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α-磷酸三钙(α-TCP):不同钙前体的固相合成及水合反应性。

Alpha-tricalcium phosphate (α-TCP): solid state synthesis from different calcium precursors and the hydraulic reactivity.

机构信息

Graduate Department of Biomedical Engineering, Middle East Technical University, 06531 Ankara, Turkey.

出版信息

J Mater Sci Mater Med. 2011 Apr;22(4):809-17. doi: 10.1007/s10856-011-4283-x. Epub 2011 Mar 29.

Abstract

The effects of solid state synthesis process parameters and primary calcium precursor on the cement-type hydration efficiency (at 37 °C) of α-tricalcium phosphate (Ca(3)(PO(4))(2) or α-TCP) into hydroxyapatite (Ca(10-x)HPO(4)(PO(4))(6-x)(OH)(2-x) x = 0-1, or HAp) have been investigated. α-TCP was synthesized by firing of stoichiometric amount of calcium carbonate (CaCO(3)) and monetite (CaHPO(4)) at 1150-1350 °C for 2 h. Three commercial grade CaCO(3) powders of different purity were used as the starting material and the resultant α-TCP products for all synthesis routes were compared in terms of the material properties and the reactivity. The reactant CaHPO(4) was also custom synthesized from the respective CaCO(3) source. A low firing temperature in the range of 1150-1350°C promoted formation of β-polymorph as a second phase in the resultant TCP. Meanwhile, higher firing temperatures resulted in phase pure α-TCP with poor hydraulic reactivity. The extension of firing operation also led to a decrease in the reactivity. It was found that identical synthesis history, morphology, particle size and crystallinity match between the α-TCPs produced from different CaCO(3) sources do not essentially culminate in products exhibiting similar hydraulic reactivity. The changes in reactivity are arising from differences in the trace amount of impurities found in the CaCO(3) precursors. In this regard, a correlation between the observed hydraulic reactivities and the impurity content of the CaCO(3) powders--as determined by inductively coupled plasma mass spectrometry--has been established. A high level of magnesium impurity in the CaCO(3) almost completely hampers the hydration of α-TCP. This impurity also favors formation of β- instead of α-polymorph in the product of TCP upon firing.

摘要

研究了固相反响参数和初级钙前体对 α-磷酸三钙(Ca(3)(PO(4))(2)或α-TCP)向羟磷灰石(Ca(10-x)HPO(4)(PO(4))(6-x)(OH)(2-x),x=0-1,或 HAp)的水泥型水合效率(37°C)的影响。α-TCP 通过在 1150-1350°C 下煅烧化学计量比的碳酸钙(CaCO(3))和单磷酸钙(CaHPO(4))2 小时。使用三种不同纯度的商业级 CaCO(3)粉末作为起始材料,比较了所有合成路线的反应物 CaHPO(4),并比较了所有合成路线的反应性。结果表明,反应温度在 1150-1350°C 范围内,促进了β-多晶型物作为 TCP 中第二相的形成。同时,较高的煅烧温度导致单相α-TCP 的形成,但其水合反应性较差。煅烧操作的延长也导致反应性降低。研究发现,不同 CaCO(3)来源的α-TCP 具有相同的合成历史、形态、粒径和结晶度,并不一定导致具有相似水合反应性的产品。反应性的变化是由于 CaCO(3)前体中痕量杂质的差异造成的。在这方面,已经建立了观察到的水合反应性与 CaCO(3)粉末中杂质含量之间的相关性——通过电感耦合等离子体质谱法确定。CaCO(3)中高水平的镁杂质几乎完全阻碍了α-TCP 的水合作用。这种杂质也有利于在 TCP 的产物中形成β-而不是α-多晶型物。

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