Formation of Highly Dispersed Metals Via Chemical Reduction Methods
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 MoC15 is described. The preparation of pure starting materials is crucial to the success of the subsequent chemical reduction. Reduction of MoC13(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 M2C M = 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. 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 deg C). The solids isolated from these experiments could be redispersed in THF to form colloidal black solutions.
Document Details
- Document Type
- Technical Report
- Publication Date
- May 22, 1992
- Accession Number
- ADA251657
Entities
People
- A. Datye
- D. Zeng
- M. J. Hampden-smith
Organizations
- University of New Mexico