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Sensors 2003, 3(10), 415-423;

Morphology, Structure and Nonstoichiometry of ZnCr2O4 Nanophased Powder

Institute of Technical Sciences of Serbian Academy of Sciences and Arts, Knez Mihailova 35/IV, 11000 Belgrade, Serbia-Montenegro
Center for Multidsciplinary Studies, University of Belgrade, Kneza Viseslava 1a, 11 000 Belgrade, Serbia-Montenegro
Faculty of Mining and Geology, Department of Crystallography, Djusina 7, 11000 Belgrade, Serbia- Montenegro
University Carlos III, la Universidad 30, 28911 Leganes, Madrid, Spain
Author to whom correspondence should be addressed.
Received: 15 May 2003 / Accepted: 17 August 2003 / Published: 31 October 2003
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It is well established that gas/humidity-sensing properties of spinels are markedly influenced by their stoichiometry and microstructure. In this work nucleation and spinel phase development in the Zn-Cr-O system were investigated from the viewpoint of structural and morphological phenomena occurred during nanophased particle synthesis through aerosol reaction. The aerosol was generated from nitrates precursor solution using ultrasonic atomizer operated at 1.7 MHz. The influence of different decomposition schedules on the particle chemical content and morphology was determined by adjusting the processing parameters (aerosol droplet density 3.9x106 droplets/cm3, droplet velocity 0.035m/s, max. temperature 900oC and residence times 3, 6 and 9s). A composite particle structure comprised of primary crystallites sized from 22 to 44nm is revealed by SEM and TEM analysis. XRD structural analysis (crystallite size, microstrains, unit cell and ionic occupancies) is performed in accordance with procedure based on Koalariet-Xfit program. A certain degree of non-stochiometry is characteristic for all powders. Homogenous distribution of the constituting elements and Zn/Cr ratio of about 0.68 are proved by EDAX mapping analysis in 470nm sized as-prepared particles. After additional treatment at 1000oC octahedral crystals form with the (111) surface dominat. Evaluated spinel non-stochiometry (Zn/Cr=0.58) is a result of the ZnO dissolving (1.9%wt) in the stoichiometric ZnCr2O4. Determination of the way by which the ZnO is incorporated into the spinel lattice is performed according to the procedure based on calculation of both formation and attachment energies. View Full-Text
Keywords: Spray pyrolysis; nanostructure; nonstoichiometry; ZnCr2O4 Spray pyrolysis; nanostructure; nonstoichiometry; ZnCr2O4

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Mancic, L.; Marinkovic, Z.; Vulic, P.; Moral, C.; Milosevic, O. Morphology, Structure and Nonstoichiometry of ZnCr2O4 Nanophased Powder. Sensors 2003, 3, 415-423.

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