为了进一步促进钠快离子导体磷酸锆钠(NaZr2(PO4)3)粉体的实际应用, 本文提出了一种以氧氯化锆(ZrOCl2?8H2O)和二水磷酸二氢钠(NaH2PO4?2H2O)为原料的低温固相反应法制备NaZr2(PO4)3粉体。通过XRD, SEM和Raman等测试手段系统研究了磷酸盐用量对制备磷酸锆钠粉体的影响。结果表明: 采用超量的 磷酸盐有利于纯相磷酸锆钠粉体的合成。同时当锆盐与磷酸盐的摩尔比为2∶5.4时, 能够合成平均粒径1 μm, 尺寸均匀, 分散性良好的磷酸锆钠粉体。研究发现研磨时发生的固相反应对磷酸锆钠粉体的制备有重要作用, 一方面促进了无定型磷酸锆钠的产生, 有利于磷酸锆钠晶体形成; 另一方面原位生成的氯化钠为晶体的生长提供了良好的液相环境, 促进了磷酸锆钠粉体的低温合成。该工作为磷酸锆钠粉体的大规模生产提供了一条简单有效的方法。

For the purpose of accelerating the practical application of NaSICON NaZr2(PO4)3 powders, a solid-state reaction method at low- temperature was developed to prepare NaZr2(PO4)3 powders using ZrOCl2?8H2O and NaH2PO4?2H2O as raw materials. The influence of phosphate content on the synthesis of NaZr2(PO4)3 powders was investigated by XRD, SEM and Raman techniques. The results show that excess amount of phosphate is beneficial to obtain the pure phase of NaZr2(PO4)3. In addition, the as-prepared powders with average particle size of 1 μm show uniform size and good dispersion when the mole ratio of ZrOCl2?8H2O to NaH2PO4?2H2O is 2∶5.4. The occurrence of solid-state reaction during grinding process is found to play an essential role in the preparation of NaZr2(PO4)3 powders. On the one hand, the amorphous NaZr2(PO4)3 produced by solid-state reaction contributes to the formation of crystalline NaZr2(PO4)3. On the other hand, the in-situ generation of NaCl provides favorable liquid environment for the crystal growth. Furthermore, this work develop a facile and effective route for the mass production of NaZr2(PO4)3 powders.