In Situ X-ray Diffraction Studies on the Reduction of V 2 O 5 and WO 3 by Using Hydrogen.

The reduction of metal oxides with hydrogen is widely used for the production of fine chemicals and metals both on the laboratory and industry scale. In situ methods can help to elucidate reaction pathways and to gain control over such synthesis reactions. In this study, the reduction of WO 3 and V 2 O 5 with hydrogen was investigated by in situ X-ray powder diffraction with regard to intermediates and the influence of heating rates and hydrogen flow rates. Mixtures of V 4 O 9 , V 6 O 13 and VO 2 in two modifications were identified as intermediates on the way to phase-pure V 2 O 3 . None of the intermediates occurs in a single phase and therefore cannot be prepared this way. In contrast, the intermediates of the WO 3 reduction, H 0.23 WO 3 and W 10 O 29 , appear consecutively and can be isolated. For both reactions, the heating and flow rates have little influence on the formation of intermediates.