Synthesis and thermal behaviour of β tricalcium phosphate precipitated from aqueous solutions

E. Salahi, J. Heinrich
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引用次数: 17

Abstract

Abstract In the present study, β tricalcium phosphate (β-TCP) was prepared by precipitation from aqueous solutions. Calcium nitrate tetrahydrate Ca(NO3)2.4H2O and diammonium hydrogen phosphate (NH4)2HPO4 salts with an initial Ca/P molar ratio of 1·5 were dissolved in distilled water and mixed at 20°C and pH 10. Phase evolution of the as received precipitate was studied by X-ray diffraction and infrared spectroscopy before and after calcination in a dry air atmosphere at temperatures in the range 200-1400°C for 1 h. Thermal behaviour was investigated by simultaneous thermal analysis (DTA-TG). Calcium and phosphorus contents of the as received precipitate were determined by the inductively coupled plasma technique, and a Ca/P molar ratio of 1·49 ± 0·01 was found. The densities of the as received precipitate and of powder calcined at 800°C were determined by picnometery to be 2·43 and 3·01 ± 0·05 g cm-3 respectively. The experimental data suggest the formation of an amorphous phase corresponding to a TCP-like composition, which is calcium deficient and contains a very small amount of HPO42- groups.
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从水溶液中沉淀的β磷酸三钙的合成及其热行为
摘要本研究采用沉淀法从水溶液中制备了β磷酸三钙(β- tcp)。将四水硝酸钙Ca(NO3)2.4H2O和初始Ca/P摩尔比为1.5的磷酸氢二铵(NH4)2HPO4盐溶解于蒸馏水中,在20℃、pH 10条件下混合。通过x射线衍射和红外光谱研究了接收到的沉淀在干燥空气中在200-1400℃范围内煅烧1小时前后的相演变。通过同步热分析(DTA-TG)研究了热行为。采用电感耦合等离子体技术测定了接收沉淀物中钙、磷的含量,Ca/P摩尔比为1.49±0.01。经皮测,800℃煅烧后的沉淀和粉末的密度分别为2.43和3.01±0.05 g cm-3。实验数据表明,形成了一种非晶相,对应于tcp样成分,该成分缺钙,含有极少量的HPO42-基团。
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