反应条件下Ni/Mo2CTx MXene催化剂结构演变调节CO2还原性能

doi:10.1016/S1872-2067(25)64681-X

催化学报 ›› 2025, Vol. 72: 243-253.DOI: 10.1016/S1872-2067(25)64681-X

反应条件下Ni/Mo₂CT_x MXene催化剂结构演变调节CO₂还原性能

马军^a^,^b, 徐冰^b, 曹硕^b^,^c, 李世艳^b^,^d, 储伟^a^,^*(), Siglinda Perathoner^e, Gabriele Centi^e, 刘岳峰^b^,^*()

^a四川大学化工学院, 四川成都 610065, 中国
^b中国科学院大连化学物理研究所, 辽宁大连 116023, 中国
^c中国石化石油化工研究院有限公司, 北京 100083, 中国
^d中国科学院大学, 北京 100049, 中国
^e墨西拿大学ChiBioFarAm系, 墨西拿, 意大利

收稿日期:2024-12-14 接受日期:2025-03-21 出版日期:2025-05-18 发布日期:2025-05-20
通讯作者: *电子信箱: yuefeng.liu@dicp.ac.cn (刘岳峰),chuwei1965@scu.edu.cn (储伟).
基金资助:
国家自然科学基金(21972140);国家自然科学基金(22172161);国家自然科学基金(22472168);大连市科技创新基金(2024JJ12RC034);大连化学物理研究所创新基金(DICP I202421);榆林市清洁能源创新研究院能源革命科技计划(E411020705);中国科学院国际人才计划(PIFI)

Structural dynamics of Ni/Mo₂CT_x MXene catalysts under reaction modulate CO₂ reduction performance

Jun Ma^a^,^b, Bing Xu^b, Shuo Cao^b^,^c, Shiyan Li^b^,^d, Wei Chu^a^,^*(), Siglinda Perathoner^e, Gabriele Centi^e, Yuefeng Liu^b^,^*()

^aCollege of Chemical Engineering, Sichuan University, Chengdu 610065, Sichuan, China
^bDalian National Laboratory for Clean Energy, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, Liaoning, China
^cSINOPEC Research Institute of Petroleum Processing Co., Ltd., Beijing 100083, China
^dUniversity of Chinese Academy of Sciences, Beijing 100049, China
^eDepartment ChiBioFarAm, University of Messina, 98166 Messina, Italy

Received:2024-12-14 Accepted:2025-03-21 Online:2025-05-18 Published:2025-05-20
Contact: *E-mail: yuefeng.liu@dicp.ac.cn (Y. Liu), chuwei1965@scu.edu.cn (W. Chu).
Supported by:
National Natural Science Foundation of China(21972140);National Natural Science Foundation of China(22172161);National Natural Science Foundation of China(22472168);Dalian Science and Technology Innovation Fund(2024JJ12RC034);Dalian Institute of Chemical Physics(DICP I202421);Energy Revolution S&T Program of Yulin Innovation Institute of Clean Energy(E411020705);CAS President's International Fellowship Initiative (PIFI) Program

摘要/Abstract

摘要：

过渡金属碳化物MXene作为典型的二维材料, 具有丰富的表面端基和独特的物理化学性质被视为一种新型的催化载体材料. 然而, 催化反应中所表现的金属-载体相互作用及结构演变机制尚未明晰. 众所周知, 传统负载型催化剂中金属纳米颗粒在高温和反应气氛下往往会经历烧结、熟化及再分散等多种结构变化, 这些结构变化则直接决定了催化剂的活性和选择性. 因此, 研究催化剂在实际反应条件下的结构演变, 不仅能深入理解金属与载体之间的相互作用方式, 也可为调控催化性能提供重要理论依据. 基于此, 本工作以Mo₂CT_x MXene材料负载Ni纳米粒子为研究对象, 深入探究了Ni/Mo₂CT_x催化剂在CO₂加氢过程中的结构演变, 解析MXene载体的表面结构变化以及与金属颗粒的相互作用, 进而关联催化性能并理解其构-效关系.

本文首先通过HCl刻蚀Mo₂Ga₂C的方法制备了Mo₂CT_x, 然后采用浸渍法合成了用于CO₂加氢反应的Ni/Mo₂CT_x负载型催化剂. 在CO₂加氢过程中, 该催化剂的CO选择性随温度升高呈先降后升的趋势. 然而, 在第二轮升温测试中, CO选择性始终保持在93%以上, 而CO₂转化速率几乎不变. 这表明Ni/Mo₂CT_x催化剂在使用过程中发生了结构转变, 导致CH₄生成速率下降. 电子显微镜和X射线表征研究揭示了催化剂的结构演变. 高分辨透射电子显微镜结果表明, 经过500 °C反应2 h后, Ni的平均粒径从12.9减至3.1 nm. X射线光电子能谱分析结果表明, 使用后表面未连接端基的Mo原子比例从1.8%增加至7.1%, Ni的结合能向高结合能方向偏移0.2 eV, 表明部分Mo₂CT_x端基被移除, Ni向Mo₂CT₂转移了更多电荷. X射线衍射结果也表明, Mo₂CT_x端基被部分移除而非完全去除. 拉曼光谱分析进一步证实形成了Ni-Mo物种. 原位漫反射红外光谱实验揭示了选择性转变的反应机理. 结果表明, CO₂通过甲酸盐和碳化物路径生成CO和CH₄, 其中甲烷主要依赖于甲酸盐路径. Ni纳米颗粒的分散降低了甲酸盐中间体的生成速率, 抑制了甲酸盐路径, 增强了碳化物路径. 因此, CH₄生成速率下降, 而CO生成速率提高.

本研究通过揭示Ni/Mo₂CT_x催化剂在CO₂加氢反应中的结构演变与金属-载体相互作用形式, 对其影响反应选择性提供了重要见解, 为利用Mo₂CT_x或其他MXene材料作为催化剂载体的设计与优化提供了新的研究思路.

关键词: Mo₂CT_x MXene, 二氧化碳加氢, 金属-载体相互作用, 催化选择性, 结构演变

Abstract:

The catalyst's structural dynamics under reaction conditions critically determine their performance. We proved this indication by studying Ni nanoparticles supported on Mo₂CT_x MXene, where the average size during CO₂ hydrogenation changed from 12.9 to 3.1 nm. A parallel increase of CO selectivity from 21.1% to 92.6% at 400 °C was observed, while the CO₂ conversion rate remained at about 84.0 mmol·g_cat^-1·h^-1. This transformation involved partial removal of Mo₂CT_x terminal groups, allowing direct interaction between Ni and Mo atoms instead of indirect coupling through -O terminations. The shift from a Ni-O-Mo to a Ni-Mo interaction enhanced electron transfer from Ni to Mo₂CT_x, strengthening the metal-support interaction and driving Ni nanoparticle dispersion. In-situ mechanistic analysis and kinetic isotope studies revealed that Ni dispersion suppresses the formate and carboxyl pathway, promotes direct CO₂ dissociation, and inhibits CO hydrogenation, shifting the primary product from CH₄ to CO. These findings provide a strategy for designing highly selective and stable MXene-based catalysts through engineered metal-support interactions.

Key words: Mo₂CT_x MXene, CO₂ hydrogenation, Metal-support interactions, Catalytic selectivity, Structure evolution

马军, 徐冰, 曹硕, 李世艳, 储伟, Siglinda Perathoner, Gabriele Centi, 刘岳峰. 反应条件下Ni/Mo₂CT_x MXene催化剂结构演变调节CO₂还原性能[J]. 催化学报, 2025, 72: 243-253.

Jun Ma, Bing Xu, Shuo Cao, Shiyan Li, Wei Chu, Siglinda Perathoner, Gabriele Centi, Yuefeng Liu. Structural dynamics of Ni/Mo₂CT_x MXene catalysts under reaction modulate CO₂ reduction performance[J]. Chinese Journal of Catalysis, 2025, 72: 243-253.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(25)64681-X

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图/表 7

Fig. 1. (a) Schematic showing the synthesis of 2D Mo2CTx MXene and Ni/Mo2CTx catalyst. XRD patterns (b), XPS survey spectra (c) and Raman spectra (d) of Mo2Ga2C, Mo2CTx and Ni/Mo2CTx.

Fig. 2. (a) CO2 conversion and CO selectivity as a function of reaction temperature in three cycles. (b) CO2 conversion rate and product selectivity of Ni/Mo2CTx after reduction and after treatment on CO2 hydrogenation conditions at different temperatures for 2 h. (c) CO2 reaction rate and selectivity of Ni/Mo2CTx-R at 500 °C. (d) Stability test of Ni/Mo2CTx-T500 at 500 °C. Reaction conditions: mcat. = 50.0 mg, WHSV = 60000 mL·gcat-1·h-1, H2/CO2 = 4.

Fig. 3. BF-STEM image (a) and EELS image and corresponding EELS mapping (b) of Ni/Mo2CTx-R, EELS spectra in area (i) (c) and (ii) (d). (e) TEM image of Ni/Mo2CTx-R. (f) HR-TEM images of Ni/Mo2CTx with [001] and [100] axis view. (j) HR-TEM image of Ni/Mo2CTx-T500. HR-TEM images of Ni/Mo2CTx-T500 with [001] (k) and [100] (m) axis view. (g, i, l, n) is a schematic structural corresponding to the HR-TEM image on the left.

Fig. 4. (a) XRD patterns of Ni/Mo2CTx-R, Ni/Mo2CTx-T400, Ni/Mo2CTx-T500 and Mo2CTx-R500. (b) Raman spectra of Ni/Mo2CTx-R, Ni/Mo2CTx-T400 and Ni/Mo2CTx-T500.

Fig. 5. Mo 3d (a) andNi 2p3/2 (b) XPS spectra of Ni/Mo2CTx-R, Ni/Mo2CTx-T400 and Ni/Mo2CTx-T500 catalysts. (c) Mo-C/Mo and Ni0/Ni contents of samples calculated from XPS spectra.

Fig. 6. (a) Temperature-programmed CO2 + H2-DRIFTS ramping from 50 to 400 °C over Ni/Mo2CTx-R (a) and Ni/Mo2CTx-T500 (b). Relative intensity of carboxyl (c) and formate (d) intermediates in in-situ DRFIT spectra. (e) Scheme of Carboxyl (i), Formate (ii) and Bidentate carbonate (iii) intermediates.

Fig. 7. Kinetic D2 isotope effects experiments of CO2 hydrogenation (a) and CO hydrogenation (b). Reaction conditions: T = 220 °C, 50 mg catalyst, WHSV = 60000 mL·gcat.-1·h?1. (c) Schematic representation of the origin of the inverse kinetic isotope effect and thermodynamic isotope effect in the CO2 hydrogenation reaction. (d) The scheme of the catalytic pathway for the CO2 hydrogenation over Ni/Mo2CTx-R and Ni/Mo2CTx-T500.

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反应条件下Ni/Mo₂CT_x MXene催化剂结构演变调节CO₂还原性能

Structural dynamics of Ni/Mo₂CT_x MXene catalysts under reaction modulate CO₂ reduction performance

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