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) A # 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 d = 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.
