口腔正畸用磁块镀氮化钛膜后抗腐蚀实验研究
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摘要
目前，口腔正畸用磁性材料大多是稀土钕铁硼(neodymium-iron-boron，Nd2Fe14B)。因其含铁和钕，而易于氧化及腐蚀，尤其在口腔特殊的环境中应用一定时间后便会发生表面腐蚀，甚至崩解，导致磁块性能的衰退，制约了磁力正牙技术在临床的应用及推广。
近年来，氮化钛(titanium nitride，TiN)膜优良的理化性能、抗腐蚀性能受到了人们的关注，并已开始应用于某些工业领域。为此，我们借鉴工业镀膜方法，选用等离子体增强化学气相沉积法(plasma enhanced chemical vapor deposition，PCVD)，首次在磁块表面成功镀以TiN膜，测定了镀TiN膜磁块的有关物理机械性能。在此基础上，应用人工唾液浸泡法及电化学法，从定性、定量两方面着重研究了镀TiN膜磁块的抗腐蚀性能。此外，还按照ISO标准，以MTT法检测了镀TiN膜磁块对L—929小鼠成纤维细胞的毒性，并观察镀膜磁块对日本大耳白兔口腔粘膜刺激情况，评价了磁块镀TiN膜后的生物安全性。
【结果】 镀TiN膜磁块耐腐蚀性能显著增强，且镀TiN膜不影响磁块的磁性能，具有良好的生物相容性，安全可靠。
【结论】 (1)等离子体增强化学气相沉积法用于口腔正畸磁块表面镀膜效果良好；(2)正畸用磁块表面镀TiN膜不影响磁块的磁学性能；(3)磁块镀TiN膜后抗腐蚀性能显著增强；(4)磁块镀TiN膜后，具有良好的
昆明医学院硕士学位论文
生物安全性;(5)口腔正畸用磁块表面镀TIN膜具有良好的推广应用前景。
The magnetic materials used in orthodontics at present are rare earth neodymium-iron-boron, which are easily oxidized and corroded because of containing iron and neodymium when they are used intra-orally. These lead to the disintegration of the magnets and the decay of the magnetic force and limit their application and popularization in orthodontics.
In recent years, titanium nitride (TiN) is increasingly important in industry. The anticorrosion and physio-chemical properties of TiN are excellent and thin TiN coating is able to improve the properties of metallic materials. In this study, TiN coating was deposited by direct current pulse plasma enhanced chemical vapor deposition (PCVD) and the physio-mechanical properties of the magnets with TiN coating were tested. Then the corrosion resistance of the magnets with TiN coating was qualitatively and quantitatively studied by immersing into the artificial saliva and by electrochemical test. Moreover, according to ISO standard, the biocompatibilities of magnets coated TiN were evaluated by cytotoxicity test using L-929 mouse fibroblasts with 3-(4,5-dimetnyltniazol-2-yl)-2,5-dipnenyltetra-zoliumbromide (MTT) method and by oral mucous irritation test
in Japanese white rabbit.
Results: Coating TiN film on the surface of the orthodontic magnets does not change magnetic force of the magnets and greatly improves the anticorrosion resistance of the magnets and the biocompatibilities of the magnets coating TiN are excellent.
Conclusion: (1) Direct current PCVD is a desirable method and can be employed to coat the magnets used in orthodontics. (2) Magnetic force of the magnets with TiN film does not be changed. (3) The anticorrosion resistance of the magnets with TiN coating is significantly strengthened. (4) The biocompatibilities of the magnets with TiN film are excellent. (5) Coating TiN film on the surface of the orthodontic magnets has the worth of popularization and application.
近年来，氮化钛(titanium nitride，TiN)膜优良的理化性能、抗腐蚀性能受到了人们的关注，并已开始应用于某些工业领域。为此，我们借鉴工业镀膜方法，选用等离子体增强化学气相沉积法(plasma enhanced chemical vapor deposition，PCVD)，首次在磁块表面成功镀以TiN膜，测定了镀TiN膜磁块的有关物理机械性能。在此基础上，应用人工唾液浸泡法及电化学法，从定性、定量两方面着重研究了镀TiN膜磁块的抗腐蚀性能。此外，还按照ISO标准，以MTT法检测了镀TiN膜磁块对L—929小鼠成纤维细胞的毒性，并观察镀膜磁块对日本大耳白兔口腔粘膜刺激情况，评价了磁块镀TiN膜后的生物安全性。
【结果】 镀TiN膜磁块耐腐蚀性能显著增强，且镀TiN膜不影响磁块的磁性能，具有良好的生物相容性，安全可靠。
【结论】 (1)等离子体增强化学气相沉积法用于口腔正畸磁块表面镀膜效果良好；(2)正畸用磁块表面镀TiN膜不影响磁块的磁学性能；(3)磁块镀TiN膜后抗腐蚀性能显著增强；(4)磁块镀TiN膜后，具有良好的
昆明医学院硕士学位论文
生物安全性;(5)口腔正畸用磁块表面镀TIN膜具有良好的推广应用前景。
The magnetic materials used in orthodontics at present are rare earth neodymium-iron-boron, which are easily oxidized and corroded because of containing iron and neodymium when they are used intra-orally. These lead to the disintegration of the magnets and the decay of the magnetic force and limit their application and popularization in orthodontics.
In recent years, titanium nitride (TiN) is increasingly important in industry. The anticorrosion and physio-chemical properties of TiN are excellent and thin TiN coating is able to improve the properties of metallic materials. In this study, TiN coating was deposited by direct current pulse plasma enhanced chemical vapor deposition (PCVD) and the physio-mechanical properties of the magnets with TiN coating were tested. Then the corrosion resistance of the magnets with TiN coating was qualitatively and quantitatively studied by immersing into the artificial saliva and by electrochemical test. Moreover, according to ISO standard, the biocompatibilities of magnets coated TiN were evaluated by cytotoxicity test using L-929 mouse fibroblasts with 3-(4,5-dimetnyltniazol-2-yl)-2,5-dipnenyltetra-zoliumbromide (MTT) method and by oral mucous irritation test
in Japanese white rabbit.
Results: Coating TiN film on the surface of the orthodontic magnets does not change magnetic force of the magnets and greatly improves the anticorrosion resistance of the magnets and the biocompatibilities of the magnets coating TiN are excellent.
Conclusion: (1) Direct current PCVD is a desirable method and can be employed to coat the magnets used in orthodontics. (2) Magnetic force of the magnets with TiN film does not be changed. (3) The anticorrosion resistance of the magnets with TiN coating is significantly strengthened. (4) The biocompatibilities of the magnets with TiN film are excellent. (5) Coating TiN film on the surface of the orthodontic magnets has the worth of popularization and application.
引文
1 Assano T. The effects of mandibular retractive force on the growing rat mandibule. Am J Orthod Dentofac Orthop, 1986, 90:464
2 候志明，邓燕，尚伟．钕铁硼磁力矫治器的研制．口腔材料器械杂志，1999，8(1)：14-16
3 贾成厂，李汶霞，郭志猛等．陶瓷基复合材料导论．北京：冶金工业出版社，1998,8．56-57
4 Rapisarda E, Bonaccorso A, Tripi TR, et al. The effect of surface treatments of nickel-titanium files on wear and cutting efficiency. Oral surgery, oral medicine, oral pathology, oral radiology, and endodontics. 2000, 89(3): 363-8
5 RAwlings RD, Robinson PB, Rogers PS. The durability of ceramic coated dental instruments. European journal of prosthodontics and restorative. dentisty, 1995, 3(5): 211-6
6 中华人民共和国国家标准，金属维氏硬度试验：GB／T 4340．3—1999
7 李璞，余兵，徐芸等．正牙用小磁块的力学、磁学研究．云南医药，1997，18(4)：275-276
8 沈延山，陈贞祥，朱英臣．氮化钛涂层刀具及其应用．华东理工大学学报，1994，20(2)：141—44
9 马峰，蔡殉．膜基界面结合强度表征和评价．表面技术，2001，30(5)：50-54
10 ISO TR 10271. Dentistry-determination of tarnish and corrosion of metals and alloys. Switzerland. 1993:3
11 中华人民共和国国家标准，金属和合金的腐蚀．腐蚀试样上腐蚀产物的清除：GB／T16545—1996
12 刘安福．Nd-Fe-B永磁材料镀镍和镀锌．电镀与精饰，1999，2l(5)：24-26
13 Yada I. A basic study on gallium alloy for dental restoration, Improvement of liguid gallium alloy. Fuknoke-Shika-Daigakm-Gakkai-Zasshi, 1989, 16(2): 1758
14 ISO/TC 194. Biological testing of medical and dental materials and device. 10993-1992
15 上海第二医科大学生物材料研究室编．非直接接触血液的医用生物材料生物性能测试标准．上海市试行规，1985
16 张彩霞，孙皎，孟爱英．紫外分关光度仪测定不同含铜量银汞合金细胞毒性的新方法．中华口腔医学杂志，1990，25(4)：216-18
17 Mosroam T, Rapid colorimetric assay for cellular growth and survival: Application to proliferation and cytotoxicity assay. J Immunol Methods, 1983, 65(1～2): 55
18 杨晓芳，奚廷斐．生物材料生物相容性评价研究进展．生物医学工程学杂志，
18(1)：123-28
19 赵桂枝，陈华，徐如生．磁力作用下猴牙周组织改建的扫描电镜观察．口腔医学纵横，1992，8(1)：27-28
20 徐芸，梁文勇，余兵．钕铁硼磁体对机体微量元素影响的初步研究．华西口腔医学杂志，1997，15(2)：108-9
21 Aronson LA, Lindskog S, Rygh P. Orthodontic mgnets: effects on gingival epithelium and alveolar bone in monkeys. Eur J Ortho, 1992, 14:255
22 薛淼，晏真．国际标准化组织7406技术报告：牙科材料的生物学评价(续Ⅷ)．口腔材料器械杂志，1997，6(3)：147
2 候志明，邓燕，尚伟．钕铁硼磁力矫治器的研制．口腔材料器械杂志，1999，8(1)：14-16
3 贾成厂，李汶霞，郭志猛等．陶瓷基复合材料导论．北京：冶金工业出版社，1998,8．56-57
4 Rapisarda E, Bonaccorso A, Tripi TR, et al. The effect of surface treatments of nickel-titanium files on wear and cutting efficiency. Oral surgery, oral medicine, oral pathology, oral radiology, and endodontics. 2000, 89(3): 363-8
5 RAwlings RD, Robinson PB, Rogers PS. The durability of ceramic coated dental instruments. European journal of prosthodontics and restorative. dentisty, 1995, 3(5): 211-6
6 中华人民共和国国家标准，金属维氏硬度试验：GB／T 4340．3—1999
7 李璞，余兵，徐芸等．正牙用小磁块的力学、磁学研究．云南医药，1997，18(4)：275-276
8 沈延山，陈贞祥，朱英臣．氮化钛涂层刀具及其应用．华东理工大学学报，1994，20(2)：141—44
9 马峰，蔡殉．膜基界面结合强度表征和评价．表面技术，2001，30(5)：50-54
10 ISO TR 10271. Dentistry-determination of tarnish and corrosion of metals and alloys. Switzerland. 1993:3
11 中华人民共和国国家标准，金属和合金的腐蚀．腐蚀试样上腐蚀产物的清除：GB／T16545—1996
12 刘安福．Nd-Fe-B永磁材料镀镍和镀锌．电镀与精饰，1999，2l(5)：24-26
13 Yada I. A basic study on gallium alloy for dental restoration, Improvement of liguid gallium alloy. Fuknoke-Shika-Daigakm-Gakkai-Zasshi, 1989, 16(2): 1758
14 ISO/TC 194. Biological testing of medical and dental materials and device. 10993-1992
15 上海第二医科大学生物材料研究室编．非直接接触血液的医用生物材料生物性能测试标准．上海市试行规，1985
16 张彩霞，孙皎，孟爱英．紫外分关光度仪测定不同含铜量银汞合金细胞毒性的新方法．中华口腔医学杂志，1990，25(4)：216-18
17 Mosroam T, Rapid colorimetric assay for cellular growth and survival: Application to proliferation and cytotoxicity assay. J Immunol Methods, 1983, 65(1～2): 55
18 杨晓芳，奚廷斐．生物材料生物相容性评价研究进展．生物医学工程学杂志，
18(1)：123-28
19 赵桂枝，陈华，徐如生．磁力作用下猴牙周组织改建的扫描电镜观察．口腔医学纵横，1992，8(1)：27-28
20 徐芸，梁文勇，余兵．钕铁硼磁体对机体微量元素影响的初步研究．华西口腔医学杂志，1997，15(2)：108-9
21 Aronson LA, Lindskog S, Rygh P. Orthodontic mgnets: effects on gingival epithelium and alveolar bone in monkeys. Eur J Ortho, 1992, 14:255
22 薛淼，晏真．国际标准化组织7406技术报告：牙科材料的生物学评价(续Ⅷ)．口腔材料器械杂志，1997，6(3)：147