Chapter 1. Thermal analysis: a guide through catalyst’s synthesis and reaction process

Various thermal analysis methods trace all stages of catalyst formation. This chapter deals with a sequential study of the main stages of catalyst formation from widely used thermogravimetry to specially developed in situ calorimetry through precursor synthesis to the catalytic reaction. Particular focus is given to Cu, Zn-based catalytic systems for methanol synthesis and Ni, Mg-based catalysts for dry methane reforming. The calcination of hydroxocarbonates and their decomposition kinetics were investigated by the simultaneous thermal analysis-mass spectrometry (STA-MS) method. Using temperature-programmed reduction technique, the composition of oxide systems, their reduction, and activation of the metal catalyst was analyzed. Additional diffraction, spectroscopic, and microscopic methods characterized the change in metal-support interaction during successive oxidative and reducing temperature treatments. Structural-functional relationships can be identified based on thermochemical, structural, and catalytic data. High-pressure thermogravimetry was used to probe the adsorption layer on the catalyst surface under methanol synthesis and coking under dry methane reforming conditions. Finally, the application of in situ calorimetry for studying the catalyst restructuring in oxidative reactions is shown.