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Solvent‐Free Synthesis of Nano Zirconium Phenylphosphonates with Molten Phenylphosphonic Acid
Author(s) -
ContrerasRamirez Aida,
Tomlin Bryan E.,
Day Gregory S.,
Clearfield Abraham,
Zhou HongCai
Publication year - 2020
Publication title -
chemistry – a european journal
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.687
H-Index - 242
eISSN - 1521-3765
pISSN - 0947-6539
DOI - 10.1002/chem.201905110
Subject(s) - crystallinity , zirconium , x ray photoelectron spectroscopy , zirconium phosphate , ion exchange , chemistry , solvent , inorganic chemistry , fourier transform infrared spectroscopy , nanoparticle , cubic zirconia , particle size , nuclear chemistry , chemical engineering , materials science , phosphate , ion , ceramic , organic chemistry , crystallography , nanotechnology , engineering
Abstract Nanosized α‐zirconium phenylphosphonate particles were successfully prepared by the reaction between different zirconium sources 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 a topotactic anion exchange method starting from α‐zirconium phosphate instead resulted in the generation of 15 to 180 nm plates, while also resulting in nanoparticles with a higher degree of crystallinity. The topotactic anion exchange 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, TGA, FTIR spectroscopy, TEM, solid‐state NMR and XPS.