Advanced Biomaterials and Tissue Engineering Center, Huazhong University of Science and Technology, Wuhan 430074, People's Republic of China.
Biomed Mater. 2012 Aug;7(4):045009. doi: 10.1088/1748-6041/7/4/045009. Epub 2012 Jun 1.
Si-doped hydroxyapatite (Si-HA) has been intensively investigated as a promising bone biomaterial because of the biomineralization and bone formation benefit from silicon addition. In the current work, Si-HA samples were synthesized by the aqueous precipitation method. The sintering property of Si-HA was studied in terms of phase composition and transition, which was influenced by the Si doping percentage and sintering temperature. The results indicate that all the as-prepared and sintered low Si doping samples (Si% ≤ 1.6 wt%) possess HA phases; while the high Si doping samples (Si% ≥ 2 wt%) present amorphous phases as prepared, and largely or even completely transform to β-tricalcium phosphate (β-TCP) phase after sintering at 1250 °C. The Rietveld refinement on x-ray diffraction patterns was conducted to determine the particle sizes, microstrain factors and anisotropic distributions. According to the refined results, the calculated anisotropic particle sizes correspond to the observations made by transmission electron microscopy. The microstrains also present anisotropic distributions in all refinements. The accurate variation in the fine structure of Si-HA has been studied by the improved refinements after considering the anisotropic distribution.
掺硅羟基磷灰石(Si-HA)作为一种很有前途的骨生物材料受到了广泛的研究,因为硅的添加有利于生物矿化和骨形成。在本工作中,采用水热沉淀法合成了 Si-HA 样品。通过相组成和转变研究了 Si-HA 的烧结性能,其受到 Si 掺杂百分比和烧结温度的影响。结果表明,所有制备和烧结的低 Si 掺杂样品(Si%≤1.6wt%)都具有 HA 相;而高 Si 掺杂样品(Si%≥2wt%)在制备时呈非晶相,在 1250°C 烧结后大部分或甚至完全转变为β-磷酸三钙(β-TCP)相。通过 X 射线衍射图谱的 Rietveld 精修确定了晶粒尺寸、微应变因子和各向异性分布。根据精修结果,计算出的各向异性晶粒尺寸与透射电子显微镜观察结果一致。在所有精修中,微应变也呈现各向异性分布。通过考虑各向异性分布,对 Si-HA 的精细结构进行了改进后的精确变化研究。