A study of preparation of tungsten nitride catalysts with high surface area

Tungsten oxides, to be used as precursors for tungsten nitride catalysts, were prepared by a sol-gel method. The preparation conditions were as follows: the solution molar ratio of 1 : 1 (methanol and water), temperature of 80 degrees C, and the range of R (methanol/H2WO4 mole ratio) between 15 and 30. The XRD results showed that the prepared gels were amorphous and suggested they were tungsten oxide hydrate. However, this result disagreed with that of Raman spectroscopy and XANES. The highest surface area was 28.57 m(2)/g, which was obtained from the tungsten oxide with the R ratio of 25. After the gel was heated at 500 degrees C, it was crystallized tungsten oxide (WO3). The results of Raman spectroscopy and XANES showed that the unheated gel had a considerable amount of structural water in its structure. Such structural water may have an effect on nitriding the sample. Tungsten nitride catalysts were prepared in NH3 flow with the flow rate of 100 ml/min, at 670-700 degrees C with the heating rate of 1.0 degrees C/min by the temperature programmed reaction (TPR) method. The prepared nitride catalysts were found to be mostly beta-W2N from the XRD results. The surface area of the nitride from unheated gel was 79.53 m(2)/g, which was higher than that of the nitride from a commercial tungsten trioxide. The temperature for nitriding the prepared gels of this present study was lower than that of the commercial tungsten trioxide. (C) 1999 Elsevier Science B.V. All rights reserved.