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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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The high-temperature phase stability of Ca10−x Cs x (PO4)6(OH)2, (x = 0–3) compositions synthesized by various wet chemical methods was investigated. The thermal expansion property of Ca10(PO4)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%. Cs3(PO4) 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 αa = 12.42 × 10−6 K−1, αc = 14.98 × 10−6 K−1; and αa = 12.62 × 10−6 K−1, αc = 12.57 × 10−6 K−1 for CaHAp and Ca9.78Cs0.2(PO4)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:Ca 10−x Cs x (PO 4 6 (OH)<的高温相稳定性研究了用各种湿化学方法合成的sub> 2 (x = 0–3)组合物。 Ca 10 (PO 4 6 (OH) 2 (缩写为CaHAp)的热膨胀性质和通过高温X射线衍射和膨胀法测量Cs-取代的CaHAp。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10–50 nm。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。然而,Cs-取代体系的高温稳定性被限制为≤5mol%。观察到加热到773 K以上的材料时,对于取代了Ca子晶格中超过5 mol%Cs的成分,Cs 3 (PO 4 )会被分离出来。 HTXRD测量的热膨胀系数为α a = 12.42×10 -6 K -1 ,α c = 14.98×10 −6 K −1 ;和α a = 12.62×10 −6 K -1 ,α c = 12.57×10 CaHAp和Ca 9.78 Cs 0.2 (PO 4 K −1 > 298 (OH) 1.96 ,分别在298-1083 K的温度范围内。体热膨胀测量结果与晶格膨胀结果一致。

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