张宪明,蔡丁森,钱仕.医用钛表面石墨烯薄膜的PECVD法制备及其性能[J].表面技术,2024,53(8):156-162, 190.
ZHANG Xianming,CAI Dingsen,QIAN Shi.Preparation and Properties of Graphene Films on Medical Titanium by PECVD Method[J].Surface Technology,2024,53(8):156-162, 190
医用钛表面石墨烯薄膜的PECVD法制备及其性能
Preparation and Properties of Graphene Films on Medical Titanium by PECVD Method
投稿时间:2023-07-16  修订日期:2023-12-10
DOI:10.16490/j.cnki.issn.1001-3660.2024.08.014
中文关键词:  等离子体增强化学气相沉积  医用钛  石墨烯  耐腐蚀性  细胞相容性
英文关键词:plasma enhanced chemical vapor deposition  medical titanium  graphene films  corrosion resistance  cell compatibility
基金项目:宁波市高层次人才和高端创业创新团队资助项目(2018A-09-C);国家自然科学基金面上项目(31971259)
作者单位
张宪明 慈溪生物材料表面工程中心,浙江 宁波 315300;中国科学院上海硅酸盐研究所 高性能陶瓷与超微结构国家重点实验室,上海 200050 
蔡丁森 慈溪生物材料表面工程中心,浙江 宁波 315300 
钱仕 慈溪生物材料表面工程中心,浙江 宁波 315300;中国科学院上海硅酸盐研究所 高性能陶瓷与超微结构国家重点实验室,上海 200050 
AuthorInstitution
ZHANG Xianming Cixi Center of Biomaterials Surface Engineering, Zhejiang Ningbo, 315300, China;State Key Laboratory of High Performance Ceramics and Superfine Microstructure, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China 
CAI Dingsen Cixi Center of Biomaterials Surface Engineering, Zhejiang Ningbo, 315300, China 
QIAN Shi Cixi Center of Biomaterials Surface Engineering, Zhejiang Ningbo, 315300, China;State Key Laboratory of High Performance Ceramics and Superfine Microstructure, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China 
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中文摘要:
      目的 在医用钛表面制备石墨烯薄膜,研究生长时间对石墨烯薄膜理化性能和生物学性能的影响。方法 采用等离子体增强化学气相沉积设备,在医用钛表面制备石墨烯薄膜,控制石墨烯薄膜生长时间为5、10、30 min。通过拉曼光谱、扫描电子显微镜、接触角测量仪和电化学工作站对石墨烯薄膜的结构、表面形貌、表面润湿性和耐腐蚀性进行表征,通过小鼠成骨细胞培养评价石墨烯薄膜的细胞相容性。结果 薄膜的拉曼结果呈现石墨烯的D、G和2D特征峰。生长时间为10 min和30 min的石墨烯薄膜在医用钛表面呈现垂直纳米片状态。随着生长时间的延长,医用钛表面石墨烯薄膜的水接触角逐渐增大。3组样品中,生长时间为5 min的样品具有最小的腐蚀电流密度(1.822×10‒7 A/cm2),生长时间为10 min的样品具有最高的腐蚀电位(‒0.404 V);生长时间为5 min和10 min的样品有利于细胞的黏附与铺展,生长时间为30 min的样品对小鼠成骨细胞活性具有一定的抑制作用。结论 石墨烯薄膜可以有效提高医用钛的耐腐蚀性。石墨烯薄膜生长时间影响其形貌,进而改变水接触角。不同生长时间的石墨烯薄膜对小鼠成骨细胞的黏附和铺展表现出明显的差异。
英文摘要:
      Graphene is a two-dimensional carbon nanomaterial consisting of a single layer of carbon atoms arranged in a hexagonal lattice. It has attracted extensive attention in many fields due to its unique chemical structure and excellent performance. Many researchers confirm that graphene-based nanomaterials have certain antibacterial and osteogenic properties. However, there is little study on in-situ preparation of graphene on medical titanium. In order to construct graphene films on medical titanium, plasma enhanced chemical vapor deposition (PECVD) method was used in this study. Methane, argon, and hydrogen were flowed into the reaction chamber as carbon source, carrier gas, and etching gas, respectively. The influences of growth time on the physical, chemical and biological properties of graphene films were studied. The growth time of graphene was set to be 5 min, 10 min, and 30 min. The structure, surface morphology, surface wettability, and corrosion resistance of graphene films were analyzed by Raman, scanning electron microscope, contact angle tester, and electrochemical workstation, respectively. The cytocompatibility of graphene films was evaluated by culturing mouse osteoblasts. Cell adhesion and spreading, cell proliferation, and cell morphology of mouse osteoblasts on the graphene films were systemically studied. The Raman results indicated that graphene films contained D, G, and 2D characteristic peaks. The graphene films with a growth time of 10 min and 30 min presented a vertical nano sheet state on the medical titanium surface. The water contact angle of graphene films with a growth time of 5 min, 10 min, and 30 min was 94.7°, 100.5°, and 122.7°, respectively. With the increasing of growth time, water contact angle of graphene films on the medical titanium surface increased gradually, which might be the influence of vertical nanosheet structure. Among the three graphene films groups, the sample with graphene growth time of 5 min had the minimum corrosion current density of 1.822×10‒7 A/cm2. The sample with graphene growth time of 10 min had the highest corrosion potential of ‒0.404 V. Graphene films improved corrosion resistance of titanium. Graphene films growing for 5 min and 10 min were beneficial to the cell adhesion and spreading. Graphene films growing for 30 min had an inhibitory effect to some extent on the cell adhesion and spreading, and viability of mouse osteoblasts, which attributed to surface morphology and hydrophobic properties. In short, graphene films are prepared with different morphology on medical titanium by adjusting the growth time in this study. Graphene films can effectively improve the corrosion resistance of medical titanium. The morphology of graphene films is affected by the growth time and then the water contact angle is changed. Graphene films with different growth time show obvious differences in the adhesion and spread of mouse of mouse osteoblasts.
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