纳米非晶金刚石薄膜在牙科钴铬合金及纯钛表面处理中的应用
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摘要
金属是口腔义齿修复中必不可少的一种材料。由于口腔内复杂的酸碱环境和微生物环境，金属材料义齿在口腔内使用一段时间后其表面会出现不同程度的腐蚀、变色、细菌粘附等现象，既影响修复体的美观和使用寿命，又会导致一些严重的不良反应和并发症，威胁人体健康。因此对金属义齿材料进行表面处理以改善其表面性能具有十分重要的临床意义。本研究将西安交通大学研制的纳米非晶金刚石薄膜应用于牙科钴铬合金以及纯钛的表面处理，其目的旨在为改善义齿金属材料表面性能探索新的途径，同时也为纳米非晶金刚石薄膜的临床应用提供理论及实验依据。
本课题研究采用西安交通大学研制的过滤阴极真空电弧沉积系统在牙科钴铬合金及纯钛表面制备纳米非晶金刚石薄膜。首先，采用扫描电镜、原子力显微镜、拉曼光谱以及X射线光电子能谱表征纳米非晶金刚石薄膜的表面形貌、空间结构、元素成分和化学键构成，同时探讨样品偏压这一工艺参数对该薄膜质量的影响。随后，按照医疗器械生物学评价标准，通过体外细胞毒性实验和口腔粘膜接触实验，对纳米非晶金刚石薄膜的生物相容性能进行评价。接下来，采用常规划痕实验，测量不同样品偏压条件下以及Ti和TiN两种中间层预处理条件下纳米非晶金刚石薄膜的膜基临界载荷，并探讨样品偏压和中间层预处理对该薄膜结合强度的影响。最后，采用粗糙度仪和接触角测量系统测量镀膜前后钴铬合金及纯钛表面粗糙度和三种液体接触角，并计算镀膜前后两种牙科金属的表面自由能；通过细菌粘附实验比较镀膜前后钴铬合金及纯钛表面变形链球菌、白色念珠菌、粘性放线菌的粘附数量，并结合表面粗糙度和自由能的变化，深入探讨钴铬合金和纯钛表面所镀纳米非晶金刚石薄膜影响细菌粘附的机制。本课题研究的结果如下：
1.采用过滤阴极真空电弧沉积系统在钴铬合金及纯钛表面制备的薄膜具有纳米级厚度，由sp~3键和sp~2键碳原子组成，且sp3键含量大于70%，符合纳米非晶金刚石薄膜的质量标准。随样品偏压的增大，两种牙科金属镀膜的sp3键含量均呈现先升高后降低的趋势，钴铬合金和纯钛镀膜的最佳样品偏压分别为200v及250v。
2.纳米非晶金刚石薄膜的细胞相对增殖率均大于90%，细胞毒性评级≤1级，粘膜刺激指数为0，具备非常良好的生物相容性。
3.随样品偏压的增大，钴铬合金和纯钛镀膜的结合强度均呈现先升高后降低的趋势，其最佳样品偏压值分别为200v及250v。Ti和TiN两种中间层预处理后，纳米非晶金刚石薄膜与衬底的结合强度显著提高，钴铬合金采用Ti中间层时膜基结合强度最好，纯钛采用TiN中间层时膜基结合强度最佳。
4.镀膜后钴铬合金及纯钛的表面粗糙度均显著降低，同时，钴铬合金的表面能增大明显，但是纯钛表面能的变化不显著。经纳米非晶金刚石薄膜表面处理后，钴铬合金及纯钛表面变形链球菌、白色念珠菌及粘性放线菌的粘附数量均出现了显著降低，表明纳米非晶金刚石薄膜可以改善这两种义齿金属材料表面的细菌粘附性能。
As a very important dental material, metals are widely used in completeand removable partial dentures. Owing to the complicated microbial andacid-base circumstances in oral cavity, the surfaces of dental metal materialsmay suffer corrosion, discoloration and bacterial adhesion. These phenomenamay not only affect the appearance and useful life of dentures but also lead tosome denture-induced adverse effects and complications which will severelythreaten the health of human body. Therefore, it is very significant to find aneffective method of surface treatment to improve the surface properties of dentalmetal materials. In this study, nanometer amorphous diamond films researchedand developed by Xi'an Jiaotong University were applied to the surfacetreatment of dental Co-Cr alloys and pure Ti. The aims of this study were to finda new method to improve the surface properties of dental metal materials andprovide the theoretical and experimental bases for the clinical applications ofnanometer amorphous diamond films.
In this study, a filtered cathodic vacuum arc (FCVA) system was used toprepare nanometer amorphous diamond films on dental Co-Cr alloys and pureTi. Then, scanning electronic microscopy (SEM), Atomic force microscopy(AFM), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS) wereused to analyze some characteristics of the coatings including the surfacemorphology, microstructure, elemental composition and the chemical bindingstates, and simultaneously the effects of substrate bias voltage on sp3fraction ofthe coatings were investigated. The biocompatibility of the deposited nanometeramorphous diamond films was investigated through in vitro cytotoxicity test andoral mucous membrane irritation test. Using the method of scratch test, thecritical loads of the films deposited at different substrate bias voltages and underthe conditions of Ti and TiN interlayer pretreatment were measured to researchthe effects of substrate bias voltages and interlayer pretreatment on adhesionstrength of nanometer amorphous diamond films. A portable surface roughnesstester and a drop shape analysis system were used to measure respectively theroughness and static contact angle of the coated and uncoated surfaces of Co-Cralloys and pure Ti, and the surface free energy was calculated then. Bycomparing the adhesion of Streptococcus mutans, Actinomyces viscosus andCandida albicans to the coated surfaces with that to the uncoated ones, weinvestigated the effects of nanometer amorphous diamond films deposited ondental Co-Cr alloys and pure Ti on bacterial adhesion. The main results of thisstudy were listed as the following.
1. The films deposited on the surfaces of dental Co-Cr alloys and pure Tiby the FCVA system had a nano-sized thickness and were composed of sp2andsp3bonded carbon atoms. Over70%of the carbon atoms in the films are sp3bonded. These results indicated that the deposited films came up to thequalitative standards of nanometer amorphous diamond films. With theincreased substrate bias voltages, the changes of sp3fraction in the films deposited on Co-Cr alloys and pure Ti presented a first increasing and thendecreasing tendency. The maximum sp3fraction in the films deposited on Co-Cralloys and pure Ti was obtained respectively at200v and250v.
2. The cell relative growth rate of nanometer amorphous diamond filmswas over90%and their graduations of cytotoxicity were0or1, which means nocytotoxicity. In addition, their mucosal stimulation index was0, which means nostimulation. Therefore, nanometer amorphous diamond films had verysatisfactory biocompatibility.
3. With the increased substrate bias voltages, the changes of adhesionstrength of nanometer amorphous diamond films to Co-Cr alloys and pure Tipresented a first increasing and then decreasing tendency. The optimal adhesionstrength of the films to Co-Cr alloys and pure Ti was obtained respectively at200v and250v. Ti and TiN interlayer pretreatment could significantly increasethe adhesion strength of nanometer amorphous diamond films to Co-Cr alloysand pure Ti. The optimal interlayer pretreatment on the substrate of Co-Cr alloysand pure Ti was Ti and TiN interlayer respectively.
4. After the surface treatment of nanometer amorphous diamond films, thesurface roughness of Co-Cr alloys and pure Ti significantly decreased. Inaddition, the films could significantly increase the surface free energy of Co-Cralloys but had no significant effects on that of pure Ti. Most importantly, afterthe coating surface treatment, the adhesion of Streptococcus mutans,Actinomyces viscosus and Candida albicans to Co-Cr alloys and pure Ti wassignificantly decreased. This result showed that nanometer amorphous diamondfilm surface treatment on dental Co-Cr alloys and pure Ti could significantlyreduce the bacterial adhesion.
本课题研究采用西安交通大学研制的过滤阴极真空电弧沉积系统在牙科钴铬合金及纯钛表面制备纳米非晶金刚石薄膜。首先，采用扫描电镜、原子力显微镜、拉曼光谱以及X射线光电子能谱表征纳米非晶金刚石薄膜的表面形貌、空间结构、元素成分和化学键构成，同时探讨样品偏压这一工艺参数对该薄膜质量的影响。随后，按照医疗器械生物学评价标准，通过体外细胞毒性实验和口腔粘膜接触实验，对纳米非晶金刚石薄膜的生物相容性能进行评价。接下来，采用常规划痕实验，测量不同样品偏压条件下以及Ti和TiN两种中间层预处理条件下纳米非晶金刚石薄膜的膜基临界载荷，并探讨样品偏压和中间层预处理对该薄膜结合强度的影响。最后，采用粗糙度仪和接触角测量系统测量镀膜前后钴铬合金及纯钛表面粗糙度和三种液体接触角，并计算镀膜前后两种牙科金属的表面自由能；通过细菌粘附实验比较镀膜前后钴铬合金及纯钛表面变形链球菌、白色念珠菌、粘性放线菌的粘附数量，并结合表面粗糙度和自由能的变化，深入探讨钴铬合金和纯钛表面所镀纳米非晶金刚石薄膜影响细菌粘附的机制。本课题研究的结果如下：
1.采用过滤阴极真空电弧沉积系统在钴铬合金及纯钛表面制备的薄膜具有纳米级厚度，由sp~3键和sp~2键碳原子组成，且sp3键含量大于70%，符合纳米非晶金刚石薄膜的质量标准。随样品偏压的增大，两种牙科金属镀膜的sp3键含量均呈现先升高后降低的趋势，钴铬合金和纯钛镀膜的最佳样品偏压分别为200v及250v。
2.纳米非晶金刚石薄膜的细胞相对增殖率均大于90%，细胞毒性评级≤1级，粘膜刺激指数为0，具备非常良好的生物相容性。
3.随样品偏压的增大，钴铬合金和纯钛镀膜的结合强度均呈现先升高后降低的趋势，其最佳样品偏压值分别为200v及250v。Ti和TiN两种中间层预处理后，纳米非晶金刚石薄膜与衬底的结合强度显著提高，钴铬合金采用Ti中间层时膜基结合强度最好，纯钛采用TiN中间层时膜基结合强度最佳。
4.镀膜后钴铬合金及纯钛的表面粗糙度均显著降低，同时，钴铬合金的表面能增大明显，但是纯钛表面能的变化不显著。经纳米非晶金刚石薄膜表面处理后，钴铬合金及纯钛表面变形链球菌、白色念珠菌及粘性放线菌的粘附数量均出现了显著降低，表明纳米非晶金刚石薄膜可以改善这两种义齿金属材料表面的细菌粘附性能。
As a very important dental material, metals are widely used in completeand removable partial dentures. Owing to the complicated microbial andacid-base circumstances in oral cavity, the surfaces of dental metal materialsmay suffer corrosion, discoloration and bacterial adhesion. These phenomenamay not only affect the appearance and useful life of dentures but also lead tosome denture-induced adverse effects and complications which will severelythreaten the health of human body. Therefore, it is very significant to find aneffective method of surface treatment to improve the surface properties of dentalmetal materials. In this study, nanometer amorphous diamond films researchedand developed by Xi'an Jiaotong University were applied to the surfacetreatment of dental Co-Cr alloys and pure Ti. The aims of this study were to finda new method to improve the surface properties of dental metal materials andprovide the theoretical and experimental bases for the clinical applications ofnanometer amorphous diamond films.
In this study, a filtered cathodic vacuum arc (FCVA) system was used toprepare nanometer amorphous diamond films on dental Co-Cr alloys and pureTi. Then, scanning electronic microscopy (SEM), Atomic force microscopy(AFM), Raman spectroscopy and X-ray photoelectron spectroscopy (XPS) wereused to analyze some characteristics of the coatings including the surfacemorphology, microstructure, elemental composition and the chemical bindingstates, and simultaneously the effects of substrate bias voltage on sp3fraction ofthe coatings were investigated. The biocompatibility of the deposited nanometeramorphous diamond films was investigated through in vitro cytotoxicity test andoral mucous membrane irritation test. Using the method of scratch test, thecritical loads of the films deposited at different substrate bias voltages and underthe conditions of Ti and TiN interlayer pretreatment were measured to researchthe effects of substrate bias voltages and interlayer pretreatment on adhesionstrength of nanometer amorphous diamond films. A portable surface roughnesstester and a drop shape analysis system were used to measure respectively theroughness and static contact angle of the coated and uncoated surfaces of Co-Cralloys and pure Ti, and the surface free energy was calculated then. Bycomparing the adhesion of Streptococcus mutans, Actinomyces viscosus andCandida albicans to the coated surfaces with that to the uncoated ones, weinvestigated the effects of nanometer amorphous diamond films deposited ondental Co-Cr alloys and pure Ti on bacterial adhesion. The main results of thisstudy were listed as the following.
1. The films deposited on the surfaces of dental Co-Cr alloys and pure Tiby the FCVA system had a nano-sized thickness and were composed of sp2andsp3bonded carbon atoms. Over70%of the carbon atoms in the films are sp3bonded. These results indicated that the deposited films came up to thequalitative standards of nanometer amorphous diamond films. With theincreased substrate bias voltages, the changes of sp3fraction in the films deposited on Co-Cr alloys and pure Ti presented a first increasing and thendecreasing tendency. The maximum sp3fraction in the films deposited on Co-Cralloys and pure Ti was obtained respectively at200v and250v.
2. The cell relative growth rate of nanometer amorphous diamond filmswas over90%and their graduations of cytotoxicity were0or1, which means nocytotoxicity. In addition, their mucosal stimulation index was0, which means nostimulation. Therefore, nanometer amorphous diamond films had verysatisfactory biocompatibility.
3. With the increased substrate bias voltages, the changes of adhesionstrength of nanometer amorphous diamond films to Co-Cr alloys and pure Tipresented a first increasing and then decreasing tendency. The optimal adhesionstrength of the films to Co-Cr alloys and pure Ti was obtained respectively at200v and250v. Ti and TiN interlayer pretreatment could significantly increasethe adhesion strength of nanometer amorphous diamond films to Co-Cr alloysand pure Ti. The optimal interlayer pretreatment on the substrate of Co-Cr alloysand pure Ti was Ti and TiN interlayer respectively.
4. After the surface treatment of nanometer amorphous diamond films, thesurface roughness of Co-Cr alloys and pure Ti significantly decreased. Inaddition, the films could significantly increase the surface free energy of Co-Cralloys but had no significant effects on that of pure Ti. Most importantly, afterthe coating surface treatment, the adhesion of Streptococcus mutans,Actinomyces viscosus and Candida albicans to Co-Cr alloys and pure Ti wassignificantly decreased. This result showed that nanometer amorphous diamondfilm surface treatment on dental Co-Cr alloys and pure Ti could significantlyreduce the bacterial adhesion.
引文
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