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Formation of Highly Dispersed Metal Carbides, M2C (M=Mo, W) via Chemical Reduction Methods

Published online by Cambridge University Press:  15 February 2011

Dongshui Zeng ,
M.J. Hampden-Smith  and
A. Datye
Dongshui Zeng
Affiliation:
Department of Chemistry and Center for Micro-Engineered Ceramics, University of New Mexico, Albuquerque NM 87131, USA
M.J. Hampden-Smith
Affiliation:
Department of Chemistry and Center for Micro-Engineered Ceramics, University of New Mexico, Albuquerque NM 87131, USA
A. Datye
Affiliation:
Chernical Engineering and Center for Micro-Engineered Ceramics, University of New Mexico, Albuquerque NM 87131, USA
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Abstract

A new reduction method for the preparation of the molybdenum halides MoCl3(THF)3 and MoCl4(THF)2 in high yield and with high purity directly from MoCl5 is described. The preparation of pure starting materials is crucial to the success of the subsequent chemical reduction. Reduction of MoCl3(THF)3, MoCl4(THF)2 or WCl4 in THF with LiBEt3H at room temperature did not.result in formation of Mo and W as anticipated but instead resulted in formation of nanophase M2CM = Mo and W binary metal carbides. These species were characterized by SEM, TEM, energy dispersive spectroscopy, electron diffraction, elemental analysis, thermogravimetric analysis and X-ray diffraction techniques. These techniques showed the black solids were crystalline and comprised 1–2 nm sized crystallites Which could be grown by heating to higher temperatures (450 – 500°C). The solids isolated from these experiments could be redispersed in THF to form colloidal black solutions.

Type
Research Article
Information
MRS Online Proceedings Library (OPL) , Volume 272: Symposium O – Chemical Processes in Inorganic Materials: Metal and Semiconductor Clusters , 1992 , 103
Copyright
Copyright © Materials Research Society 1992

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References

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