本文以明胶、硝酸钙Ca(NO3)2和磷酸氢二铵(NH4)2HPO4为前驱体,初始Ca/P为1.5,制备了纯相的β-磷酸三钙.红外谱图和X射线晶体衍射结果表明,溶液中直接沉淀得到的产物为缺钙磷灰石,该产物在明胶浓度≥0.22％(质量分数)时热转化为纯相的β-磷酸三钙.通过晶体尺寸计算和比表面积测定,缺钙磷灰石的晶体大小随着明胶用量的增加而变小.透射电镜结果显示溶液中直接沉淀的缺钙磷灰石呈针状形貌,经过高温煅烧后,针状的缺钙磷灰石将相互融合形成葡萄状的β-磷酸三钙.差热/热重结果表明,明胶与生成的缺钙磷灰石形成了化学键合,这将有助于吸附较多的水分子,随后水分子与缺钙磷灰石发生化学反应生成羟基磷灰石,羟基磷灰石继续与沉淀中的偏磷酸钙反应生成β-磷酸三钙.本文还研究了明胶对纯相β-磷酸三钙的生成机理.
Pure β-tricalcium phosphate(β-TCP)was synthesized using the precipitation method,starting from the gelatin,Ca(NO3)2 and(NH4)2 HPO4 precursors by adopting the initial Ca/P ratio of 1.5.FT-IR spectroscopy and X-ray diffractometry indicated the solution derived precipitate was calcium deficient phosphate(Ca-dHAP)and it would thermally transform into pure β-TCP as the amount of gelatin exceeds 0.22％(mass concentration).The Ca-dHAP crystal dimensions decreased with increasing gelatin amount as shown by crystallite calculation and SSA measurement.TEM results showed that the as prepared Ca-dHAP powders were needle-like and formed a botryoidal shape characteristic of β-TCP when being calcined at high temperatures.The DTA/TG results showed thatgelatin chemically bonded with the Ca-dHAP crystals which could be beneficial for the absorption of water molecules and the absorbed water molecules,then subsequently reacted with Ca-dHAP to form HA which would react with a second phase calcium pyrophosphate(Ca2P2O7)(CPP)to prepare pure β-TCP.In this paper,we also studied the mechanism of gelatin on the formation of β-TCP.
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