钛表面微弧氧化-微波水热法铜铌涂层的制备及抗菌性研究  

Preparation and antibacterial properties of a copperniobium coating on a titanium surface by a microarc oxidationmicrowave hydrothermal method

作　　者：王天琦 杜青[2] 谢伟丽[1] WANG Tianqi;DU Qing;XIE Weili(Department of Prosthodon-tics,College of Stomatology,Harbin Medical University,Harbin 150001,China;School of Materials Science and Engi-neering,Harbin Institute of Technology,Harbin 150001,China)

机构地区：[1]哈尔滨医科大学口腔医学院修复科,黑龙江哈尔滨150001 [2]哈尔滨工业大学材料科学与工程学院,黑龙江哈尔滨150001

出　　处：《口腔疾病防治》2021年第11期733-739,共7页Journal of Prevention and Treatment for Stomatological Diseases

基　　金：黑龙江省科技攻关项目(GC12C3053)。

摘　　要：目的在钛表面通过微弧氧化微波水热两步法制备铜铌抗菌涂层,对其表面结构和抗菌性能进行探究。方法以包覆微弧氧化涂层(MAO组)的钛为基体,通过微波水热法分别在低(MHLCu组)、中(MHMCu组)、高(MHHCu组)浓度的氯化铜溶液及草酸铌(MHNb组)溶液中引入铜、铌元素。通过能谱分析确定引入铜最多的组分,与草酸铌混合微波水热制备铜铌复合涂层(MHCu/Nb组)。通过扫描电子显微镜、X射线能谱仪及X射线衍射仪对各组试件微观结构、元素分布和物相成分进行表征;贴膜法测定涂层对大肠杆菌和金黄色葡萄球菌的抑菌效果。结果X射线能谱仪显示MHLCu、MHMCu、MHHCu组表面均引入了Cu元素,各组铜元素原子比例依次为(0.68±0.04)%、(1.17±0.06)%、(1.64±0.03)%,组间差异有统计学意义(P<0.01)。扫描电子显微镜显示MAO组表面呈火山口状多孔结构,MHLCu、MHMCu、MHHCu、MHNb、MHCu/Nb组均保持微孔形貌,随Cu^(2+)浓度增加,粗糙度增加;其中MHNb、MHCu/Nb组同时出现沟壑状结构。X射线衍射仪显示MAO组涂层主要由钛和锐钛矿相TiO_(2)组成,MHLCu、MHMCu、MHHCu、MHNb、MHCu/Nb组涂层主要由锐钛矿和金红石相TiO_(2)组成。与MAO组菌落相比,MHHCu、MHNb、MHCu/Nb组大肠杆菌和金黄色葡萄球菌均有不同程度减少,差异具有统计学意义(P<0.001);MHHCu组与MHCu/Nb组相比,菌落数差异无统计学意义(P>0.05)。结论微弧氧化微波水热两步法制备的含铜铌粗糙多孔的涂层可有效抑制大肠杆菌和金黄色葡萄球菌生长。Objective To prepare a coppernobium antibacterial coating on a titanium surface by a microarc oxidationmicrowave hydrothermal twostep method and to study its surface structure and antibacterial properties.Methods Using titanium coated with a microarc oxidation coating(MAO group)as the substrate,copper and niobium were introduced by a microwave hydrothermal method in low(MHLCu group),medium(MHMCu group)and high(MHHCu group)copper chloride solutions and niobium oxalate(MHNb group)solutions,respectively.The component with the highest copper content was determined by energy spectrum analysis,and the copperniobium composite coating(MHCu/Nb group)was prepared by microwave hydrothermal mixing with niobium oxalate.The microstructure,element distribution and phase composition of the specimens were characterized by scanning electron microscopy,energy dispersive spectrometry and Xray diffraction,and the bacteriostatic effect of the coating on Escherichia coli and Staphylococcus aureus was determined by the film method.Results Energy dispersive spectrometry showed that Cu was introduced onto the surface of the MHLCu,MHMCu,and MHHCu groups,and the atomic ratios of copper in each group were(0.68±0.04)%,(1.17±0.06)%,and(1.64±0.03)%.The difference between groups was statistically significant(P<0.01).Scanning electron microscopy showed a craterlike porous structure on the surface of the MAO group,and the MHLCu,MHMCu,MHHCu,MHNb,MHCu/Nb groups maintained micropore morphology.The roughness increased with increasing Cu^(2+)concentration,in which the MHNb and MHCu/Nb groups showed gully like structures simultaneously.Xray diffraction showed that the coating of the MAO group was mainly composed of titanium and anatase phase TiO_(2),and the coatings of the MHLCu,MHMCu,MHHCu,MHNb,MHCu/Nb groups were mainly composed of anatase and rutile phase TiO_(2).Compared with the MAO group,Escherichia coli and Staphylococcus aureus in the MHHCu,MHNb,MHCu/Nb groups decreased to varying degrees,with significant differences(P<0.001);compared with th

关 键 词：钛 涂层 表面处理 微弧氧化 微波水热 铜 铌 抗菌 大肠杆菌 金黄色葡萄球菌 

分 类 号：R78[医药卫生—口腔医学]