Decomposition of W(CO)(6) at high pressures and temperatures

作者:Rademacher Nadine*; Bayarjargal Lkhamsuren; Friedrich Alexandra; Morgenroth Wolfgang; Avalos Borja Miguel; Vogel Sven C; Proffen Thomas; Winkler Bjoern
来源:Journal of Applied Crystallography, 2011, 44: 820-830.
DOI:10.1107/S0021889811021285

摘要

The decomposition of hexacarbonyltungsten, W(CO)(6), has been studied. The decomposition was induced by heating W(CO)(6) in an autoclave at 523 K and pressures up to 1.8 MPa, and by laser heating in a diamond anvil cell at pressures between 5 and 18 GPa. The products have been characterized using synchrotron X-ray diffraction, pair distribution function analysis, Raman spectroscopy and scanning electron microscopy. Decomposition in the autoclave at the lower pressures resulted in the formation of a metastable tungsten carbide, W2C, with an average particle size of 1-2 nm, and an unidentified nanocrystalline tungsten oxide and nanocrystalline graphite with average particle sizes of 1-2 and 11 nm, respectively. The existence of nanocrystalline graphite was deduced from micro-Raman spectra and the graphite particle size was extracted from the intensities of the Raman modes. The high-pressure decomposition products obtained in the diamond anvil cell are the monoclinic tungsten oxide phase WO2 and the high-pressure phase W3O8(I). The approximate average size of the graphite particles formed here was 6-8 nm. The bulk modulus of W(CO)(6) is B-0 similar or equal to 13 GPa.

  • 出版日期2011-8