Adrián Barroso-Bogeat

Particle size distribution and morphological changes in activated carbon-metal oxide hybrid catalysts prepared under different heating conditions.

In catalysis processes, activated carbon (AC) and metal oxides (MOs) are widely used either as catalysts or as catalyst supports because of their unique properties. A combination of AC and a MO in a single hybrid material entails changes not only in the composition, microstructure and texture but also in the morphology, which may largely influence the catalytic behaviour of the resulting product. This work is aimed at investigating the modifications in the morphology and particle size distribution (PSD) for AC‐MO hybrid catalysts as a result of their preparation under markedly different heating conditions. From a commercial AC and six MO (Al2O3, Fe2O3, ZnO, SnO2, TiO2 and WO3) precursors, two series of such catalysts are prepared by wet impregnation, oven‐drying at 120ºC, and subsequent heat treatment at 200ºC or 850ºC in inert atmosphere. The resulting samples are characterized in terms of their morphology and PSD by scanning electron microscopy and ImageJ processing program. Obtained results indicate that the morphology, PSD and degree of dispersion of the supported catalysts are strongly dependent both on the MO precursor and the heat treatment temperature. With the temperature rise, trends are towards the improvement of crystallinity, the broadening of the PSD and the increase in the average particle size, thus suggesting the involvement of sintering mechanisms. Such effects are more pronounced for the Fe, Sn and W catalysts due to the reduction of the corresponding MOs by AC during the heat treatment at 850ºC.

A single slice approach for simulating two-beam electron diffraction of nanocrystals

A simple computational method that can be used to simulate TEM image contrast of an electron beam diffracted by a crystal under two-beam dynamical scattering conditions is presented. The approach based on slicing the shape factor is valid for a general crystal morphology, with and without crystalline defects, avoids the column approximation, and provides the complex exit wave at the focal and the image planes also under weak-beam conditions. The approach is particularly efficient for large crystals and the 3D model required for the calculations can be measured experimentally using electron tomography. The method is applied to show that the shape of a diffracted spot can be affected by shifts, broadening and secondary maxima of appreciable intensity, even for a perfect crystal. The methodology is extended for the case of electron precession diffraction, and to show how can be used to improve nanometrology from diffraction patterns. The method is used also to perform simulations of simple models of crystalline defects. The accuracy of the method is demonstrated through examples of experimental and simulated dark-field images of MgO and ZrO2 nanocrystals and thin layers of CeO2.