Operando XPS in reactive plasmas: The importance of the wall reactions

Diulus, John Trey; Head, Ashley R.; Boscoboinik, Jorge Anibal; Kolmakov, Andrei

doi:10.1116/6.0004569

Operando XPS in reactive plasmas: The importance of the wall reactions

Journal Article · Thu May 15 00:00:00 EDT 2025 · Journal of Vacuum Science and Technology A

DOI:https://doi.org/10.1116/6.0004569· OSTI ID:2569466

Diulus, John Trey ^[1]; ^[2]; ^[2]; ^[1]

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

In this article, advancements in differential pumping and electron optics over the past few decades have enabled x-ray photoelectron spectroscopy (XPS) measurements at (near-)ambient pressures, bridging the pressure gap for characterizing realistic sample chemistries. Recently, we have demonstrated the capabilities of an ambient pressure XPS setup for in situ plasma environment measurements, allowing plasma-surface interactions to be studied in operando rather than using the traditional before-and-after analysis approach. This new “plasma-XPS” technique facilitates the identification of reaction intermediates critical for understanding plasma-assisted surface processes relevant to semiconductor nanomanufacturing, such as physical vapor deposition, etching, atomic layer deposition, and many other plasma applications. In this paper, we apply the plasma-XPS approach to monitor real-time surface chemical changes on a model Ag(111) single crystal exposed to oxidizing and reducing plasmas. We correlate surface-sensitive data with concurrent gas-phase XPS measurements and residual gas mass-spectrum analysis of species generated during plasma exposure, highlighting the significant role of plasma-induced chamber wall reactions. Ultimately, we demonstrate that plasma-XPS provides comprehensive insights into both surface and gas-phase chemistry, establishing it as a versatile and dynamic characterization tool with broad applications in microelectronics research. Finally, we outline potential enhancements and future metrology directions to advance plasma-XPS investigations further.

View Accepted Manuscript (DOE)

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:: 2569466

Report Number(s):: BNL--228273-2025-JAAM

Journal Information:: Journal of Vacuum Science and Technology A, Journal Name: Journal of Vacuum Science and Technology A Journal Issue: 4 Vol. 43; ISSN 1520-8559; ISSN 0734-2101

Publisher:: American Vacuum Society / AIPCopyright Statement

Country of Publication:: United States

Language:: English

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Operando XPS in reactive plasmas: The importance of the wall reactions

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