SOLVENT MEDIATED METATHETICAL APPROACH TO THE ROOM TEMPERATURE SYNTHESIS OF TERNARY (MIXED METAL) CHALCOGENIDE MATERIALS IN LIQUID AMMONIA
Shaw, Graham A., Parkin, Ivan P.
Main Group Metal Chemistry · 2002
doi:10.1515/mgmc.2002.25.7.453 (opens in a new tab)
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Abstract
Liquid ammonia mediated metathetical reactions of disodium chalcogenide (Na2E; Ε = S, Se, Te) and metal halides afforded ternary chalcopyrite-type materials of general formula ABE 2 (A = Cu, Ag; Β = Ga, In; Ε = S, Se), CuSbE 2 (E = S, Se, Te), Cu 12 Sb 4 S ( i 6 .x) , and CuFeS 2 in good yield (> 90 %), in addition to co-produced salt.The reactions, carried out in liquid ammonia at room temperature, afforded X-ray amorphous aggregates.Annealing the purified products at 200-250 °C for 3 hours resulted in single phase, crystalline products of the desired stoichiometry.The annealed products were characterised by X-ray Powder Diffraction (XRD), Energy Dispersive X-ray Analysis (EDXA), Scanning Electron Microscopy (SEM), Fourier Transform Infra-red Spectroscopy (FT-IR) and microanalysis.Attempts at forming ABE 2 (A = Cu, Ag; Β = Al; Ε = S, Se), MFeS 2 (M = Cu, Zn, Cd), AB 2 E 4 (A = Zn, Cd; Β = Cr, Ε = S; Β = V, Ε = Se) and Cd x Hg y Te (χ + y = 1.00) resulted in phase segregation to mixtures of binary metal chalcogenides with similar morphology to the ternary materials.
Abstract licence: CC BY-NC-ND
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