Hydrothermal synthesis of nanocrystalline powders of various crystalline phases of ZrO2 and TiO2

Yu V. Kolen'ko, A. A. Burukhin, B. R. Churagulov, N. N. Oleinikov, V. A. Mukhanov

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18 Citations (Scopus)


Nanocrystalline ZrO2 and TiO2 powders were hydrothermally synthesized from 0.01-1.8 M ZrO(NO3)2 and TiO(NO3)2 precursor solutions under high pressures of 4.0-5.0 GPa at temperatures from 403 to 523 K. The samples synthesized were characterized by X-ray powder diffraction, X-ray line broadening analysis (XLB), thermogravimetry (TG), and transmission electron microscopy (TEM). The BET specific surface area was determined by capillary nitrogen adsorption. From ZrO(NO3)2 solutions, the stable monoclinic m-ZrO 2 was synthesized with the grain size d = 6-8 nm. From TiO(NO 3)2 aqueous solutions at 523 K (τ = 10 min), nanocrystalline samples of anatase (the metastable TiO2 phase) with d = 10 nm were first formed; after 6 h of hydrothermal exposure, they converted to the thermodynamically stable rutile (d = 50 nm). High-temperature hydrolysis of zirconyl nitrate solutions at 523 K and 4.0 GPa for 30 min yielded a mixture of the monoclinic and tetragonal phases; from titanyl nitrate solutions, only rutile (the stable phase) was formed. Short-term hydrothermal processing (τ = 10 min) of hydroxide gels yielded metastable phases: in the case of ZrO(OH)2, tetragonal t-ZrO2 (d = 10-12 nm) was formed at 403 K, which was gradually converted by subsequent hydrothermal processing to the stable monoclinic phase; in the case of TiO2·nH 2O at 523 K, anatase (d = 27 nm) was produced.

Original languageEnglish
Pages (from-to)1609-1615
Number of pages7
JournalRussian Journal of Inorganic Chemistry
Issue number11
Publication statusPublished - Nov 2002
Externally publishedYes


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