Nanosized a-zirconium phenylphosphonate particles were successfully prepared by the reactionb etween different zirconiums ources and molten phenylphosphonic acid in the absence of solvent. The resultant nanoplates exhibit particle sizes in the range of 15 to 30 nm. The use of at opotactic anion exchange methods tarting from a-zirconium phosphate instead resultedi nt he generation of 15 to 180 nm plates, while also resulting in nanoparticles with a higher degree of crystallinity.T he topotactic anione xchange of the phosphate groups by phenylphosphonate groups could be performed to completion when performed in molten phenylphosphonic acid. Characterization of both the final products as well as the individual steps in the anion exchange were performed by powder XRD, fast neutron activation analysis,T GA, FTIR spectroscopy,T EM, solid-state NMR and XPS.[a] A.Supporting information and the ORCID identification number(s) for the author(s) of this article can be found under: https://doi.