CeO2/Co3O4催化剂界面相互作用的尺寸依赖性: 从单原子到纳米颗粒

doi:10.1016/S1872-2067(26)65120-0

摘要/Abstract

摘要：

CeO₂/Co₃O₄复合氧化物在催化氧化反应中展现出媲美贵金属的催化潜力, 但界面相互作用的原子尺度起源仍存在争议. 电子转移方向、氧活化机制以及缺陷结构的形成路径等问题长期悬而未决. 针对这些问题, 本研究通过精确构筑Co₃O₄负载的单原子Ce与CeO₂纳米颗粒两种截然不同的界面模型, 从原子尺度揭示了Ce物种尺寸对界面相互作用的调控本质, 明确了长期以来关于电子转移方向的争议, 并为理性设计高性能氧化物-氧化物催化剂提供了新的认识.
本文采用离子交换法结合水热过程, 成功在Co₃O₄表面实现了Ce单原子的原子级分散及CeO₂纳米颗粒的尺寸可控负载. 球差校正电镜、X-射线吸收谱及X-射线光电子能谱等表征结合密度泛函理论计算发现, 单原子Ce主要以Ce³⁺形态选择性占据Co₃O₄尖晶石结构的八面体Co³⁺位点. 由于Ce³⁺半径远大于Co³⁺, 这一取代诱发局域压缩应变, 显著降低相邻位点氧空位形成能(由2.1 eV降至0.96 eV), 促进Ce³⁺-Vₒ-Co活性位点的形成. 更为关键的是, Ce³⁺作为强电子供体, 将Co的d带中心由-2.04 eV上移至-1.75 eV, 显著增强了向O₂反键轨道的电子注入能力, 使O₂键级降至1.5, 解离能垒由3.83 eV大幅下降至1.87 eV. 相比之下, CeO₂纳米颗粒与Co₃O₄形成扩展界面, 电子注入范围更广但Ce³⁺比例较低. 电子由CeO₂向Co₃O₄的迁移引发界面Co³⁺向Co²⁺的还原, 伴随八面体向四面体结构的转变; 当这一电子注入速率超过结构弛豫速率时, 晶格发生局域塌陷, 在CeO₂/Co₃O₄界面形成缺陷乃至非晶区. 该结构演化对CeO₂尺寸高度敏感: 2.4 nm颗粒产生界面点缺陷, 7.3 nm颗粒则诱导非晶区域形成, 氧迁移率随之提升, 但Ce³⁺比例由25.15%降至18.68%. 苯甲醇氧化反应结果显示, 单原子催化剂活性是纳米颗粒催化剂的1.5倍, 表观活化能低27.7 kJ/mol, 且Ce归一化活性高出近两个数量级, 证实电子效应对本征活性的主导作用远高于界面重构.
综上, 本文揭示了单原子与纳米颗粒两种截然不同的促进机制: 前者以局域电子效应为核心, 后者以界面离子迁移驱动的结构重组为主导. 这一发现不仅明确了CeO₂/Co₃O₄界面作用中长期存在的争议, 更揭示了氧化物催化中“尺寸决定路径”的普适性规律. 未来研究可进一步拓展至其他稀土-过渡金属氧化物体系, 探索利用单原子掺杂或限域界面工程协同优化电子供给与氧迁移能力的可行路径, 为设计新一代高效、低成本氧化催化剂提供原子尺度的理论依据与实验范式.

关键词: 四氧化三钴催化剂, 二氧化铈, 催化氧化, 界面重构, 单原子, 纳米颗粒

Abstract:

Although CeO₂/Co₃O₄ composites exhibit excellent catalytic performance in oxidation reactions, the atomic-scale origin of their interfacial interactions remains unclear. In this work, we compare two contrasting catalysts: Co₃O₄-supported Ce single atoms and Co₃O₄-supported CeO₂ nanoparticles. We reveal that these two forms of Ce promote catalytic performance through different mechanisms. Ce single atoms occupy the octahedral Co³⁺ sites within the Co₃O₄ structure, forming Ce³⁺-Vo-Co active sites and thereby induce local compressive strain and facilitate the formation of point-defective oxygen vacancies. More importantly, Ce³⁺ acts as an electron donor, elevating the d-band center of Co and facilitating O₂ activation via enhanced electron transfer to O₂ antibonding orbitals. In contrast, the extensive interfacial contact between CeO₂ nanoparticles and Co₃O₄ triggers ion migration, which subsequently generates defects or amorphous interfacial domains with high oxygen mobility. The configuration of interfacial defects is highly dependent on the size of CeO₂ nanoparticles. Catalytic tests for the liquid-phase aerobic oxidation of benzyl alcohol confirm the superior performance of the single-atom catalyst, which exhibits 1.5 times higher activity and a 27.7 kJ/mol lower activation energy than its CeO₂ nanoparticle counterpart. Our findings demonstrate that the interaction between Ce species and Co₃O₄ is dominated by electronic effects when Ce is atomically dispersed, whereas interfacial reconstruction becomes predominant with increasing CeO₂ nanoparticles size.

Key words: Co₃O₄ catalyst, CeO₂, Catalytic oxidation, Interface reconstruction, Single atoms, Nanoparticles

曾悦, 王泓升, 轩靖, 肖萍, 冯瑶瑶, 吕帅, 朱君江. CeO₂/Co₃O₄催化剂界面相互作用的尺寸依赖性: 从单原子到纳米颗粒[J]. 催化学报, 2026, 88: 478-491.

Yue Zeng, Hongsheng Wang, Jing Xuan, Ping Xiao, Yaoyao Feng, Shuai Lyu, Junjiang Zhu. Size-dependent interfacial interactions in CeO₂/Co₃O₄ catalysts: From single atoms to nanoparticles[J]. Chinese Journal of Catalysis, 2026, 88: 478-491.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(26)65120-0

https://www.cjcatal.com/CN/Y2026/V88/I9/478

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Fig. 1. TEM characterization of Ce supported Co3O4 catalysts. Atomic-resolution STEM image of SA-Ce-Co3O4 (A) and 5.7NP-CeO2/Co3O4 (C). HAADF-STEM image and corresponding EDX elemental mappings of SA-Ce-Co3O4 (B) and 5.7NP-CeO2/Co3O4 (D).

Fig. 2. Surface chemical states and coordination information of as-prepared catalysts. (A) Ce k-edge XANES profiles for as-prepared catalysts. (B) Ce k-edge EXAFS spectra in R space for as-prepared catalysts. WT analysis of SA-Ce-Co3O4 (C), 5.7NP-CeO2/Co3O4 (D), and CeO2 (E). (F) Ce 3d XPS data of as-prepared catalysts. (G) The percentage of Ce3+ in the catalysts.

Fig. 3. Catalytic performance of as-prepared catalysts. (A) The BzOH conversion as the function time for different catalysts. (B) The BzOH conversion and BzH selectivity at 180 min for different catalyst. (C) The Arrhenius plots for calculating activation energies for SA-Ce-Co3O4, 5.7NP-CeO2/Co3O4 and Co3O4 catalyst. Reaction conditions: 80 °C, 20 μL substrates, O2: 50 mL/min, Toluene 20 mL.

Fig. 4. Microstructural analysis of the catalyst series. (A) Raman spectra of Co3O4, SA-Ce-Co3O4 and 5.7NP-CeO2/Co3O4 catalyst. Peak center (B) and FWHM (C) of A1g for different catalyst. HRTEM image of Co3O4 (D), SA-Ce-Co3O4 (E), and 5.7NP-CeO2/Co3O4 (F) catalysts. Schematic diagram of single atom Ce modified Co3O4 (G) and CeO2 nanoparticle supported on Co3O4 (H).

Fig. 5. DFT calculation. (A) Surface structure of Co3O4 (111) facet. (B) Surface structure of Ce1/Co3O4 (111) facet. (C) Oxygen vacancy formation energy on Co3O4 (111) and Ce1/Co3O4 (111) facets. (D) The density of states of Co3O4. (E) The density of states of Ce1/Co3O4. (F) Oxygen adsorption structure on the oxygen vacancy site of Ce1/Co3O4-Vo with charge density difference and Bader charge analysis. (G) Oxygen adsorption structure on the oxygen vacancy site of Co3O4-Vo with charge density difference and Bader charge analysis. (H) Oxygen dissociation pathways and corresponding energy barriers on different structures. The balls in blue, red, and yellow colors represent Co, O, and Ce atoms, respectively.

Fig. 6. Interfacial microstructure of Co3O4 with different-sized CeO2. STEM image (A) and HRTEM image (B) of 2.4NP-CeO2/Co3O4. STEM image (C) and HRTEM image (D) of 7.3NP-CeO2/Co3O4. (E) Schematic diagram of the interfacial microstructure of Co3O4 tuned by CeO2 size. (F) Raman spectra of synthesized Co3O4-Supported CeO2 Catalysts. (G) Position of the A1g peak of the catalyst as a function of CeO2 size. (H) FWHM of the A1g peak of the catalyst as a function of CeO2 size.

Fig. 7. XRD patterns (A) and Raman spectra (B) of 5.7CeO2/Co3O4 catalyst calcined at 400 °C for different time. (C) STEM and the corresponding EDX line scan image of 5.7CeO2/Co3O4. (D) Schematic illustration of the octahedral to tetrahedral structural transformation driven by electron transfer. (E) The formation mechanism schematic diagram of the amorphous region at the interface.

Fig. 8. (A) The BzOH conversion as the function time for different catalysts. (B) The BzOH conversion and BzH selectivity at 180 min for different catalysts. (C) The Arrhenius plots for calculating activation energies for different catalyst. (D) Activation energies of the catalyst as a function of CeO2 size. Ov percentage (E) and Co3+ percentage (F) in the catalyst as a function of CeO2 size. H2-TPR profiles (G) and O2-TPD profiles (H) of different catalysts. (I) Ce3+ percentage in the catalyst as a function of CeO2 size.

Fig. 9. Schematic illustrating the enhanced catalytic oxidation activity of Co3O4 promoted by single atom Ce and CeO2 nanoparticles with different size.

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CeO₂/Co₃O₄催化剂界面相互作用的尺寸依赖性: 从单原子到纳米颗粒

Size-dependent interfacial interactions in CeO₂/Co₃O₄ catalysts: From single atoms to nanoparticles

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