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Combination of a reaction cell and an ultra-high vacuum system for the in situ preparation and characterization of a model catalyst

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Abstract

An in-depth understanding of the structure–activity relationship between the surface structure, chemical composition, adsorption and desorption of molecules, and their reaction activity and selectivity is necessary for the rational design of high-performance catalysts. Herein, we present a method for studying catalytic mechanisms using a combination of in situ reaction cells and surface science techniques. The proposed system consists of four parts: preparation chamber, temperature-programmed desorption (TPD) chamber, quick load-lock chamber, and in situ reaction cell. The preparation chamber was equipped with setups based on the surface science techniques used for standard sample preparation and characterization, including an Ar+ sputter gun, Auger electron spectrometer, and a low-energy electron diffractometer. After a well-defined model catalyst was prepared, the sample was transferred to a TPD chamber to investigate the adsorption and desorption of the probe molecule, or to the reaction cell, to measure the catalytic activity. A thermal desorption experiment for methanol on a clean Cu(111) surface was conducted to demonstrate the functionality of the preparation and TPD chambers. Moreover, the repeatability of the in situ reaction cell experiment was verified by CO2 hydrogenation on the Ni(110) surface. At a reaction pressure of 800 Torr at 673 K, turnover frequencies for the methanation reaction and reverse water–gas shift reaction were 0.15 and 7.55 Ni atom−1 s−1, respectively.

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Data availability

The data that support the findings of this study are openly available in Science Data Bank at https://doi.org/10.57760/sciencedb.j00186.00074 and https://cstr.cn/31253.11.sciencedb.j00186.00074.

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Author notes

  1. Yi-Jing Zang and Shu-Cheng Shi have contributed equally to this work.

Authors and Affiliations

  1. State Key Laboratory of Functional Materials for Informatics, Shanghai Institute of Microsystem and Information Technology, Chinese Academy of Sciences, Shanghai, 200050, China

    Yi-Jing Zang, Hui Zhang, Mao Ye & Zhi Liu

  2. School of Physical Science and Technology, ShanghaiTech University, Shanghai, 201210, China

    Shu-Cheng Shi, Yong Han, Wei-Jia Wang & Zhi Liu

  3. Center for Transformative Science, ShanghaiTech University, Shanghai, 201210, China

    Yong Han, Peng Liu & Zhi Liu

  4. University of Chinese Academy of Sciences, Beijing, 100049, China

    Yi-Jing Zang

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Contributions

All authors contributed to the study conception and design. Material preparation, data collection and analysis were performed by Yi-Jing Zang, Shu-Cheng Shi, and Yong Han. Zhi Liu, Hui Zhang, Wei-Jia Wang, Peng Liu, and Mao Ye provided a great help to the study. The first draft of the manuscript was written by Yi-Jing Zang, Shu-Cheng Shi and Yong Han, and all authors commented on previous versions of the manuscript. All authors read and approved the final manuscript.

Corresponding authors

Correspondence to Yong Han or Zhi Liu.

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Conflict of interest

Zhi Liu is an editorial board member for Nuclear Science and Techniques and was not involved in the editorial review, or the decision to publish this article. All authors declare that there are no competing interests.

Additional information

This work was supported by the National Natural Science Foundation of China (Nos. 21802096, 21832004, 21902179, 21991152, and 21991150) and the Shanghai XFEL Beamline Project (SBP) (31011505505885920161A2101001). H.Z. acknowledges the support of the Shanghai Sailing Program (19YF1455600).

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Zang, YJ., Shi, SC., Han, Y. et al. Combination of a reaction cell and an ultra-high vacuum system for the in situ preparation and characterization of a model catalyst. NUCL SCI TECH 34, 65 (2023). https://doi.org/10.1007/s41365-023-01228-w

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