微弧氧化联合溶胶-凝胶工艺制备钛表面复合生物涂层的研究

目的探讨微弧氧化联合溶胶-凝胶工艺制备钛表面复合生物涂层。方法钛片根据表面处理工艺不同分为5组:对照组,MAO(微弧氧化组),MAO+Sol/gel(微弧氧化+溶胶-凝胶组),MAO+Sol/gel-LowZn(微弧氧化+溶胶-凝胶低锌组),MAO+Sol/gel-HighZn(微弧氧化+溶胶-凝胶高锌组)。利用扫描电镜(SEM)观察涂层表面形貌,X射线能谱分析仪(EDX)和X射线衍射仪(XRD)分析元素分布和成分,测厚仪测量涂层厚度;粗糙度测试仪测量表面粗糙度。结果 SEM下可见MAO组钛表面粗糙多孔,联合溶胶-凝胶处理后,钛表面更加平整紧密,EDX得出MAO+Sol/gel组钙磷元素的质量百分比分别为25.00%和15.49%,MAO+Sol/gel-Low Zn组和MAO+Sol/gel-High Zn组钙、磷、锌元素的质量百分比分别为22.87%、15.01%、1.82%与18.66%、15.60%、7.45%,XRD得出MAO+Sol/gel组、MAO+Sol/gel-Low Zn组和MAO+Sol/gel-High Zn组均可见特征性羟基磷灰石(HA)峰和Ca3(PO4)2峰,MAO+Sol/gel-High Zn组表面涂层厚度最高(10.40±0.49)μm(P<0.05),MAO+Sol/gel组表面粗糙度最高(1.17±0.10)μm(P<0.05)。结论应用微弧氧化联合溶胶-凝胶工艺,可在钛金属表面制备出HA涂层,并通过调节溶胶凝胶中Zn(NO3)2·6H2O的含量,制备出HA和不同含量锌离子的复合生物涂层。经过两种不同工艺联合处理后,钛表面涂层厚度逐渐增加,而粗糙度随着溶胶凝胶中锌离子的增加逐渐降低。

Preparation of composite coatings on titanium surface by micro-arc oxidation combined with sol/gel process

Objective To investigate the the preparation of titanium surface composite coatings by micro-arc oxidation combined with sol/gel process Methods The Ti specimens were divided into the following five groups according to different surface treatment methods: the control group, MAO, MAO+Sol/gel, MAO+Sol/gel-Low Zn, MAO+Sol/gel-High Zn. The SEM(scanning electron microscopy), EDX(energy dispersive X-ray analysis), XRD(X-ray diffraction), the thickness gauge and roughness tester were used to detected the properties of Ti specimens. Results Under the SEM, the surface of titanium in the MAO group was rough and porous. After the sol/gel treatment, the surface of the titanium was smoother and more compact.The EDX showed that the wt% of calcium and phosphorus in the MAO+Sol/gel group was 25.00% and 15.49%, the wt% of calcium, phosphorus and zinc in the MAO+Sol/gel-Low Zn group and the MAO+Sol/gelHigh Zn group were 22.87%, 15.01%, 1.82% and 18.66%, 15.60%, 7.45%, respectively.The XRD showed that characteristic hydroxyapatite peak and Ca3(PO4)2 peak were observed in MAO+Sol/gel group, MAO+Sol/gel-Low Zn group and MAO+Sol/gel-High Zn group. The surface coating thickness of the sol/gel-High Zn group was the highest(10.40±0.49) μm(P <0.05)and the surface roughness of the MAO+Sol/gel group was the highest(1.17±0.10)μm(P <0.05).Conclusion The hydroxyapatite coatings can be prepared on the surface of titanium by micro-arc oxidation combined with sol/gel process. The composite coatings of hydroxyapatite and different content of zinc ions can be prepared by adjusting the content of Zn(NO3)2·6 H2O in the sol-gel. After the combination of two different processes, the thickness of the titanium surface coatings gradually increases, and the roughness gradually decreases with the increase of zinc ions in the sol/gel.