effects of pretreatment procedures on shear bond strength

2092014年 6月

Effects of Pretreatment Procedures on Shear Bond Strength in Repair of Composite Resin Restorations

KOBAYASHI Mikihiro, FUJISHIMA Akihiro＊ and MANABE Atsufumi

Department of Conservative Dentistry, Division of Aesthetic Dentistry and Clinical Cariology,Showa University School of Dentistry

＊Department of Conservative Dentistry, Division of Oral Biomaterials and Engineering, Showa University School of Dentistry

Abstract　Purpose: We examined the effects on composite resin filling repair of differences in pretreatment condi-tions（e.　g., primer treatment）and the surface roughness of the adhesive surface.　Methods: Two types of resin, namely, Clearfil AP-X（AP）and Beautifil Flow F02（BE）, which differed in composition and fluidity, were compared under various pretreatment conditions（no treatment, bonding treat-ment（Clearfil Photo Bond）, silane coupling treatment（Clearfil Photo Bond and Clearfil Porcelain Bond mixture））for different adhesive surfaces（pressure-contact surface or diamond-point ground surface）. Filling was performed with the same resin material as the adhesive surface, and the shear bond strength was com-pared after the resins were stored for 1 week in water.　Results: When comparing between the adhesive surface types, a significant difference in shear bond strength was observed for only BE with bonding treatment, and no significant differences were observed for the other BE cases or any of the AP cases. When comparing between the adhesion treatments, the bonding treatment group and the silane coupling group for AP with the pressure-contact surface exhibited a signifi-cant difference in shear bond strength compared with the no-treatment group. In the case of BE, significant differences were observed in the case of the diamond-point ground surface and silane coupling processing. On the pressure-contact surface, a significant difference was observed only between no treatment and silane coupling treatment.　Conclusion: The effective method for treating the adhesive surface differs depending on the composite resin, and it is necessary to perform the surface treatment that is optimal for the composite resin to be applied. Good fluidity of the component resin is effective for ensuring good adhesive properties.

Key words: silane coupling, filling repair, composite resin, bonding material

　Corresponding author: Dr. KOBAYASHI, Department of Conservative Dentistry, Division of Aesthetic Dentistry and Clinical Cariology, Showa University School of Dentistry, 2‒1‒1, Kitasenzoku, Ohta-ku, Tokyo 145‒8515, Japan　TEL: ＋81‒3‒3787‒1151, FAX: ＋81‒3‒3787‒1229, E-mail: [email protected]　Received for Publication: February 7, 2014/Accepted for Publication: February 20, 2014　DOI: 10.11471/shikahozon.57.209

日歯保存誌 57（3）：209～218，2014

210 日　本　歯　科　保　存　学　雑　誌第 57巻　第 3号

Introduction

　As a result of the development and improvement of materials used in composite resin restoration, it has become possible to restore teeth to their previous state simply by removing the decayed area, without needing to drill out a significant amount of healthy tooth for the sake of convenience, leading to the establishment of the minimal intervention concept1）. Furthermore, there have been reports on improvements in cavity compati-bility as a result of improved wear and abrasion resis-tance, better long-term color stability, and decreased polymerization shrinkage2‒4）. Also, the primary method of posterior restoration previously involved restoration using amalgams or metal inlays, but owing to the devel-opment of dental bonding systems, it is now possible to use composite resin repair materials in place of metallic restoration materials. There are many kinds of compos-ite resins, such as composite resin with various filler types, low-viscosity composite resin（flowable composite resin）, and composite resin of many different colors. Therefore, the appropriate composite resin can be selected for different situations, making it easier for the practitioner to perform aesthetic restoration. Even among flowable composite resins, there are many dif-ferent types of resin with different fluidities, filler con-figurations, and properties. Moreover, flowable compos-ite resins with improved properties that can be used in molar restoration have recently been developed and are expected to be used5,6）. It has thus become possible to use flowable composite resin as the plastic restoration material in cavity base restoration, in normal direct res-toration, and in the restoration of all types of teeth, from the front teeth to the molars. For these reasons, the frequency of using flowable composite resin is expected to increase in the future.　However, there are an increasing number of cases of patients undergoing repeated restorations due to prob-lems such as fractures, degradation, discoloration, or secondary caries after restoration using an old type of composite resin or after restoration of old composite resin7,8）. The conventional method of dealing with cases of comparatively small resin fractures, discoloration, or secondary caries, or with cases of local clinical issues, is to remove all of the composite resin in order to perform a new restoration. In contrast, based on the concept of

minimal intervention that was proposed by Federation Dental International in 2002, it is now possible to per-form filling repair using new composite resins9）, and the guidelines for dental caries issued by the Japanese Soci-ety of Conservative Dentistry clearly note the effective-ness of such repairs10）. The basic concept of filling repair is to conserve healthy tooth and to prevent a transient decrease in oral function, which should help to improve the quality of life of patients. However, the base material of composite resins is bisphenol A-glyc-idyl methacrylate（BisGMA）, which has a network structure11）, and therefore once the material has been polymerized, it cannot chemically bond to BisGMA. This is very unlike the behavior of straight-chain mono-mers with methyl methacrylate as a base which are used in dentures and false teeth12）. In ongoing research into the bonding of resin cement with ceramics or zir-conia, silane coupling agents, carboxylic acid monomers, and even phosphate ester monomers are expected to bond effectively to ceramics and zirconia13）. Therefore, to evaluate the possibility of clinical filling repair by bonding these monomers to unpolymerized BisGMA in comparison to polymerized BisGMA, the effects of dif-ferences in the surface roughness of adhesive surfaces and differences in pretreatment conditions（e.　g., primer treatment）on composite resin filling repair were com-pared and tested with respect to bond strength.

Materials and methods

1 ．Materials　Table　1 lists the types of light-cured composite resin, the bonding material used as the primer, and the silane coupling agents used in this research. Hybrid AP resin（Clearfil AP-X, Kuraray Noritake Dental）and flowable BE resin（Beautifil Flow F02, Shofu）were used as the light-cured composite resins.

2 ．Experimental methods 1 ）Preparation of deposited composite resin　Fig.　1 shows the method used to prepare the speci-mens. The composite resin was packed into a stainless steel mold（10×10×2 mm）containing square holes. After pressing with a glass plate via celluloid strips, a light irradiator（Dentcraft Curemaster, Yoshida；≥800 mW/cm2）was used to irradiate the material for 60 s in order to prepare the test specimens. The prepared test specimens were placed in an acrylic ring（6×2 mm）and

2112014年 6月 Composite Resin Repair Bond Strength

a self-curing resin（Palapress Vario, HeraeusKulzer）was injected into the ring in order to embed and fix the composite resin specimen. All the specimens were then stored in water at 37℃ for 1 week.　Two types of adhesive surface were prepared on the deposited composite resins: a smooth surface for use as the pressure-contact surface, and a diamond-point ground surface. A diamond point of the regular type（108R, Shofu）was attached to an air turbine, and 5 passes were made over the surface while irrigating the surface with the free hand to make the ground surface parallel to the sample adhesive surface in order to pre-pare the diamond-point ground surface. Seals with an inner diameter of 6 mm and a thickness of 20μm were affixed to the two adhesive surfaces with different roughnesses that were prepared in order to regulate the adhesive surface. Then, a polytetrafluoroethylene mold with an inner diameter of 7 mm was set on top of

the seal. Pretreatment was performed using various pretreatment conditions: no treatment, bonding treat-ment, and silane coupling treatment（bonding material: silane coupling agent mixture）. Composite resin of the same type as the adhesive surface was applied, and the material was irradiated from above for 60 s in order to prepare the adhesion test specimens. Table　2 shows the storage conditions for the adhesion test specimens. The specimens were stored in water at 37℃ for 1 week. Also, for the adhesive surface pretreatment groups, thermal cycle loading was applied to the bonding treat-ment and silane coupling treatment by immersing the specimens in 5℃ and 60℃ water for 30 s each, repeat-ing this cycle 20,000 times. Ten adhesion test specimens were prepared using each set of conditions, for a total of 200 test specimens. 2 ）Measurement of surface roughness　The surface roughness（arithmetic average rough-

Table　1　Study materials

Material（Code）

Components（Filler content wt％）

Bath No. Manufacturer

Clearfil AP‒X（AP）

BisGMA, TEGDMA, barium glass, microfiller, photoinitiator, others（85 wt％）

01404A Kuraray Noritake Dental

Beautifil Flow F02（BE）

BisGMA, TEGDMA, glass filler, photoinitiator, others（54.5 wt％）

071157 Shofu

Clearfil Photo BondBisGMA, HEMA, MDP, ethanol, photoinitiator, chemical polym-erization catalyst, others

00448A, B Kuraray Noritake Dental

Clearfil Porcelain Bond Activator

γ-MPS, methacrylate monomer, others

00254A Kuraray Noritake Dental

HEMA: hydroxyethylmethacrylate, MDP: methacryloyloxydecyl dihydrogen phosphate

Fig.　1　Methods for preparing the test specimens and performing the adhesion test　a: Resin adhesive surface, b: Resin was added after setting the polytetrafluoroethylene mold, c: Completed adhesion test specimen, d: Shear bond test（1.0 mm/min）

a b c d


ness［Ra］）of the two types of adhesive surface was measured using a surface texture measuring instru-ment（Surfcom 130A, Tokyo Seimitsu）, with measure-ments made at 10 locations in a direction perpendicular to the cutting streaks; the measurement length was 4.0 mm and the cutoff value was 0.8 mm. The average value was calculated as the surface roughness for each adhesive surface. 3 ）SEM observation of adhesive surface

　Samples were prepared using the same surface treat-ments, and after platinum deposition, the surfaces were observed by scanning electron microscopy（SEM; S-2360N, Hitachi）using an accelerating voltage of 25 kV. 4 ）Measurement of bond strength

　A universal testing machine（Type 1125, Instron）was used to perform shear bond testing on each sample using a cross-head speed of 1.0 mm/min. The shear bond strength was determined by dividing the breaking load by the adhesion area, and the mean value was cal-culated as the shear bond strength（n＝10 for each group）. 5 ）Statistical processing

　Statistical analysis was performed on the measured bond strength values obtained under the various condi-tions using Tukey’s honest significant differences test with the significance level set at 5％. Also, with the sig-nificance level set at 5％, t-testing was used to perform statistical testing on the shear bond strength after ther-mal cycle loading and after storage in water for 1 week.

Results

1 ．Surface roughness of adhesive surfaces　The roughness（Ra）of the adhesive surfaces having two types of surface property were 0.34（±0.04）μm for the AP pressure-contact surface, and 0.32±0.04μm

for the BE pressure-contact surface. For the diamond-point ground surface, Ra was 3.80±0.45μm for AP and 3.20±0.53μm for BE. For each surface treatment con-dition, no significant difference was observed in Ra between AP and BE（p＞0.05）.

2 ．SEM observation of adhesive surfaces　Fig.　2 shows SEM images of the polished surfaces for the composite resin specimens after polymerization. For AP, comparatively large and amorphous filler is present at high density. For BE, the image shows a low density of round filler that is comparatively smaller than the filler observed for AP. Fig.　3 shows the SEM image of the composite resin adhesive surface for each adhesive surface type（pressure-contact surface, dia-mond-point ground surface）. The AP and BE pressure-contact surfaces are flat, showing almost no irregulari-ties. The diamond-point ground surfaces show irregu-larities of various sizes, with deep cutting traces. Filler dropout was observed in some places.

3 ．Shear bond strength　Fig.　4 shows the results of the shear bond testing conducted 1 week after adhesion. Regarding the AP combinations, the combination of the diamond-point ground surface and silane coupling treatment（silane coupling and bonding mixture）showed approximately the same high values as the pressure-contact surface combined with the silane coupling treatment（silane coupling and bonding mixture）. Also, the lowest values were observed for the combination of the pressure-con-tact surface and no pretreatment. Regarding the BE combinations, the highest values were observed for the diamond-point ground surface combined with silane coupling treatment（silane coupling and bonding mix-ture）, while the lowest values were observed for the combination of the pressure-contact surface and no pre-treatment. When comparing the different adhesive sur-faces, a significant difference in shear bond strength was observed for only the BE bonding treatment, and no significant differences were observed for the other BE cases or for any of the AP cases. There were sig-nificant differences between the adhesion treatment methods for both the AP and the BE groups. Signifi-cant differences were observed for both the bonding treatment group and the silane coupling treatment compared with the no-treatment group for AP with the pressure-contact surface. Also, a significant difference was observed for AP with the diamond-point ground

Table　2　Conditions in each group

GroupAdhesive surface

Resin used in the repair

Storage conditions

1 AP AP 1 week2 BE BE 1 week3 AP AP TC4 BE BE TC

1 week: storage in water at 37℃ for 1 week, TC: 20,000 thermal cycle loads


surface between silane coupling treatment and no treat-ment. For BE with the pressure-contact surface, a sig-nificant difference was observed between only silane coupling treatment and no treatment. Fig.　5 shows the results of shear bond testing that was conducted after 20,000 repetitions of thermal cycle loading. No signifi-cant differences were observed between the surface

treatment groups with the same surface properties for either AP or BE under thermal cycling conditions（p＜0.05）.

Fig.　2　SEM images of the polished surface following hardening of each composite resin（×3,000）AP BE

Fig.　3　SEM images of the adhesive surface of each composite resin（×1,000）

Pressure-contact surface of AP Diamond-point ground surface of AP

Pressure-contact surface of BE Diamond-point ground surface of BE


Fig.　5　 Shear bond strength（MPa）after 20,000 thermal cycle loads following resin adhesionThe graph shows the mean±standard deviation.1 week: Storage for 1 week in 37℃ water, TR: 20,000 thermal cycle loads, p＜0.05

0

10

20

30

40

Pressure-contactsurface

Bondig only


Silane coupling and bondingmixture

Diamond-point groundsurface

Bondig only



Shaer bond strength（MPa） AP

1 week

TR

0

10

20

30

40


Bondig only




Bondig only



Shaer bond strength（MPa） BE

1 week

TR

Fig.　4　 Shear bond strength（MPa）after 1 week of storage in 37℃ water following resin adhesion Graph shows mean±standard deviation.

　＊: p＜0.05 when comparing the treatment groups, ＊＊: p＜0.05 when comparing the adhesive surfaces

0

10

20

30

40



Shear bond strength（MPa） AP＊＊

＊

0

10

20

30

40



Shear bond strength（MPa）

BE

＊

＊＊

No treatmentBonding onlySilane coupling andbonding mixture


Discussion

　During composite resin filling repair, one recommen-dation is to grind the surface of the adhesive body in order to expose a fresh surface, to increase the surface roughness, and to increase the adhesive area, and it is also recommended to perform silane coupling treat-ment14‒19）. Once hardened, the surface of the composite resin will be covered by a dense, light-cured matrix resin and fi l ler , which is disadvantageous when attempting adhesion. Also, it has been reported that the presence of an unpolymerized layer has no effects on the adhesive properties20）. In light of this information, when performing composite resin filling repair, it is necessary to look at the types of effects that the char-acteristics of the adhesive surface or pretreatment will have on the adhesive properties. Here, we investigated the state of the adhesive surfaces using the pressure-contact surface and the adhesive surface after increas-ing the surface roughness using a diamond point, as well as when performing bonding and silane coupling treatment as pretreatment.　Two kinds of conventional composite resin were used. Two different kinds of composite resin was used to examine the effects of difference in fluidity and com-position. Based on the results obtained in the present study, when considering the effects of cutting the adhe-sive surface on the surface roughness, the composition of AP consisted of 85 wt％ barium glass powder and silica-based microfiller（containing the filler）21）, and the other materials（BisGMA, triethyleneglycol-dimethacry-late［TEGDMA］）provided the remaining 14.5 wt％.　Furthermore, the BE consisted of 54.5％ glass filler（containing the filler）22,23） and 35.5 wt％ other materials（BisGMA, TEGDMA）. As is clear from the SEM imag-ing, the different filler configurations or content had no impact on the surface roughness. The filler configura-tion and content would also have no effect on the sur-face roughness of the composite resin after diamond-point cutting in clinical applications. The surface rough-ness of the pressure-contact surface is thought to be created by subsidence of the filler due to the pressure contact, and although there were differences in fluidity in an unpolymerized state（AP is a paste-type resin; BE is a flowable resin）, no significant differences were found between AP and BE. Furthermore, the SEM

imaging in this study revealed no differences in the adhesive surface characteristics of the two materials.　Because the shear bond test revealed no differences in bond strength based on the surface characteristics when using AP, it was determined that the surface roughness of the adhesive surface did not contribute to bond strength. When using BE, a significant difference was observed only in the case of bonding treatment, indicating that the fluidity of the composite resin used had an effect on bond strength. Significant differences were observed only in some parts, but it was specu-lated that the tendency for higher overall shear bond strength was due to the fact that the good fluidity of the flowable resin acted on the mechanical interlocking force. Compared with the case in which no pretreat-ment was performed for AP surface treatment, bonding treatment and silane coupling treatment showed signifi-cantly higher bond strength. This is attributed to the effects of the bonding material penetrating into the hardened surface during bonding treatment. It has been reported that unreacted monomer is present in compos-ite resin after polymerization24）. In the present study, the ratio of the base resin was high due to the pres-sure-contact surface, and the presence of unreacted monomer is therefore possible. Also, there were indica-tions that the functional monomers contained within the bonding material had an effect. In the silane coupling treatment, the unpolymerized base resin is thought to have bonded with the filler within the hardened mate-rial, which is the same behavior that occurs in silane treatment, which is used when bonding a resin inlay or ceramic filling material to resin cement13）. However, there were no indications of the effectiveness of silane coupling treatment in comparison with that of bonding treatment. Again, though silane coupling agents are superior surface modifiers for fillers25,26）, this result is attributed to the efficacy of the silane coupling agent not being reflected as a result of differences in filler content or morphology. A significant difference was observed for BE only in the case of silane coupling treatment on the pressure-contact surface. In the case of BE, there were indications that adhesive properties were affected by silane coupling treatment, and that the fluidity of the resin used also had an effect.　When looking at the shear bond strength after ther-mal cycle loading, no significant differences were observed between the surface treatments or between


the same surface characteristics for either AP or BE. The silane coupling layer undergoes hydrolysis of the siloxane bond due to the effects of water and heat, resulting in a drop in bond strength27）. Based on the present experimental results, heat treatment promoted polymerization of the permeated bonding layer, result-ing in a strong bond and thus degradation of bond strength was not observed as in the previous study.　As described above, in the present experiments, the significant issue in filling repair of restoration material（composite resin）is that grinding a single layer of the surface of the old resin is related to the removal of the contaminated area by increasing the roughness and cleaning up the contact points. In the case of AP, there were indications that differences in surface treatment had a greater effect than differences in surface rough-ness. In contrast, in the case of BE, there were indica-tions that differences in surface roughness were more effective than differences in surface treatment. There may be differences in fluidity depending on the compos-ite resin that is to be applied, and there may be differ-ences in the composition of the composite resin. Even when performing a repair using a composite resin of the same type, if the composition is different, there may be differences in surface roughness, surface treatment, or in the fluidity of the composite resin to be applied; therefore, the optimal filling repair method should be selected for each resin. The present results demon-strate that the effectiveness will differ depending on the type of composite resin, but when restoring composite resin, there are many cases where the composition of the old composite resin is unknown; the results here show that bonding and silane coupling treatment con-tributed to an improvement in adhesiveness when applying the unpolymerized resin. Also, the fluidity of the flowable resin contributes to the bond strength when performing a filling repair using composite resin. In the future, it will be necessary to compare and test other types of composite resin and composite resins with different fluidity, as well as to investigate surface modification methods for the base resin.

Conclusions

　This experiment simulated composite resin filling repair, and investigated the effects of differences in sur-face characteristics and pre-bonding treatment on the

adhesive properties when using a composite resin of the same type by comparing the results of shear bond test-ing. As a result, the following conclusions were reached.　1．No significant differences were observed in the surface roughness of the adhesive surfaces of the differ-ent composite resins.　2．The effective adhesive surface treatment was found to differ depending on the type of composite resin, so it is necessary to perform surface treatment that is optimal for the composite resin to be used.　3．Good fluidity of composite resins is effective for ensuring good adhesive properties.

　Conflict of interest: The authors declare that there is no conflict of interest.　Sources of funding: None.

References

1） Mount GJ, Ngo H. Minimal intervention: a new concept for operative dentistry. Quintessnce Int 2000; 31: 527‒533.

2） Akimoto N, Takamizu M, Momoi Y. 10-year clinical evaluation of a self-etching adhesive system. Oper Dent 2007; 32: 3‒10.

3） Kubo Y, Nakasa R, Hayashi Y. Survival rates of compos-ite resin and cast restoration. Jpn J Conserv Dent 2001; 44: 802‒809.（in Japanese）

4） Nikaido T, Takada T, Kitasako Y, Ogata M, Shimada Y, Yoshikawa T, Nakajima M, Otsuki M, Tagami J, Bur-row MF. Retrospective study of five-year clinical per-formance of direct composite restorations using a self-etching primer adhesive system. Dent Mater J 2006; 25: 611‒615.

5） Shinno Y, Kishimoto M, Anabuki Y, Kamiya E, Omae M, Nishitani S, Yoshiyama M. The physical properties of resin composites for posterior direct restoration in solu-tions. Jpn J Conserv Dent 2008; 51: 622‒629.（in Japa-nese）

6） Morigami M, Yukisada K, Tajima K, Sugisaki J, Uno S, Yamada T. A clinical survey on the frequency of flow-able resin composite restorations. Adhes Dent 2011; 29: 55‒59.（in Japanese）

7） Kubo S, Kawasaki A, Hayashi Y. Factors associated with the longevity of resin composite restorations. Dent Mater J 2011; 30: 374‒383.

8） Shinkai K, Kato Y. Factors affecting long-term clinical performance of posterior resin composites. Jpn J Con-serv Dent 2000; 43: 121‒133.（in Japanese）

9） Tyas MJ, Anusarice KJ, Frencken JE, Mount GJ. Mini-


mal Intervention dentistry―a review, FDI Commission Project 1‒97. Int Dent J 2000; 50: 1‒12.

10） Momoi Y, Hayashi M, Fujitani M, Fukushima M, Imazato S, Kubo S, Nikaido T, Shimizu A, Umemori M, Yamaki C. Clinical guidelines for treating caries in adults follow-ing a minimal intervention policy―Evidence and con-sensus based report. J Dent 2012; 40; 95‒105.

11） Tagami J, Senda A, Nara Y, Momoi Y. Operative den-tistry 21. 4th ed. Nagasue Shoten: Kyoto; 2011. 144‒147.（in Japanese）

12） Tanaka T, Ino S, Odagiri A, Hamano N, Watanabe T, Katsumata Y, Hojo S, Toyota M. In-vitro assessment of hard relining material. Kanagawa Shigaku 2011; 42: 134‒139.（in Japanese）

13） Komine T, Matsumura H. Adhesive bonding and luting of restorations and fixed prostheses. Ann Jpn Prostho-dont Soc 2012; 4: 343‒352.（in Japanese）

14） Hisamatsu N, Atsuta M, Matsumura H. Effect of surface conditioning agents on the repair bond strength of an indirect hybrid composite. Int Chin J Dent 2002; 2: 5‒14.

15） Chan KC, Boyer DB. Repair of conventional and micro-filled composite resins. J Prosthet Dent 1989; 50: 345‒350.

16） Chiba K, Hosoda H, Fusayama T. The addition of an adhesive composite resin to the same material: bond strength and clinical techniques. J Prosthet Dent 1989; 61: 669‒675.

17） Bouschlicher MR, Reinhardt JW, Vargas MA. Surface treatment techniques for resin composite repair. Am J Dent 1997; 10: 279‒283.

18） Tezvergil A, Lassila LVJ, Vallittu PK. Composite-com-posite repair bond strength: effect of different adhesion primers. J Dent 2003; 31: 521‒525.

19） Nikaido T, Tagami J. Filling repair that utilizes bonding. Dent Outlook 2006; Suppl: 130‒136.（in Japanese）

20） Suh BI. Oxygen-inhibited layer in adhesion dentistry. Tsurumi Univ Dent J 2006; 32: 1‒7.

21） Miyaji H. Study on repair of resin composite restora-tions. Jpn J Conserv Dent 2006; 49: 108‒119.（in Japa-nese）

22） Hoshika T, Nishitani S, Takahashi K, Tanaka T, Nakada T, Yamaji K, Yoshiyama M. A study of flow on flowable resin composite. Adhes Dent 2009; 27: 118‒124.（in Japa-nese）

23） Kinomoto K, Nakatsuka T, Deguchi M. Characteristics of PRG technology-applied“BEAUTIFIL Flow”. J Jpn Soc Dent Prod 2006; 19: 53‒61.（in Japanese）

24） Hirabayashi S, Hirazawa T, Nasu K, Nakanishi S. Com-positions of various visible light-cured composite resins and elutions of residual monomer from these cured res-ins. J Jpn Soc Dent Equip 1984; 3: 655‒664.（in Japanese）

25） Nishiyama N, Hayakawa T. Silane coupling agents. J Jpn Soc Adhes Dent 1987; 5: 129‒133.（in Japanese）

26） Jo H, Blum FD. Characterization of the interface in polymer-silica composites containing an acrylic silane coupling agent. Chem Mater 1999; 11: 2548‒2553.

27） Ishida S, Nishiyama N. Study on surface treatment of silica filler: Hydrolytic deterioration of the silane cou-pling layer. J Jpn Soc Dent Equip 1989; 8: 601‒607.（in Japanese）


　責任著者連絡先：小林幹宏　〒 145‒8515　東京都大田区北千束 2‒1‒1　昭和大学歯学部歯科保存学講座美容歯科学部門　TEL：03‒3787‒1151，FAX：03‒3787‒1229，E-mail：[email protected]　受付：平成 26年 2月 7日/受理：平成 26年 2月 20日

コンポジットレジンに対する接着前処理方法が補修修復後のせん断接着強さに及ぼす影響

小　林　幹　宏藤　島　昭　宏＊真　鍋　厚　史

昭和大学歯学部歯科保存学講座美容歯科学部門＊昭和大学歯学部歯科保存学講座歯科理工学部門

抄録　目的：コンポジットレジンの補修修復における被着面の表面粗さならびにプライマー処理などの前処理条件の相違がコンポジットレジンの補修修復に及ぼす影響について比較，検討した．　材料と方法：2種類の組成，流動性の異なるコンポジットレジン Clearfil AP‒X（AP），Beautifil Flow F02（BE）を用いて表面性状が異なる 2種類の被着面を作製した（圧接面とダイヤモンドポイント切削面）．接着前処理条件として未処理，ボンディング処理（Clearfil Photo Bond），シランカップリング処理（Clearfil Photo Bondと Clearfil Porcelain Bondの混合液）で前処理を行い被着面と同じコンポジットレジンを充塡し，1週間水中保管後にせん断接着試験を行い比較，検定を行った．　結果：せん断接着強さでは，同じ被着面の表面性状間でBEのボンディング処理のみに有意な差が認められ，その他のAPならびに BEでは有意な差は認められなかった．被着面の表面処理間では，APの圧接面の表面未処理に対してボンディング処理群，シランカップリング群，いずれの群でも有意な差が認められた．BEでは，ダイヤモンドポイント切削面に対してシランカップリング処理で有意な差が認められた．圧接面の未処理に対して，シランカップリング処理のみに有意な差が認められた．　結論：コンポジットレジンの種類により有効な被着面の処理が異なり，それぞれに適した表面処理が必要である．コンポジットレジンの流動性の良さは接着性に有効である．

キーワード：シランカップリング，補修修復，コンポジットレジン，ボンディング材

effects of pretreatment procedures on shear bond strength

Documents