A series of nanocrystalline Gd 2 Zr 2 O 7 powders has been studied using a combination of X-ray diffraction and X-ray spectroscopy with synchrotron radiation. It has been shown that isothermal annealing of an X-ray amorphous mixed hydroxide first leads to the formation of an oxide nanomaterial with a defect fluorite structure and clearly pronounced nonequivalence of the local environment of the Gd 3+ and Zr 4+ ions. Increasing heat treatment temperature results in initiation and growth of nanodomains with pyrochlore-type superstructure ordering of cations inside bulkier crystallites of defect fluorite. To adequately describe the evolution of the real nanocrystalline structure of gadolinium zirconate, a combination of X-ray structural methods sensitive to the averaged crystal structure and local atomic structure should be used.
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Popov et al. (2014) studied this question.
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