牙科陶瓷偶联剂的相关性能研究
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摘要
现代粘结技术已经广泛应用于口腔医学的各个领域，粘结技术的应用不但为临床操作提供了便利，而且使修复过程更具保存性，也在一定程度上满足了患者日益增长的美容需要。尤其是应用陶瓷材料进行的间接粘结修复，如全瓷冠、瓷贴面等倍受临床医生和患者的欢迎。通常各类全瓷修复体应用粘结性树脂粘固于牙体表面。且各类瓷修复体崩瓷后在口内直接修补用的也是复合树脂，所以瓷与树脂的粘结成为瓷修复体临床应用的一个关键问题。
硅烷偶联剂是促进瓷与树脂粘结的重要手段。应用偶联剂可在瓷与树脂之间建立一定程度的化学粘结。γ-MPS的浓度和各种添加成分对偶联剂作用效果有显著影响。目前国外一些成品陶瓷偶联剂加入了酸性催化剂和引发体系等添加成分，使偶联剂的效能显著提高。
为了进一步探讨硅烷偶联剂的不同浓度和各种添加成分对偶联剂作用效果的影响，验证偶联剂对瓷表面润湿性以及瓷和树脂粘结密合度的影响，为陶瓷偶联剂的应用提供一定理论依据，本研究根据影响陶瓷偶联剂作用效果的主要因素，在预试验的基础上，配制了具有代表性的6种陶瓷偶联剂配方。将试制的6种偶联剂与Cerinate Prime偶联剂相比较，观察了非酸蚀和酸蚀条件下不同偶联剂对2种瓷和树脂粘结强度的影响，探讨了γ-MPS的不同浓度、引发剂及粘结单体4-META对偶联剂作用效果的影响。
第四军医大学硕士学位论文
实验发现C配方陶瓷偶联剂可以在瓷和树脂之间产生最高的剪切
粘结强度。而后我们又使用接触角测定仪和扫描电子显徽镜对试
制陶瓷偶联剂在改善瓷表面润湿性和提高粘结界面密合度，减少
边缘微渗漏等方面进行了实验研究，验证了陶瓷偶联剂在这些方
面的作用。并发现该陶瓷偶联剂在这些方面的粘结性能优于目前
临床使用的Cerinate Prime偶联剂。为保证临床应用的安全，我
们还对试制陶瓷偶联剂进行了急性全身毒性实验，皮肤刺激实验
和细胞毒性实验，初步评价了其生物安全性。
根据实验结果可以得出如下结论:
1.陶瓷偶联剂中朴MPS的浓度在5%左右可以取得较好的粘结
效果，其浓度过高或过低均不利于瓷和树脂的粘结。
2.粘结单体4一META作为陶瓷偶联剂的添加成分，对瓷和树脂
的粘结无帮助。
3.C配方陶瓷偶联剂在瓷与树脂之间产生的粘结强度最高，用
于烤瓷或全瓷表面处理均有良好效果。临床应用时，应将瓷修复
体用氢氟酸酸蚀后再使用陶瓷偶联剂，可以获得理想的粘结强度。
4.试制陶瓷偶联剂可以明显改善瓷表面的润湿性。粘结树脂在
瓷表面形成的接触角大小与粘结强度有一定相关性。改善瓷表面
润湿性可能是陶瓷偶联剂提高瓷与树脂之间粘结强度的作用机理
之一。
5.试制陶瓷偶联剂能提高瓷和树脂的粘结密合度，若与氢氟酸
酸蚀配合使用效果更好。瓷和树脂粘结界面微缝隙大小与粘结强
度有一定相关性。
6.试制陶瓷偶联剂属实际无毒材料，对皮肤无刺激，用于瓷修
复体的粘结，不会经边缘微渗漏对口腔组织细胞造成毒性损害，
具有良好的生物安全性。
Bonding techniques today are widely used in every branches of dentistry. It has not only facilitated the clinical procedures, but also produced more conservative restorative techniques and met in some extent the growing cosmetic needs of patients. Indirect porcelain-bonded restorations are warmly welcomed by both dentists and patients. We usually use composite resin adhesive for attaching porcelain restorations to teeth or repairing the fractured porcelain of a metalloceramic restoration. Both of these applications require adequate bond strength of composite resin to the surface of porcelain.
Using silane coupling agent in enhancing the bonding of composite resin to porcelain is well accepted. The silane treatment is thought to contribute to chemical bond formation between porcelain and composite resin. Concentration and additioners have significant influence on effects of silane coupling agent. Some foreign commercially available silane coupling agents have different components with functional monomer, catalyst and activator. They are vastly improved over the earlier versions.
For discussing the effects of different concentrations and
additioners in porcelain silane coupling agent, testifying its effects on wetting and sealing capability, and choosing a new silane coupling agent to improve clinical procedure, we made out some new prescriptions of porcelain silane coupling agent.
After pilot study, we chose 6 prescriptions for further experimental selection. Six new silane coupling agents were applied to etched or unetched porcelain surfaces respectively, Cerinate Prime was used as control. The shear bond strengths between porcelain and composite resin were determined. The effects of activators, 4 -META and concentrations of y-MPS were also discussed. Results suggested the type C silane coupling agent can generate the highest shear bond strength. Then we testified effects of silane coupling agent on wetting and sealing capability with SEM and contact angle machine. After a series study, we found that the new silane coupling agent was better than Cerinate Prime on improving bonding of composite resin to porcelain . To study the biological safety of new silane coupling agent, we also did acute toxicity test, skin irritation test and cytotoxicity test. The main findings of this study are as follows:
1. 5% -MPS in porcelain silane coupling agent can generate the best effect on porcelain-composite resin bonding. Above or below this concentration may adverse.
2. As an additioner in silane coupling agent, the functional monomer of 4-META can not help the bonding between porcelain and composite resin.
3. Type C silane coupling agent can generate the highest shear bond strength between different porcelains and composite resin. To get the ideal bond strength in clinical procedures, we should
combine etching and silane treatment.
4. New silane coupling agent can obviously improve the wetting of porcelain surface. There may be some relations between contact
v
angle on porcelain surface and bond strength of porcelain-composite resin. Improving the wetting on porcelain surface may be one of mechanisms of silane coupling agent.
5. New silane coupling agent can improve the sealing capability and diminish microleakage between porcelain and composite resin. There may be some relations between sealing capability and bond strength.
6. New silane coupling agent has good biological safety. In fact, it does not have acute toxicity, skin irritation and cytotoxicity from microleakage.
硅烷偶联剂是促进瓷与树脂粘结的重要手段。应用偶联剂可在瓷与树脂之间建立一定程度的化学粘结。γ-MPS的浓度和各种添加成分对偶联剂作用效果有显著影响。目前国外一些成品陶瓷偶联剂加入了酸性催化剂和引发体系等添加成分，使偶联剂的效能显著提高。
为了进一步探讨硅烷偶联剂的不同浓度和各种添加成分对偶联剂作用效果的影响，验证偶联剂对瓷表面润湿性以及瓷和树脂粘结密合度的影响，为陶瓷偶联剂的应用提供一定理论依据，本研究根据影响陶瓷偶联剂作用效果的主要因素，在预试验的基础上，配制了具有代表性的6种陶瓷偶联剂配方。将试制的6种偶联剂与Cerinate Prime偶联剂相比较，观察了非酸蚀和酸蚀条件下不同偶联剂对2种瓷和树脂粘结强度的影响，探讨了γ-MPS的不同浓度、引发剂及粘结单体4-META对偶联剂作用效果的影响。
第四军医大学硕士学位论文
实验发现C配方陶瓷偶联剂可以在瓷和树脂之间产生最高的剪切
粘结强度。而后我们又使用接触角测定仪和扫描电子显徽镜对试
制陶瓷偶联剂在改善瓷表面润湿性和提高粘结界面密合度，减少
边缘微渗漏等方面进行了实验研究，验证了陶瓷偶联剂在这些方
面的作用。并发现该陶瓷偶联剂在这些方面的粘结性能优于目前
临床使用的Cerinate Prime偶联剂。为保证临床应用的安全，我
们还对试制陶瓷偶联剂进行了急性全身毒性实验，皮肤刺激实验
和细胞毒性实验，初步评价了其生物安全性。
根据实验结果可以得出如下结论:
1.陶瓷偶联剂中朴MPS的浓度在5%左右可以取得较好的粘结
效果，其浓度过高或过低均不利于瓷和树脂的粘结。
2.粘结单体4一META作为陶瓷偶联剂的添加成分，对瓷和树脂
的粘结无帮助。
3.C配方陶瓷偶联剂在瓷与树脂之间产生的粘结强度最高，用
于烤瓷或全瓷表面处理均有良好效果。临床应用时，应将瓷修复
体用氢氟酸酸蚀后再使用陶瓷偶联剂，可以获得理想的粘结强度。
4.试制陶瓷偶联剂可以明显改善瓷表面的润湿性。粘结树脂在
瓷表面形成的接触角大小与粘结强度有一定相关性。改善瓷表面
润湿性可能是陶瓷偶联剂提高瓷与树脂之间粘结强度的作用机理
之一。
5.试制陶瓷偶联剂能提高瓷和树脂的粘结密合度，若与氢氟酸
酸蚀配合使用效果更好。瓷和树脂粘结界面微缝隙大小与粘结强
度有一定相关性。
6.试制陶瓷偶联剂属实际无毒材料，对皮肤无刺激，用于瓷修
复体的粘结，不会经边缘微渗漏对口腔组织细胞造成毒性损害，
具有良好的生物安全性。
Bonding techniques today are widely used in every branches of dentistry. It has not only facilitated the clinical procedures, but also produced more conservative restorative techniques and met in some extent the growing cosmetic needs of patients. Indirect porcelain-bonded restorations are warmly welcomed by both dentists and patients. We usually use composite resin adhesive for attaching porcelain restorations to teeth or repairing the fractured porcelain of a metalloceramic restoration. Both of these applications require adequate bond strength of composite resin to the surface of porcelain.
Using silane coupling agent in enhancing the bonding of composite resin to porcelain is well accepted. The silane treatment is thought to contribute to chemical bond formation between porcelain and composite resin. Concentration and additioners have significant influence on effects of silane coupling agent. Some foreign commercially available silane coupling agents have different components with functional monomer, catalyst and activator. They are vastly improved over the earlier versions.
For discussing the effects of different concentrations and
additioners in porcelain silane coupling agent, testifying its effects on wetting and sealing capability, and choosing a new silane coupling agent to improve clinical procedure, we made out some new prescriptions of porcelain silane coupling agent.
After pilot study, we chose 6 prescriptions for further experimental selection. Six new silane coupling agents were applied to etched or unetched porcelain surfaces respectively, Cerinate Prime was used as control. The shear bond strengths between porcelain and composite resin were determined. The effects of activators, 4 -META and concentrations of y-MPS were also discussed. Results suggested the type C silane coupling agent can generate the highest shear bond strength. Then we testified effects of silane coupling agent on wetting and sealing capability with SEM and contact angle machine. After a series study, we found that the new silane coupling agent was better than Cerinate Prime on improving bonding of composite resin to porcelain . To study the biological safety of new silane coupling agent, we also did acute toxicity test, skin irritation test and cytotoxicity test. The main findings of this study are as follows:
1. 5% -MPS in porcelain silane coupling agent can generate the best effect on porcelain-composite resin bonding. Above or below this concentration may adverse.
2. As an additioner in silane coupling agent, the functional monomer of 4-META can not help the bonding between porcelain and composite resin.
3. Type C silane coupling agent can generate the highest shear bond strength between different porcelains and composite resin. To get the ideal bond strength in clinical procedures, we should
combine etching and silane treatment.
4. New silane coupling agent can obviously improve the wetting of porcelain surface. There may be some relations between contact
v
angle on porcelain surface and bond strength of porcelain-composite resin. Improving the wetting on porcelain surface may be one of mechanisms of silane coupling agent.
5. New silane coupling agent can improve the sealing capability and diminish microleakage between porcelain and composite resin. There may be some relations between sealing capability and bond strength.
6. New silane coupling agent has good biological safety. In fact, it does not have acute toxicity, skin irritation and cytotoxicity from microleakage.
引文
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77．纪云晶．实用毒理学手册．第一版．中国环境科学出版社：1993．126～142．
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81. Hank CT, Wataha JC,Zhilin Sun. In vitro models of biocompatibility: A review. Dent Mater, 1996,66:1～9.
82. Silva VV, Lameiras FS, Lobato ZI. Biological reactivity of zirconia-hydroxyapatite composites. J Biomed Mater Res. 2002,63(5):583-90.
83. Schamls G ,Gymnlich L. A simple dentin barrier test:cytotoxicity of dental cement. J Dent Res, 1993,72:367～371.
84．孙皎，高桑美代子，佐藤和子等．复合树脂单体对人牙髓细胞毒性的研究．实用口腔医学杂志，2000，16(4)：264～267．
85. Cattani Lorente MA,Dupuis V, Moya F, et al. Comparative study of the physical porperties of a polyacid-modified composite resin and a resin modified glass ionomer cement. Dent Mater, 1999:15(1):21～32.