【作者】 罗平辉；

【导师】 赵玉涛；

【作者基本信息】 江苏大学 ， 材料加工工程， 2006， 硕士

【摘要】 本文利用磁控溅射技术在有机基体聚酰亚胺（PI）表面成功制备了HA/YSZ复合涂层。通过合理选择溅射工艺参数的优化后处理工艺，制备得到了成分均匀分布、生物活性优良的HA/YSZ生物活性复合涂层。利用X-射线衍射仪（XRD）、扫描电镜（SEM）、X射线能量色散谱（EDS）、傅立叶红外光谱（FTIR）等多种现代分析手段，研究了HA/YSZ复合涂层的物相组成、表面和界面微结构以及后处理工艺对涂层物相和微结构的影响，同时分析了HA/YSZ复合涂层在模拟体液（SBF）条件下生物活性及其机理。 采用溶胶—凝胶法制备微纳米级HA粉体以及HA/YSZ复合粉体。实验检测结果显示以磷酸三甲酯[（CH₃O）₃PO₄]和硝酸钙[Ca（NO₃）₂．4H₂O]为原料，乙二醇为表面活性剂，采用溶胶—凝胶法，静置过程对溶胶进行机械搅拌和超声振荡，可以制备出物相较纯、粒度均匀的HA粉体，粉体以短棒状为主，颗粒长度约为80nm，宽度约为20nm。 溅射靶材通过粉体热压烧结工艺制备而成。合理控制烧结工艺，可以制备得到成分与原始粉体一致的靶材。靶材致密较高，满足溅射用靶材的质量要求。 对溅射和后处理涂层XRD物相检测结果发现，用磁控溅射法制备的涂层HA为非晶结构；大气条件下对涂层200℃×2h热处理后，可使涂层中非晶相向晶相转化。EDS检测涂层表面特定点的n（Ca）/n（P）比约为1.62，与HA的化学计量值1.67还存在一定距离。SEM表面微观检测结果显示涂层厚度为6～8μm。涂层表面为粗糙多孔结构。 SBF浸泡实验发现本研究制备的复合涂层能够有效的诱导类骨磷灰石的形核和生长。新沉积涂层都结晶度较低，同时n（Ca）/n（P）为1.59（人体骨组织的化学计量值1.67），为缺钙磷灰石。通过测定SBF溶液中钙离子浓度变化发现热处理复合涂层具有较高的结晶度和结构完整性，因此浸泡SBF中降解速度较慢，而涂层中的杂质相CaO和TCP加速了涂层的降解。同时研究表明浸泡过程新生成的磷灰石晶粒平均尺寸很小，接近于无定形相，与自然骨中磷灰石结构相似。从而证实了本研究中制备的HA/YSZ复合涂层具有一定的生物活性。更多还原

【Abstract】 Yttria stabilized zirconia (YSZ) reinforced hydroxyapatite (HA) bio-composite coatings on polyimide (PI) substrate had been developed by R.F. magnetron sputtering technique. Bioactive HA/YSZ composite coatings with homogeneous composition were prepared by radio-frequency magnetron sputtering with proper processing parameter of sputtering and optimized post-treatment. Phase constitution, surface morphology and interfacial characterization of the composite coating were investigated with X-ray diffraction (XRD), scanning electronic microscopy (SEM), X-ray energy dispersion spectrum (EDS) and Fourier transform infrared spectroscopy( FTIR).The effect of post-treatment process on phase and microstructure of coatings were also studied. Furthermore, bioactivity of composite coatings and its mechanics in simulated body fluid (SBF) were discussed.Nano-hydroxyapatite powder was prepared by sol-gel technique and HA/YSZ composite powder was prepared by mixing ball milling process. The results indicated that HA powder with pure phase and homogeneous granularity could be prepared through the process as follows, trimethyl phosphate and calcium nitrate were used as starting material, and ethylene glycol was used surface activator, sol-gel technique was introduced aided with agitation and ultrasonic vibration. HA with homogeneous granularity were composed of short bar granule with 80nm length, 20nm width.After XRD analyzing for as-grown coating and post-treated coating, it was found that the HA coatings by magnetron sputtering were amorphous, but amorphous phase in coatings could be transform into crystalline via heat treatment with 200℃ × 2h in atmosphere. The Ca/P atomic ratios of the coating measured by EDS was 1.62 which slightly deviated from the ideal composition of Ca/P=1.67. The coating with 6～8μm thickness presented rough and porous surface configuration measured by cross-section SEM.It was found that composite coatings immersed in SBF prepared by magnetron sputtering could effectively induce bone-like apatite to nucleate and grow. The precipitate was of low crystallinity, and of which Ca/P=1.59 (Ca/P of osseous tissue更多还原