CN108441805A - 一种采用复合技术制备钛基表面ha涂层的方法 - Google Patents
一种采用复合技术制备钛基表面ha涂层的方法 Download PDFInfo
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Abstract
本发明公开了一种采用复合技术制备钛基表面HA涂层的方法,具体包括如下步骤:步骤一:选用钛合金板作为基体材料,用砂纸打磨再使用丙酮将钛合金板表面清洗干净;步骤二:将羟基磷灰石粉末、钛粉末和氧化钇粉末按照48.4%:50%:0.6%的质量比均匀混合,并预先均匀铺设在钛合金板的表面;步骤三:用激光熔覆技术将步骤二中钛合金表表面预置的混合粉末熔覆;步骤四:在步骤三形成的混合粉末涂层的表面进行等离子喷涂;本发明采用激光熔覆技术制备出羟基磷灰石粉末、钛粉末和氧化钇粉末熔覆后形成的混合粉末过渡层,实现基体与表面层之间成分和结构上的过渡,以利于涂层与基体之间实现较高的结合强度,并减少残余应力。
Description
技术领域
本发明涉及生物医用材料领域,更具体的说,尤其涉及一种采用复合技术制备钛基表面HA涂层的方法,该方法用于制备骨组织植入物。
背景技术
钛及钛合金因其优良的综合力学性能与加工性能,在较早时期就被人们将其作为人体硬组织的修复和骨科植入物的材料。然而,当纯金属或其金属合金植入到体内后,由于体内环境具有一定的腐蚀性,因此金属植入物表面氧化膜会受到影响和破坏,光鲜的金属表面会暴露于体液中,金属材料释放出大量的金属离子到体液中,释放出的金属离子导致各种对人体健康有害的现象产生,如金属过敏、肉芽肿瘤,甚至肝癌。为了更好地制备出理想的植入物假体,根据临床的需要,在金属表面制备涂层,一方面保留金属优良的力学性能,另一方面发挥陶瓷涂层的生物相容性。
羟基磷灰石(HA)涂层作为一种生物活性陶瓷涂层,在植入物植入人体以后,HA涂层会与人体骨组织相互作用,从而形成骨性结合。HA涂层由于其成分与人体骨成分相似,并且具有优良的生物活性以及无毒、无害、不致癌等优点,同时对骨组织具有良好的诱导生长作用,因此成为了骨科植入物最主要的制作材料。
目前制备HA涂层的方法有:热喷涂、脉冲激光烧蚀动态混合、浸涂法、溶胶-凝胶法、电泳沉积法、仿生涂层、热等静压等。在上述这些方法中,等离子喷涂由于其制备的涂层与其他涂层比较具有更好的性能,是唯一一种被美国食品与药品管理局(FDA)批准来制备生物医学涂层的方法,但是利用等离子喷涂的方法制备的HA涂层存在以下缺点:
1、HA涂层的基本材料-HA粉末在高温的条件下容易分解;
2、等离子喷涂制备的HA涂层,其涂层与基体之间结合类型为机械结合,因此结合强度较低,HA涂层容易脱落;
3、HA涂层在体内短期内能表现出较好的性能,但从长期来看,由于HA涂层在体液中的易溶解性,不具备优良的长期稳定性。
激光熔覆作为表面改性技术得到了快速的发展,其作为一种表面改性技术已广泛应用于航空、航海,化学工业级生物医学装置,而制备的生物陶瓷涂层也表现出较大的优越性。但是激光熔覆的制备方法也不是完美的,其在制备过程钟也存在一些问题,如高温条件下HA易分解,在XRD中主要观察到的是HA分解后的一些杂相,需要进行热处理来重新结晶生成HA。
因此,设计一种充分利用激光熔覆和等离子喷涂这两种表面改性技术的优先,结合这两种技术制备出具有更好综合性能的钛基表面HA涂层的方法显得尤为必要。
发明内容
本发明的目的在于激光熔覆和等离子喷涂这两种表面改性技术在单独制备HA涂层时往往不能满足临床需求的问题,提出了一种采用复合技术制备钛基表面HA涂层的方法,结合激光熔覆和等离子喷涂这两种表面改性技术的优点,弥补彼此的不足,制备出综合性能更好,长期稳定性更好的涂层。
本发明通过以下技术方案来实现上述目的:一种采用复合技术制备钛基表面HA涂层的方法,该方法选用羟基磷灰石粉末和钛粉末,采用激光熔覆和等离子喷涂技术相结合的方法在钛合金板表面制备HA涂层,具体包括如下步骤:
步骤一:选用钛合金板作为基体材料,用砂纸打磨钛合金板的表面去除钛合金板表面的氧化层,再使用丙酮将钛合金板表面清洗干净;
步骤二:将羟基磷灰石粉末、钛粉末和氧化钇粉末按照48.4%:50%:0.6%的质量比均匀混合,并预先均匀铺设在步骤一种清洗干净后的钛合金板的表面,预置的羟基磷灰石粉末、钛粉末和氧化钇粉末的混合粉末厚度为0.4mm;
步骤三:用激光熔覆技术将步骤二中钛合金表表面预置的混合粉末熔覆,激光的功率为1200W,激光速度为3.8mm/s,激光熔覆后钛合金表面的混合粉末涂层厚度为0.19~0.21mm;步骤四:在步骤三形成的混合粉末涂层的表面进行等离子喷涂,喷涂的材料为质量分数为100%的羟基磷灰石粉末,喷涂电压为500V,喷涂电流为500A,喷涂距离为12cm,喷涂速度为400mm/s,喷涂的主气流压力为60PSI,辅助气流压力为30PSI,载气流压力为30PSI,送粉速度为2.0RPM,采用等离子喷涂技术喷涂的羟基磷灰石粉末涂层厚度为0.15mm。
进一步的,步骤二和步骤四中采用的羟基磷灰石粉末的纯度级别为BR,羟基磷灰石粉末的含量为99.5%,羟基磷灰石的平均粒径为5~20mm。
进一步的,步骤二中采用的钛粉的纯度级别为LR,钛粉的含量大于等于99.0%,粒度为2N(目)。
进一步的,步骤二中采用的氧化钇粉末的纯度级别为GR,氧化钇粉末的含量为99.99%。
进一步的,步骤三种激光熔覆后钛合金表面的混合粉末涂层厚度为0.2mm。
本发明的有益效果在于:本发明采用激光熔覆技术制备出羟基磷灰石粉末、钛粉末和氧化钇粉末熔覆后形成的混合粉末过渡层,实现基体与表面层之间成分和结构上的过渡,以利于涂层与基体之间实现较高的结合强度,并减少残余应力;在混合粉末过渡层上采用用等离子喷涂制备的羟基磷灰石粉末涂层则将直接与体液接触,有高的耐磨性和致密的表层与高结晶度、单一的物相,且该涂层的摩擦磨损小,在体液中的溶解速度慢,提高整体涂层的长期稳定性;本发明的关键技术是结合激光熔覆与等离子喷涂技术的优点,对相关的工艺参数进行优化,制备出综合性能优异、长期稳定性较好的复合涂层。
附图说明
图1是本发明HA涂层的制备示意图。
图2是本发明采用复合技术制备钛基表面HA涂层的宏观图。
图3是本发明采用复合技术制备钛基表面HA涂层在扫描电子显微镜下的视图。
具体实施方式
下面结合附图对本发明作进一步说明:
本发明激光熔覆技术所采用的设备是YAG激光器,YAG激光器属子固体激光器,是目前除CO2激光器以外应用最广泛的激光加工用激光器,其工作介质为YAG晶体,YAG是钇铝石榴石的简称,化学式为Y3Al5O12;本发明等离子喷涂技术所采用的设备是上海瑞法喷涂机械有限公司生产的DH1080型等离子喷涂系统。
如图1~3所示,本发明的钛合金板采用钛合金Ti-6Al-4V板材,即TC4钛合金板材,式样的几何尺寸为20mm×20mm×5mm,先用砂纸将钛合金板需要制备涂层的表面打磨去除表面氧化层,再用丙酮清洗掉油污。
再将羟基磷灰石粉末、钛粉末和氧化钇粉末按照48.4%:50%:0.6%的质量比均匀混合,并预先均匀铺设在步骤一种清洗干净后的钛合金板的表面,预置的羟基磷灰石粉末、钛粉末和氧化钇粉末的混合粉末厚度为0.4mm;其中采用的羟基磷灰石粉末的纯度级别为BR,羟基磷灰石的平均粒径为5~20mm;采用的钛粉纯度大于等于99.0%,粒度为2N(目);采用的氧化钇粉末纯度为99.99%。
再用激光熔覆技术将步骤二中钛合金表表面预置的混合粉末熔覆,激光形成的矩形光斑尺寸12mm×2mm,激光的功率为1200W,激光速度为3.8mm/s,激光熔覆后钛合金表面的混合粉末涂层厚度为0.19~0.21mm;
最后在混合粉末涂层的表面进行等离子喷涂,喷涂的材料为质量分数为100%的羟基磷灰石粉末,喷涂电压为500V,喷涂电流为500A,喷涂距离为12cm,喷涂速度为400mm/s,喷涂的主气流压力为60PSI,辅助气流压力为30PSI,载气流压力为30PSI,送粉速度为2.0RPM,采用等离子喷涂技术喷涂的羟基磷灰石粉末涂层厚度为0.15mm。
对制成的HA涂层进行测试,HA涂层的HA结晶度为96.7%,硬度为540HV,HA涂层孔隙率为5.4%。所制备的HA涂层的结合强度为20.1MPa,大于HA涂层植入物结合强度的标准要求≥15MPa(ISO 13779-2),与目前等离子喷涂制备的涂层结合强度16MPa相比要高出25%。
上述实施例只是本发明的较佳实施例,并不是对本发明技术方案的限制,只要是不经过创造性劳动即可在上述实施例的基础上实现的技术方案,均应视为落入本发明专利的权利保护范围内。
Claims (5)
1.一种采用复合技术制备钛基表面HA涂层的方法,其特征在于:该方法选用羟基磷灰石粉末和钛粉末,采用激光熔覆和等离子喷涂技术相结合的方法在钛合金板表面制备HA涂层,具体包括如下步骤:
步骤一:选用钛合金板作为基体材料,用砂纸打磨钛合金板的表面去除钛合金板表面的氧化层,再使用丙酮将钛合金板表面清洗干净;
步骤二:将羟基磷灰石粉末、钛粉末和氧化钇粉末按照48.4%:50%:0.6%的质量比均匀混合,并预先均匀铺设在步骤一种清洗干净后的钛合金板的表面,预置的羟基磷灰石粉末、钛粉末和氧化钇粉末的混合粉末厚度为0.4mm;
步骤三:用激光熔覆技术将步骤二中钛合金表表面预置的混合粉末熔覆,激光的功率为1200W,激光速度为3.8mm/s,激光熔覆后钛合金表面的混合粉末涂层厚度为0.19~0.21mm;
步骤四:在步骤三形成的混合粉末涂层的表面进行等离子喷涂,喷涂的材料为质量分数为100%的羟基磷灰石粉末,喷涂电压为500V,喷涂电流为500A,喷涂距离为12cm,喷涂速度为400mm/s,喷涂的主气流压力为60PSI,辅助气流压力为30PSI,载气流压力为30PSI,送粉速度为2.0RPM,采用等离子喷涂技术喷涂的羟基磷灰石粉末涂层厚度为0.15mm。
2.根据权利要求1所述的一种采用复合技术制备钛基表面HA涂层的方法,其特征在于:步骤二和步骤四中采用的羟基磷灰石粉末的纯度级别为BR,羟基磷灰石粉末的含量为99.5%,羟基磷灰石的平均粒径为5~20mm。
3.根据权利要求1所述的一种采用复合技术制备钛基表面HA涂层的方法,其特征在于:步骤二中采用的钛粉的纯度级别为LR,钛粉的含量大于等于99.0%,粒度为2N(目)。
4.根据权利要求1所述的一种采用复合技术制备钛基表面HA涂层的方法,其特征在于:步骤二中采用的氧化钇粉末的纯度级别为GR,氧化钇粉末的含量为99.99%。
5.根据权利要求1所述的一种采用复合技术制备钛基表面HA涂层的方法,其特征在于:步骤三种激光熔覆后钛合金表面的混合粉末涂层厚度为0.2mm。
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