等离子体电解氧化法制备不同锌含量的钙磷活性涂层与抗菌性能的关系

Study of relationship between different contents of zinc and antibacterial activity on calcium phosphate coating modified by plasma electrolytic oxidation method

目的:利用等离子体电解氧化技术,在纯钛表面制备不同锌含量的钙磷活性涂层,比较纯钛表面不同锌含量活性涂层的理化性能差异及其对牙龈卟啉单胞菌(P.gingivalis,Pg)及伴放线放线杆菌(A.actinomycetemcomitans,Aa)抗菌性能的影响。方法:在等离子体电解氧化的电解液中,每组各加入0.08 mol/L钙和0.06 mol/L磷,再分别向各组加入0.01、0.03、0.05 mol/L锌处理纯钛片,制成低、中、高3种不同锌含量的钙磷活性涂层,以不加锌组作为对照组。利用电子万能测试机检测涂层与钛基底的结合力,扫描电镜(SEM)观察钛片表面形貌,X线衍射(XRD)分析材料表面晶相结构,X射线光电子能谱仪(XPS)分析材料表面化学组成及元素成分。材料表面培养Pg和Aa后,应用扫描电镜和贴膜法评价锌含量与抗菌性能的关系。采用SPSS13.0软件包对数据进行统计学分析。结果:随着锌含量的提高,涂层的孔径及粗糙度随之增加;低锌组结晶优于高锌组;低锌组HA和Zn3P2含量较多,高锌组ZnO含量多。扫描电镜观察,随着锌含量的提高,材料表面Pg和Aa细菌数量逐渐减少,高锌组部分细菌出现裂解、坏死。通过贴膜法观察,随着锌含量的提高,材料表面Pg和Aa细菌数量逐渐减少,且4组间差异显著。结论:锌含量的变化会改变涂层的理化性能。高含量锌的钙磷涂层,抗菌性能最佳。

PURPOSE： Calcium phosphate activity coating containing different contents of zinc was deposited onto the surface of pure titanium modified by plasma electrolytic oxidation. The physical and chemical properties of different contents of zinc were compared among three groups, and the influence on antibacterial activity of P.gingivalis （Pg） and A. actinomycetemcomitans （Aa） was evaluated. METHODS： Pure titanium samples were treated in the electrolyte of plasma electrolytic oxidation with 0.08 mol/L calcium and 0.06 mol/L phosphorus, and 0.01, 0.03, 0.05 zinc was added to each group in order to deal with pure titanium plate. Titanium samples were divided into three groups： low, middle and high group according to zinc contents. The group without zinc was as control. The binding force of coating and titanium was tested by electric universal test machine. The topography of surfaces was observed under scanning electron microscope （SEM）. The crystalline structure of surfaces was determined by XRD. The chemistry and elements of surfaces were determined by XPS. Pg and Aa were seeded onto samples surfaces, and the antibacterial properties of four kinds of materials were evaluated by using scanning electron microscopy and the paster method. Statistical analysis was performed using SPSS 13.0 software package. RESULTS： It was found that the aperture and roughness were increased with theincrease of content of zinc. The crystallization of low zinc group was superior to high zinc group. The content of HA and Zn3P2 in low zinc group was more, but ZnO in high zinc group was more. Scanning electron microscope demonstrated that the number of Pg and A a decreased on the surface with the increase of the content of zinc, while the bacteria of high zinc group underwent lysis and necrosis. By using the paster method, the number of Pg and A a decreased on the surface with the increase of the content of zinc, and there was significant difference among the four groups. CONCLUSIONS： The change of zinc content will change the physical and chemical properties of the coating; at the same time, the antimicrobial property of calcium phosphate coating with high content zinc was the best.Supported by Science and Technology Projects of Shenyang City （F11-264-1-25）, Science and Technology Projects of Liaoning Province （2013225049） and Scientific Foundation for Youth of Stomatology Hospital of China Medical University （K101593-14-45）.