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不同烧结温度下中空羟基磷灰石微球的物相、组织与织构性能的研究
Research on the Phase,Morphology and Textual Properties of the Hollow HAP Microspheres at Different Sintering Temperatures
【摘要】 利用锂钙硼玻璃的原位转化反应制备了表面由介孔组成的中空羟基磷灰石(HAP)微球。研究了不同烧结温度对微球的物相、组织、织构等性能的影响。通过X射线衍射仪(XRD)、扫描电镜(SEM)、比表面积分析仪、压汞仪与化学分析方法研究了不同烧结温度下中空HAP微球的物性与特征。结果表明,所制备的微球由缺钙HAP组成。随着烧结温度的提高,微球的结晶性能提高,晶粒尺寸增加。烧结温度700℃时,缺钙HAP发生分解,生成磷酸三钙新物相。所制备的HAP微球(90℃热处理)球壳由2~40nm的介孔组成,平均孔径最小。随着烧结温度的提高,平均孔径增加。烧结温度900℃时,微球表面出现微米级的小孔。所制备的中空HAP微球(90℃热处理)的比表面积最大,总孔体积最大,随着烧结温度的增加,比表面积与总孔体积减少。调节烧结温度,可获得不同物相、表面形貌、比表面积、总孔体积与小孔孔径的中空HAP微球,有利于获得具有缓释速率可在一定范围内调节的生物医用材料。
【Abstract】 Hollow hydroxappatite(HAP) microspheres with mesoporous surfaces were prepared by a Li-Ca-B glass in situ conversion process.The effects of sintering temperature on the morphology,phase composition,and textual properties of the HAP microspheres were investigated.The property and characterization of the hollow HAP microspheres were studied by scanning electron microscope,X-ray diffractometer,specific surface area analyzer,Hg porosimetry,and chemical analysis method,respectively.The results show that the resulting microspheres consisted of calcium deficient hydroxyapatite.With the increase of sintering temperature,the degree of crystallization was enhanced and the crystal size was increased.When the sintering temperature was 700 °C,calcium deficient HAP decomposed into biphasic mixture of β-calcium phosphate(new phase) and HAP.The as-prepared microspheres were mainly the mesopores in the range of 2~40 nm.The mean pore size increased with increasing sintering temperature,and at 900 °C,the pores in micrometer occurred on the surface of the HAP microspheres.The as-prepared microspheres had the highest specific surface and the biggest total pore volume.The specific surface area and total pore volume decreased with increasing sintering temperature.The surface morphology,phase composition,specific surface area and pore size can be modified by sintering the samples in a certain temperature range,which may be beneficial for its usage as drug delivers or biomedical materials with controlled delivery rate in a certain range.
【Key words】 calcium deficient hydroxyapatite; textual property; hollow microspheres; sintering; mesoporous materials;
- 【文献出处】 稀有金属材料与工程 ,Rare Metal Materials and Engineering , 编辑部邮箱 ,2012年S2期
- 【分类号】R318.08
- 【被引频次】4
- 【下载频次】272