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From Gel to Crystal: Mechanism of HfO2 and ZrO2 Nanocrystal Synthesis in Benzyl Alcohol.


ABSTRACT: Nonaqueous sol-gel syntheses have been used to make many types of metal oxide nanocrystals. According to the current paradigm, nonaqueous syntheses have slow kinetics, thus favoring the thermodynamic (crystalline) product. Here we investigate the synthesis of hafnium (and zirconium) oxide nanocrystals from the metal chloride in benzyl alcohol. We follow the transition from precursor to nanocrystal through a combination of rheology, EXAFS, NMR, TEM, and X-ray total scattering (PDF analysis). Upon dissolving the metal chloride precursor, the exchange of chloride ligands for benzylalkoxide liberates HCl. The latter catalyzes the etherification of benzyl alcohol, eliminating water. During the temperature ramp to the reaction temperature (220 °C), sufficient water is produced to turn the reacti

SUBMITTER: Goossens E 

PROVIDER: S-EPMC11027147 | biostudies-literature | 2024 Apr

REPOSITORIES: biostudies-literature