Adapting an Electron Microscopy Microheater for Correlated and Time-Resolved Ambient Pressure X-ray Photoelectron Spectroscopy

Karagoz, Burcu; Carpena-Núñez, Jennifer; Zhu, Yi; Baker, Lukas; Attenkofer, Klaus; Maruyama, Benji; Stacchiola, Dario; Zakharov, Dmitri N.; Head, Ashley R.

doi:10.1021/acs.chemmater.3c00615

Title: Adapting an Electron Microscopy Microheater for Correlated and Time-Resolved Ambient Pressure X-ray Photoelectron Spectroscopy

Journal Article · Thu Jul 27 00:00:00 EDT 2023 · Chemistry of Materials

DOI:https://doi.org/10.1021/acs.chemmater.3c00615· OSTI ID:1996202

Karagoz, Burcu ^[1]; Carpena-Núñez, Jennifer ^[2]; Zhu, Yi ^[3]; Baker, Lukas ^[1]; Attenkofer, Klaus ^[4]; Maruyama, Benji ^[5];

^[1]; Zakharov, Dmitri N. ^[1];

^[1]

Brookhaven National Laboratory (BNL), Upton, NY (United States). Center for Functional Nanomaterials (CFN)
Air Force Research Lab. (AFRL), Wright-Patterson AFB, OH (United States); UES, Inc., Dayton, OH (United States)
Brookhaven National Laboratory (BNL), Upton, NY (United States). National Synchrotron Light Source II (NSLS-II)
ALBA Synchrotron Radiation Facility (Spain)
Air Force Research Lab. (AFRL), Wright-Patterson AFB, OH (United States)

Environmental transmission electron microscopy (ETEM) can follow structural and chemical changes in nanomaterials under reaction conditions, including at temperatures up to 1300 °C and pressures up to ~20 mbar. However, ETEM studies are limited to localized areas of a sample and can benefit from correlative studies of a similar sample on larger length scales. Here, in this work, we describe the customization of a commercial microheater holder used in ETEM to anode-based ambient pressure X-ray photoelectron spectroscopy (APXPS), where chemical and electronic structure information is averaged over several hundred square micrometers. To benchmark heating capabilities in the APXPS instrument, core level binding energies were followed during surface chemical reactions of a Pd film, including CO adsorption–desorption, Pd oxidation, and PdO reduction. The fast heating feature of the microheaters advanced XPS experimental capabilities, including the collection of subsecond time-resolved spectra of the Pd 3d_5/2 peak during the reduction of an oxidized Pd film. The potential to use these heaters in a closed gas cell was also demonstrated by oxidizing Pd in a partial pressure of air locally dosed to the sample surface. General tips and considerations for the application of commercial ETEM heaters to any XPS system with a focused X-ray beam are discussed.

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Research Organization:: Brookhaven National Laboratory (BNL), Upton, NY (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES). Scientific User Facilities (SUF)

Grant/Contract Number:: SC0012704

OSTI ID:: 1996202

Report Number(s):: BNL-224698-2023-JAAM

Journal Information:: Chemistry of Materials, Vol. 35, Issue 15; ISSN 0897-4756

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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37 INORGANIC
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
binding energy
palladium
redox reactions
x-ray photoelectron spectroscopy
x-rays

Title: Adapting an Electron Microscopy Microheater for Correlated and Time-Resolved Ambient Pressure X-ray Photoelectron Spectroscopy

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