A new continuous two-step molecular precursor route to rare-earth oxysulfides Ln{sub 2}O{sub 2}S
- Institute of Condensed Matter and Nanosciences/MOST, Universite Catholique de Louvain, Place Louis Pasteur, 1, L4.01.03, B-1348 Louvain-la-Neuve (Belgium)
A continuous two-step molecular precursor pathway is designed for the preparation of rare-earth oxysulfides Ln{sub 2}O{sub 2}S (Ln=Y, La, Pr, Nd, Sm-Lu). This new route involves a first oxidation step leading to the rare-earth oxysulfate Ln{sub 2}O{sub 2}SO{sub 4} which is subsequently reduced to the rare-earth oxysulfide Ln{sub 2}O{sub 2}S by switching to a H{sub 2}-Ar atmosphere. The whole process occurs at a temperature significantly lower than usual solid state synthesis (T{<=}650 Degree-Sign C) and avoids the use of dangerous sulfur-based gases, providing a convenient route to the synthesis of the entire series of Ln{sub 2}O{sub 2}S. The molecular precursors consist in heteroleptic dithiocarbamate complexes [Ln(Et{sub 2}dtc){sub 3}(phen)] and [Ln(Et{sub 2}dtc){sub 3}(bipy)] (Et{sub 2}dtc=N,N-diethyldithiocarbamate; phen=1,10-phenanthroline; bipy=2,2 Prime -bipyridine) and were synthesized by a new high yield and high purity synthesis route. The nature of the molecular precursor determines the minimum synthesis temperature and influences therefore the purity of the final Ln{sub 2}O{sub 2}S crystalline phase. - Graphical abstract: A continuous two-step molecular precursor pathway was designed for the preparation of rare-earth oxysulfides Ln{sub 2}O{sub 2}S (Ln=Y, La, Pr, Nd, Sm-Lu), starting from heteroleptic dithiocarbamate complexes. The influence of the nature of the molecular precursor on the minimum synthesis temperature and on the purity of the final Ln{sub 2}O{sub 2}S crystalline phase is discussed. Highlights: Black-Right-Pointing-Pointer A new high yield and high purity synthesis route of rare earth dithiocarbamates is described. Black-Right-Pointing-Pointer These compounds are used as precursors in a continuous process leading to rare-earth oxysulfides. Black-Right-Pointing-Pointer The oxysulfides are obtained under much more moderate conditions than previously described.
- OSTI ID:
- 22012192
- Journal Information:
- Journal of Solid State Chemistry, Journal Name: Journal of Solid State Chemistry Vol. . 191; ISSN 0022-4596; ISSN JSSCBI
- Country of Publication:
- United States
- Language:
- English
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