Surface and Bulk Approach to Time-resolved Characterization of Heterogeneous Catalysts

• Published in: ChemCatChem 2012-06, Vol.4 (6), p.725-737
• Main Authors: Kubacka, Anna, Iglesias-Juez, Ana, Martínez-Arias, Arturo, Di Michiel, Marco, Newton, Mark A., Fernández-García, Marcos
• Format: Article
• Language: English
• Subjects: heterogeneous catalysis; operando approach; vibrational techniques; X-ray absorption; X-ray diffraction
• ISSN: 1867-3880; 1867-3899
• DOI: 10.1002/cctc.201200131

The evolution of time‐resolved experiments, covering a multipurpose surface and bulk characterization of catalytic solids, during their preparation process and under reaction conditions, is presented. Particular emphasis is given to recent studies that attempt to unveil contemporary unresolved questions concerning the control of physicochemical properties of nanosolids, as well as the evolution of such solid materials under reactive atmospheres. To reach this goal, representative in situ and in operando works, using either modern (mostly synchrotron radiation based) approaches or multi‐technique methods (mainly, although not exclusively, X‐ray–vibrational coupling), and considering experiments in liquid and gas phase, as well as with amorphous, nanocrystalline and surface‐deposited materials, are reviewed. The incredible bulk: Catalytic solid preparation and performance at reaction conditions are analyzed through a multipurpose operando prism accounting for a complete surface and bulk characterization.