等离子喷涂生物压电陶瓷复合涂层的制备与性能研究

发布时间：2018-04-22 19:59

本文选题：等离子喷涂 + 生物材料　；参考：《新疆大学》2015年硕士论文

【摘要】：随着现代医学的发展,组织替代和重建已经成为人们关注的热点,其关键性技术就是仿生材料的研发。Ti合金,羟基磷灰石(HA),聚乳酸(PLA)等是常用的生物材料。本文采取等离子喷涂工艺在Ti合金基体上喷涂制备生物压电陶瓷复合涂层,将羟基磷灰石(HA)与钛酸钡(BaTiO3)压电陶瓷复合制备生物活性材料,使其兼具生物活性与力电性能。Ti基体上等离子喷涂HA涂层已经被广泛研究,研究表明制备的涂层具有一定的生物性能和力学性能,但生物诱导活性并不高,在人体中也极容易剥落。为了进一步提高涂层的性能,作者在前人的基础上加入钛酸钡压电陶瓷,希望涂层具有一定的压电性能,利用骨生长的力电效应原理,来改善生物涂层的诱导活性,通过控制等离子喷涂工艺参数来提高涂层与基体的结合性能。为了确定试验最佳的工艺参数,采用正交试验设计合理的喷涂HA的工艺参数,选取喷涂距离、喷涂电压、喷涂电流为变量因素,喷涂电压在60-70V,喷涂电流500-700A,喷涂距离80-120mm,以附着强度为考察因素,最终确定合适的工艺参数为喷涂距离80mm,喷涂电压65V,喷涂电流600A,此时羟基磷灰石与Ti合金的附着强度达到最大值为25N。80-120mm内,随着喷涂距离的增大,涂层的附着强度减小,60-70V内,随着喷涂电压的增大,涂层的附着强度先增大后减小,500-700A内,随着喷涂电流的增大,涂层的附着强度先增大后减小。为了进一步提高陶瓷涂层与金属基体界面的润湿性,在羟基磷灰石中加入纯钛粉,采取以上得到的最佳工艺参数喷涂制备Ti/HA涂层,最后再加入钛酸钡陶瓷粉末,采取同样的工艺参数制备Ti/HA/Ba TiO3涂层。通过SEM/EDS对涂层进行形貌分析和成分分析,用划痕仪测试涂层与基体的附着强度,用Image J图像处理软件测试涂层孔隙率,通过对纯Ti、Ti/HA涂层、Ti/HA/BaTiO3涂层进行细胞培养试验,在37℃,0.25%CO2浓度下分别培养1d,4d,7d后,用CCK-8法测试细胞增值率,评价细胞毒性,然后用扫描电镜观察细胞的黏附状态。涂层SEM形貌结果表明:在喷涂距离80mm,喷涂电压65V,喷涂电流600A的喷涂工艺下,制备的三种涂层具有层叠状的组织结构,涂层熔化良好,有明显的熔滴铺展形貌。孔隙率测试结果表明:涂层具有一定的微孔结构,孔隙率大约在2.6%-8.6%之间。通过划痕试验测试附着强度表明:最优工艺参数下制备的三种涂层具有较高的附着强度,HA涂层为25N,Ti/HA涂层为35N,Ti/HA/BaTi O3涂层为27N,涂层与基体在界面处发生剥落失效。细胞毒性测试结果表明:纯Ti、Ti/HA涂层的细胞等级为1级,Ti/HA/BaTiO3的细胞毒性等级趋于0级,能够作为生物材料使用。通过对细胞的SEM形貌观察,细胞在涂层上面附着良好,有较多的细胞伪足伸出。通过细胞增值率的比较,Ti/HA/Ba TiO3涂层的细胞增值率比其他两种涂层的要高,这也说明了钛酸钡的加入对涂层的生物活性有了一定提高。以上结果表明,通过等离子喷涂工艺能够制备具有一定附着强度的Ti/HA/BaTiO3复合涂层,利用压电陶瓷的力电效应,能够改善HA的生物诱导活性,为进一步开发高性能的生物活性材料提供了参考依据。
[Abstract]:With the development of modern medicine, the replacement and reconstruction of tissue has become a hot spot of attention. The key technology is the research and development of biomimetic materials,.Ti alloys, hydroxyapatite (HA), polylactic acid (PLA) and so on as the common biomaterials. Hydroxyapatite (HA) and barium titanate (BaTiO3) piezoelectric ceramics are combined to prepare bioactive materials. The plasma spraying HA coating on.Ti substrate has been widely studied. The study shows that the coating has some biological and mechanical properties, but the bioactivity is not high, and it is also very important in the human body. In order to further improve the performance of the coating, the author added barium titanate piezoelectric ceramics on the basis of the predecessors. It is hoped that the coating has a certain piezoelectricity and the principle of the force and electricity effect of bone growth to improve the induction activity of the biological coating, and to improve the bonding performance of the coating and the substrate by controlling the parameters of the plasma spraying process. In order to determine the optimum technological parameters of the test, the orthogonal experiment was used to design the reasonable spraying process parameters of HA. The spraying distance, the spraying voltage and the spraying current were selected as the variables, the spraying voltage was 60-70V, the spraying current was 500-700A, the spraying distance was 80-120mm, and the adhesion strength was taken as the investigation factor. Finally, the suitable technological parameters were determined as the spraying distance. From 80mm, spraying voltage 65V and spraying current 600A, the adhesion strength of hydroxyapatite and Ti alloy reached the maximum value of 25N.80-120mm. With the increase of spray distance, the adhesion strength of the coating decreased, and the adhesion strength of the coating increased and then decreased with the increase of spraying voltage. In 500-700A, with the increase of spraying current, the coating was coated. The adhesion strength of the layer increases first and then decreases. In order to further improve the wettability of the interface between the ceramic coating and the metal matrix, the pure titanium powder is added to the hydroxyapatite, and the Ti/HA coating is prepared by the best technological parameters obtained above. Finally, the barium titanate ceramic powder is added, and the same process parameters are used to prepare the Ti/HA/Ba TiO3 coating. The coating was analyzed and analyzed by SEM/EDS. The adhesion strength of the coating and the substrate was tested by scratch tester. The porosity of the coating was tested by Image J image processing software. The cell culture test was carried out on pure Ti, Ti/HA coating and Ti/HA/BaTiO3 coating, and 1D, 4D and 7d were cultured at 37 degrees and 0.25%CO2 concentration, and the cell growth was tested by CCK-8 method. The adhesion status of cells was observed by scanning electron microscopy (SEM), and the morphology of the coated SEM showed that the three coatings prepared by spraying distance 80mm, spraying voltage 65V and spraying current 600A were stacked structure, the coating melted well, the droplet spreading morphology was obvious. The porosity test results were found. The results show that the coating has a certain microporous structure and the porosity is about 2.6%-8.6%. The adhesion strength of the three kinds of coatings prepared under the optimal process parameters shows that the coating has high adhesion strength, the HA coating is 25N, the Ti/HA coating is 35N, the Ti/HA/BaTi O3 coating is 27N, and the coating and the matrix are exfoliated at the interface. The results of toxicity test showed that the cell grade of pure Ti, Ti/HA coating was grade 1, the cytotoxicity grade of Ti/HA/BaTiO3 tended to 0, and could be used as biomaterial. By observing the SEM morphology of the cells, the cells were attached well on the coating and more cells were protruded out. Through comparison of cell value added rate, Ti/HA/Ba TiO3 coated cells The added value is higher than that of the other two kinds of coatings. It also shows that barium titanate has a certain increase in the biological activity of the coating. The above results show that the Ti/HA/BaTiO3 composite coating with certain adhesion strength can be prepared by plasma spraying process, and the bioactivity of HA can be improved by using the piezoelectric effect of the piezoelectric ceramic. It provides a reference for further developing high performance bioactive materials.

【学位授予单位】：新疆大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TG174.4

【参考文献】