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Review Article | Open Access

Probe of nanocatalysts in-action by ambient pressure photoelectron spectroscopy

Zikang Su1,§ Chen Zhang1,§ Xianze Zhang1 Shanshan Wang2Yaoxian Yang1 Zhi Wang1 Wenxing Chen3 Xueqiang Zhang1 ( )
Laser Micro/Nano Fabrication Laboratory, School of Mechanical Engineering, Beijing Institute of Technology, Beijing 10081, China
Analysis & Testing Center, Beijing Institute of Technology, Beijing 10081, China
Energy & Catalysis Center, School of Materials Science and Engineering, Beijing Institute of Technology, Beijing 100081, China

§ Zikang Su and Chen Zhang contributed equally to this work.

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Abstract

Elucidation of a physicochemical process on nanocatalysts, especially under continuously evolving conditions, is often heavily tool-driven because of technical challenges. Recently, ambient pressure X-ray photoelectron spectroscopy (APXPS) emerges as an emerging photon-in-electron-out technique in in-situ/operando analysis by bridging the pressure-gap between conventional ultra-high vacuum (UHV) and near ambient or even close to operating conditions, rendering the advancement of XPS from a UHV-based technique to a versatile and powerful tool that enables the specific probe of numerous events taking place at the gas–solid, liquid–solid and liquid–gas nanoscale interfaces which are critical to nanocatalysis research. For example, APXPS probes information on catalytically active phase and reaction kinetics in nanocatalytic processes; details inside the electric double-layer at an electrolyte/electrode interface can now be accessed; more efficient nanocatalyst design can be achieved and energy transfer venues can be optimized. Here, we aim to critically review the recent advances in instrumentation and the probe of the gas–solid, liquid–solid, and gas–liquid nanoscale interfaces using APXPS-based methodologies, followed by putting forward an outlook of the development of APXPS as a rising in-situ/operando analytical means in surface science, nanocatalysis, nanoscience and materials science.

Graphical Abstract

Benefiting from its capability to bridge the pressure gap between ultra-high vacuum and practical environments, ambient pressure X-ray photoelectron spectroscopy (APXPS) provides unprecedented insights into the dynamic interfacial processes of nanocatalysts across gas–solid, liquid–solid and gas–liquid interfaces, enabling in-depth mechanistic understanding and rational design of heterogeneous catalytic systems. By integrating cutting-edge instrumental advancements and interdisciplinary case studies, this review systematically highlights APXPS’s pivotal role in dissecting catalytic reaction pathways, identifying active sites, and optimizing nanomaterials for energy conversion applications.

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Nano Research
Article number: 94907709

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Cite this article:
Su Z, Zhang C, Zhang X, et al. Probe of nanocatalysts in-action by ambient pressure photoelectron spectroscopy. Nano Research, 2025, 18(9): 94907709. https://doi.org/10.26599/NR.2025.94907709
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Received: 19 April 2025
Revised: 19 June 2025
Accepted: 20 June 2025
Published: 01 September 2025
© The Author(s) 2025. Published by Tsinghua University Press.

This is an open access article under the terms of the Creative Commons Attribution 4.0 International License (CC BY 4.0, https://creativecommons.org/licenses/by/4.0/).