CN112063878B - 一种表面具有微纳结构的减磨医用钛合金及其制备方法 - Google Patents
一种表面具有微纳结构的减磨医用钛合金及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种表面具有微纳结构的减磨医用钛合金及其制备方法，该减磨医用钛合金表面具有微米级孔隙，微米级孔隙内部分布有纳米多孔结构，纳米多孔结构内附着有纳米Si3N4/TiN复相陶瓷；该制备方法包括以下步骤：(1)将纳米硅粉与医用钛合金粉末混合均匀；(2)将复合材料粉末采用真空感应熔炼工艺，制造医用钛基复合材料；(3)利用飞秒激光热源在医用钛基复合材料表面进行扫略加工。该钛基复合材料孔隙内附着的纳米Si3N4与TiN复相陶瓷，能够增强孔壁的支撑强度，Si3N4陶瓷具有自润滑功能，有助于耐磨性的提升，医用钛合金植入体与周围组织的嵌骨结合强度更高；钛基复合材料上的孔隙能够作为关节液的存储器，提高医用钛合金的耐磨性。
Description
技术领域
本发明涉及一种减磨医用钛合金及其制备方法，更具体地，涉及一种表面具有微纳结构的减磨医用钛合金及其制备方法。
背景技术
人工植入体长期与活体组织接触，在生物条件下须具有良好的稳定性，且不能对人体的组织、血液、免疫等系统产生不良影响。生物医用金属材料因具有较高的机械强度、韧性及抗疲劳性能是承载植入体的首选材料。钛及其合金与人体骨相近的弹性模量、优良的抗腐蚀性能及良好的生物相容性在临床上得到越来越广泛的应用。作为承载植入体而言，必然涉及应力作用下植入体与人骨间的腐蚀摩擦与磨损行为，而钛合金的一个缺点是耐磨性不足，导致钛合金植入体在人体生理环境中服役时因磨损而产生的磨屑极易引发细菌感染，甚至引发二次手术，给患者带来更严重的痛苦和经济负担。通过物理或化学气相沉积、溶胶凝胶、电化学沉积等表面改性方法，在医用钛合金沉积不同种类的陶瓷涂层一定程度上能有效提升其耐磨性。但钛合金植入体在人体服役过程中必然承载自然骨传递的压应力和腐蚀摩擦作用，对钛合金表面陶瓷涂层的膜/基结合强度提出了较高的要求，而陶瓷涂层与钛合金间物性差异大，造成膜/基界面应力大，给界面结合强度的提升带来较大难度，最终表现为涂层的过早失效。
发明内容
发明目的：本发明的目的是提供一种耐磨性能好、陶瓷相与基体结合界面强度高、使用过程中不产生磨屑的表面具有微纳结构的减磨医用钛合金，本发明的另一目的是提供该减磨医用钛合金的制备方法。
技术方案：本发明所述的表面具有微纳结构的减磨医用钛合金，表面具有微米级孔隙，微米级孔隙内部分布有纳米多孔结构，纳米多孔结构内附着有纳米Si3N4/TiN复相陶瓷。
其中，微米级孔隙尺寸为10～80μm，医用钛合金为TiNi合金。
本发明所述的表面具有微纳结构的减磨医用钛合金的制备方法，包括以下步骤：
(1)将纳米硅粉与医用钛合金粉末采用高能球磨工艺混合，获得混合均匀的复合材料粉末；
(2)将复合材料粉末采用真空感应熔炼工艺，制造医用钛基复合材料；
(3)利用飞秒激光热源在医用钛基复合材料表面进行扫略加工，形成负载有原位纳米Si3N4/TiN复相陶瓷的减磨医用钛合金。
其中，步骤1中混合纳米硅粉与医用钛合金粉末时在在氩气保护气氛下进行，纳米硅粉粒径20～100nm、医用钛合金粉末粒径15～62μm、纳米硅粉占总粉末的质量比为0.1～1.5wt.％，医用钛合金粉末为TiNi合金；步骤2中真空感应熔炼工艺温度为1350～1450℃；步骤3中飞秒激光脉冲能量为50～90μJ，在氮气与氩气的流量比为1～5:100的混合气氛环境下对医用钛基复合材料进行飞秒激光扫略加工。
工作原理：纳米硅粉与医用钛合金粉末经球磨均匀混合，采用真空感应熔炼工艺成形钛基复合材料，借助飞秒激光热源在钛基复合材料植入体表面扫略熔凝成形微米尺度的孔隙，孔隙内壁负载具有减磨功能的原位纳米Si3N4与TiN复相陶瓷分布均匀的纳米多孔结构，Si3N4与TiN复相陶瓷具有强化作用及润滑功能，附着在孔隙内提高了医用钛合金的耐磨性；同时高比面积纳米多孔结构具有较强的机械嵌合能力，以促进医用钛合金植入体与周围组织的嵌骨结合强度，提高钛合金的综合服役性能和使用寿命。
有益效果：本发明与现有技术相比，其显著优点是：1、在钛基复合材料孔隙内附着的纳米Si3N4与TiN复相陶瓷，能够增强孔壁的支撑强度，并降低钛合金摩擦过程中孔隙边缘应力，提高耐磨性；2、纳米Si3N4/TiN复合陶瓷相与钛合金基体具有较高的冶金结合界面强度，且Si3N4陶瓷具有自润滑功能，有助于耐磨性的显著提升；3、微米尺度孔隙为钛合金植入体周围组织向孔隙内生长提供了通道，且纳米多孔结构和原位纳米陶瓷相的比面积大，促进钛合金与骨组织间形成纤维组织膜，形成机械嵌合，使得医用钛合金植入体与周围组织的嵌骨结合强度更高；4、钛基复合材料上的孔隙直径仅为10～80μm，在单位面积能够表面具有更多数量的孔隙，作为关节液的存储器，有效润湿摩擦表面和避免干摩擦，从而提高医用钛合金的耐磨性。
附图说明
图1是实施例1表面形貌图。
具体实施方式
实施例1
(1)取1g纳米硅粉与999g医用TiNi合金粉末在氩气保护气氛下，纳米硅粉质量分数为0.1wt.％，采用高能球磨工艺，获得混合均匀的复合材料粉末；
(2)将复合材料粉末在1350℃温度下采用真空感应熔炼工艺，制造得到医用钛基复合材料；
(3)在氮气与氩气流量比为1:100的混合气氛环境下，利用激光脉冲能量为50μJ的飞秒激光热源在医用钛基复合材料表面进行扫略加工，形成负载有原位纳米Si3N4/TiN复相陶瓷的减磨医用钛合金。
图1为实施例1中制造的医用钛合金表面原位陶瓷减磨的微纳多孔结构的显微组织形貌图，可发现原位纳米Si3N4与TiN陶瓷相及钛合金基体界面结合较好，无明显冶金缺陷，同时，可看出原位纳米相分散于微米尺度多孔结构内壁，孔隙尺寸约20μm。
实施例2
(1)取8g纳米硅粉与992g医用TiNi合金粉末在氩气保护气氛下，纳米硅粉质量分数为0.8wt.％，采用高能球磨工艺，获得混合均匀的复合材料粉末；
(2)将复合材料粉末在1400℃温度下采用真空感应熔炼工艺，制造得到医用钛基复合材料；
(3)在氮气与氩气流量比为2:100的混合气氛环境下，利用激光脉冲能量为65μJ的飞秒激光热源在医用钛基复合材料表面进行扫略加工，形成负载有原位纳米Si3N4/TiN复相陶瓷的减磨医用钛合金。
实施例3
(1)取12g纳米硅粉与988g医用TiNi合金粉末在氩气保护气氛下，纳米硅粉质量分数为1.2wt.％，采用高能球磨工艺，获得混合均匀的复合材料粉末；
(2)将复合材料粉末在1450℃温度下采用真空感应熔炼工艺，制造得到医用钛基复合材料；
(3)在氮气与氩气流量比为4:100的混合气氛环境下，利用激光脉冲能量为75μJ的飞秒激光热源在医用钛基复合材料表面进行扫略加工，形成负载有原位纳米Si3N4/TiN复相陶瓷的减磨医用钛合金。
实施例4
(1)取15g纳米硅粉与985g医用TiNi合金粉末在氩气保护气氛下，纳米硅粉质量分数为1.5wt.％，采用高能球磨工艺，获得混合均匀的复合材料粉末；
(2)将复合材料粉末在1450℃温度下采用真空感应熔炼工艺，制造得到医用钛基复合材料；
(3)在氮气与氩气流量比为5:100的混合气氛环境下，利用激光脉冲能量为90μJ的飞秒激光热源在医用钛基复合材料表面进行扫略加工，形成负载有原位纳米Si3N4/TiN复相陶瓷的减磨医用钛合金。
实施例2、3和4中制造的医用钛合金表面原位陶瓷减磨的微纳多孔结构的磨损率在1.72～1.95×10-4mm3·N-1·m-1范围内，说明本发明提供的减磨医用钛合金能够实现有效提升医用钛合金植入体的耐磨性能。
Claims (6)
1.一种表面具有微纳结构的减磨医用钛合金的制备方法，其特征在于，所述医用钛合金表面具有微米级孔隙，所述微米级孔隙内部分布有纳米多孔结构，所述纳米多孔结构内附着有纳米Si3N4/TiN复相陶瓷，包括以下步骤：
（1）将纳米硅粉与医用钛合金粉末采用高能球磨工艺混合，获得混合均匀的复合材料粉末；
（2）将复合材料粉末采用真空感应熔炼工艺，制造医用钛基复合材料；
（3）利用飞秒激光热源在医用钛基复合材料表面进行扫略加工，形成负载有原位纳米Si3N4/TiN复相陶瓷的减磨医用钛合金；
飞秒激光脉冲能量为50～90 μJ，在氮气与氩气的流量比为1~5:100的混合气氛环境下对医用钛基复合材料进行飞秒激光扫略加工。
2.根据权利要求1所述的表面具有微纳结构的减磨医用钛合金的制备方法，其特征在于，所述微米级孔隙尺寸为10~80μm。
3.根据权利要求1所述的表面具有微纳结构的减磨医用钛合金的制备方法，其特征在于，所述步骤（1）中混合纳米硅粉与医用钛合金粉末时在氩气保护气氛下进行。
4.根据权利要求1所述的表面具有微纳结构的减磨医用钛合金的制备方法，其特征在于，所述步骤（1）中纳米硅粉粒径20～100 nm、医用钛合金粉末粒径15～62μm、纳米硅粉占总粉末的质量比为0.1～1.5 wt.%。
5.根据权利要求1所述的表面具有微纳结构的减磨医用钛合金的制备方法，其特征在于，所述步骤（1）中医用钛合金粉末为TiNi合金。
6.根据权利要求1所述的表面具有微纳结构的减磨医用钛合金的制备方法，其特征在于，所述步骤（2）中真空感应熔炼工艺温度为1350～1450℃。
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