以二水磷酸氢钙(CaHPO4·2H2O)与碳酸钙(CaCO3)为原料,采用固相反应法合成α-磷酸钙(α-TCP)粉末,系统研究分散介质去离子水和乙醇,以及添加剂氟化钙(CaF2)的加入对合成α-TCP的影响及相转变的作用。结果表明:以水为分散介质的混合料球磨后由结晶较差的非化学计量的碳羟基磷灰石组成;经高温煅烧,由这种羟基磷灰石所制得的高温相α-TCP具有较好的室温稳定性。本实验在CaHPO4·2H2O与CaCO3的混合料中加入1.0或1.5wt％CaF2,分别在1350-1450℃和1250-1480℃煅烧,随炉自然冷却至室温,可获得高纯α-TCP粉末。CaF2可以降低β-TCP向α-TCP转变的相变势垒,有利于高温亚稳相α-TCP保留至室温,α-TCP的稳定性与CaF2的添加量有关。
The starting powders selected for solid-state reaction to synthesize alpha-tricalcium phosphate (α-TCP) were CaHPO4·2H2O and CaCO3. The effects of dispersed medium and
mineralizer CaF2 on the synthesis of α-TCP and phase transformation were investigated. The results show that a metastable high temperature phase (α-TCP) prepared by calcining the
nonstoichiometric hydroxyapatite powder with poor crystallization obtained by grinding the mixture in distilled water is more stable than those prepared by grinding the mixture in an ethanol system. A new
and easy route, based on the solid-state reaction and the addition of CaF2, was developed to synthesize alpha-calcium phosphate (α-TCP). For samples containing 1.0wt% and 1.5 wt% CaF2, calcined in
the range of 1350℃ to 1450℃ and 1350℃ to 1480℃, respectively, a pure phase α-TCP was obtained. The transition energy of β-TCP to α-TCP during cooling
process is decreased by adding some mineralizer CaF2. It will be helpful to keep the metastable high temperature phase (α-TCP) at room temperature. The stability of α-TCP in the course
of furnace cooling is also related to the content of CaF2.
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