氧化物表面覆盖层稳定活性氧化铁催化苛刻高温水气变换反应

doi:10.1016/S1872-2067(25)64900-X

催化学报 ›› 2026, Vol. 82: 327-336.DOI: 10.1016/S1872-2067(25)64900-X

氧化物表面覆盖层稳定活性氧化铁催化苛刻高温水气变换反应

李荣坦, 杜相泽, 冯小辉, 王建洋, 塔娜, 傅强^*(), 包信和^*()

中国科学院大连化学物理研究所, 能源催化转化全国重点实验室, 辽宁大连 116023

收稿日期:2025-08-10 接受日期:2025-09-18 出版日期:2026-03-18 发布日期:2026-03-05
通讯作者: * 电子信箱: qfu@dicp.ac.cn (傅强),xhbao@dicp.ac.cn (包信和).
基金资助:
国家重点研发项目(2021YFA1502800);国家重点研发项目(2022YFA1504800);国家重点研发项目(2022YFA1504500);国家自然科学基金(22332006);国家自然科学基金(22288201);国家自然科学基金(22321002);国家自然科学基金(22402194);大连高层次人才创新支持计划(2023RG002);中国科学院碳中和光子科学中心;中央高校基本科研业务费专项资金资助(20720250005);中国博士后科学基金(2023M743425);中国博士后科学基金(2025T180267)

Shielding active Fe oxide by surface oxide overlayers for harsh high-temperature water-gas shift reaction

Rongtan Li, Xiangze Du, Xiaohui Feng, Jianyang Wang, Na Ta, Qiang Fu^*(), Xinhe Bao^*()

State Key Laboratory of Catalysis, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, Liaoning, China

Received:2025-08-10 Accepted:2025-09-18 Online:2026-03-18 Published:2026-03-05
Contact: * E-mail: qfu@dicp.ac.cn (Q. Fu),xhbao@dicp.ac.cn (X. Bao).
Supported by:
National Key R&D Program of China(2021YFA1502800);National Key R&D Program of China(2022YFA1504800);National Key R&D Program of China(2022YFA1504500);National Natural Science Foundation of China(22332006);National Natural Science Foundation of China(22288201);National Natural Science Foundation of China(22321002);National Natural Science Foundation of China(22402194);Dalian Innovation Support Plan for High Level Talents(2023RG002);Photon Science Center for Carbon Neutrality;Fundamental Research Funds for the Central Universities(20720250005);China Postdoctoral Science Foundation(2023M743425);China Postdoctoral Science Foundation(2025T180267)

摘要/Abstract

摘要：

高温水气变换(HT-WGS)反应作为工业上大规模制氢的核心工艺, 在构建清洁低碳能源体系中具有重要战略意义. HT-WGS反应的活性相为四氧化三铁(Fe₃O₄), 其在反应条件下易过度还原和烧结,这一稳定性问题制约着该过程的发展. 目前工业上通过添加铬助剂和采用高水气比(H₂O/CO ≥ 2.5)来稳定活性Fe₃O₄相, 但是高水气比原料气的使用增加了能耗, 而铬助剂也带来了潜在的环境问题. 因此, 开发适用于低水气比反应条件下的高活性、高稳定性、无铬Fe基HT-WGS催化剂对实现高效可持续制氢至关重要.

本研究提出构建氧化物表面覆盖层来稳定活性氧化物催化剂的策略. 基于低熔点前驱体的高流动性特性, 发展了一种熔润法制备催化剂的新方法, 在氧化铁(Fe₂O₃)颗粒表面实现了亚单层二氧化铈(CeO₂)覆盖层的精确构筑. X射线光电子能谱(XPS)和X射线衍射(XRD)结果表明, CeO₂在Fe₂O₃表面的分散阈值为1.8 wt%(约0.5个单层). 利用准原位XPS、扫描透射电镜、低能离子散射谱、一氧化碳程序升温还原、飞行时间二次离子质谱、原位XRD等表征技术, 深入揭示了CeO₂覆盖层对Fe₂O₃颗粒的屏蔽效应: 每个CeO₂盖层岛的周围形成“屏蔽作用区”, CeO₂覆盖层对“屏蔽区”内的Fe₂O₃具有双重作用, 既能促进Fe₂O₃部分还原为具有催化活性的Fe₃O₄, 又可有效抑制活性Fe₃O₄进一步深度还原为金属铁(Fe⁰). 在分散阈值以下, 屏蔽效应与Fe-O-Ce界面数量呈线性关系, 证实该效应来自于CeO₂覆盖层与Fe₂O₃颗粒之间的强氧化物-载体相互作用(SOSI). 进一步研究发现, 这种屏蔽效应在多种MO_x/Fe₂O₃体系(M = Ce, Cr, Mn, Mg, Al, Zn)中具有普适性, 而NiO_x, CoO_x, CuO_x覆盖层则不具备这一屏蔽效应. 结果表明, 氧化物-氧化物作用受表面氧化物中金属-氧键强弱的影响, 金属-氧键越强, 氧化物-氧化物作用越强. 基于氧化物覆盖层修饰策略, 设计开发的无铬CeO_x/Fe₂O₃催化剂表现出卓越的稳定性, 在150 h的稳定性测试中活性仅衰减4.5%, 显著优于无CeO₂覆盖层修饰的Fe₂O₃催化剂(20 h失活26.0%)和工业铁铬催化剂(100 h失活19.7%).

综上, 本研究表明氧化物表面覆盖层可通过SOSI作用调控衬底氧化物的氧化还原行为与催化性能, 也为高稳定性氧化物催化剂的设计提供了普适性策略. 该策略未来可拓展至低碳烷烃脱氢、CO₂加氢等其他涉及氧化物催化的重要反应体系, 对推动高效界面催化剂的理性设计具有重要指导意义.

关键词: 表面氧化物覆盖层, 强氧化物-载体相互作用, 界面限域效应, 氧化铁, 高温水气变换反应

Abstract:

Oxide supports are well known to significantly influence the structure and properties of active oxide overlayers through strong oxide-support interactions. However, the effect of oxide overlayers on the underlying active oxide substrates remains poorly understood. Here, we report the controllable formation of ceria (CeO₂) overlayers on a hematite (Fe₂O₃) surface (CeO₂/Fe₂O₃) via a melting-wetting method. Submonolayer CeO₂ patches facilitate the partial reduction of surrounding Fe₂O₃ to active magnetite (Fe₃O₄) while effectively suppress further reduction of Fe₃O₄ to inactive metallic iron (Fe⁰) under harsh high-temperature water-gas shift (HT-WGS) conditions. We demonstrate this stabilization effect of surface oxide patches (MO_x, M = Ce, Cr, Mn, Mg, Al and Zn) on surrounding active Fe oxide sites via creating a shielding zone around each oxide patch. As a result, Fe₂O₃ catalysts covered with a small amount of CeO₂ surface overlayers (~1.8 wt%) exhibit remarkable stability at 450 °C for over 100 h, in contrast to rapid deactivation observed in pure Fe₂O₃ and industrial iron-chromium (6.5 wt% Cr) catalysts. Building on these findings, we have developed an advanced HT-WGS process that utilizes Cr-free catalysts and significantly reduces steam consumption. This study highlights the critical role of surface oxide overlayers in modulating the redox behavior and reactivity of underlying active oxide substrates, developing an interface confinement strategy for the design of robust and efficient oxide catalysts.

Key words: Surface oxide overlayers, Strong oxide-support interaction, Interface confinement effect, Fe₂O₃, High-temperature water-gas shift

李荣坦, 杜相泽, 冯小辉, 王建洋, 塔娜, 傅强, 包信和. 氧化物表面覆盖层稳定活性氧化铁催化苛刻高温水气变换反应[J]. 催化学报, 2026, 82: 327-336.

Rongtan Li, Xiangze Du, Xiaohui Feng, Jianyang Wang, Na Ta, Qiang Fu, Xinhe Bao. Shielding active Fe oxide by surface oxide overlayers for harsh high-temperature water-gas shift reaction[J]. Chinese Journal of Catalysis, 2026, 82: 327-336.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(25)64900-X

https://www.cjcatal.com/CN/Y2026/V82/I3/327

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Fig. 1. Preparation and structure of CeOx/Fe2O3 catalysts. (a) Schematic diagram of preparation of CeOx/Fe2O3 catalysts by the melting-wetting method. (b) XRD patterns of CeOx/Fe2O3 catalysts. (c) Monolayer dispersion threshold of CeOx on Fe2O3 determined by XRD and XPS. (d) STEM and EDX mapping images of 2CeOx/Fe2O3 catalyst.

Fig. 2. Interface-dependent reduction behavior of CeOx/Fe2O3 catalysts. (a) CO-TPR of CeOx/Fe2O3 catalysts. CO MS signal (m/z = 28 5%CO/Ar balance. (b) Quasi in-situ Fe 2p3/2 XPS spectra of CeOx/Fe2O3 catalysts after CO-TPR at 330 and 600 °C. (c) ToF-SIMS spectra of CeOx/Fe2O3 catalysts. (d) Correlation of IFe2+/IFe and IFe0/IFe calculated from XPS results with IFe-O-Ce/IFe-O-Fe.

Fig. 3. Effect of surface oxide overlayers on the reduction behavior of surrounding Fe2O3. (a) Quasi in-situ Fe 2p3/2 XPS spectra of oxide/Fe2O3 catalysts after HT-WGS at 450 °C; 10%CO/10%H2O/80%N2, 30000 mL/(h·gcat). (b) In-situ XRD spectra of Fe2O3, 2CeOx/Fe2O3 and 2NiOx/Fe2O3 catalysts in simulated HT-WGS reaction gases at 450 °C for 1 h (the bottom line represents t = 0 and the upper line represents t = 1 h); 10%CO2/10%H2/80%N2, 60000 mL/(h·gcat). (c) Quasi in-situ XPS spectra of metal elements from oxide overlayers of oxide/Fe2O3 catalysts after HT-WGS at 450 °C; 10%CO/10%H2O/80%N2, 30000 mL/(h·gcat).

Fig. 4. Activity, long-term stability and structural evolution of oxide/Fe2O3 catalysts. CO conversion of CeOx/Fe2O3 catalysts at temperatures from 350 to 450 °C (a) and oxide/Fe2O3 catalysts (b) at t = 3 min and 10 h, at 450 °C. (c) Stability test of Oxide/Fe2O3 and industrial FeCrOx catalysts at 450 °C. Reaction conditions in (a-c): 10%CO/10%H2O/80%N2, 36000 mL/(h·gcat). (d) Quasi in-situ Fe 2p XPS spectra of the spent CrOx/Fe2O3 and industrial FeCrOx catalysts after stability test at 450 °C for 5 h. In-situ XRD patterns of industrial FeCrOx (e) and CrOx/Fe2O3 (f) catalysts in simulated HT-WGS reaction gases at 450 °C for 1 h (the bottom line represents t = 0 h and the upper line represents t = 1 h), 10%CO2/10%H2/80%N2, 60000 mL/(h·gcat).

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氧化物表面覆盖层稳定活性氧化铁催化苛刻高温水气变换反应

Shielding active Fe oxide by surface oxide overlayers for harsh high-temperature water-gas shift reaction

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