Electron tomography in transmission electron microscopy provides valuable three-dimensional structural, morphological and chemical information of condensed matter at nanoscale. Current image acquisitions require at least tens of minutes, which prohibits the analysis of nano-objects evolving rapidly such as under dynamic environmental conditions. Reducing the acquisition duration to tens of seconds or less permits to follow in 3D the same object during its evolution under varying temperatures and pressures. We report Operando Electron nanotomography using image series acquired in less than 230 seconds instead of typically 15 min in the best cases so far. The in situ calcination of silica zeolites encaging silver nanoparticles, a catalytic nanosystem of potential interest for, e.g., nuclear waste treatments or selective heterogeneous catalysis, was successfully studied. Kinetic environmental Operando 3D electron microscopy becomes possible, as well as real time observation of beam sensitive samples (polymers, biological objects) without prior preparation, which reduces their contrast and reactivity.
Keywords: Ag nanoparticles; Operando electron nanotomography; environmental transmission electron microscopy (ETEM); heterogeneous catalysis; in situ calcination; silicates.
© 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.