Rhenium and molybdenum poorly crystalline disulfides and their mesophases with hexadecylamine

Sulfides of molybdenum and rhenium poorly crystalline were prepared by solvothermal oxidative decarbonylation of the respective metal carbonyls with sulfur using p-xylene as solvent. The same reaction, but in presence of hexadecylamine (HDA), was used for preparing the nanocomposites MoS 2 /HDA and...

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Bibliographic Details
Published in:Journal of coordination chemistry 2014-12, Vol.67 (23-24), p.3884-3893
Main Authors: Aliaga, Juan Antonio, Araya, Juan Francisco, Villarroel, Roberto, Lozano, Harold, Alonso-Nuñez, Gabriel, González, Guillermo
Format: Article
Language:English
Subjects:
Amorphous materials
Composite materials
Crystal structure
Disulfides
Evaporation
Microscopy
Molybdenum
Molybdenum disulfide
Molybdenum sulfide
Nanocomposites
Rhenium
Rhenium sulfide
Solvents
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Summary:Sulfides of molybdenum and rhenium poorly crystalline were prepared by solvothermal oxidative decarbonylation of the respective metal carbonyls with sulfur using p-xylene as solvent. The same reaction, but in presence of hexadecylamine (HDA), was used for preparing the nanocomposites MoS 2 /HDA and ReS 2 /HDA. The products were analyzed by X-ray diffraction analysis, scanning electron microscopy, atomic force microscopy, and Fourier-transform infrared spectroscopy. The products, MoS 2 and ReS 2 , are structurally similar but morphologically different: small undefined particles (150-300 nm) and well-defined, almost perfect microspheres (0.4-2.8 μm), respectively. Preparations containing HDA lead to the corresponding layered nanocomposites. MoS 2 /HDA is a dark solid easily separable from the reaction mixture, while ReS 2 /HDA remains as a suspension in p-xylene, from which it is obtained by evaporating the solvent under vacuum. Both are layered species with basal spacing of 33.8 Å (Mo) and 30.4 Å (Re), respectively. The preparation of thin films of ReS 2 /HDA from its suspension by evaporating the solvent in the air produces small cylindrical particles of about 0.4 × 1.0 μm in size. Differences in the behavior of Mo and Re derivatives are discussed considering the coordination of the metal and the electronic structures of both metal disulfides.
ISSN:0095-8972
1029-0389
DOI:10.1080/00958972.2014.975220