热处理渗氮技术对镍钛合金根管预备器械表面防护作用研究  

Study on surface protection of Nitinol alloy for root canal preparation instruments by heat treatment nitriding process

作　　者：刘美霞 徐延[2] 顾贵松 林浩 张炳春[1] 张桂荣[2] 高淑春 王逸琳 LIU Mei-xia;XU Yan;GU Gui-song;LIN Hao;ZHANG Bing-chun;ZHANG Gui-rong;GAO Shu-chun;WANC Yi-lin(Institute of Metal Research,Chinese Academy of Sciences,Shenyang 110016,China;Shenyang Stomatological Hospital,Shenyang 110002,China;不详)

机构地区：[1]中国科学院金属研究所,辽宁沈阳110016 [2]沈阳市口腔医院,辽宁沈阳110002 [3]沈阳天贺新材料开发有限公司,辽宁沈阳110179

出　　处：《中国实用口腔科杂志》2022年第6期715-719,共5页Chinese Journal of Practical Stomatology

基　　金：辽宁省“兴辽英才计划”项目(XLYC1902073);沈阳市科技计划项目(20-205-4-070)。

摘　　要：目的研究热处理渗氮技术对镍钛(Ni-Ti)合金根管预备器械表面的防护作用。方法研究于2022年4—6月在中国科学院金属研究所基础实验室、东北大学科技园腐蚀中心进行。选取30个Ni-Ti合金试件随机分为Ni-Ti-N组和Ni-Ti组,每组各15个。Ni-Ti-N组试件采用热处理渗氮工艺制备氮化钛(TiN)涂层,在扫描电镜下观察涂层厚度,并通过X射线光电子能谱分析(XPS)对涂层表面成分进行确认。Ni-Ti组试件不做任何处理。采用纳米压痕方法及电化学实验检测2组试件的表面硬度和耐腐蚀性能。选取60支Ni-Ti根管锉随机分成2组进行Ni离子溶出实验,Ni-Ti-N′组(30支)采用与Ni-Ti-N组相同的涂层制备方法,Ni-Ti′组(30支)不做任何处理,并设置阴性对照组,检测浸泡1、10 d各组浸提液中Ni离子溶出量。结果扫描电镜观测Ni-Ti-N组试件表面涂层厚度为22.97~30.08μm,平均(25.34±4.10)μm。XPS分析结果提示,Ni-Ti-N组试件表面可以观测到TiN峰值,且N元素含量随着溅射时间的延长而增加,在溅射30 s后,N元素含量趋于稳定。Ni-Ti-N组试件表面硬度为2.34 GPa,与Ni-Ti组(2.37 GPa)相似。Ni-Ti-N组极化曲线整体向正电位方向移动,且自腐蚀电位(Ecorr)高于NiTi组。浸泡1、10 d后,3组Ni离子溶出量总的比较,差异均具有统计学意义(F值分别为44.542、27.383,均P<0.05);其中,Ni-Ti-N′组Ni离子溶出量均低于Ni-Ti′组,差异具有统计学意义(均P<0.05)。结论经热处理渗氮技术加工后的Ni-Ti合金防护涂层TiN能够提高Ni-Ti合金的耐腐蚀性,并对于Ni离子的溶出有着显著的抑制作用,且不影响Ni-Ti合金的硬度,为其临床研究奠定基础。Objective To investigate the protective effect of heat nitriding technology on the surface of Nitinol(Ni-Ti)alloy root canal instruments.Methods The research was conducted from April to June 2022 in the Basic Laboratory of Institute of Metal Research,Chinese Academy of Sciences and the Corrosion Center of Science Park,Northeastern University.A total of 30 specimens of Ni-Ti alloy were randomly divided into Ni-Ti-N group and Ni-Ti group,with 15 specimens in each group.The specimens in the Ni-Ti-N group were nitrided by heat treatment nitriding process to prepare titanium nitride(TiN)coating.The thickness of the coating was observed by scanning electron microscope(SEM),and the surface composition of the coating was confirmed by X-ray photoelectron spectroscopy(XPS).The specimens in the Ni-Ti group were not treated.The surface hardness and corrosion resistance of the two groups of specimens were measured by nano-indentation method and electrochemical test.A total of 60 root canal files were randomly divided into two groups for Nickel ion dissolution experiment.The 30 root canal files from the Ni-Ti-N′group was prepared by the same coating method as the Ni-Ti-N group,while the other 30 root canal files from Ni-Ti′group was not treated,and a negative control group was set up.The amount of Nickel ion dissolved in the leaching solution of each group after immersion for 1 and 10 days was detected.Results Scanning electron microscopy showed that the surface coating thickness of Ni-Ti-N group was 22.97-30.08μm,with an average o(f25.34±4.10)μm.XPS analysis showed that TiN peak could be observed on the surface of the Ni-TiN group,the content of N element increased with the extension of sputtering time,and the content of N element tended to be stable after sputtering for 30 s.The surface hardness of the specimens in the Ni-Ti-N group was 2.34 GPa,which was similar to that of the Ni-Ti group(2.37 GPa).The polarization curve of the Ni-Ti-N group shifted to the positive potential,and the Ecorrof the Ni-Ti-N group was high

关 键 词：热处理渗氮技术 镍钛合金 根管预备器械 镍离子溶出 

分 类 号：R78[医药卫生—口腔医学]