Catalyst aging effects were analyzed using X-ray absorption micro-computed tomography in combination with conventional characterization methods on various length scales ranging from nm to μm to gain insight into deactivation mechanisms.
For this purpose, a 4 wt% Pt/Al2O3 model exhaust gas catalyst was coated on a cordierite honeycomb and subjected to sequential thermal aging in static air at 950 °C for 4, 8, 12 and 24 hours. The aging was followed on the one hand by traditional methods, i.e. CO-oxidation activity, scanning and transmission electron microscopy (SEM, TEM), and X-ray diffraction (XRD). On the other hand, all intermediate aging steps were captured by X-ray absorption micro-computed tomography (μ-CT) with 1.27 μm voxel size using a quasi in situ approach as complementary tool. The μ-CT data allowed comparing exactly the same position after each treatment using a special alignment procedure during data analysis which took into account that the sample was remounted on the sample holder. A growth of the initially nanometer-sized Pt particles into larger crystals as well as its agglomeration was found, preferentially in voids between support grains. Sintering occurred especially around the larger particles, which is in line with the Ostwald ripening mechanism reported for this system on a nanometer scale. The distribution of chemical elements in an embedded and mechanically cross-sectioned honeycomb was additionally mapped by an electron probe micro analyzer (EPMA), which in agreement to the μ-CT results shows no diffusion of Pt into the cordierite. Together with studies on the nanometer scale, these results allow a more thorough multi-scale modeling of exhaust gas catalysts, especially also during aging.