Dynamic imaging of structural changes in silver catalysts by environmental scanning electron microscopy

Polycrystalline silver catalysts are used extensively for the partial oxidation of methanol to formaldehyde, which is then primarily incorporated in the synthesis process for adhesives and resins. In order to maximize formaldehyde production it is essential to gain a comprehensive understanding of the complex microstructural changes which occur in the catalyst during reaction conditions. However, conventional electron microscopic techniques are incapable of imaging catalysts at high temperatures and in the presence of a gaseous atmosphere. Therefore, an environmental scanning electron microscope (ESEM) has been used to image polycrystalline silver catalysts during simulated industrial conditions. The most dramatic effect of heating various catalysts to 700 degrees C in the ESEM chamber was the formation of "pinholes" in the silver surface. These "pinholes" occur at specific temperatures and are inherently associated with the catalytic process, resulting from near-surface explosions caused by subsurface hydroxyl recombination. Of particular interest was the nature and location of the holes, which preferentially occur in the vicinity of surface defects such as platelets and edge structures. To the best of our knowledge, this study represents the first time that the progress of a catalytic reaction has been observed under in situ conditions by scanning electron microscopy.