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Article

The Various Silane Agents in Universal Adhesives on Repair Strength of Resin Composite to Resin Composite

by
Seelassaya Leelaponglit
1,2,
Apichai Maneenacarith
1,
Tuksadon Wutikhun
3 and
Awiruth Klaisiri
1,2,*
1
Division of Restorative Dentistry, Faculty of Dentistry, Thammasat University, Pathum Thani 12120, Thailand
2
Thammasat University Research Unit in Restorative and Esthetic Dentistry, Thammasat University, Pathum Thani 12120, Thailand
3
National Nanotechnology Center, National Science and Technology Development Agency, Pathum Thani 12120, Thailand
*
Author to whom correspondence should be addressed.
J. Compos. Sci. 2023, 7(1), 7; https://doi.org/10.3390/jcs7010007
Submission received: 3 December 2022 / Revised: 17 December 2022 / Accepted: 19 December 2022 / Published: 3 January 2023
(This article belongs to the Section Biocomposites)
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Abstract

:
The aim of this investigation was to examine the bonding efficacy of a universal adhesive containing various silane agents to repair aged resin composite with new resin composite. Ninety resin composite specimens were created with nanofilled resin composite and aged for 5000 cycles in a thermocycler. The specimens were sorted into nine groups (n = 10) at random based on the methods used to treat the surfaces with/without silane agent (Si), and adhesive agents (Single bond universal, SU; Single bond universal plus, SUP; Clearfil Tri-S bond universal, CFU; and Single bond 2, SB2). A template was placed on the treated surface of the aged resin composite, and then the resin composite was filled into the template. The shear bond strength (SBS) test was conducted using a universal tester and failure patterns were determined. The statistical analysis was performed using a one-way ANOVA and a Tukey’s test. The lowest SBS values were exhibited in the no surface treatment group (7.69 ± 2.57 MPa). The highest SBS values were exhibited in Si + SUP group (28.04 ± 1.62 MPa), with a significant difference compared to SUP group (22.69 ± 2.21 MPa), Si + SU group (22.08 ± 1.83 MPa), Si + CFU group (21.98 ± 1.54 MPa), and Si + SB2 group (21.85 ± 2.18 MPa). The experimental group demonstrated a predominance of adhesive failure at the junctions between the aged resin composite and the new resin composite. In conclusion, The SUP, which incorporates 3-(aminopropyl)triethoxysilane (APTES) and 3-methacryloxypropyltriethoxysilane (3-MPTES), has a positive effect on the repaired shear bond strength of resin composite to resin composite both with and without the use of a silane agent prior to the use of the SUP when compared with a conventional adhesive agent (SB2) and other universal adhesives (SU and CFU). Moreover, an additional silane agent used prior to the SUP application has the highest shear bond strength.

1. Introduction

The practical practice of restorative dentistry now includes resin composite restorations on a frequent basis. Resin composite materials are widely chosen due to their great esthetics, tooth structure conservation, ability to adhere to teeth, and ability to reinforce repaired tooth structure [1]. Even though resin composites’ qualities have evolved, failure can still happen for a number of reasons, including restoration fracture, marginal leakage, secondary caries, discoloration, and wear [2,3,4].
According to Opdam et al., posterior resin composite restorations had a decent survival record, with yearly failure rates at 5 years and 10 years of service being 1.8% and 2.4%, respectively [4]. The repair of resin composites is a conservative technique that begins with the preparation of the damaged portion of the restoration and ends with the restoration of the prepared defect. Restoration repair is an effective approach to raising the quality of restorations and is widely accepted [5]. For a successful repair, choosing the appropriate adhesive technique, restorative substance, and surface preparation of the aged composite resin are all key [6,7,8]. According to several studies, repaired resin composite restorations last as long as or even longer than replacements [9,10]. The clinical method for repair of resin composite involved treating the damaged resin composite surface or any exposed tooth structure with abrasion or a diamond bur, acid etching, silane agent application, an appropriate adhesive system application, and resin composite placement [11,12].
Universal adhesives are the most current advancements in adhesive restorative materials. They were created to simplify the clinical process for direct and indirect adhesive restorations. Universal adhesives are all-in-one self-etching systems that are additionally suggested for use in two-step total etching adhesives or selective enamel etching when phosphoric acid is utilized to treat enamel and/or dentin [13]. The composition of phosphate and/or carboxylate functional monomers and/or silane agents in universal adhesives is the main difference between them and conventional all-in-one self-etch systems. A variety of these functional monomers can chemically bond with tooth structure and restorations [14,15,16,17]. However, some silane agents in universal adhesives are unstable in acidic solutions [16].
The purpose of this study was to test the bonding efficacy of a universal adhesive containing various silane agents to repair aged resin composite with new resin composite. The null hypothesis was that the universal adhesive containing various silane agents has no impact on the repaired shear bond efficacy of aged resin composite and new resin composite.

2. Materials and Methods

Table 1 demonstrates the materials employed in the research.

2.1. Aged Resin Composite Preparation

Ninety Filtex Z350 XT resin composite block specimens in shade A4B (3M ESPE, St. Paul, MN, USA) were made by pushing Filtex Z350 XT resin composite into a clear silicone template (6 mm in diameter and 2 mm in thickness). A transparent strip was put on the top of the specimen for a flat surface. A light-emitting diode (LED) curing device (MiniLED, Acteon, Merignac, France) was applied for 40 s to cured resin composite specimens. A specimen was taken out of the clear silicone mold. In order to simulate an old resin composite, the specimens were aged 5000 times at 5 °C and 55 °C with a dwell time of 5 s in water by a thermocycler device (Proto-tech, Microforce, Portland, OR, USA) [7].
The old resin composite samples were inserted in the poly(vinylchloride) pipe, with resin acrylic in the center. The surfaces of the samples were polished while wet using 320- and 600-grit silicon carbide abrasive sheets (RS Component, Bangkok, Thailand). After being cleaned with an ultrasonic cleaner for ten minutes in distilled water, the old resin composite specimen was dried with triple syringe air syringes for ten s.

2.2. Surface Treatment Procedures

2.2.1. Phosphoric Acid Treatment

All specimen surfaces were treated with an etching gel containing phosphoric acid for 15 s (37% phosphoric acid, Pentron, Ornage, CA, USA), and then carefully dried by air drying after thorough water cleaning.

2.2.2. Silane Agent Treatment

A disposable microbrush applicator (Kerr Corporation, Orange, CA, USA) was used to treat the silane agent (RelyX ceramic primer (Si), 3M ESPE, Minnesota, USA) to the aged resin composite surface. After one minute, it was air dried with triple syringes until no silane agent movement was detected or it was completely dry.

2.2.3. Adhesive Agent Treatment

The adhesive agents [(i) Single bond universal (SU), 3M, Neuss, Germany; (ii) Single bond universal plus (SUP), 3M, Neuss, Germany; (iii) Clearfil Tri-S bond universal (CFU), Kuraray Noritake Dental Inc., Okayama, Japan; and (iv) Single bond 2 (SB2), 3M ESPE, St. Paul, MN, USA] were utilized in this research. The adhesive agent was coated onto the aged resin composite surface using a microbrush and an agitated application technique. The adhesive agent was air dried with a triple syringe until no apparent movement was seen, and it was then light-cured for 20 s.
The specimens were sorted into 9 groups (n = 10/group) at random based on the methods used to treat the surfaces with/without silane agent, and adhesive agents, along these lines;
Group 1: no surface treatment with the silane agent and the adhesive agent
Group 2: SU
Group 3: SUP
Group 4: CFU
Group 5: SB2
Group 6: Si + SU
Group 7: Si + SUP
Group 8: Si + CFU
Group 9: Si + SB2

2.3. Bond Specimen Procedures

The ultradent template with 2 mm of height and 2 mm of diameter (Ultradent product, South Jordan, UT, USA) was put in the aged resin composite surface center. The Filtex Z350 XT resin composite in shade A3B was packed into the ultradent template using a plastic instrument, and then irradiated by a LED curing device for 40 s to cure it. After removing the ultradent mold, the area was again exposed to a LED curing device for 40 s. All samples were maintained in distilled water at 37 °C for 1 day.

2.4. Shear Bond Strength (SBS) and Failure Mode Inspection

According to SBS, the specimens were attached to the mechanic’s universal tester (EZ-S 500N, Shimadzu Corporation, Kyoto, Japan) using a notched-edge shearing blade. The bonding region was in close proximity to the shearing blade. A crosshead speed was set to 1.0 mm per minute during the bond strength test. The SBS value is determined in terms of megapascals (MPa).
All de-bonded specimens were inspected using ×40 magnification of a stereomicroscope-ML9300 (Meiji Techno Co., Ltd., Saitama, Japan) to analyze the fracture pattern, which was categorized into 3 groups: (i) adhesive failure in aged and new resin composite interfaces, (ii) cohesive failure in aged or new resin composites, and (iii) mixed failure, which is a mixture of cohesive and adhesive failure [7,8].
The representative fractured specimens were evaluated using a scanning electron microscope-Versa 3D (SEM, FEI company, Eugene, OR, USA) at ×250 magnification to analyze fractured surfaces.

2.5. Statistical Analysis

The SBS values were computed using SPSS 23.0 (SPSS Inc., Chicago, IL, USA) to determine the data. A one-way ANOVA was employed to determine the effect of universal adhesive containing various silane agents on the repair bond efficacy of old and fresh resin composites in SBS values, and post-hoc with a Tukey’s test to determine pairwise comparisons. In all test groups, the confidence level and p-values were set to 95% and 0.05, respectively.

3. Results

3.1. SBS Values

In this investigation, the SBS values of the repaired samples are detailed in Table 2. The experimental groups demonstrated significant differences in one-way ANOVA (p < 0.05). The lowest SBS values were exhibited in the no surface treatment group (7.69 ± 2.57 MPa). Between groups 2, 4, and 5, there was no significant difference (p > 0.05). On the other hand, the highest SBS values were exhibited in group 7 (28.04 ± 1.62 MPa), with a significant difference compared to group 3 (22.69 ± 2.21 MPa), group 6 (22.08 ± 1.83 MPa), group 8 (21.98 ± 1.54 MPa), and group 9 (21.85 ± 2.18 MPa) (p < 0.05).

3.2. Analysis of Failure Pattern and SEM Surface Fractured

Table 2 presents the outcomes of the mode of failure observations. With higher SBS, there was a trend for mixed type fracture percentages to increase. Group 7, which had the highest portion of mixed failure modes (30% mixed failure), displayed the highest SBS values (28.04 ± 1.62 MPa). Figure 1 and Figure 2 demonstrate examples of SEM pictures of adhesive and mixed failure patterns.

4. Discussion

The investigation aims to determine the bonding efficacy of a universal adhesive containing various silane agents to repair old resin composites with fresh resin composites. In this in vitro investigation, it was discovered that the effectiveness of the repair bond between an aged resin composite and a new resin composite was affected by a universal adhesive that contained different silane agents. Group 3 has a higher SBS significant difference than groups 2 and 4. Furthermore, the highest significant SBS is obtained when SUP is combined with a silane agent prior to the adhesive agent. As a result, the investigation’s hypothesis was denied.
Three potential processes might be used to attach new resin composites to old resin composites during the repair of resin composites [8]; (i) micromechanical retention to the aged resin composite surface, (ii) chemical adhesion of the fresh resin matrix with the uncured carbon double bonds of the aged resin composite via copolymerization, and (iii) chemical adhesion with the exposed aged resin composite filler particles by applying silane agents. The resin composite repair protocol is built on the principles of micromechanical surface treatment [18]. Thus, the clinicians should make an effort to enhance the pre-existing restoration’s surface area before beginning the repair process. According to Klaisiri et al., the aged resin composite’s micromechanical characteristics were created using 320- and 600-grit abrasive sheets [7]. In the current study, resin composite surfaces were micromechanically refined with 320- and 600-grit abrasive sheets before adhesive preparation. Previous studies showed that mechanical preparation of the resin composite surface increases surface micro-roughness and strengthens the bonding to the resin composite repair [19,20,21].
The adhesive ability between the material and the repair resin composite may be strengthened by silanization before the use of an adhesive system [6,22]. Silane agents have the potential to form covalent connections with exposed fillers and improve the resin composite surface’s wettability, which facilitates better penetration of the adhesive employed for the repair and restoration [23]. The resin composite Z350 XT consists of zirconia, silica, and ceramic that has been silane-treated. According to reports, adding silane-treated fillers to the matrix of a resin composite enhances the material’s mechanical and physical characteristics, including its mechanical properties and hydrolytic durability [24]. This might affect how the surface is treated during repair [25]. The clinical procedure for repairing aged resin composites involved mechanically treating the composites’ surfaces with a silane agent and an appropriate adhesive system, and then applying the resin composite afterwards [11,12].
In the previous investigation, bonding with the silica base materials was negatively affected by the universal adhesive’s 3-methacryloxypropyltrimethoxysilane (3-MPTS) component [16,25]. The 3-MPTS is unstable in the universal adhesive’s aqueous acidic condition, and separate silanization is advised when using a universal adhesive that contains 3-MPTS [16]. However, the manufacturer does not disclose the quantity of silane agent in its formulation, and it could not be enough to enhance the repair bond [25]. According to Michelotti et al., the investigated universal adhesive’s bonding strength between resin composites does not improve when a silane agent is used before, regardless of the mechanical roughening technique [21]. In this research, the repair SBS of groups 2 and 4 were not significantly different compared to group 5. The SU and CFU are composed of 3-MPTS, which have no influence on the repaired shear bond ability of aged resin composites to new resin composites when compared to conventional adhesive agents. Dehydration-induced self-condensation of functional silanols in SU and CFU as a result of 3-MPTS molecular instability in an aqueous acidic condition may be the cause of the weaker bonding performance of SU and CFU [26,27]. Additionally, our findings also supported a recent study [16,21,28] that found the bonding effectiveness was greatly improved when a silane agent was added before the adhesive agent. In this study, the SBS of adhesive or universal adhesive treated with separate prior silanization still functioned significantly greater than when adhesive or universal adhesive was not treated with a silane agent.
In our study, the SUP incorporates the functional monomer 3-(aminopropyl)triethoxysilane (APTES) as well as 3-methacryloxypropyltriethoxysilane (3-MPTES), which features a vinyl group that may be polymerized. The SBS performance of SUP bonded to the aged resin composite and treated without a silane agent showed no significant difference compared to silanization prior to treating the universal adhesives in groups 6 and 8. Moreover, the use of a silane agent before the SUP application has a significantly higher SBS. The possible explanations of SUP to resin composite repair may have three mechanisms; (i) APTES is a bifunctional silane, allowing its silanol end to react with silane-treated silica filler in aged resin composites, while the amino component may assist in stabilizing the hydrolyzed silanols at the aged resin composite surface. (ii) 3-MPTES gives a vinyl group to interact with the new resin composite. Additionally, 3-MPTES hydrolyzed relatively slowly compared to 3-MPTS, which reduced potential dehydration self-condensation. Finally, (iii) it may have a high elastic modulus, flexural strength, and polymerization conversion [16]. For these mechanisms, group 3 has a higher SBS significant difference than groups 2 and 4. Moreover, SUP, applied with a separate silane agent prior to the adhesive agent, has the highest significant SBS.
As the fractured mode, the experimental group demonstrated a predominance of adhesive failure at the junctions between the old resin composite and the fresh resin composite (group 1, 100%; group 2, 100%; group 3, 80%; group 4, 100%; group 5, 100%; group 6, 80%; group 7, 70%; group 8, 80%; and group 9, 80%), which is completely consistent with prior reports where adhesive breakdowns were frequently linked to weak bonds [7,16]. In groups 3, 6, 7, 8, and 9, mixed failure modes (group 3, 20%; group 6, 20%; group 7, 30%; group 8, 20%; and group 9, 20%) were commonly correlated with high SBS (group 3, 22.69 ± 2.21 MPa; group 6, 22.08 ± 1.83 MPa; group 7, 28.04 ± 1.62 MPa; group 8, 21.98 ± 1.54 MPa; and group 9, 21.85 ± 2.18 MPa). This investigation has no cohesive failure mode.
The design of this research was focused on the application of three universal adhesives and one conventional adhesive; therefore, it was not applicable to other universal and conventional adhesives, which was a limitation. Future studies on the longevity and bond stability of repaired resin composites should consider more universal and conventional adhesives, as well as long-term mimicked oral cavity environments. The clinical success of an adhesion procedure is influenced by a number of parameters, not only the bond strength. The findings of our investigation must thus be carefully interpreted.

5. Conclusions

Within the limitations of our results, the universal adhesives containing 3-MPTS have not enhanced the repaired shear bond ability of resin composites when compared with conventional adhesive agents. However, an additional silane agent used prior to the use of universal adhesives containing 3-MPTS has enhanced shear bond strength. In addition, the universal adhesive containing 3-MPTES and APTES has a positive effect on the repaired shear bond ability of resin composite to resin composite both with and without the use of a silane agent prior to the universal adhesive application. Moreover, an additional silane agent used prior to the universal adhesive containing 3-MPTES and APTES application has the highest repaired shear bond ability.

Author Contributions

S.L., A.M. and A.K. conceived and designed the study; S.L., T.W. and A.K. performed the experiments and interpreted the results; S.L., A.M. and A.K drafted the manuscript; S.L., A.M., T.W. and A.K. revised the manuscript. All authors have read and agreed to the published version of the manuscript.

Funding

This research was supported by the Thammasat University Research Unit in Restorative and Esthetic Dentistry, Thammasat University, Thailand.

Institutional Review Board Statement

Not applicable.

Informed Consent Statement

Not applicable.

Data Availability Statement

Not applicable.

Conflicts of Interest

The authors declare no conflict of interest.

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Jcs 07 00007 g001 550
Figure 1. SEM pictures of adhesive failure pattern: (A) group 1; (B) group 2; (C) group 4; and (D) group 5.
Figure 1. SEM pictures of adhesive failure pattern: (A) group 1; (B) group 2; (C) group 4; and (D) group 5.
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Figure 2. SEM pictures of mixed failure pattern: (A) group 3; (B) group 6; (C) group 7; (D) group 8; and (E) group 9.
Figure 2. SEM pictures of mixed failure pattern: (A) group 3; (B) group 6; (C) group 7; (D) group 8; and (E) group 9.
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Table
Table 1. Materials used in the research.
Table 1. Materials used in the research.
MaterialsMain Compositions
RelyX ceramic primer (3M ESPE, Minnesota, USA)
Lot: N988623		Ethanol, water, methacryloxypropyltrimethoxysilane
Single bond 2 (3M ESPE, Minnesota, USA)
Lot: NE92635		Bis-GMA, HEMA, DMA, methacrylate functional copolymer, filler, photoinitiators, ethanol, water
Singlebond universal (3M, Neuss, Germany)
Lot: 483316		10-MDP, Bis-GMA, HEMA, DMA, methacrylate functional copolymer, silane, filler, initiators, ethanol, water
Scotchbond universal plus (3M, Neuss, Germany)
Lot: 8321974		HEMA, 2-propenoic acid, 2-methyl-, diesters with 4,6-dibromo-1,3-benzenediol 2-(2-hydroxyethoxy)ethyl 3-hydroxypropyl diethers, 2-propenoic acid, 2-methyl-, reaction products with 1,10-decanediol and phosphorus oxide, 2-propenoic acid, 2-methyl-, 3(triethoxysilyl)propyl
ester, reaction products with silica and 3(triethoxysilyl)-1-propanamine, synthetic amorphous silica, fumed, crystalline-free, ethanol, water, (3-aminopropyl)triethoxysilane, camphorquinone, N,N-dimethylbenzocaine, methacrylic acid, Acetic acid, copper(2+) salt, monohydrate
Clearfil Tri-S bond universal (Kuraray Noritake Dental Inc., Okayama, Japan)
Lot: 4K0025		10-MDP, Bis-GMA, HEMA, colloidal silica, ethanol, silane, sodium fluoride, camphoquinone, ethanol, water
Resin composite (Filtex Z350 XT (A3B, A4B), 3M ESPE, Minnesota, USA)
Lot: NA77397, NF40326		Silane treated ceramic, silane treated silica, silane treated zirconia, Bis-EMA-6, Bis-GMA, UDMA, PEGDMA and TEGDMA
Abbreviations: Bis-GMA, bisphenol A-glycidyl methacrylate; HEMA, 2-hydroxyethyl methacrylate; DMA, dimethacrylate; 10-MDP, 10-methacryloyloxydecyl dihydrogen phosphate; UDMA, urethane dimethacrylate; Bis-EMA-6, bisphenol A polyethylene glycol diether dimethacrylate; PEGDMA, polyethylene glycol dimethacrylate; TEGDMA, triethylene glycol dimethacrylate.
Table
Table 2. The SBS’s means and standard deviation (MPa) and percentage of failure pattern.
Table 2. The SBS’s means and standard deviation (MPa) and percentage of failure pattern.
GroupMean SBS ± SD Failure Pattern
AdhesiveMixedCohesive
1. No surface treatment7.69 ± 2.57 a10000
2. SU14.63 ± 2.05 b10000
3. SUP22.69 ± 2.21 c80200
4. CFU15.01 ± 3.07 b10000
5. SB214.59 ± 2.17 b10000
6. Si + SU22.08 ± 1.83 c80200
7. Si + SUP28.04 ± 1.62 d70300
8. Si + CFU21.98 ± 1.54 c80200
9. Si + SB221.85 ± 2.18 c80200
The value with identical letters indicates no statistically significant difference.
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MDPI and ACS Style

Leelaponglit, S.; Maneenacarith, A.; Wutikhun, T.; Klaisiri, A. The Various Silane Agents in Universal Adhesives on Repair Strength of Resin Composite to Resin Composite. J. Compos. Sci. 2023, 7, 7. https://doi.org/10.3390/jcs7010007

AMA Style

Leelaponglit S, Maneenacarith A, Wutikhun T, Klaisiri A. The Various Silane Agents in Universal Adhesives on Repair Strength of Resin Composite to Resin Composite. Journal of Composites Science. 2023; 7(1):7. https://doi.org/10.3390/jcs7010007

Chicago/Turabian Style

Leelaponglit, Seelassaya, Apichai Maneenacarith, Tuksadon Wutikhun, and Awiruth Klaisiri. 2023. "The Various Silane Agents in Universal Adhesives on Repair Strength of Resin Composite to Resin Composite" Journal of Composites Science 7, no. 1: 7. https://doi.org/10.3390/jcs7010007

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