Crystal Growth, Structure, and Stoichiometry of the Superconducting Pyrochlore Cd2Re2O7
Authors: He, J.; Jin, R.; Chakoumakos, B.C.; Gardner, J.S.; Mandrus, D.; Tritt, Terry
Source: Journal of Electronic Materials, Volume 36, Number 7, July 2007 , pp. 740-745(6)
Abstract:We report single-crystal growth of the superconducting pyrochlore Cd2Re2O7 using a vapor transport technique. Several parameters of the growth conditions, including hot-zone temperature and starting stoichiometry, were varied in order to control the formation of ReO2 inclusions, as confirmed by the electron microscopy, resistivity, and magnetic susceptibility measurements. The Rietveld refinement of x-ray (neutron) powder diffraction was found to be consistent with a cubic structure Fd3m with lattice constant a = 10.2250 (10.2358) Å and reduced coordinate of O1 = 0.3184 (0.3177) at 293 K (250 K). We also studied the oxygen stoichiometry by means of redox reactions, electron microprobe analysis (EMPA), and x-ray/neutron diffractions. Particularly, the neutron powder diffraction on the 114Cd-enriched specimens yielded an oxygen deficiency = 0.14 ± 0.03 solely at the O2 site, which was consistent with the EMPA results. The EMPA indicated that the oxygen deficiency is homogeneous in the bulk and in a range of 0.01 ± 0.18–0.23 ± 0.19.
Document Type: Research Article
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Publication date: July 2007