This study presents a novel approach to impedance measurements. The methodology discussed is limited to contact in the sample-probe system under ambient conditions without the presence of electrolyte. Comparison with results of direct and alternating current measurements for well-defined metallic surfaces are made. In spite of idealization related to the type of contact examined, the proposed technique provides an improvement of traditional impedance measurement related to sequential changes in system perturbation compared with the sine wave superposition type.

A tomographic heating holder for transmission electron microscopy that can be used to study supported catalysts at temperatures of up to ~1,500°C is described. The specimen is placed in direct thermal contact with a tungsten filament that is oriented perpendicular to the axis of the holder without using a support film, allowing tomographic image acquisition at high specimen tilt angles with minimum optical shadowing. We use the holder to illustrate the evolution of the active phases of Pt nanoparticles on carbon black and PtPd nanoparticles on γ-alumina with temperature. Particle size distributions and changes in active surface area are quantified from tilt series of images acquired after subjecting the specimens to increasing temperatures. The porosity of the alumina support and the sintering mechanisms of the catalysts are shown to depend on distance from the heating filament.