Simultaneous measurement of X-ray small angle scattering, absorption and reactivity: A continuous flow catalysis reactor

A fixed-bed, continuous flow catalysis reactor is described, in which GISAXS (grazing incidence small angle X-ray scattering)/GIXAS (grazing incidence X-ray absorption spectroscopy) and TPR (temperature-programmed reaction) can be measured simultaneously on samples with low metal coverage. The capabilities offered by this setup are illustrated in the example of the dehydrogenation of cyclohexene, where the size, oxidation state and reactivity of supported cobalt clusters were investigated under ambient pressure conditions. The GIXAS data reveal an evolution of the oxidation state of the catalytic particles with temperature. Simultaneously recorded GISAXS data show stable clusters, without any indication of sintering under employed reaction conditions.