Title : Operando and in-situ characterisation of energy materials: Understanding dynamic processes in catalysis and hydrogen technologies
Abstract:
Energy materials rarely behave in steady-state — catalysts restructure under reaction conditions, electrode surfaces evolve during charge-discharge, and hydrogen storage materials undergo phase transitions invisible to post-mortem analysis. Understanding these dynamic processes is the prerequisite for designing systems that remain reliable and efficient across operational lifetimes, and operando and in situ characterisation methods have transformed this landscape by making it possible to observe structure-property relationships as they unfold. This talk presents an integrated framework built around synchrotron XAS/XANES/EXAFS, AP-XPS, and HE-XRD, applied across electrocatalysis, alkaline water electrolysis, and hydrogen carrier systems, enabled by purpose-designed in situ electrochemical cells that replicate realistic operating conditions of temperature, pressure, electrolyte composition, and applied potential.
Across several material systems, the talk demonstrates how these methods resolve questions static techniques cannot: oxidation state trajectories in Ni-Fe OER catalysts under applied overpotential; coordination environment changes in Mo-based HER electrocatalysts during hydrogen evolution; and reversible structural transitions in LOHC dehydrogenation catalysts across hydrogenation-dehydrogenation cycles. Practical aspects of cell design — window material selection, beam path geometry, electrolyte compatibility, and minimising X-ray induced artefacts — are discussed as transferable guidelines accumulated across multiple beamtime campaigns at the Canadian Light Source, NSLS-II, APS, SSRL, MAX-IV, and INDUS-2. The talk closes with a forward look at multi-modal pipelines combining operando XAS with in situ Raman, impedance spectroscopy, and X-ray fluorescence to resolve increasingly complex degradation phenomena in next-generation electrochemical energy systems.
