MOF衍生多壳层Pd@Co3O4表面氧空位调控及催化甲烷高效燃烧

doi:10.1016/S1872-2067(26)65134-0

催化学报 ›› 2026, Vol. 88: 492-505.DOI: 10.1016/S1872-2067(26)65134-0

MOF衍生多壳层Pd@Co₃O₄表面氧空位调控及催化甲烷高效燃烧

张春雷^a, 谭涵予^a, 隋超阳^a, 冯莹^a, 陈心宇^b, 范晓强^a, 于学华^a^,^*(), 赵震^a^,^b^,^*()

^a 沈阳师范大学化学化工学院, 能源与环境催化研究所, 辽宁沈阳 110034
^b 中国石油大学(北京)理学院, 重质油国家重点实验室, 北京 102249

收稿日期:2025-12-28 接受日期:2026-02-13 出版日期:2026-09-18 发布日期:2026-09-05
通讯作者: *电子信箱: yuxuehua1986@163.com (于学华),
zhenzhao@cup.edu.cn/zhaozhen1586@163.com (赵震).
基金资助:
国家自然科学基金(22572132);国家自然科学基金(22372107);国家自然科学基金(22402129);广西重大专项项目(桂科AA24206022);辽宁省杰出青年科学基金(2025-JQ-08);辽宁省教育厅高等学校基本科研项目(LJ212410166052);辽宁省教育厅高等学校基本科研项目(LJ212410166046);辽宁省兴辽英才计划青年拔尖人才项目(XLYC2203007);辽宁省兴辽英才计划青年拔尖人才项目(XLYC2203138);辽宁省国际科技合作计划项目(2024JH2/102100004);沈阳师范大学研究生教育改革重点项目(YJSJG220240064);先进催化材料教育部重点实验室及浙江师范大学固体表面反应化学浙江省重点实验室(KLMEACM202508)

Efficient methane combustion by engineering surface oxygen vacancies on MOF-derived multi-shell Pd@Co₃O₄

Chunlei Zhang^a, Hanyu Tan^a, Chaoyang Sui^a, Ying Feng^a, Xinyu Chen^b, Xiaoqiang Fan^a, Xuehua Yu^a^,^*(), Zhen Zhao^a^,^b^,^*()

^a Institute of Catalysis for Energy and Environment, College of Chemistry and Chemical Engineering, Shenyang Normal University, Shenyang 110034, Liaoning, China
^b State Key Laboratory of Heavy Oil Processing, China University of Petroleum, Beijing 102249, China

Received:2025-12-28 Accepted:2026-02-13 Online:2026-09-18 Published:2026-09-05
Supported by:
National Natural Science Foundation of China(22572132);National Natural Science Foundation of China(22372107);National Natural Science Foundation of China(22402129);The Science and Technology Major Program of Guangxi Province(桂科AA24206022);The Outstanding Youth Science Foundation of Liaoning Province(2025-JQ-08);The Fundamental Research Funds for the Liaoning Universities(LJ212410166052);The Fundamental Research Funds for the Liaoning Universities(LJ212410166046);The Liaoning Xingliao Talented Youth Top Talent Program(XLYC2203007);The Liaoning Xingliao Talented Youth Top Talent Program(XLYC2203138);The Liaoning Province International Science and Technology Cooperation Program Project(2024JH2/102100004);The Shenyang Normal University postgraduate education reform key project(YJSJG220240064);The Key Laboratory of the Ministry of Education for Advanced Catalysis Materials and Zhejiang Key Laboratory for Reactive Chemistry on Solid Surfaces, Zhejiang Normal University(KLMEACM202508)

摘要/Abstract

摘要：

甲烷作为重要高热值清洁能源, 同时也是地球大气中第二大温室气体, 已经成为导致全球气候变暖的重要因素. 因此, 在较低温度下实现甲烷的高效催化净化, 对于控制温室气体排放和环境保护具有重要意义. 然而, 由于甲烷分子具有高度对称且稳定的C-H键, 加之催化剂中晶格氧物种的迁移速率相对缓慢, 导致其低温催化转化面临巨大挑战. 尽管负载型钯(Pd)基催化剂在甲烷燃烧中表现出优异的C-H键裂解能力, 但传统方法制备的催化剂常面临活性组分易团聚烧结、金属-载体界面接触不充分以及晶格氧补给缓慢等缺点. 因此, 合理设计并构建兼具高分散Pd活性位点与丰富表面氧空位的多级结构催化体系, 对于打破反应能垒限制, 提升晶格氧迁移率及甲烷低温催化燃烧性能具有重要的科学意义和应用价值.
本文提出了一种拓扑导向的缺陷工程策略, 以沸石咪唑酯骨架结构材料(ZIF-67)为前驱体模板, 通过精准调控热解动力学(焙烧气氛和升温速率), 成功合成了一系列具有可调壳层结构(实心、单壳、三壳及四壳层)的金属有机框架(MOF)衍生多壳层Pd@Co₃O₄纳米笼催化剂, 并系统探究了不同壳层拓扑结构对催化剂电子构型、缺陷密度及甲烷催化燃烧性能的影响. 实验结果表明, 在温和焙烧条件(低氧分压和缓慢升温)下制备的四壳层1%Pd@Co₃O₄-Q催化剂表现出最优异的催化性能. 该催化剂催化50%甲烷转化率的温度(T₅₀)低至305 °C, 相较于纯Co₃O₄-Q载体显著降低了51 °C; 在260 °C时的反应速率高达4.06 mmol·g^-1·s^-1, 是纯载体的2.8倍. 此外, 得益于多壳层结构的物理限域效应, 该催化剂在长达50 h的连续活性评价中展现出优异的抗烧结能力与热稳定性. 静态表征(X-射线衍射、电子顺磁共振、O₂-程序升温脱附和X射线光电子能谱等)与原位红外光谱分析表明, 独特的多壳层拓扑结构不仅有效抑制了高温下晶粒的过度生长, 还诱导产生了高密度的表面氧空位(V₀); 同时, Pd纳米颗粒与Co₃O₄载体间形成了强烈的电子-金属载体相互作用. 结合反应动力学与密度泛函理论计算, 深入揭示了Pd-Co界面与氧空位的双重促进协同机制: 一方面, 电子从Pd向Co₃O₄转移显著削弱了界面处的Co-O键强度, 使氧空位形成能从3.02 eV大幅降至1.21 eV, 极大促进了晶格氧物种的迁移与再生; 另一方面, 高活性的Pd位点将甲烷解离路径由氧化物表面的异裂转变为金属介导的均裂, 将决速步骤(C-H键断裂)的表观活化能大幅降低至66.6 kJ·mol^-1. 二者共同加速了Mars-van Krevelen机制中的氧化还原循环.
综上, 本文不仅开发了一种用于甲烷低温高效消除的高性能多壳层Pd@Co₃O₄催化剂原型, 还深入阐明了Pd-Co界面电子态与表面缺陷协同催化甲烷深度氧化的微观反应机制. 该拓扑导向的缺陷工程策略, 为利用MOF衍生物的拓扑结构精准调控催化剂表面缺陷化学提供了全新的普适性视角, 对未来设计与开发高效绿色且经济的催化材料具有重要的理论参考意义.

关键词: 金属有机骨架衍生材料, 甲烷催化燃烧, 多壳层结构, 氧空位构建, 催化剂

Abstract:

ABSTRACT: Implementing low-temperature catalytic methane combustion is imperative for curbing the release of greenhouse gases. However, this process is fundamentally limited by the high energy barrier for C-H bond activation and the slow migration of lattice oxygen species. In this work, we introduced a topology-directed defect engineering strategy to synthesize a series of Pd@Co₃O₄ nanocages with adjustable shell numbers by precisely controlling the pyrolysis kinetics of ZIF-67. Among the synthesized catalysts, the quadruple-shell 1%Pd@Co₃O₄-Q system exhibits the best catalytic performance (T₅₀ = 305 °C), marking a 2.8-fold enhancement in reaction rate relative to the pristine Co₃O₄-Q catalyst, along with outstanding stability. Results of multidimensional characterizations (electron paramagnetic resonance, O₂-temperature programmed desorption, X-ray photoelectron spectroscopy) confirm that the unique multi-shell topology not only induces a high density of surface oxygen vacancies, but also optimizes the electronic configuration of Pd through strong electron-metal-support interactions. Kinetic analysis and in-situ diffuse reflectance Fourier transform infrared spectroscopy experiments verify that the reaction proceeds via the Mars-van Krevelen mechanism. The Pd sites significantly lower the activation barrier associated with C-H bond rupturing during the rate-determining step (with E_a decreasing to 66.6 kJ·mol^-1), and the abundant oxygen vacancies boost the transport efficiency of lattice oxygen species. Furthermore, density functional theory calculations unveil that electron donation from Pd to Co₃O₄ weakens the Co-O bond, thereby simultaneously depressing the energy required for oxygen vacancy formation and the barrier for methane dissociation. This work not only introduces an efficient catalyst for methane combustion, but also proposes a universal mechanism for regulating the chemistry of surface defects through the topological structure of MOF derivatives.

Key words: Metal-organic frameworks-derived materials, Methane catalytic combustion, Multi-shelled structure, Oxygen vacancy construction, Catalyst

张春雷, 谭涵予, 隋超阳, 冯莹, 陈心宇, 范晓强, 于学华, 赵震. MOF衍生多壳层Pd@Co₃O₄表面氧空位调控及催化甲烷高效燃烧[J]. 催化学报, 2026, 88: 492-505.

Chunlei Zhang, Hanyu Tan, Chaoyang Sui, Ying Feng, Xinyu Chen, Xiaoqiang Fan, Xuehua Yu, Zhen Zhao. Efficient methane combustion by engineering surface oxygen vacancies on MOF-derived multi-shell Pd@Co₃O₄[J]. Chinese Journal of Catalysis, 2026, 88: 492-505.

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https://www.cjcatal.com/CN/Y2026/V88/I9/492

图/表 8

Fig. 1. XRD patterns (A), N2 adsorption-desorption isotherms (B), and pore size distributions (C) of prepared catalysts. (a) Co3O4-Q; (b) 1%Pd@Co3O4-Z; (c) 1%Pd@Co3O4-S; (d) 1%Pd@Co3O4-T; (e) 1%Pd@Co3O4-Q).

Fig. 2. TEM images of as-prepared catalysts (A1-D1); SAED patterns of as-prepared catalysts (A2-D2); EDS elemental mapping images (A3-D5). (A: 1%Pd@Co3O4-Q, B: 1%Pd@Co3O4-T, C: 1%Pd@Co3O4-S, D: 1%Pd@Co3O4-Z).

Fig. 3. XPS spectra of Pd 3d (A), O 1s (B), and Co 2p (C). (D) EPR spectra of as prepared catalysts. O2-TPD (E) and H2-TPR (F) curves of as-prepared catalysts. (a) Co3O4-Q; (b) 1%Pd@Co3O4-Z; (c) 1%Pd@Co3O4-S; (d) 1%Pd@Co3O4-T; (e) 1%Pd@Co3O4-Q.

Table 1 Parameters of the fitted components on surface from Pd 3d, Co 2p and O 1s XPS spectra.

Catalyst
	Pd			Co			O
	Pd²⁺	Pd⁴⁺	Co³⁺		Co²⁺	O_sur		O_ads	O_latt
Co₃O₄-Q	—	—	49.8		50.2	6.8		25.7	67.6
1%Pd@Co₃O₄-Z	54.5	45.5	45.5		54.5	4.1		28.4	67.6
1%Pd@Co₃O₄-S	56.6	43.4	44.2		55.8	4.6		29.6	65.8
1%Pd@Co₃O₄-T	57.6	42.4	34.9		65.1	3.2		31.8	64.9
1%Pd@Co₃O₄-Q	58.8	41.2	31.7		68.3	2.6		33.3	64.1

Fig. 4. CH4-TPR curves of as-prepared catalysts. (A) Co3O4-Q; (B) 1%Pd@Co3O4-Z; (C) 1%Pd@Co3O4-S; (D) 1%Pd@Co3O4-T; (E) 1%Pd@Co3O4-Q.

Fig. 5. (A,B) The catalytic activity of the as-prepared catalysts for methane combustion. (C) Arrhenius plots for methane combustion over the as-prepared catalysts. (D) Evaluation of the catalyst stability at 335 °C. Reaction conditions: 50 mg catalyst, reactant gas mixture of 1 vol% CH4 and 20 vol% O2 balanced with Ar, SV = 20000 mL·g-1·h-1.

Table 2 Catalytic activities and Ea of the catalysts for methane combustion at SV = 20000 mL·g-1·h-1.

Catalyst	Methane combustion			Methane combustion at 260 °C		E_a (kJ·mol^-1)
Catalyst	T₁₀ (°C)	T₅₀ (°C)	T₉₀ (°C)	Conversion (%)	Reaction rate (mmol·g^-1·s^-1)	E_a (kJ·mol^-1)
Co₃O₄-Q	277	356	434	5.90	1.47	85.40
1%Pd@Co₃O₄-Z	262	324	377	8.98	2.23	77.93
1%Pd@Co₃O₄-S	260	322	375	9.96	2.48	74.07
1%Pd@Co₃O₄-T	254	317	371	11.63	2.89	71.15
1%Pd@Co₃O₄-Q	243	305	356	16.34	4.06	66.58

Fig. 6. In-situ DRIFT spectra of methane combustion carried out over Co3O4-Q (A) and 1%Pd@Co3O4-Q (B) catalyst. Differential charge density map of the Pd13/Co3O4 (311) interface. The green and blue isosurfaces represent electron accumulation and depletion respectively. (C) The calculated Bader charge indicates that approximately 0.1627 e- of electrons are transferred from the Pd cluster to the Co3O4 support. PDOS of Co 3d orbitals on the surfaces of pure Co3O4 and Pd/Co3O4 catalysts. (D) The vertical dashed line represents the calculated position of the d-band center, the Fermi level is set to 0 eV. (E) Comparison of oxygen vacancy formation energies of Co3O4 and Pd/Co3O4 catalysts. (F) Comparison of C-H bond dissociation energies of Co3O4 and Pd/Co3O4 catalysts. (G) Comparison of free energies for surface intermediate conversion of Co3O4 and Pd/Co3O4 catalysts.

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MOF衍生多壳层Pd@Co₃O₄表面氧空位调控及催化甲烷高效燃烧

Efficient methane combustion by engineering surface oxygen vacancies on MOF-derived multi-shell Pd@Co₃O₄

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