We report a unique in situ instrument development effort dedicated to studying gas/solid interactions relevant to heterogeneous catalysis and early stages of oxidation of materials via Atom Probe Tomography and Microscopy (APT/M). An in situ reactor cell has been developed to expose nanoscale volumes of material to reactive gas environments, in which temperature, pressure, and gas chemistry are well controlled. We demonstrate that the combination of this reactor cell with APT/M techniques can aid in building a better mechanistic understanding of resultant composition and surface and subsurface structure changes accompanying gas/surface reactions in metal and metal alloy systems through a series of case studies: O2/Rh, O2/Co, and O2/Zircaloy-4. In addition, the basis of a novel in operando mode of analysis within an atom probe instrument is also reported, which is inspired by Prof. Norbert Kruse’s earlier work on the development and use of the 1-Dimensionnal Atom Probe. The work presented here supports the implantation of APT/M techniques dedicated to atomic to near-atomically resolved gas/surface interaction studies of materials broadly relevant to heterogeneous catalysis and oxidation.
Revised: December 31, 2020 |
Published: November 2, 2020