Lin F H, Liao C J, Chen K S, Sun J S
Center for Biomedical Engineering, College of Medicine, National Taiwan University, Taipei, ROC.
Biomaterials. 1998 Jun;19(11-12):1101-7. doi: 10.1016/s0142-9612(98)00040-4.
In this paper, the high-temperature stabilized beta-tricalcium phosphate (betaTCP, beta-Ca3(PO4)2) were prepared by heating the deficient HAP (d-HAP, Ca10-x(HPO4)x(PO4)6-x(OH)2-x) with tetra-sodium diphosphate decahydrate (NP, Na4P2O7 x 10H2O) addition. The betaTCP, d-HAP and d-HAP doped with 2.5, 5, 7.5 and 10 wt % NP were heated to different temperatures and were investigated by X-ray diffraction analysis (XRD) and Fourier-transformed infrared spectroscopy (FTIR). The results demonstrated that the HPO4(2-) of d-HAP condensed into P2O7(4-) occurred before 650 degrees C. The P2O7(4-) ions could be traced in the FTIR spectrum when the d-HAP was heated up to 750 degrees C. The reaction of P2O7(4-) with OH- did not occur instantly but over a wide range of temperatures. The d-HAP doped with NP would decrease the decomposition temperature of d-HAP. NP doped into d-HAP not only induced the d-HAP decomposition at lower temperature but also stabilized the betaTCP crystal structure at higher-temperature. It could also increase the conversion temperature of betaTCP to alphaTCP from 1180 degrees C up to 1300 degrees C. We could successfully prepare high-temperature (up to 1300 C) stabilized ffTCP by heating NP doped d-HAP.
本文通过加热添加十水合二磷酸四钠（NP，Na4P2O7·10H2O）的缺钙羟基磷灰石（d-HAP，Ca10-x(HPO4)x(PO4)6-x(OH)2-x）制备了高温稳定的β-磷酸三钙（βTCP，β-Ca3(PO4)2）。将βTCP、d-HAP以及掺杂2.5、5、7.5和10 wt%NP的d-HAP加热到不同温度，并通过X射线衍射分析（XRD）和傅里叶变换红外光谱（FTIR）进行研究。结果表明，d-HAP中的HPO4(2-)在650℃之前缩合形成P2O7(4-)。当d-HAP加热到750℃时，FTIR光谱中可以检测到P2O7(4-)离子。P2O7(4-)与OH-的反应不是立即发生，而是在很宽的温度范围内发生。掺杂NP的d-HAP会降低d-HAP的分解温度。掺杂到d-HAP中的NP不仅能在较低温度下诱导d-HAP分解，还能在较高温度下稳定βTCP晶体结构。它还能将βTCP向αTCP的转变温度从1180℃提高到1300℃。通过加热掺杂NP的d-HAP，我们能够成功制备出高温（高达1300℃）稳定的βTCP。
