6533b7d2fe1ef96bd125e0a4
RESEARCH PRODUCT
Large scale synthesis of nanostructured zirconia-based compounds from freeze-dried precursors
M. VicentAndrés GómezEnrique SánchezFernando SapiñaDavid VieAurelio BeltránRegina VillanuevaE. MartínezS. Murcia-mascarossubject
Materials scienceDopantRietveld refinementMicrostructure-finalThermal decompositionThermal treatmentPowders-chemical preparationCondensed Matter PhysicsGrain sizeNanocrystalline materialElectronic Optical and Magnetic MaterialsInorganic ChemistryCrystallographyTetragonal crystal systemChemical engineeringFreeze-dryingMaterials ChemistryCeramics and CompositesZrO2Cubic zirconiaPhysical and Theoretical ChemistryYttria-stabilized zirconiadescription
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. This study has been supported by the Spanish Ministry of Science and Technology and EU FEDER Program (MAT2009-14144-C03-01, MAT2009-14144-C03-03, MAT2012-38364-C03-01, MAT2012-38364-C03-02). The SCSIE of the Universitat de València is gratefully thanked for the use of the X-ray diffraction, electron microscopy, and analytical facilities. R. Moreno and T. Molina, from Instituto de Cerámica y Vidrio, CSIC, Madrid, are acknowledged by the realization of the agglomerate size measurements.
year | journal | country | edition | language |
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2013-01-01 | Journal of Solid State Chemistry |