微波烧结法制备TCP/TTCP复合生物陶瓷材料的研究

Study on the TCP/TTCP Calcium Phosphate Composite Bio-ceramics Prepared by Microwave Sintering Method

采用微波烧结方法制备TCP/TTCP复合磷酸钙生物陶瓷材料,以四水硝酸钙(Ca(NO3)2.4H2O)和磷酸氢二铵((NH4)2HPO4)为初始原料制备磷酸三钙(TCP)和磷酸四钙(TTCP)。研究了当TCP/TTCP(物质的量)配比为1:1时,不同的烧结温度对复合钙磷陶瓷的结构和晶相的影响。对烧结后的样品在模拟体液中进行了浸泡实验,监测了浸泡过程中的pH值变化,通过扫描电镜、X射线衍射分析对浸泡后试样的结构和晶相的变化进行了分析。结果表明微波烧结制备的磷酸钙生物陶瓷的主晶相是HA,其结构均匀,致密度较好。且在1200℃下微波烧结HA能稳定存在,陶瓷具有良好的表面生物活性。浸泡溶液的pH值变化幅度小(在7.40～7.72之间),接近中性。

TCP/TTCP calcium phosphate composite bio-ceramics were prepared by microwave sintering method, TCP and TTCP was synthesized from Ca（ NO3 ）2·4H2O and （NH4）2HPO4 respectively. The influence of sintering temperature on the structure and crystalline phases of the composite ceramics was studied as TCP/TrcP （mole） ratio was 1. The immersion tests of the samples sintered by microwave was done in simulation body fluid （ SBF）, the variety of fluid pH during immersion process was tested. The structure and crystalline phases of the samples immersed in simulation fluid for different periods were also analyzed by SEM and XRD. The results showed that the main phase of the microwave sintered bioceramics was HA, the microstructure of the bio-ceramics was uniform and its density was good. HA existed stably in the bio-ceramics as sintered by microwave at 1200 ℃, and the ceramics had good bioactivity. The pH value of SBF solution changed from 7.2 to 7.8 during immersion, closed to neutral.