Operando XPS for Plasma Process Monitoring: A Case Study on the Hydrogenation of Copper Oxide Confined under h-BN

Diulus, J. Trey; Naclerio, Andrew E.; Boscoboinik, Jorge Anibal; Head, Ashley R.; Strelcov, Evgheni; Kidambi, Piran R.; Kolmakov, Andrei

doi:10.1021/acs.jpcc.4c00253

Title: Operando XPS for Plasma Process Monitoring: A Case Study on the Hydrogenation of Copper Oxide Confined under h-BN

Journal Article · 28 April 2024 · Journal of Physical Chemistry. C

DOI: https://doi.org/10.1021/acs.jpcc.4c00253 · OSTI ID:2349260

^[1]; Naclerio, Andrew E. ^[2];

^[3];

^[3]; Strelcov, Evgheni ^[1];

^[2];

^[1]

National Inst. of Standards and Technology (NIST), Gaithersburg, MD (United States)
Vanderbilt Univ., Nashville, TN (United States)
Brookhaven National Laboratory (BNL), Upton, NY (United States)

Here, we demonstrate that ambient pressure x-ray photoelectron spectroscopy (APXPS) can be used for in situ studies of dynamic changes in surface chemistry in a plasma environment. This opens a new and vast application space for XPS and greatly complements modern spectroscopy techniques to probe plasma-solid/liquid interactions relevant to process monitoring in the semiconductor industry, bio-medical plasma applications and plasma remediation technologies. Hexagonal boron nitride (h-BN) grown on Cu was used in this study as a well-defined model system for plasma process monitoring and because of its unique chemical, optical and electrical properties that make it a prospective material for advanced electronics. To better understand the stability and surface chemistry of h-BN during plasma assisted processing, we track in real time the plasma-induced chemical state changes of B, N and the underlying Cu substrate using APXPS equipped with an AC discharge plasma source operating at 13 Pa. Residual gas analysis (RGA) mass-spectra were concurrently collected during plasma-XPS to track reaction products formed during plasma exposure. A clear reduction of Cu_xO is seen, while an h-BN layer remains intact, suggesting hydrogen radical (H^•) species can attack the exposed and h-BN covered Cu oxide patches and partially reduce the underlying substrate without significantly damaging the overlaying h-BN, which is of practical importance for development of h-BN encapsulated devices and interfaces. In addition to demonstration of plasma-XPS capabilities we discuss the observed challenges (e.g., parasitic plasma-chamber walls reactions and charging effects) and propose potential solutions.

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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); National Science Foundation (NSF)

Grant/Contract Number:: SC0012704; SC0022915

OSTI ID:: 2349260

Report Number(s):: BNL--225597-2024-JAAM; {"","Journal ID: ISSN 1932-7447"}

Journal Information:: Journal of Physical Chemistry. C, Journal Name: Journal of Physical Chemistry. C Journal Issue: 18 Vol. 128; ISSN 1932-7447

Publisher:: American Chemical SocietyCopyright Statement

Country of Publication:: United States

Language:: English

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