节点文献
羟基磷灰石粉末的水热合成及动力学研究
Study on Kinetics of Hydrothermal Synthesis of Hydroxyapatite Powders
【摘要】 以CaHPO4·2H2O(DCPD)为前驱物,在0.1mol·L-1NaOH溶液中,100~200℃,2~12h条件下水热合成羟基磷灰石(HA)粉末。结果表明:HA晶粒尺寸和结晶程度随反应温度的提高和时间的延长而增大。提高反应温度,有利于晶粒沿c轴方向生长;延长反应时间,有利于晶粒沿a轴方向生长。在120~160℃、2~10h条件下可以得到HA纳米棒。水热合成过程中有缺钙磷灰石(DAP,Ca10~(HPO4)x(PO4)6-x(OH)2-x,0≤x≤1)形成,并经历β-TCP→DAP→HA这一转化过程。转化反应为二级反应,活化能为72.91kJ·mol-1,推测反应为表面控制反应。
【Abstract】 Hydroxyapatite(HA) powders were hydrothermal synthesized by using CaHPO4 ,2H20(DCPD) in 0.1mol. L-1 NaOH solution in an autoclave at 100-200C for 2 ~ 12h. X-ray diffraction(XRD), transmission electron microscopy (TEM) and fouier transform infrared spectroscopy(FTIR) were used to characterized the morphology, structure, crystal grain size and chemical composition of hydroxyapatite powder. The experiment results show that the width and length of the crystal particle and crystallinity of crystals increased continuously with the electrolyte temperature and reaction time. Increasing the electrolyte temperature make for hydroxyapatite crystal growing along the c axis, whereas, increasing reaction time make for hydroxyapatite crystal growing along the a axis. The sizes of the crystal grain for the Bragg reflection of (002) and (300) planes were 45 ~ 98nm and 30 ~ 64nm at 120 ~ 160C for 2 ~ 10h. The TEM micrograph showed that the nano-hydroxyapatite powders could be obtain under these conditions. Calcium-deficient hydroxyapatite (DAP, Ca10-x(HPO4)x(PO4)6-x(OH)2-x, 0< x<1) was formed under hydrothermal synthesis , because the powders had radicals of HPO42- and the powders were decomposed into the mixture of hydroxyapatite and B-calcium phosphate after sintering at 800C. The hydrothermal reaction underwent the following process: transferring form DCPD to B-calcium phosphate (B-TCP) rapidly, and then from B-TCP to DAP and HA. The reaction of hydrothermal hydroxyapatite was second order and the active energy was 72. 91kJ.mol-1 and therefore it was inferred that the rate of reaction was surface reaction control process.
- 【文献出处】 无机化学学报 ,Chinese Journal of Inorganic Chemistry , 编辑部邮箱 ,2003年10期
- 【分类号】O614.23;O643.1
- 【被引频次】40
- 【下载频次】413