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Chem. Mater. 2001, 13, 3962-3968
Preparation of Nanocrystalline Molybdenum Disilicide (MoSi2) by a Chlorine-Transfer Reaction Timothy J. Trentler,† R. Suryanarayanan Iyer,‡ Shankar M. L. Sastry,‡ and William E. Buhro*,† Departments of Chemistry and Mechanical Engineering, Washington University, St. Louis, Missouri 63130-4899 Received March 27, 2001. Revised Manuscript Received July 10, 2001
Reaction of MoCl3 and Si at 500 °C produces phase-pure MoSi2 powders in nearquantitative yields. Use of an inert diluent (LiCl or ZnCl2) enables the production of nanocrystalline powders. The diluent can be subsequently removed by washing with methanol or by sublimation. Consolidation of diluent-free powders by hot pressing at 1400 °C and 375 MPa for 0.5-4 h affords dense compacts (>95% theoretical density) possessing nanocrystalline grains (