Nanoscale Perspectives of Metal Degradation via In Situ Atom Probe Tomography
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ORIGINAL PAPER
Nanoscale Perspectives of Metal Degradation via In Situ Atom Probe Tomography Sten V. Lambeets1 · Elizabeth J. Kautz2 · Mark G. Wirth1 · Graham J. Orren1 · Arun Devaraj3 · Daniel E. Perea1
© The Author(s) 2020
Abstract 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 (APM). An in situ reactor cell, similar in concept to other reports, 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 APM 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: O 2/Rh, O2/Co, and O 2/Zircaloy-4. In addition, the basis of a novel operando mode of analysis within an atom probe instrument is also reported. The work presented here supports the implementation of APM techniques dedicated to atomic to near-atomically resolved gas/surface interaction studies of materials broadly relevant to heterogeneous catalysis and oxidation. Keywords Atom probe tomography · Atom probe microscopy · Oxidation · In situ · Operando · Cobalt · Rhodium · Zircaloy-4
1 Introduction The physics governing chemical reactions at surfaces and interfaces, involved in both heterogeneous catalysis and oxidation processes, share fundamental synergistic interactions between reactant gases and specific surface structures [1]. Additionally, gas phase reactions on surfaces have Electronic supplementary material The online version of this article (https://doi.org/10.1007/s11244-020-01367-z) contains supplementary material, which is available to authorized users. * Sten V. Lambeets [email protected] * Daniel E. Perea [email protected] 1
Environmental Molecular Sciences Laboratory, Earth and Biological Sciences Directorate, Pacific Northwest National Laboratory, Richland, WA 99352, USA
2
National Security Directorate, Pacific Northwest National Laboratory, Richland, WA 99352, USA
3
Physical and Computational Sciences Directorate, Pacific Northwest National Laboratory, Richland, WA 99352, USA
significant socioeconomic impact worldwide; heterogeneous catalysis directly impacts the productivity of all major chemical processes, whereas oxidation has serious implications for the safety and economic viability of national and private infrastructure. Importantly, scientific research into these phenomena are heavily pursued. However, a fundamental mechanistic understanding of gas-surface reactions leading to the development of oxide scale on metal substrates relevant to catalysis and oxidation remains inadequate, highlighting the need for the development and application of novel analytical techniques that can
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