温和水热法制备MZr_2(PO_4)_3(M=Na,K,Rb)

Mild Hydrothermal Preparation of MZr_2(PO_4)_3(M=Na,K,Rb)

在温和的水热条件下分别制备出纯净的磷酸锆钠 [NaZr2 (PO4) 3 ]、磷酸锆钾 [KZr2 (PO4) 3 ]和磷酸锆铷 [RbZr2 (PO4) 3 ]。研究了原料配比、矿化剂 (氟离子 )、反应时间和温度等水热晶化条件对产物生成的影响。发现在较宽的温和水热条件下可以制得这三种磷酸锆盐 ;随着碱金属离子的增大 ,产物的生成条件越来越窄 ;最佳制备条件是 :F- ZrO2 =2、P2 O5 ZrO2 =3 (均为摩尔比 )、[ZrOCl2 ]=0 6mol L、反应温度 1 5 0℃、反应时间 2天。用水热法没有制备出同一系列磷酸锆盐中的磷酸锆锂 [LiZr2 (PO4) 3 ]和磷酸锆铯 [CsZr2 (PO4) 3 ]。采用XRD、SEM、IR。

Three pure compounds of sodium dizirconium phosphate (NaZr 2(PO 4) 3),potassium dizirconium phosphate (KZr 2(PO 4) 3) and rubidium dizirconium phosphate (RbZr 2(PO 4) 3) have been prepared respectively by mild hydrothermal synthesis methods under the optimum conditions:F -/ZrO 2=2,P 2O 5/ZrO 2=3 (both in molar ratio),(ZrOCl 2)=0.6mol/L,150℃ and 2 days,which are very soft hydrothermal conditions with a high rate of output.The effects of the hydrothermal conditioins (initial composition,mineralizer,temperature and time) on the kind of products have been investigated.The phases and purity of final products have been identified by XRD、SEM、IR、Raman and XPS.