CN106435544A - 一种钛合金基体上制备纳米羟基磷灰石梯度涂层的方法 - Google Patents

一种钛合金基体上制备纳米羟基磷灰石梯度涂层的方法 Download PDF

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CN106435544A
CN106435544A CN201610985992.7A CN201610985992A CN106435544A CN 106435544 A CN106435544 A CN 106435544A CN 201610985992 A CN201610985992 A CN 201610985992A CN 106435544 A CN106435544 A CN 106435544A
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尹海清
邱俊杰
曲选辉
何剑桥
张桐
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Abstract

一种钛合金基体上制备纳米羟基磷灰石梯度涂层的方法，涉及一种在钛合金基体上以生物惰性瓷作为过渡层的纳米HA/惰性瓷梯度涂层。提供工艺为浸涂‑烧结法。钛合金基体预处理，配制惰性瓷悬浮液和纳米HA/惰性瓷悬浮液，惰性瓷过渡层浸涂‑烧结和纳米HA/惰性瓷复合层浸涂‑烧结，烧结气氛为氩气。本发明制备梯度涂层引入了低熔点生物惰性瓷作为过渡层，解决了钛合金与HA因热膨胀系数和弹性模量的失配造成的结合力强度不够的问题。另一方面在800‑850℃的低温烧结不会造成HA的分解，保留了羟基磷灰石的生物活性和稳定性。此外该工艺简单易行，生产周期短，成本较低且可在复杂形状植入体上进行涂层制备。

Description

一种钛合金基体上制备纳米羟基磷灰石梯度涂层的方法
技术领域
本发明涉及一种制备纳米羟基磷灰石梯度涂层的方法，尤其是以低熔点生物惰性瓷作为过渡层进行低温烧结制备梯度涂层的方法，所得的梯度涂层保持了HA的生物活性和稳定性，与基体结合力良好。可作为生物植入医用材料。
背景技术
钛合金生物相容性较好，力学性能优良，但其硬度较低，耐磨性差，其耐蚀性依赖于表面的一层氧化膜，一旦氧化膜破坏又不能立即生成新的氧化膜，因此发生严重腐蚀，此外钛合金为生物惰性，不能有效促进骨粘附与生长。为防止钛合金磨损并提升钛合金材料的生物相容性，常在其上制备生物涂层。
羟基磷灰石(hydroxyapatite,HA)是钙磷灰石(Ca5(PO4)3(OH))的自然矿物。动物骨的无机成分主要是HA，HA具有良好的生物活性和组织相容性，并能与骨组织形成强有力的化学结合，但是其脆性大、韧性差因而限制了其单独应用(徐淑华,罗承萍,王迎军.羟基磷灰石生物活性梯度涂层材料的界面特点[J].中国有色金属学报,2002,12:163-167.)。因此，常在钛合金上制备HA涂层以获得优良的生物相容性、耐磨性、耐蚀性以及良好力学性能。在制备生物涂层时除了HA还可以引入其他具有优良生物相容性的材料。
目前常用HA涂层有以下几类:单一HA涂层、复合涂层、梯度涂层和纳米涂层。常用的钛合金/HA涂层制备技术包括电化学沉积法、溶胶-凝胶法、等离子喷涂法，此外还有热化学法、离子注入法、放电离子烧结法、涂敷-烧结法以及仿生矿化法等(Durdu S,Usta M.Thetribological properties of bioceramic coatings produced on Ti6Al4V alloy byplasma electrolytic oxidation[J].Ceramics International,2014,40(2):3627–3635.)。各种方法都有自己的缺陷如结合强度不高以及HA分解等问题。目前已投入商业应用的等离子喷涂制备工艺得到的HA涂层会由于高温而分解，造成涂层在植入后分解过快，不利于长期植入。因此寻找一种既能保证HA稳定性又能使涂层与基体结合良好的方法势在必行。生物植入用惰性瓷具有良好的生物相容性又有较低的熔融温度(约685℃开始软化)可作为过渡层在钛合金基体上上制备羟基磷灰石涂层。
发明内容
本发明涉及一种钛合金基体上制备纳米羟基磷灰石梯度涂层的方法，梯度涂层的获得包括钛合金的表面预处理、涂层悬浮液的制备、过渡层的浸涂-烧结和纳米HA/惰性瓷复合层的浸涂-烧结，其具体步骤如下：
1)钛合金基体预处理：
钛合金基体预处理采用砂纸机械打磨(150、400、600、800grit)、丙酮超声清洗、去离子水冲洗、酸蚀(10％HF+30％HNO3，蚀刻时间为6-10min)、酒精超声清洗、干燥。
2)悬浮液配制：
悬浮液包括过渡层和复合层悬浮液两种，过渡层悬浮液由惰性瓷粉和酒精按1:9的重量比例配置，复合层悬浮液由纳米HA:惰性瓷:酒精＝(17-20):(0-3):180的重量比配置，其中HA和惰性瓷占总重量的10％。两种悬浮液配制后都用超声波振荡25-35min，再磁力搅拌25-35min，使粉末充分混合且尽量减少团聚。
惰性瓷成分及其重量百分数(wt％)如下：60SiO2-(10～15)Al2O3-(10～15)K2O-(5～10)Na2O-(2～5)CaO-(1～3)ZrO2-(1～2)BaO-(0.1～0.5)TiO2-(0.1～0.5)Fe2O3-(0.1～0.5)MgO或CeO2、B2O3、Li2O、F、B2O3和CeO2。
3)过渡层的制备
在基体上先浸涂再烧结：
以浸涂(提拉速度为5mm/s)的方式在基体上涂覆惰性瓷悬浮液，还可以用其他涂覆方法如喷涂、电泳沉积、旋涂、静电吸附等。浸涂后室温放置24h干燥，再在鼓风干燥箱中以60℃干燥10-30min。
过渡层的烧结工艺为管式电阻炉中氩气气氛(流速2L/min)下以10℃/min的升温速度到800-850℃保温20-30min，以1℃/min的速度冷却。在钛合金基体上得到镜面的过渡瓷层。
4)复合层的制备
是在过渡层上先浸涂后烧结：
在步骤3)烧结后得到的过渡层上进行纳米HA/惰性瓷的浸涂，浸涂的方式是以浸涂(提拉速度为5mm/s)的方式在过渡层上涂覆纳米HA/惰性瓷悬浮液，还可以用其他涂覆方法如喷涂、电泳沉积、旋涂、静电吸附等。浸涂后室温放置24h干燥，再在鼓风干燥箱中以60℃干燥10-30min。
复合层的烧结工艺参数为管式电阻炉中氩气气氛(流速2L/min)下以10℃/min的升温速度到800-850℃保温20-30min，以1℃/min的速度冷却。在过渡层上得到复合层。
二次烧结后，在钛合金基体上得到成分呈梯度变化的纳米HA/惰性瓷梯度涂层。该梯度涂层内层为较致密的惰性瓷釉质层，由于瓷粉熔点较低，HA粉末会在瓷粉熔融状态下向液相中扩散，最后得到惰性瓷/HA梯度涂层，最外层主要为成分为HA且相对较疏松。
本发明的基体材料为Ti6Al4V、Ti13Nb13Zr以及其他生物医用钛合金。
本发明的优点在于：
本发明制备梯度涂层引入了低熔点生物惰性瓷作为过渡层，解决了钛合金与HA因热膨胀系数和弹性模量的失配造成的结合力强度不够的问题。另一方面在800-850℃的低温烧结不会造成HA的分解，保留了羟基磷灰石的生物活性和稳定性。此外该工艺简单易行，生产周期短，成本较低且可在复杂形状植入体上进行涂层制备。
附图说明
图1涂层示意图；其中C为钛合金基底，B为惰性瓷过渡层，A为纳米HA涂层。
图2为惰性瓷过渡层与基体结合截面SEM照片，(a、b、c、d、e、f样品为在基体上以800-850℃烧结惰性瓷过渡层后，再浸涂HA，然后分别在800℃、810℃、820℃、830℃、840℃和850℃烧结20-30分钟得到的涂层截面)。
具体实施方式
例1：Ti13Nb13Zr钛合金基体上以810℃保温30分钟烧结惰性瓷过渡层后，再在过渡层上以810℃保温30分钟进行HA涂层烧结，得到涂层结合截面如图2(a)所示，可以发现在此工艺参数下得到的涂层结合界面间隙较大，涂层结合性能也不佳。测得涂层结合力在7MPa到10MPa。
例2：Ti13Nb13Zr钛合金基体上以830℃保温30分钟烧结惰性瓷过渡层后，再在过渡层上以830℃保温30分钟进行HA涂层烧结，得到涂层结合截面如图2中c、d所示，可以发现在此工艺参数下得到的涂层结合界面间隙较例1所得涂层间隙更小，涂层结合性能也更佳。测得涂层结合力在12MPa到17MPa。
例3：Ti13Nb13Zr钛合金基体上以850℃保温30分钟烧结惰性瓷过渡层后，再在过渡层上以850℃保温30分钟进行HA涂层烧结，得到涂层结合截面如图2中c、d所示，可以发现在此工艺参数下得到的涂层结合界面间隙较例1和例2所得涂层间隙都更小，涂层结合性能也更佳。测得涂层结合力在15MPa到21MPa。

Claims (9)

1.一种钛合金基体上制备纳米羟基磷灰石梯度涂层的方法，其特征在于：梯度涂层的获得包括钛合金的表面预处理、涂层悬浮液的制备、惰性瓷过渡层的浸涂-烧结和纳米HA/惰性瓷复合层的浸涂-烧结，其具体步骤如下：
1)钛合金基体预处理：
2)悬浮液配制：
悬浮液包括过渡层悬浮液和复合层悬浮液两种，
3)过渡层的制备方式是在基体上先浸涂再烧结：
4)复合层的制备方式是在过渡层上先浸涂后烧结：
复合层烧结后，在钛合金基体上得到成分呈梯度变化的纳米HA/惰性瓷梯度涂层。
2.如权利要求1所述的一种钛合金基体上制备纳米羟基磷灰石梯度涂层的方法，其特征在于：所述步骤1中基体预处理采用砂纸机械打磨到800grit，再以丙酮进行超声清洗、以去离子水冲洗，酸蚀成分为HF体积百分比为10％且HNO3体积百分比为30％，蚀刻时间为6-10min，最后进行酒精超声清洗和干燥。
3.如权利要求1所述的一种钛合金基体上制备纳米羟基磷灰石梯度涂层的方法，其特征在于：过渡层悬浮液由惰性瓷粉和酒精按1:9的重量比例配置，复合层悬浮液由纳米HA:惰性瓷:酒精＝(17-20):(0-3):180的重量比配置，其中HA和惰性瓷占总重量的10％；两种悬浮液配制后都用超声波振荡25-35min，再磁力搅拌25-35min，使粉末充分混合且尽量减少团聚。
4.如权利要求3所述的一种钛合金基体上制备纳米羟基磷灰石梯度涂层的方法，其特征在于：所述惰性瓷成分及其重量百分数如下：60SiO2-(10～15)Al2O3-(10～15)K2O-(5～10)Na2O-(2～5)CaO-(1～3)ZrO2-(1～2)BaO-(0.1～0.5)TiO2-(0.1～0.5)Fe2O3-(0.1～0.5)MgO或CeO2、B2O3、Li2O、F、B2O3和CeO2。
5.如权利要求1所述的一种钛合金基体上制备纳米羟基磷灰石梯度涂层的方法，其特征在于：步骤3)所述的浸涂是以提拉速度为5mm/s的方式在基体上涂覆惰性瓷悬浮液，或者用喷涂、电泳沉积、旋涂、静电吸附的方式在基体上涂覆惰性瓷悬浮液；浸涂后室温放置24h干燥，再在鼓风干燥箱中以60℃干燥10-30min。
6.如权利要求1所述的一种钛合金基体上制备纳米羟基磷灰石梯度涂层的方法，其特征在于：步骤3)所述的烧结是在管式电阻炉中流速2L/min的氩气气氛以10℃/min的升温速度到800-850℃保温20-30min，以1℃/min的速度冷却。
7.如权利要求1所述的一种钛合金基体上制备纳米羟基磷灰石梯度涂层的方法，其特征在于：步骤4)所述的浸涂是在步骤3)烧结后得到的过渡层上进行纳米HA/惰性瓷的浸涂，浸涂的方式是以提拉速度为5mm/s的方式在过渡层上涂覆纳米HA/惰性瓷悬浮液，或者用喷涂、电泳沉积、旋涂、静电吸附的方式在过渡层上涂覆纳米HA/惰性瓷悬浮液；浸涂后室温放置24h干燥，再在鼓风干燥箱中以60℃干燥10-30min。
8.如权利要求1所述的一种钛合金基体上制备纳米羟基磷灰石梯度涂层的方法，其特征在于：所述步骤4)所述的复合层的烧结是在管式电阻炉中流速2L/min的氩气气氛以10℃/min的升温速度到800-850℃保温20-30min，以1℃/min的速度冷却；在过渡层上得到复合层。
9.如权利要求1所述的一种钛合金基体上制备纳米羟基磷灰石梯度涂层的方法，其特征在于基体材料为Ti6Al4V、Ti13Nb13Zr以及其他生物医用钛合金。
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