Published online by Cambridge University Press: 15 February 2011
We report, for the first time, direct studies of the dynamic VOHPO4·1/2H2O precursor to (VO)2P2O7 catalyst transformation using recently developed in-situ environmental-cell, high-resolution, electron microscopy (in-situ ECELL-HREM) under controlled environments. Our observations provide fundamental evidence concerning the nature of the topotactic transformation and associated temperature regimes critical to the formation of active catalysts. The direct ECELL-HREM studies show that the structural transformation begins at ˜ 400°C, and a mixture of the precursor and pyrophosphate phases exists at ˜ 425°C. At 450°C, most of the conversion to VPO has taken place. These atomic-scale studies reveal no amorphous phases during the transformation, and that the atomic periodicity is maintained throughout. No other phases have so far been identified in the transformation. The direct studies are important in the development of selective catalysts.