Is the Freeze Drying Method Effect on the Phase Transition Temperature ofβ/β́́ Lithium Zirconium Phosphate?

Spherical granules of the superionic conductor β/β́ LiZr2(PO4)3 in the range of sub 100 nm sizewere synthesizedvia freeze drying methodand fully reviewed in all aspects. Samples were characterized by the X-ray diffractometry (XRD), the Thermal analysis (TG, DSC), theFourier Transform Infra-Red Spectroscopy (FTIR) and the Scanning Electron Microscopy (SEM).Their structuredepends largely on the method of synthesis, thermaltreatment, and conditions of storing samples. Degree of Crystallinity and phase purity in different annealing time were tested. The synthesize temperature does not exceed 873 K in any step of the synthesis.The low temperature phases (β with the Pbna space group and β́ with the P21/n space group) were preparedat optimum condition. By the Differential Scanning Calorimetry it was shown the phase transition from β↔β́ occurred at about 567-597 K. The temperature of annealing the phosphate and calcination time is not very effective to phase transition temperature.