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Preparation And Crystallinity Of Molybdenum And Tungsten Sulfides

J. C. Wildervanck, F. Jellinek
Published 1964 · Chemistry

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The sulfides of molybdenum and tungsten in the composition range MS3 to MS2 have been investigated. Molybdenum trisulfide was prepared by a variety of methods; the products were amorphous in all cases. The thermal decomposition of the trisulfide, leading to crystalline molybdenum disulfide, was studied by X-ray diffraction and a model for the crystallization process is proposed. Molybdenum disulfide prepared by this method or from the elements always was of the hexagonal form. The rhombohedral form of molybdenum disulfide can be prepared from a molten medium; again, a model for the crystallization process is proposed. Quite analogous results were obtained for the tungsten sulfides: Tungsten trisulfide was always found to be amorphous. Tungsten disulfide prepared by thermal decomposition of the trisulfide or from the elements is of the hexagonal form, but a rhombohedral modification of tungsten disulfide could be prepared in the same way as the isotypic molybdenum compound. The unit-cell dimensions of the disulfides are communicated. Die Molybdan- und Wolframsulfide der Zusammensetzungen MS3 bis MS2 wurden untersucht. Molybdantrisulfid wurde nach verschiedenen Methoden dargestellt; die erhaltenen Produkte waren in allen Fallen amorph. Die thermische Zersetzung von Molybdantrisulfid zum kristallinen Disulfid wurde rontgenanalytisch untersucht; fur den Kristallisationsprozes wird ein Modell vorgeschlagen. Das auf diese Weise oder durch Synthese aus den Elementen dargestellte Molybdandisulfid gehorte immer der hexagonalen Modifikation an. Rhomboedrisches Molybdandisulfid kann aus Carbonat-Schmelzen dargestellt werden; auch fur diesen Vorgang wird ein Modell vorgeschlagen. Ganz analoge Ergebnisse wurden fur die Wolframsulfide erhalten: Auch reines Wolframtrisulfid erwies sich in allen Fallen als amorph. Durch thermische Zersetzung des Trisulfids oder durch Synthese aus den Elementen wurde die hexagonale Modifikation des Wolframdisulfids erhalten. Eine rhomboedrische Form des Wolframdisulfids konnte auf dieselbe Weise wie die isotype Molybdanverbindung dargestellt werden. Die Gitterkonstanten der Disulfide werden mitgeteilt.

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