Synthesis Of Zirconium Phosphate Crystals And Initial Exploring Of XRPD Crystal Structure Solving Method

Layered zirconium phosphates have attracted much attention because of their potential applications in the fields of catalysis, sorption and protonic conduction. In this paper, a layered zirconium phosphate [HDAH2]0.5[Zi(PO4)(HPO4)]1.5H2O with 1, 6-hexyldiamine(HDA) templated was first hydrothermally synthesized and studied by single crystal X-Ray diffraction analysis, powder X-Ray diffraction analysis(XRD), Infrared spectrascopy (IR), thermalgravimatric analysis(TGA) and microscopy. The results of single crystal X-Ray diffraction analysis showed that the crystal structure is similar to that of γ-ZrP. The inorganic layer is in γ-type and the protonated 1, 6-hexyldiamine locates between the inorganic layers through hydrogen bonds. A new method to prepare γ-ZrP with high yield was first put forward. The synthesis conditions of α-zirconium phosphate templated by 1, 6-hexyldiamine or benzidine were also explored. XRD results revealed that the crystals are with large layer-to-layer distance (dmax= 15.3 A and dmax= 17.7 A respectively). The crystal structure of hexagonal NH4Zr2(PO4)2 was solved by X-Ray powder diffraction crystal structure analysis technology (XRPD). With Patterson method and Difference Fourier method, the final Rp=13.8.