纯钛表面微弧氧化法制备含羟基磷灰石氧化膜的实验研究

Preparation of Hydroxyapatite-containing Titania Film on the Surface of Pure Titanium by Micro-arc Oxidation Technique

应用微弧氧化技术在纯钛表面制备含羟基磷灰石的氧化物膜。在氧化过程中,将钛试件放入含Ca、P电解液中,用直流脉冲电源处理。用扫描电镜(SEM)观察试件的表面和横断面形貌,X射线能谱(EDS)及X射线衍射(XRD)分析其元素成分和晶相结构。结果表明微弧氧化处理后,纯钛表面生成微孔结构的氧化膜,膜层厚度约20μm,由O、Ti、Ca和P四种元素组成。膜层表面有分布不均匀的火山丘状的微孔分布,直径小于5μm。膜层表面的钙磷原子比为1.63,界面处的钙磷原子比为0.51。膜层由金红石型和锐钛矿型二氧化钛及少量结晶相羟基磷灰石组成。微弧氧化技术在纯钛表面生成了内层致密外层多孔的晶相二氧化钛膜,同时含有少量羟基磷灰石,表明该技术在人工种植牙和人工骨关节等领域具有良好的医学应用前景。

A porous hydroxylapatite-containing titania film was prepared by an electrochemical oxidation method, i. e. micro-arc oxidation （MAO）. During the oxidation treatment, the titanium sample was immersed in electrolytic solution containing calcium acetate monohydrate and sodium biphosphate dihydrate by using a pulse power supply. The thickness, phase, composition and morphology of the oxide coating were monitored with X-ray diffraction （XRD） and scanning electron microscopy （SEM） with energy dispersive X-ray spectrometer （EDS）. The thickness of the MAO film is about 20 μm and the coating where each porous size is no more than 5μm was porous and uneven, without apparent interface to the titanium substrates. The coating formed in the Ca- and P-containing solution with MAO contained Ca and P along with Ti and O. The Ca/P ratio on the surface is 1.63, while that in the interface is 0.51. XRD showed that the porous coating was made up of anatase, mille and hydroxyapatite. Such MAO films are expected to have significant medical applications as dental implants and artificial bone joints.