Preparation of (NH4)Zr2(PO4)3 and HZr2(PO4)3
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(NH4)Zr2(PO4)3 has been prepared, hydrothermally, from α-zirconium phosphate in three different ways; (1) from amine intercalates at 300°C, (2) from mixtures of ZrOCl2·8H2O in excess (NH4)H2PO4 and (3) reaction of NH4Cl with Zr(NaPO4)2. Ammonium dizirconium triphosphate is rhombohedral with a = 8.676(1) and c = 24.288(5) A ̊. It decomposed on heating to HZr2(PO4)3. Below 600°C a complex, as yet unindexed, X-ray pattern was obtained. A very similar X-ray pattern was obtained by washing LiTi0.1Zr1.9(PO4)3 with 0.3N HCl. Heating this phase or NH4Zr2(PO4)3, above 600°C resulted in the appearance of a rhombohedral phase of HZr2(PO4)3 with cell dimensions a = 8.803(5) and c = 23.23(1) A ̊. The protons were not completely removed until about 1150°C. Decomposition of (NH4)Zr2(PO4)3 at 450°C yielded an acidic gas whereas at 700°C NH3 was evolved. A possible explanation for this behavior is presented. © 1984.
author list (cited authors)
Clearfield, A., Roberts, B. D., & Subramanian, M. A.