高品质羟基磷灰石纳米粉体的制备及物理化学过程研究

以含结晶水的硝酸钙和五氧化二磷的醇溶液为前驱体精心控制反应过程用溶胶-凝胶法制备出高纯且粒度均匀的纳米级羟基磷灰石粉体.通过TEM,XRD,IR和TG-DTA等方法研究了不同温度下羟基磷灰石合成各阶段的相组成、相结构变化.结果表明,在200、300、400℃反应产量很低,产物主要由Ca（NO₃）₂、磷酸乙酯和非晶HA组成,随着温度的升高,HA的含量逐渐增多,Ca（NO₃）₂和磷酸乙酯含量逐渐减少.其中在300、400℃出现少量的β-Ca₂P₂O₇,和CaO.在500℃×2h处理下获得高品质的纳米级HA,与其它溶胶-凝胶法相比,本制备工艺简单,获得HA纯度高,粒度均匀,性能明显好于以前用类似方法所获得的产品,并适合大批量、纳米级HA的生产制备.

Preparation and Physicochemical Process of Nanosized Hydroxyapatite Powders with High Purity

In this paper, nano-sized hydroxyapatite powders were prepared by a sol-gel method with Ca(NO₃)₂·4H₂O and P₂O₅ ethanol solution as precursors. This process was simple without refluxing and the reactants were cheap compared with other sol-gel methods. The morphology and the phase structure were studied by TEM, XRD, IR, and TG-DTA. The nano-sized HA powders with high quality were prepared after the as-prepared powders were sintered at 500℃ for 2h. The results show that the mixture is composed of Ca (NO₃)₂, amorphous HA and ester phosphate at 200, 300 and 400℃. The amount of HA increases while the amount of Ca(NO₃)₂ and ester phosphate decreases with the increase of temperature. A small amount of β-Ca₂P₂O₇ and CaO is present at 300 and 400℃. This process is simple and appropriate to produce nano-sized HA powders in large quantities.