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 me...