Molybdenum cluster chalcogenides: In situ x-ray studies on the formation of Cu[sub x]Mo[sub 6]S[sub 8] via electron/ion transfer

Systematic structural investigations have been performed on the formation of the ternary Chevrel phase system Cu[sub x]Mo[sub 6]S[sub 8] by topotactic intercalation of copper into Mo[sub 6]S[sub 8] via electron/ion transfer reactions. In high-temperature synthesis the homogeneity range of Cu[sub x]M...

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Bibliographic Details
Published in:Journal of solid state chemistry 1993-01, Vol.102:1
Main Authors: Fischer, C., Gocke, E., Stege, U., Schoellhorn, R.
Format: Article
Language:English
Subjects:
360602 - Other Materials- Structure & Phase Studies
CHALCOGENIDES
COHERENT SCATTERING
COPPER COMPOUNDS
COPPER SULFIDES
DIFFRACTION
ELECTRON TRANSFER
MATERIALS SCIENCE
MOLYBDENUM COMPOUNDS
MOLYBDENUM SULFIDES
REFRACTORY METAL COMPOUNDS
SCATTERING
STRUCTURAL CHEMICAL ANALYSIS
SULFIDES
SULFUR COMPOUNDS
SUPERCONDUCTORS
SYNTHESIS
TRANSITION ELEMENT COMPOUNDS
X-RAY DIFFRACTION
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Summary:Systematic structural investigations have been performed on the formation of the ternary Chevrel phase system Cu[sub x]Mo[sub 6]S[sub 8] by topotactic intercalation of copper into Mo[sub 6]S[sub 8] via electron/ion transfer reactions. In high-temperature synthesis the homogeneity range of Cu[sub x]Mo[sub 6]S[sub 8] formation corresponds to 1.8 [le] x [le] 3.66, while by galvanostatic or potentiostatic reduction of binary Mo[sub 6]S[sub 8] at ambient temperature in aqueous CuSO[sub 4] or aprotic CuCl/CH[sub 3]CN electrolyte the terminal rhombohedral phase Cu[sub 4]MO[sub 6]S[sub 8] with the maximum number of electrons per Mo[sub 6] cluster can be obtained. The phase range 1 [le] x [le] 4 of Cu[sub x]Mo[sub 6]S[sub 8] as obtained by galvanostatic reduction of Mo[sub 6]S[sub 8] in aqueous CuSO[sub 4] electrolyte has been determined by in situ x-ray experiments. Warburg oxygen manometry has proved to be a new and powerful analytical tool for examination of the Cu content of ternary phase Cu[sub x]Mo[sub 6]S[sub 8]. Thermodiffractometry and [sup 63]Cu NMR studies of Cu[sub 2]Mo[sub 6]S[sub 8] (high-temperature phase) reveal a phase-transition rhombohedral/triclinic in a broad temperature range between 285 and 200 K. Superconducting properties (temperature-dependent ac susceptibility) of high temperature and electrochemically prepared Cu phases are reported.
ISSN:0022-4596
1095-726X
DOI:10.1006/jssc.1993.1007