Large scale synthesis of nanostructured zirconia-based compounds from freeze-dried precursors

Journal Article · Tue Jan 15 00:00:00 EST 2013 · Journal of Solid State Chemistry

DOI:https://doi.org/10.1016/J.JSSC.2012.07.045· OSTI ID:22131165

Gomez, A.; Villanueva, R.; Vie, D.; Murcia-Mascaros, S.; Martinez, E.; Beltran, A. ^[1]; Vicent, M.; Sanchez, E. ^[2]

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1. Institut de Ciencia dels Materials, Parc Cientific, Universitat de Valencia, PO Box 22085, 46071 Valencia (Spain)
2. Instituto de Tecnologia Ceramica-Asociacion de Investigacion de las Industrias Ceramicas, Universitat Jaume I, 12006 Castellon (Spain)

Nanocrystalline zirconia powders have been obtained at the multigram scale by thermal decomposition of precursors resulting from the freeze-drying of aqueous acetic solutions. This technique has equally made possible to synthesize a variety of nanostructured yttria or scandia doped zirconia compositions. SEM images, as well as the analysis of the XRD patterns, show the nanoparticulated character of those solids obtained at low temperature, with typical particle size in the 10-15 nm range when prepared at 673 K. The presence of the monoclinic, the tetragonal or both phases depends on the temperature of the thermal treatment, the doping concentration and the nature of the dopant. In addition, Rietveld refinement of the XRD profiles of selected samples allows detecting the coexistence of the tetragonal and the cubic phases for high doping concentration and high thermal treatment temperatures. Raman experiments suggest the presence of both phases also at relatively low treatment temperatures. - Graphical abstract: Zr{sub 1-x}A{sub x}O{sub 2-x/2} (A=Y, Sc; 0{<=}x{<=}0.12) solid solutions have been prepared as nanostructured powders by thermal decomposition of precursors obtained by freeze-drying, and this synthetic procedure has been scaled up to the 100 g scale. Highlights: Black-Right-Pointing-Pointer Zr{sub 1-x}A{sub x}O{sub 2-x/2} (A=Y, Sc; 0{<=}x{<=}0.12) solid solutions have been prepared as nanostructured powders. Black-Right-Pointing-Pointer The synthetic method involves the thermal decomposition of precursors obtained by freeze-drying. Black-Right-Pointing-Pointer The temperature of the thermal treatment controls particle sizes. Black-Right-Pointing-Pointer The preparation procedure has been scaled up to the 100 g scale. Black-Right-Pointing-Pointer This method is appropriate for the large-scale industrial preparation of multimetallic systems.

• OSTI ID: 22131165
• Journal Information: Journal of Solid State Chemistry, Vol. 197; Other Information: Copyright (c) 2012 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; Country of input: International Atomic Energy Agency (IAEA); ISSN 0022-4596
• Country of Publication: United States
• Language: English

Related Subjects

36 MATERIALS SCIENCE
77 NANOSCIENCE AND NANOTECHNOLOGY
CHEMICAL PREPARATION
CONTROL
CRYSTALS
DOPED MATERIALS
GRAIN SIZE
HEAT TREATMENTS
IMAGES
MONOCLINIC LATTICES
NANOSTRUCTURES
PARTICLE SIZE
POWDERS
PRECURSOR
PYROLYSIS
SCANNING ELECTRON MICROSCOPY
SOLID SOLUTIONS
SOLIDS
X-RAY DIFFRACTION
YTTRIUM OXIDES
ZIRCONIUM OXIDES