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Crystallographic study of lead-substituted hydroxyapatite synthesized by high temperature mixing method under hydrothermal conditions

机译:水热条件下高温混合法合成铅取代羟基磷灰石的晶体学研究

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摘要

The solid solutions in the system of Ca and Pb hydroxyapatite, Ca10-χPbχHA (χ= 0-10), were successfully synthesized by high-temperature mixing method (HTMM) at 200ºC for 12 hours under hydrothermal conditions. The samples were characterized by X-ray diffraction, chemical analysis and electron microscopic observation, and the site of the metal ions in the solid solutions was analyzed with the Rietveld method. The lattice parameters of the solid solutions prepared by both of the methods didn’t vary linearly with Pb contents, and they have two turning points of 0.4 and 0.6 of Pb content. It was found that Pb ions in the solid solutions preferentially occupied the M (2) site in the apatite structure. HTMM gives Ca-Pb HA solid solutions much better crystallization. However, due to the formation of intermediate compound of Pb3O2(OH)2 in the Pb(NO3)2•4H2O solution before mixing with (NH4)2HPO4 solution at 200°C, HTMM causes the decrease of crystallization of the samples with high Pb content.
机译:在高温水热条件下,通过高温混合法(HTMM)在200ºC下成功地合成了Ca和Pb羟基磷灰石体系中的固溶体Ca10-χPbχHA(χ= 0-10)。通过X射线衍射,化学分析和电子显微镜观察对样品进行表征,并通过Rietveld方法分析固溶体中金属离子的位置。两种方法制得的固溶体的晶格参数均不随Pb含量线性变化,其转折点分别为Pb含量的0.4和0.6。已发现固溶体中的Pb离子优先占据磷灰石结构中的M(2)位置。 HTMM使Ca-Pb HA固溶体更好地结晶。但是,由于在200°C下与(NH4)2HPO4溶液混合之前,在Pb(NO3)2•4H2O溶液中形成了Pb3O2(OH)2中间化合物,因此HTMM导致高Pb样品的结晶减少内容。

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