Zero- and one-dimensional thioindates synthesized under solvothermal conditions yielding {alpha}-In{sub 2}S{sub 3}, {beta}-In{sub 2}S{sub 3} or MgIn{sub 2}S{sub 4} as thermal decomposition products

Journal Article · Wed Dec 15 00:00:00 EST 2010 · Journal of Solid State Chemistry

DOI:https://doi.org/10.1016/j.jssc.2010.09.024· OSTI ID:21494137

Quiroga-Gonzalez, E ^[1]; Kienle, L ^[2]; Naether, C ^[1]; Chakravadhanula, V S.K. ^[2]; Luehmann, H ^[1]; Bensch, W ^[1]

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1. Institute for Inorganic Chemistry of the University of Kiel, Max-Eyth-Str. 2, 24118 Kiel (Germany)
2. Institute of Material Science of the University of Kiel, Synthesis and Real Structure, Kaiserstr. 2, 24143 Kiel (Germany)

The first cationic thioindate with composition [In(en){sub 2}S]{sub 2}.2Cl (zero-dimensional) (1) and the first thioindate being charge compensated by a main group metal complex with composition [Mg(en){sub 3}][In{sub 2}S{sub 4}] (one-dimensional) (2) have been prepared with ethylenediamine under solvothermal conditions. The main structural motif of [In(en){sub 2}S]{sub 2}.2Cl is the centro-symmetric rhomboidal [In(en){sub 2}S]{sub 2}{sup 2+} ring which is formed by S-S edge-sharing of two symmetry related [InN{sub 4}S{sub 2}] octahedra. The structure of [Mg(en){sub 3}][In{sub 2}S{sub 4}] is composed of a straight one-dimensional {l_brace}[InS{sub 2}]{sup -{r_brace}}{sub {infinity}} chain surrounded by [Mg(en){sub 3}]{sup 2+} complexes. Both compounds are wide band-gap semiconductors. The thermal decomposition reaction of [In(en){sub 2}S]{sub 2}.2Cl stopped at 500 {sup o}C yielded cubic {alpha}-In{sub 2}S{sub 3} and reflections of {beta}-In{sub 2}S{sub 3} are seen in the X-ray powder pattern of the residue obtained at 900 {sup o}C. In the case of [Mg(en){sub 3}][In{sub 2}S{sub 4}] the thiospinel MgIn{sub 2}S{sub 4} was identified as decomposition product. The size of the MgIn{sub 2}S{sub 4} crystals are in the nanometer range as evidenced by a pronounced broadening of the reflections in the powder pattern and with transmission electron microscopy. -- Graphical abstract: The structure of [In(en){sub 2}S]{sub 2}.2Cl contains a cationic core and [Mg(en){sub 3}][In{sub 2}S{sub 4}] is the first thioindate with a charge compensating Mg{sup 2+} complex. Thermal decomposition yields {alpha}- or {beta}-In{sub 2}S{sub 3} resp. spinel-type nanocrystalline MgIn{sub 2}S{sub 4}.

• OSTI ID: 21494137
• Journal Information: Journal of Solid State Chemistry, Vol. 183, Issue 12; Other Information: DOI: 10.1016/j.jssc.2010.09.024; PII: S0022-4596(10)00423-8; Copyright (c) 2010 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; ISSN 0022-4596
• Country of Publication: United States
• Language: English

Related Subjects

77 NANOSCIENCE AND NANOTECHNOLOGY
CRYSTAL STRUCTURE
CRYSTALS
INDIUM SULFIDES
MAGNESIUM COMPLEXES
MAGNESIUM IONS
NANOSTRUCTURES
PRECURSOR
PYROLYSIS
SEMICONDUCTOR MATERIALS
SPINELS
SYNTHESIS
TRANSMISSION ELECTRON MICROSCOPY
ALKALINE EARTH METAL COMPLEXES
CHALCOGENIDES
CHARGED PARTICLES
CHEMICAL REACTIONS
COMPLEXES
DECOMPOSITION
ELECTRON MICROSCOPY
INDIUM COMPOUNDS
IONS
MATERIALS
MICROSCOPY
MINERALS
OXIDE MINERALS
SULFIDES
SULFUR COMPOUNDS
THERMOCHEMICAL PROCESSES