Catalyst characterization plays an important role in developing catalytic
materials because it helps to identify active catalytic phases or centers and to elucidate
reaction mechanisms. Several characterization methods have been parallelized and
successfully applied in the high-throughput workflow of catalyst development. We
present characterization equipment developed at the Leibniz Institute for Catalysis and
show applications in three research areas: (i) in catalyst synthesis for identifying
suitable preparation conditions, (ii) in understanding factors governing catalytic
performance for identifying structure-reactivity relationships, and (iii) in understanding
catalyst deactivation for elucidating the deactivation mechanisms. 6-fold and 8-fold
reactors are used for temperature programmed reduction (TPR), oxidation (TPO),
desorption (TPD) and chemical titration experiments. TPR has been successfully
applied for studying the reducibility of supported Ni-containing catalysts for CO2
reforming of CH4 and for investigating the interaction between metal oxide species and
support materials. Chemisorption of H2 and CO2 has provided information about Ni
dispersion and basic properties of said catalysts, and with TPO of spent catalysts coke
formation was monitored. To prepare catalysts for visible-light induced water splitting,
we studied the formation of nitrides and oxynitrides from oxides upon their temperature
programmed treatment under a flow of ammonia. We also used 6-fold and 36-fold
parallel reactors utilizing UV/vis catalyst analysis in reflectance mode to study changes
in valence state and coordination of supported VOx during oxidative dehydrogenation of
propane, and to follow coke formation during catalyst deactivation in non-oxidative
dehydrogenation of propane.
Keywords: Ammonolysis, band gap, CO2 reforming of methane, diffuse
reflectance UV/vis spectroscopy, dry reforming of methane, high throughput
catalysis, high throughput characterization, high throughput experimentation,
high-throughput synthesis, metal dispersion, mixed-metal oxynitrides, operando
spectroscopy, parallel reactors, propane dehydrogenation, pulse experiments,
steady-state isotopic transient kinetic analysis, temperature programmed
desorption, temperature programmed oxidation, temperature programmed
reactions, temperature programmed reduction, water splitting.
