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Thermal Expansion and Phase Stability Investigations on Cs-Substituted Nanocrystalline Calcium Hydroxyapatites

机译:Cs取代的纳米晶羟基磷灰石的热膨胀和相稳定性研究

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摘要

The high-temperature phase stability of Ca_(10-x)Cs_x(PO_4)_6(OH)_2, (x = 0-3) compositions synthesized by various wet chemical methods was investigated. The thermal expansion property of Ca_(10)(PO_4)_6(OH)_2 (abbreviated as CaHAp) and Cs-substituted CaHAp was measured by high-temperature XRD and dilatometry. The average crystallite size of the powders synthesized by wet chemical methods was found to be 10-50 nm range as shown by XRD and TEM. Up to 30 mol% Cs loading was observed to show only the apatite phase by XRD when the apatite powder was nanocrystalline in nature. However, high-temperature stability of the Cs-substituted system is limited to ≤5 mol%. Cs_3(PO_4) is observed to be separated out on heating the material above 773 K for compositions substituted with more than 5 mol% of Cs in the Ca-sublattice. The coefficient of thermal expansion measured by HTXRD is α_a = 12.42 × 10~(-6) K~(-1), α_c = 14.98 × 10~(-6) K~(-1); and α_a = 12.62 × 10~(-6) K~(-1), α_c = 12.57 × 10~(-6) K~(-1) for CaHAp and Ca_(9.78)Cs_(0.2)(PO_4)_6(OH)_(1.96), respectively, in the temperature range of 298-1083 K. Bulk thermal expansion measurements are seen to be in agreement with the lattice expansion results.
机译:研究了通过各种湿化学方法合成的Ca_(10-x)Cs_x(PO_4)_6(OH)_2,(x = 0-3)组合物的高温相稳定性。 Ca_(10)(PO_4)_6(OH)_2(缩写为CaHAp)和Cs-取代的CaHAp的热膨胀特性通过高温X射线衍射和热膨胀法测量。通过XRD和TEM显示,通过湿化学方法合成的粉末的平均微晶尺寸为10-50nm范围。当磷灰石粉末本质上是纳米晶体时,通过XRD观察到高达30mol%的Cs负载仅显示磷灰石相。但是,Cs-取代体系的高温稳定性被限制为≤5mol%。对于在Ca-亚晶格中被大于5mol%的Cs取代的组合物,观察到在加热到773 K以上的材料时,Cs_3(PO_4)被分离出来。 HTXRD测得的热膨胀系数为α_a= 12.42×10〜(-6)K〜(-1),α_c= 14.98×10〜(-6)K〜(-1);对于CaHAp和Ca_(9.78)Cs_(0.2)(PO_4)_6(α),α_a= 12.62×10〜(-6)K〜(-1),α_c= 12.57×10〜(-6)K〜(-1) OH)_(1.96)分别在298-1083 K的温度范围内。本体热膨胀测量结果与晶格膨胀结果一致。

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