,, such as potassium nitrate, potassium or ferric oxalates, and dentin sealers . Tay et al.  found that, on applying oxalate desensitizers to acid-etched dentin before adhesive application, the depleted calcium ions from the dentin surface help to diffuse the oxalate ions further down into the dentinal tubules, producing calcium oxalate crystals. These crystals result in subsurface tubular occlusion and reduction in the hydraulic conductance of dentin.
Another well-known mode of action is by precipitation of protein in dentinal tubules in addition to resin occlusion. Gluma and I-Bond bonding agents  are examples of this mode of action as they provide desensitization to dentin due to the presence of glutaraldehyde and HEMA in their component ,,.
However, many studies reported that the application of desensitizing agents had significant negative effects on the shear bond strength of adhesive system ,.
Thus, the objective of this study was to evaluate the effect of different desensitizing adhesive systems on the shear bond strength of composite resin to dentin surface.
| Materials and Methods|| |
A total of 80 freshly extracted sound human molars with periodontal involvement were collected from the Oral and Maxillofacial Surgery Department at the Faculty of Dentistry, Tanta University. All patients agreed that their extracted teeth shall be used in the study. The teeth were cleaned with pumice and water and stored in saline solution in a refrigerator at 4°C, and the solution was changed regularly until the experiment time, which was scheduled within 3 months after extraction .
The roots of each tooth were cut off 1 mm below the cementoenamel junction and the crowns were embedded in an autopolymerizing resin (Imircryl, Konya, Turkey) inside a splitted metallic holder, leaving the occlusal surfaces uncovered. These were carefully trimmed to expose clean flat dentin surfaces using a diamond disc adapted to low-speed hand piece under copious water coolant . The exposed dentin surface was finished using 600 Grit Wet Silicon Carbide abrasive papers in a circular motion and rinsed under running tap water to create a smear layer in addition to a flat dentin surface . The prepared samples were randomly divided into four equal groups according to the method of dentin treatment (20 each).
A specially prepared Teflon mold in a metallic ring was secured (zero touch) on the dentin surface to confine the area of dentin to be treated. The confined dentin surfaces for groups I, II, and III were etched with 35% phosphoric acid gel for 15 s with a special syringe and rinsed for 10 s. In group I (the control group), Adper Single Bond 2 (3M ESPE, St. paul, MN, USA) adhesive system was applied with a microbrush for 15 s, dried gently for 2–5 s with intermittent air blow free of oil, and light-cured for 10 s. In group II, oxalate desensitizer (D/Sense Crystal) was applied with a Sofneedle foam tip specially supplied with the desensitizing agent, leaving a frosty white precipitate on the surface to which the adhesive system (Adper Single Bond 2) was applied in the same manner as group I. In group III, oxalate desensitizer (D/Sense Crystal and Sofneedle, Centrix, Inc., Shelton, CT, USA) was applied in the same manner. Subsequently, the dentin surface was re-etched using 35% phosphoric acid gel for 15 s and rinsed with water for 10 s. Excess water was blotted, leaving a wet dentin surface to which the same previously used adhesive system was applied. In group IV, I-Bond One Self-Etch (Heraeus Kulzer, Inc., New York) adhesive system was applied in three successive layers to the prepared dentin using a specially supplied microbrush, followed by gentle rubbing for 30 s. Thereafter, gentle air pressure was used to remove acetone and water solvents. The adhesive system was cured for 20 s according to the manufacturer's instruction.
On all of the confined dentin surfaces, composite resin cylinders (Filtek Z250, 3M ESPE, St. paul, MN, USA) were built up in two layers measuring 1.5 mm in thickness. Each layer was cured for 20 s using a halogen light cure unit (Cromalux-E). All samples were then thermocycled for 500 cycles (5–55°C) with 30 s dwell time and 20 s transfer time ,.
After thermocycling, the samples of each group were subdivided randomly into two equal subgroups A and B (10 samples each) according to storage time in distilled water at 37°C in an incubator  of either 24 h or 6 months, respectively, and the storage medium was changed regularly (twice weekly) to minimize the risk for bacterial growth.
After each recommended storage period, the shear bond strength of eight samples of each subgroup was tested using an Instron testing machine (Instron Corporation, Canton, Massachusetts, USA) at a cross-head speed of 0.5 mm/min and a load cell capacity of 25 kN until fracture .
The fracture load was recorded in kilograms and the shear bond strength values were calculated in mega Pascal . Finally, the collected data were tabulated, calculated, and statistically analyzed using a statistical package SPSS 17.0 for Windows (SPSS Inc., Chicago, Illinois, USA). One-way analysis of variance (ANOVA) was used for comparing between the four tested groups at each subgroup when even significance was recorded. Tukey's test was used to find out as to which group was responsible for the difference. In addition, comparison between the two tested subgroups at each group was performed using the T-test.
All fractured surfaces were examined under a stereomicroscope (SZ-CTY; Olympus, Japan) at a magnification of ×40 to record the mode of failure, which was classified into adhesive, cohesive, and mixed mode of failure.
The remaining two samples of each subgroup were prepared to be examined under a scanning electron microscope (SEM) (JSM-5300 Scanning Microscope; JEOL, Peabody, Massachusetts, USA) to find out the adhesion pattern concerning different dentin treatments.
| Results|| |
The statistical analysis of collected data after 24 h of water storage (subgroup A) is illustrated in [Table 1]. The ANOVA test was used to compare all tested groups at 95% and reported a statistically significant difference. Therefore, Tukey's test was performed to find out as to which group is responsible for the recorded difference and found that it was group I, as a statistically significant difference was recorded between group I and group II (P = 0.019) and between group I and group IV (P = 0.023), whereas there were no significant differences among the other tested groups (P > 0.05).
|Table 1: Statistical analysis of the shear bond strength values (MPa) of the four tested groups after 24 h of storage|
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The statistical analysis of collected data after 6 months of water storage (subgroup B) is illustrated in [Table 2]. The ANOVA test reported no statistically significant difference among tested groups.
|Table 2: Statistical analysis of the shear bond strength values (MPa) of the four tested groups after 6 months of storage|
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Regardless of the storage time, the ANOVA test was used to compare all tested groups, which revealed a significant difference ([Table 3]). Therefore, the treatment of dentin surface is a factor affecting baseline value.
|Table 3: Statistical analysis of the shear bond strength values (MPa) of the four tested groups regardless of the storage periods|
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The interaction between all tested variables (the method of dentin surface treatment and/or period of storage in water) was assessed. The interaction between the two tested variables, the method of dentin surface treatment and the period of storage in water, showed a high significant difference, recording a P value of 0.003. This means that both variables affected each other, thus giving a negative effect on the shear bond strength in the current conditions.
Mode of failure
Data of all tested groups and subgroups represented as a percentage for each failure mode are shown in [Table 4] and [Table 5]. It was seen that there was a significant difference in the mode of failure between the tested groups after 24 h. However, using the same test, the c2 value reported no significance in the mode of failure comparing the tested groups after 6 months of storage period. Thus, this indicated that the storage period or aging is an important factor affecting the baseline values.
Finally, the relationship between the shear bond strength values recorded and the mode of failure obtained regardless of the storage period was tested. This study showed that cohesive mode of failure was accompanied by the highest shear bond strength (8.444 ± 4.039), followed by mixed mode of failure (7.797 ± 4.506) and adhesive mode of failure (5.380 ± 2.928).
Scanning electron microscope
Images were obtained to confirm and explain the current results.
| Discussion|| |
Several desensitizers have been used to provide desensitization of the postoperative hypersensitive teeth ,.
The tested desensitizers were chosen in this study according to Salz and Bock , who reported that the most common approaches to reduce permeability and sensitivity of exposed dentin are precipitate-forming agents such as potassium oxalate and protein coagulants such as glutaraldehyde, chlorhexidine, and fluoride.
Desensitizers were found to affect bond strength of restorative materials to the tooth. Thus, some studies reported that the type of desensitizer used may impact the bond strength to dentin .
Thus, the aim of the current study was to evaluate the effect of different desensitizing agents [a potassium oxalate desensitizer solution (D/Sense Crystal) and a glutaraldehyde desensitizing adhesive system] on the shear bond strength of composite resin bonded to dentin surface in vitro.
In this in-vitro study, extracted molars were used as it was stated that a reliable bonding is influenced by many variables, such as the tooth structure and morphology, contamination, or temporization. Thus, it is preferable to conduct in-vitro studies to avoid some of these factors, which related to in-vivo studies ,.
To simulate one of the most important clinical factors, in this study, all specimens were stored in distilled water for two periods of storage time (24 h and 6 months) and thermocycled as recommended for quality testing of adhesive materials according to the International Organization for Standardization in 1993 .
In the current study, group IA recorded the highest shear bond strength values. This was explained by Cavalcanti et al. , who found that removal of the smear layer and opening of the dentinal tubules by means of complete acid etching allow free diffusion of the adhesive agents and may contribute to the bond effectiveness of etch-and-rinse adhesive systems. This mechanism, added to the characteristics of the simplified etch-and-rinse adhesive used in this study, may justify its higher bond strength under both experimental conditions. In addition, the Adper Single Bond 2 adhesive system has 10% of filler nanoparticles by weight in its composition. It was found that the presence of these fillers may be important to strengthen the adhesive layer and to guarantee an adequate thickness over the hybrid layer, protecting it against stresses, which can be confirmed by SEM images ([Figure 1]). In addition, group IIA recorded the least shear bond strength value.
|Figure 1: Scanning electron microscope image of the resin–dentin interface from group IA (Adper Single Bond 2+composite, after 24 h of water storage) showing a continuous hybrid layer and long resin tags.|
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This was explained by Perdigão , who found that the effect of some dentin desensitizers provide blocking of dentinal tubules and blocking tubular fluid, which deteriorates the bonding for some current adhesives.
The current finding about group II is in agreement with those of others ,,,, who found that acid etching procedure before application of oxalate desensitizer removed the smear layer and depleted the crystals of calcium oxalate from the dentin surface, allowing the formation of a hybrid layer. In contrast, the deposition of calcium oxalate crystals on the dentinal surface could neutralize the etching procedures and consequently might inhibit the formation of a sufficient hybrid layer, interfering with the subsequent bonding procedure, leading to lower bond strength, and contributing to gaps at the bonded interface in the areas of stress.
This was confirmed by Christensen and colleagues ,,,,,,, who found that application of oxalate desensitizers blocked or covered the dentinal tubules and reduced bond strengths significantly, as shown in the current SEM image ([Figure 2]).
|Figure 2: Scanning electron microscope image of resin–dentin interface from group IIA (oxalate desensitizer application followed by Adper Single Bond 2+composite, after 24 h of water storage) showing the presence of gap formation at the dentin–adhesive interface with short resin tags and some oxalate crystals blocking some dentinal tubules.|
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This might be attributed to the presence of monohydrogen monopotassium oxalate in this desensitizer, which might have been precipitated and caused blockage of dentinal tubules, thus affecting the bond strength of dentin bonding agents .
In contrast, these results are in disagreement with those of Tay et al.  and others ,,, who have evaluated the effect of oxalate desensitizers on bond strength of etch-and-rinse adhesives to dentin and reported that it did not compromise the early bond strength of relatively neutral adhesives (such as Single Bond or One Step). They explained their finding as follows: when dentin is etched, calcium ions are depleted from the smear layer and underlying dentin. Therefore, the oxalate ions diffused further down the dentinal tubules until calcium ions were available for reaction to form calcium oxalate crystals. Reduction of dentin permeability was thus achieved through subsurface tubular occlusion, which should not be interfered with subsequent resin infiltration. Therefore, the shear bond strength of adhesive system used should not record any difference compared with dentin surfaces treated with oxalate desensitizing agents.
In the current study, group IIIA showed shear bond strength values higher than that in group IIA, which was explained by SEM images ([Figure 3]) showing some opened dentinal tubules and some remnants of oxalate crystals blocking some dentinal tubules.
|Figure 3: Scanning electron microscope image of resin–dentin interface from group IIIA (oxalate desensitizer application then re-etching then Adper Single Bond 2+composite, after 24 h of water storage) showing gap formation, short resin tags, and some dentinal tubules blocked with oxalate crystals and others opened after re-etching without resin tag penetration.|
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In the current study, group III results were comparable to those found by Yousry , who also found that re-etching after oxalate treatment compromises the bonding of single-bottle etch-and-rinse adhesives to dentin. It was found that D/Sense Crystal, which is a highly acidic desensitizer (pH<1) was probably able to liberate more calcium from dentin to form both subsurface and surface crystals of insoluble calcium oxalate inclusions that remained on the dentin surface and limit the length of resin tags, but do not interfere with bonding effectiveness. The presence of surface inclusions may interfere with resin infiltration into the demineralized intertubular dentin and impedes proper hybridization. However, after phosphoric acid re-etching, these surface oxalate crystals were not totally removed from dentin surface, obscuring most dentinal tubules. Thus, application of a resinous adhesive system in the presence of these oxalate crystals in the current tested groups II and III complicated the bonding process by the formation of an oxalate–hybrid complex layer. Moreover, the presence of these subsurface inclusions at the bonded interface could cause debonding at lower forces, due to stress concentration at these areas.
Therefore, some authors , concluded that the second re-etch does not affect the dentinal subsurface oxalate crystals. They found that there was no real advantage of re-etching. SEM observation of subsurface oxalate crystals in a fractured specimen after re-etching revealed fewer and smaller oxalate crystals in dentinal tubules. Thus, overetching might further accelerate hydrolytic degradation of the resin–dentin bond due to incomplete resin infiltration and probable activation of matrix metalloproteinase enzymes, which can negatively affect the bond strength ,.
As regards subgroup B, in the current findings, the storage time had a significant role in the reduction of bond strength in groups I, II, and III. These may be explained by the current SEM images ([Figure 4],[Figure 5],[Figure 6], respectively).
|Figure 4: Scanning electron microscope image of the resin–dentin interface from group IB (Adper Single Bond 2+composite, after 6 months of water storage) showing discontinuity of hybrid layer, in addition to the presence of long resin tags but it was torn and became detached from the hybrid layer and its dentinal tubules than that of group IA due to the effect of hydrolytic degradation of long period of water storage.|
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|Figure 5: Scanning electron microscope image of resin–dentin interface from group IIB (oxalate desensitizer application followed by Adper Single Bond 2+composite, after 6 months of water storage) showing increased gap size at the dentin–adhesive interface, remnants of short resin tags, and some oxalate crystals blocking some dentinal tubules.|
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|Figure 6: Scanning electron microscope image of resin–dentin interface from group IIIB (oxalate desensitizer application followed by re-etching and Adper Single Bond 2+composite application, after 6 months of water storage) showing discontinuous hybrid layer, short resin tags torn due to the effect of water storage, and some dentinal tubules blocked with oxalate crystals and others opened after re-etching with phosphoric acid.|
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These results are in agreement with those of others ,,,,,,,, who reported a significant decrease in bond strengths, even after relatively short storage periods, which might be attributed to degradation of interface components by hydrolysis (mainly resin and/or collagen), wherein water can also infiltrate and negatively affect the mechanical properties of the polymer matrix, by swelling and reducing the frictional forces between the polymer chains, a process known as 'plasticization'. Hydrolysis might result from degradation of resin or tooth structure collagen. It has been reported that the hydrolytic degradation of the bond can influence the bonding efficacy (bond strength and marginal seal) of the bond in the long run ,,. Decreased bond strength and increased microleakage result in tooth hypersensitivity and pulp irritation ,.
As regards group IV in the current study, the shear bond strength mean values of subgroup B showed a relatively nonsignificant decrease compared with subgroup A. This result might be explained and clarified with SEM images ([Figure 7]) showing discontinuous hybrid layer, gap formation, numerous resin tags, and some opened dentinal tubules. In addition, SEM image of resin/dentin interface from group IVB showed discontinuous hybrid layer, increasing gap formation, numerous deteriorated resin tags, and some opened dentinal tubules not infiltrated by resins ([Figure 8]).
|Figure 7: Scanning electron microscope image of resin–dentin interface from group IVA (I-Bond desensitizing adhesive system+composite, after 24 h of water storage) showing discontinuous hybrid layer, gap formation, and numerous long resin tags.|
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|Figure 8: Scanning electron microscope image of resin–dentin interface of sample from group IVB (I-Bond desensitizing adhesive system+composite, after 6 months of water storage) showing discontinuous hybrid layer, increasing gap formation, numerous deteriorated resin tags, and some opened dentinal tubules not infiltrated by resins.|
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However, the shear bond strength of group IV was still high after storage, which was explained by van Meerbeek et al. ,,, who stated that, for etch-and-rinse adhesives, the mechanisms of adhesion are mainly micromechanical because the phosphoric acid is a very strong acid (pH about 0.5). Phosphoric acid completely dissolves the mineral, and so the collagen fibers are totally exposed after etching. For the self-etch adhesives, the adhesion to the dentin is both micromechanical and chemical as in I-Bond adhesive system. The self-etch monomers are often less acidic than phosphoric acid and then some minerals (hydroxyapatite) remain attached to the collagen fibers, which may serve as a receptor for additional intermolecular interaction with specific monomers of the mild self-etch adhesive, permitting chemical links between dental substrate and functional groups of the adhesive monomers.
The current results revealed that group I using etch-and-rinse adhesive recorded a higher bond strength compared with group IV using self-etch desensitizing adhesive agent. This was explained by Joseph et al. , who reported that one-step self-etch adhesive systems generally have less cross-linking monomers. These cross-linking monomers provide most of the mechanical strength; therefore, there is a potential for lower bond strength as shown by seventh-generation bonding agent (I-Bond).
This could be explained by Senawongse et al.  and Sattabanasuk et al. , who reported that mild self-etch systems (pH≤2) are able to partially remove the smear layer and penetrate the dentinal surface, creating a less pronounced resin tag formation and hybrid layers that are thinner than those of total-etch systems.
Moreover, the presence of a glutaraldehyde desensitizing agent (included in I-Bond adhesive system) may negatively affect shear bond strength of composite to dentin surface. It was found that, after topical application of glutaraldehyde to the dentin surface, multiple transverse septa occurred in the lumen of the dentinal tubules down to a depth of 200 µm, effectively creating a barrier that eliminates the hydrodynamic mechanism of dentin hypersensitivity and can hinder adhesive infiltration ,,,,.
These findings were confirmed byAbdel-Hafez et al. , who found that Gluma desensitizing agent produced lower microshear bond strength for Solobond M and XP Bond (two-step etch and rinse) and Solobond Plus and ProBond (three-step etch and rinse). They explained that these findings may be due to blockage of dentinal tubules by the precipitate on the dentin surfaces caused by reaction between glutaraldehyde in Gluma and proteins in dentin. This precipitate may hinder adhesive infiltration and hybridization of demineralized dentin. In addition, this precipitate may also contribute to stress raiser areas that would create deboning at lower stresses.
These findings are in disagreement with previous studies by others ,,,,,,, who concluded that 'the application of selective collagen cross-linkers during adhesive restorative procedures may be a new approach to improve dentin bond strength properties' and showed that the chemical modification to the dentin matrix promoted by glutaraldehyde increased bond strengths using two types of the fifth-generation bonding agents.
| Conclusion|| |
Under the present situation of this research, the following were recorded:
- Applying a desensitizer or an adhesive system containing desensitizing agent negatively affected shear bond strength of composite resins
- Although aging (thermocycling and water storage) was a factor negatively influencing the shear bond strength of groups I, II, and III), desensitizing adhesive system (group IV) resisted the hydrolytic degradation by water.
Financial support and sponsorship
Conflicts of interest
There are no conflicts of interest.
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[Figure 1], [Figure 2], [Figure 3], [Figure 4], [Figure 5], [Figure 6], [Figure 7], [Figure 8]
[Table 1], [Table 2], [Table 3], [Table 4], [Table 5]