界面动态可逆包覆促进水气变换反应性能

doi:10.1016/S1872-2067(24)60193-2

催化学报 ›› 2025, Vol. 68: 394-403.DOI: 10.1016/S1872-2067(24)60193-2

界面动态可逆包覆促进水气变换反应性能

唐南方^a, 商庆浩^a^,^b, 陈帅^a, 马玉霞^a, 顾青青^a, 林露^a, 蒋齐可^a, 许国梁^a, 吴春田^a, 杨冰^a, 吴志杰^c, 施慧^d, 刘健^e^,^f^,^g^,^*(), 罗文豪^a^,^g^,^*(), 丛昱^a^,^*()

^a中国科学院大连化学物理研究所, 催化与新材料研究室, 辽宁大连 116023, 中国
^b中国科学院大学, 北京 100049, 中国
^c中国石油大学(北京)重质油全国重点实验室, 北京 102249, 中国
^d扬州大学化学化工学院, 江苏扬州 225009, 中国
^e中国科学院大连化学物理研究所, 催化基础国家重点实验室, 辽宁大连 116023, 中国
^f萨里大学DICP-Surrey未来材料联合中心, 萨里, 英国
^g内蒙古大学化学化工学院, 内蒙古自治区稀土催化重点实验室, 内蒙古呼和浩特 010021, 中国

收稿日期:2024-09-11 接受日期:2024-10-10 出版日期:2025-01-18 发布日期:2025-01-02
通讯作者: * 电子信箱: jian.liu@surrey.ac.uk (刘健), w.luo@imu.edu.cn (罗文豪), ycong@dicp.ac.cn (丛昱).
基金资助:
国家重点研发计划(2022YFB4300700);国家自然科学基金(21802134);国家自然科学基金(22479082);中科院青年基础研究项目(YSBR-022);内蒙古大学基金(10000-23112101/081);内蒙古青年科技英才基金(NJYT24019)

Reversible encapsulation tailored interfacial dynamics for boosting the water-gas shift performance

Nanfang Tang^a, Qinghao Shang^a^,^b, Shuai Chen^a, Yuxia Ma^a, Qingqing Gu^a, Lu Lin^a, Qike Jiang^a, Guoliang Xu^a, Chuntian Wu^a, Bing Yang^a, Zhijie Wu^c, Hui Shi^d, Jian Liu^e^,^f^,^g^,^*(), Wenhao Luo^a^,^g^,^*(), Yu Cong^a^,^*()

^aCAS Key Laboratory of Science and Technology on Applied Catalysis, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, Liaoning, China
^bUniversity of Chinese Academy of Sciences, Beijing 100049, China
^cState Key Laboratory of Heavy Oil Processing and the Key Laboratory of Catalysis of CNPC, China University of Petroleum, Beijing 102249, China
^dSchool of Chemistry and Chemical Engineering, Yangzhou University, Yangzhou 225009, Jiangsu, China
^eState Key Laboratory of Catalysis, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, 457 Zhongshan Road, Dalian 116023, Liaoning, China
^fDICP-Surrey Joint Centre for Future Materials, Department of Chemical and Process Engineering, University of Surrey, Guildford, Surrey, GU2 7XH, UK
^gInner Mongolia Key Laboratory of Rare Earth Catalysis, College of Chemistry and Chemical Engineering Inner Mongolia University, Hohhot 010021, Inner Mongolia, China

Received:2024-09-11 Accepted:2024-10-10 Online:2025-01-18 Published:2025-01-02
Contact: * E-mail: jian.liu@surrey.ac.uk (J. Liu),w.luo@imu.edu.cn (W. Luo), ycong@dicp.ac.cn (Y. Cong).
Supported by:
National Key R&D program of China(2022YFB4300700);National Nature Science Foundation of China(21802134);National Nature Science Foundation of China(22479082);CAS Project for Young Scientists in Basic Research(YSBR-022);Funding of Inner Mongolia University(10000-23112101/081);Inner Mongolia Youth Science and Technology Talents(NJYT24019)

摘要/Abstract

摘要：

水气变换反应(WGS)是重要的制氢和CO脱除过程, 广泛应用于能源相关领域. 前期研究表明, 模型催化剂上金属-载体界面在WGS反应决速步-水活化解离过程中起着重要作用; 金属键合的羟基物种直接参与了水活化过程, 可有效提高WGS反应效率. 然而, 如何精准制备富含金属-氧化物界面活性位的高性能WGS反应催化剂, 以及原位追踪反应过程中活性位、关键活性物种的动态演化仍是一项重要挑战.
本文利用“缺陷工程”策略通过两步水热法成功将Pt团簇(~0.8 nm)包覆在富含缺陷位CeO₂纳米棒中, 获得了Pt@d-CeO₂催化剂. 将Pt@d-CeO₂用于WGS反应中, 在极高空速(GHSV = 150000 h^‒1)下, 300 ^oC时CO转化率为86%, 350 ^oC时达到平衡转化率(95%). 转化频率值在350 ^oC时高达12.27 s^‒1, 比已报道的相近反应条件下同类催化剂高一个数量级. 催化剂具有良好的稳定性, 经100 h反应, CO转化率未发现明显下降. 像差校正透射电镜结果表明, Pt团簇以0.6‒1 nm尺度分散在氧化铈上, 且被氧化铈薄层包覆. 能量散射谱、电子能量损失谱、X射线光电子能谱(XPS)和原位透射模式傅里叶变换红外光谱(TM-FT-IR)结果均证实了Pt-CeO₂的界面包覆特性. 程序升温表面脱附结果初步表明, Pt@d-CeO₂催化剂上WGS反应总体历程是CO先在Pt-CeO₂界面处反应生成CO₂, 然后H₂O解离生成H₂. CO-程序升温还原、原位TM-FT-IR和原位近环境压力XPS结果表明, Pt-CeO₂包覆界面为本征活性位, 界面处的端-OH为关键活性物种. 利用一系列原位表征手段实时追踪界面活性位和端-OH在反应过程中的动态演化, 进而提出Pt@d-CeO2催化剂上WGS反应的详细反应历程: 依据一系列原位表征结果提出Pt@d-CeO₂催化剂上WGS反应的详细反应历程: 首先, CO与Pt-CeO₂包覆界面处的端-OH反应生成活性中间物种COOH, 继而分解成CO₂和H, CeO₂包覆的Pt团簇部分暴露并产生新的活性氧空位; 然后, H₂O在新生成的氧空位上解离重新生成端-OH和H, 两个H结合生成H₂, 部分裸露的Pt团簇重新被CeO₂薄层包覆, 完成催化循环.
综上所述, “缺陷工程”策略产生Pt-CeO₂界面包覆特性及其可逆动态演化促进WGS反应性能, 为高性能负载型金属/氧化物催化剂的设计开发提供了新思路.

关键词: 界面动态演化, 羟基, 水气变化反应, 原位光谱

Abstract:

Revealing the structure evolution of interfacial active species during a dynamic catalytic process is a challenging but pivotal issue for the rational design of high-performance catalysts. Here, we successfully prepare sub-nanometric Pt clusters (~0.8 nm) encapsulated within the defects of CeO₂ nanorods via an in-situ defect engineering methodology. The as-prepared Pt@d-CeO₂ catalyst significantly boosts the activity and stability in the water-gas shift (WGS) reaction compared to other analogs. Based on controlled experiments and complementary (in-situ) spectroscopic studies, a reversible encapsulation induced by active site transformation between the Pt²⁺-terminal hydroxyl and Pt^δ⁺-O vacancy species at the interface is revealed, which enables to evoke the enhanced performance. Our findings not only offer practical guidance for the design of high-efficiency catalysts but also bring a new understanding of the exceptional performance of WGS in a holistic view, which shows a great application potential in materials and catalysis.

Key words: Interfacial dynamics, Hydroxyls, Water-gas shift reaction, In-situ spectroscopy

唐南方, 商庆浩, 陈帅, 马玉霞, 顾青青, 林露, 蒋齐可, 许国梁, 吴春田, 杨冰, 吴志杰, 施慧, 刘健, 罗文豪, 丛昱. 界面动态可逆包覆促进水气变换反应性能[J]. 催化学报, 2025, 68: 394-403.

Nanfang Tang, Qinghao Shang, Shuai Chen, Yuxia Ma, Qingqing Gu, Lu Lin, Qike Jiang, Guoliang Xu, Chuntian Wu, Bing Yang, Zhijie Wu, Hui Shi, Jian Liu, Wenhao Luo, Yu Cong. Reversible encapsulation tailored interfacial dynamics for boosting the water-gas shift performance[J]. Chinese Journal of Catalysis, 2025, 68: 394-403.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(24)60193-2

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Fig. 1. Catalyst preparation and AC-STEM analysis of Pt@d-CeO2. (A) Schematic illustration of the in-situ defect engineering synthesis approach for Pt@d-CeO2. (B,C,D) Bright field AC-STEM images of Pt@d-CeO2.

Fig. 2. Catalytic performance of Pt@d-CeO2 and Pt/CeO2 catalysts in the WGS reaction. (A) CO conversion during the WGS reaction as a function of temperature over the Pt@d-CeO2 and Pt/CeO2 catalysts. (B) TOF values (mole specific activities) obtained at CO conversion levels below 15% at different reaction temperatures. (C) CO conversion as a function of time on stream during WGS reaction over Pt@d-CeO2 at 350 °C and Pt/CeO2 at 400 °C. Reaction conditions: 8% CO/20% H2O/20% N2/52% Ar, GHSV=150000 h?1.

Fig. 3. Characterization of the Pt-based catalysts. AC-HAADF-STEM image (A) and linear-scan EDS spectra (B) of Pt@d-CeO2. Linear-scan follows orange arrow on the AC-HAADF-STEM image. AC-HAADF-STEM image of Pt@d-CeO2 (C) and its corresponding EELS spectra (D) of three selected regions. The yellow circle in the figures represents the Pt clusters. (E,F) Low temperature TM-FT-IR spectra of CO upon a stepwise adsorption and evacuation on the Pt@d-CeO2 and Pt/CeO2. All the TM-FT-IR spectra were collected at ?150 °C. (G) XPS spectra of Pt@d-CeO2 and Pt/CeO2 in the Pt 4f region. (H) Low temperature TM-FT-IR spectra of CO adsorption for Pt@d-CeO2 and Pt/CeO2 with and without CO prereduction at 300 °C.

Fig. 4. Characterization of Pt-based catalysts via various temperature-programmed techniques. (A) TPSR profiles of Pt@d-CeO2. Signals of CO (m/z = 28), H2O (m/z = 18), H2 (m/z = 2) and CO2 (m/z = 44) were detected. The sample was flushed with pure He at 300 °C for 30 min before test. The signal evolution was collected under 0.5% CO/2% H2O at a ramping rated of 5 °C min?1. (B) CO-TPR profiles of Pt@d-CeO2, d-CeO2, Pt/CeO2 and CeO2. The samples were firstly pretreated with a flow of pure He at 350 °C for 30 min, and the TPR were performed from ?50 to 700 °C at a ramping rate of 10 °C min?1 under 5% CO/He. (C) TPSR profiles of H2O dissociation over Pt@d-CeO2 with or without CO introduction at 300 °C. (D) Dynamic TM-FT-IR spectra of ?OH region for CO activation over Pt@d-CeO2. The sample is first exposed to 2 mbar CO and subsequently outgassed at temperatures ranging from ?150 to 50 °C.

Fig. 5. In-situ characterization of Pt@d-CeO2 in the WGS reaction. (A) In-situ TM-FT-IR spectra of -OH region over Pt@d-CeO2 at 300 °C when altering introduction of a flow of CO or H2O. (B) In-situ TM-FT-IR spectra of -OH region with CO re-introduction at 300 °C with stepwise increase of CO pressure from 1 to 75 mbar over Pt@d-CeO2 after H2O exposure. (C) Pt 4f NAP-XPS of the Pt@d-CeO2 at 300 °C. NAP-XPS spectra conducted at 300 °C with peak fittings. The spectra of Pt@d-CeO2 were acquired after the first 10 mbar Ar exposure for 30 min, the second CO exposure for 30 min, and the final H2O exposure for 30 min. (D) Schematic illustration of the dynamic evolution of interfacial species of Pt@d-CeO2 in the WGS reaction.

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界面动态可逆包覆促进水气变换反应性能

Reversible encapsulation tailored interfacial dynamics for boosting the water-gas shift performance

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