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优化了纯钛微弧氧化膜的制备工艺。将用优化后工艺制备的微弧氧化膜进行碱化处理,然后置于模拟体液(SBF)中培养,以观察其生物活性的优劣。采用正交设计法优化了实验方案,用综合评分法分析了氧化膜的孔隙率、孔密度和孔直径,确定最佳工艺条件为:正向电压400 V,占空比60%,频率550 Hz,氧化时间25 min。对在最佳工艺条件下制备的膜层进行了XRD、SEM和EDS测试,结果表明:优化工艺后生长的膜层由锐钛矿型的TiO2组成,陶瓷层表面分布大量微孔,孔隙率为0.70×108,孔密度为12%,孔径约为3μm。经碱化处理的膜层置于模拟体液中培养14 d后,膜层表面被生长出的类骨磷灰石完全覆盖,证明其具有良好的生物活性,且生长出的缺钙型磷灰石与人体自然骨成分相似。但是,随着培养时间的延长磷灰石层发生溶解。
Optimized the preparation of pure titanium micro-arc oxidation film. The micro-arc oxidation film prepared by the optimized process was alkalized and then cultured in simulated body fluid (SBF) to observe its biological activity. The orthogonal design method was used to optimize the experimental scheme. The porosity, pore density and pore diameter of the oxide film were analyzed by the comprehensive score method. The optimum process conditions were as follows: forward voltage 400 V, duty ratio 60%, frequency 550 Hz , Oxidation time 25 min. The results of XRD, SEM and EDS tests showed that the film grown by the optimized process consisted of anatase TiO2 with a large number of micropores distributed on the surface of the ceramic and the porosity was 0.70 × 108, hole density of 12%, pore size of about 3μm. Alkali-treated membrane was placed in simulated body fluid for 14 days, the surface of the membrane was completely covered by the growth of bone-like apatite, which proved to have good biological activity, and the growth of calcium-deficient apatite Similar to the body’s natural bone composition. However, the apatite layer dissolves with increasing incubation time.