硼掺杂调控界面水取向强化CO2电还原制甲烷

doi:10.1016/S1872-2067(26)65192-3

催化学报 ›› 2026, Vol. 90: 130-144.DOI: 10.1016/S1872-2067(26)65192-3

硼掺杂调控界面水取向强化CO₂电还原制甲烷

沈悦^a, 陈冰^a, 杨洁莲^a, 吴琪^a, 廖月梅^a, 周立亚^a^,^*(), 吕乃欣^b, 郭谨^a, 许雪棠^a^,^*(), 关安翔^a^,^*(), 赵再望^c^,^*()

^a 广西大学化学化工学院, 特色金属材料与组合结构全寿命周期安全国家重点实验室, 广西电化学能源材料重点实验室, 广西高校应用化学技术与资源开发重点实验室, 广西南宁 530004, 中国
^b 卡内基梅隆大学化学工程系, 宾夕法尼亚匹兹堡, 美国
^c 内蒙古大学化学化工学院, 能源材料化学研究院, 内蒙古呼和浩特 010070, 中国

收稿日期:2026-04-21 接受日期:2026-06-15 出版日期:2026-11-18 发布日期:2026-09-09
通讯作者: *电子信箱: zhouliyatf@163.com (周立亚),
xxtang@gxu.edu.cn (许雪棠),
Axguan24@gxu.edu.cn (关安翔),
zwzhao@imu.edu.cn (赵再望).
基金资助:
国家自然科学基金(22465006);广西自然科学基金(2026GXNSFAA00640424);广西科技重大专项(AA24263003);广西青年人才普惠性支持政策研究启动基金(ZX02080030425009)

Boron-incorporation-mediated interfacial water orientation for boosting CO₂ electroreduction to CH₄

Yue Shen^a, Bing Chen^a, Jielian Yang^a, Qi Wu^a, Yuemei Liao^a, Liya Zhou^a^,^*(), Naixin Lyu^b, Jin Guo^a, Xuetang Xu^a^,^*(), Anxiang Guan^a^,^*(), Zaiwang Zhao^c^,^*()

^a School of Chemistry and Chemical Engineering, State Key Laboratory of Featured Metal Materials and Life-cycle Safety for Composite Structures, Guangxi Key Laboratory of Electrochemical Energy Materials, Guangxi Colleges and Universities Key Laboratory of Applied Chemistry Technology and Resource Development. Guangxi University, Nanning 530004, Guangxi, China
^b Department of Chemical Engineering, Carnegie Mellon University, Pittsburgh 15213, Pennsylvania, United States
^c College of Energy Materials and Chemistry, College of Chemistry and Chemical Engineering, Inner Mongolia University, Hohhot 010070, Inner Mongolia, China

Received:2026-04-21 Accepted:2026-06-15 Online:2026-11-18 Published:2026-09-09
Contact: *E-mail:zhouliyatf@163.com(L. Zhou),xxtang@gxu.edu.cn(X. Xu),Axguan24@gxu.edu.cn(A. Guan),zwzhao@imu.edu.cn(Z. Zhao).
Supported by:
National Natural Science Foundation of China(22465006);Natural Science Foundation of Guangxi Province(2026GXNSFAA00640424);Guangxi Science and Technology Major Program(Guike)(AA24263003);Guangxi Youth Talent Inclusive Support Policy Research Launch Fund(ZX02080030425009)

摘要/Abstract

摘要：

甲烷(CH₄)作为重要的高价值能源载体, 在能源存储与碳资源循环利用领域具有广阔的应用前景. 电化学二氧化碳还原(CO₂RR)可利用可再生电能将CO₂资源化转化为CH₄, 是缓解温室效应、实现碳中和目标的有效途径. 然而, CO₂电还原制CH₄涉及复杂的八质子耦合电子转移过程, 反应动力学缓慢. 其中, 界面水分子的排布方式直接决定质子供给速率与中间体稳定程度, 精准调控界面水取向、优化质子传输与中间体吸附行为, 是实现高效、高选择性CO₂甲烷化反应的核心难题. 铜基催化剂是CO₂RR制CH₄的优良催化体系, 但纯铜基材料存在界面水环境无序、副反应严重、选择性与电流密度不足等问题. 因此, 通过界面微环境调控策略构建高效铜基催化剂, 实现界面水结构优化与反应性能协同提升, 是本文的主要研究思路.

本文提出硼掺杂改性策略, 精准构筑硼、铜共掺杂二氧化铈复合催化剂, 利用杂原子硼掺杂调控催化剂界面水微环境, 实现界面水分子由氧端朝下构型向氢端朝下构型的定向重构, 以此优化质子供给并强化关键中间体稳定吸附, 突破传统铜基催化剂CO₂甲烷化性能受限的瓶颈. 本文通过电化学测试系统探究了催化剂的CO₂RR催化性能, 结果表明, 优化后的1.25BC-Cu催化剂在-1.7 V vs. RHE电位下, CH₄法拉第效率最高可达74.9%, CH₄分电流密度高达−582.4 mA·cm^-2, 催化性能显著优于多数已报道CO₂制甲烷电催化剂. 同时该催化剂具备优异的电化学稳定性, 连续电解30 h后电流密度无明显衰减, CH₄选择性可稳定保持. 依托原位衰减全反射红外光谱、原位拉曼光谱等原位表征技术证实, 氢端朝下的有序界面水结构可显著加速水解离过程, 高效生成活性*H物种, 持续促进CO₂RR关键中间体的加氢转化. 结合从头算分子动力学与密度泛函理论计算进一步阐明内在机理: 硼、铜共掺杂可有效调控二氧化铈电子结构, 实现d带中心上移, 增强催化剂对反应中间体的吸附亲和力, 显著降低CH₄生成决速步的自由能垒; 有序的氢端朝下水分子排布可优化质子转移动力学, 有效抑制析氢等竞争性副反应, 从根本上提升CO₂甲烷化的反应效率与选择性.

综上, 本文通过杂原子掺杂实现界面水分子取向精准调控, 阐明了界面水微环境与催化性能的构效关系, 建立了CO₂RR选择性调控的新思路与设计依据, 为高效CO₂甲烷化电催化剂的理性设计与可控制备提供了新的技术思路与理论支撑.

关键词: 水分子取向, 氧端朝下, 氢端朝下, 二氧化碳电还原, 硼掺杂

Abstract:

Precisely regulating interfacial water orientation to optimize proton supply and intermediate stabilization remains a critical challenge for efficient and selective electrochemical CO₂ reduction to CH₄, a high-value energy carrier with complex eight-proton-coupled electron transfer kinetics. Herein, we address this challenge by developing a boron (B) incorporation strategy to engineer the interfacial water microenvironment of Cu-doped CeO₂ catalysts, where heteroatom B doping reorients interfacial water from an O-down to H-down configuration. The optimized 1.25BC-Cu catalyst achieves a maximum Faradaic efficiency (FE) of 74.9% for CH₄ at −1.7 V vs. reversible hydrogen electrode (RHE), accompanied by a high partial current density of −582.4 mA cm^-2, outperforming most previous CO₂-to-CH₄ catalysts. This catalyst also exhibits exceptional long-term stability, with negligible current decay and well-retained CH₄ FE after 30 h of continuous electrolysis. Systematic experimental characterizations, including in-situ attenuated total reflection infrared spectroscopy, in-situ Raman spectroscopy, and electrochemical measurements, confirm that the H-down water alignment accelerates water dissociation for efficient *H generation and facilitates key CO₂RR intermediates hydrogenation. Ab initio molecular dynamics and density functional theory calculations further reveal that B and Cu co-doping modulates the electronic structure of CeO₂, upshifting the d-band center to enhance intermediate adsorption affinity, and reduces the free energy barrier of the rate-determining step for CH₄ formation. The B incorporation drives ordered H-down water arrangement, optimizing proton transfer kinetics and suppressing competitive side reactions. Our findings establish heteroatom-mediated interfacial water orientation as a pivotal design principle for tailoring CO₂RR selectivity, providing a new avenue for the rational synthesis of high-performance electrocatalysts for efficient CO₂ methanation and energy storage.

Key words: Water orientation, O-down, H-down, CO₂ electroreduction, B doping

沈悦, 陈冰, 杨洁莲, 吴琪, 廖月梅, 周立亚, 吕乃欣, 郭谨, 许雪棠, 关安翔, 赵再望. 硼掺杂调控界面水取向强化CO₂电还原制甲烷[J]. 催化学报, 2026, 90: 130-144.

Yue Shen, Bing Chen, Jielian Yang, Qi Wu, Yuemei Liao, Liya Zhou, Naixin Lyu, Jin Guo, Xuetang Xu, Anxiang Guan, Zaiwang Zhao. Boron-incorporation-mediated interfacial water orientation for boosting CO₂ electroreduction to CH₄[J]. Chinese Journal of Catalysis, 2026, 90: 130-144.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(26)65192-3

https://www.cjcatal.com/CN/Y2026/V90/I11/130

图/表 6

Fig. 1. SEM images of CeO2 (a) and 1.25BC-Cu (b). (c-e) HRTEM images of CeO2 with magnified lattice fringes. HRTEM images (f,g), inverse fast Fourier transform (IFFT) images (h), and HRTEM images (i,j) of 1.25BC-Cu sample, where white circles mark the vacancy defects. Atomic-resolution aberration-corrected HAADF-STEM image (k) and the corresponding 3D intensity surface plot (l) derived from the white dashed boxed region in (k). (m) EDS elemental mapping of 1.25BC-Cu sample. (n) XRD patterns for different Cu doped CeO2 samples. (o) Calculated profile based on Rietveld refinement for 1.25BC-Cu sample. (p) Raman spectra of the CeO2, 1.25B-CeO2, and 1.25BC-Cu samples.

Fig. 2. (a) Ce 3d XPS spectra of different samples. (b) B 1s XPS spectra of different samples. (c) Cu 2p XPS spectra of different samples. (d) O 1s XPS spectra of different samples. (e) EPR spectra of CeO2-Cu and xBC-Cu (x = 0.75, 1.25, 1.75, and 2.25) samples. (g) CO2-TPD curves of the CeO2, 1.25B-CeO2 and 1.25BC-Cu catalysts. (h) CO-TPD curves of the CeO2, 1.25B-CeO2 and 1.25BC-Cu catalysts. (i) NH3-TPD curves of the CeO2, 1.25B-CeO2 and 1.25BC-Cu catalysts.

Fig. 3. (a) Cu K-edge XANES spectra of Cu foil, Cu2O, 1.25BC-Cu, and CuO. (b) Average oxidation state of Cu in the 1.25BC-Cu sample. (c) FT-EXAFS of 1.25BC-Cu with reference to Cu foil, Cu2O, and CuO. (d) EXAFS fitting curve for 1.25BC-Cu at the Cu K edge. Wavelet transform images of EXAFS data at Cu K-edge with the optimized Morlet parameter for 1.25BC-Cu (e) and CuO (f). (g) UPS spectra of CeO2-Cu and 1.25BC-Cu samples. KPFM potential maps of CeO2-Cu (h) and 1.25BC-Cu (j). KPFM potential line profiles of CeO2-Cu (j) and 1.25BC-Cu (k).

Fig. 4. (a) LSV curves for 1.25BC-Cu catalyst measured in flow-cell with CO2- or Ar-purged 1.0 mol/L KOH as electrolyte (From 0 to −2.1 V vs. RHE). CO2 electroreduction performances of 1.25B-CeO2 (b), 1.25BC-Cu (c), and CeO2-Cu (d) samples measured in flow-cell from −1.3 to −2.1 V vs. RHE. (e) Faradaic efficiencies of CH4 for different samples measured in flow-cell at −1.7 V vs. RHE. (f) Nyquist plots over the frequency ranging from 105 to 10-2 Hz for different catalysts. (g) Tafel slopes for different catalysts. (h) Capacitive currents with different sweep rates of different catalysts. (i) Performance of 1.25BC-Cu catalyst compared with those of CO2-to-CH4 electrocatalysts. (j) Stability test of 1.25BC-Cu catalysts measured in flow-cell at −1.7 V vs. RHE.

Fig. 5. (a,b) In-situ ATR-SEIRAS spectra collected at different applied potentials over 1.25BC-Cu. (c,d) In-situ ATR-SEIRAS spectra acquired at variable applied potentials for CeO2-Cu. (e,f) Potential-dependent in situ Raman profiles of the CeO2-Cu catalyst. (g,h) Potential-dependent in-situ Raman patterns of the 1.25BC-Cu catalyst. Representative structural snapshots of interfacial water molecules and the corresponding averaged hydrogen-bond number distributions along the surface for CeO2-Cu (i) and BC-Cu (j). (k) Water concentration profiles along the direction normal to the surface over CeO2-Cu and BC-Cu. (l) Averaged hydrogen-bond counts and the corresponding numbers of water molecules for the CeO2-Cu and BC-Cu models. (m) Adsorption configurations of first-layer water molecules on CeO2-Cu and BC-Cu surfaces. (n) Distribution characteristics of water dipole orientations along the surface normal direction.

Fig. 6. (a) Charge density distribution diagram of B and Cu co-doped CeO2 (Denoted as BC-Cu). (b) Plot of electron localization function of the B and Cu co-doped CeO2. The calculated density of states for *CHO adsorbed on CeO2-Cu (c) and BC-Cu (d). (e) Adsorption energy of CO2 on CeO2, CeO2-Cu and BC-Cu. (f) H2O dissociation for CeO2, CeO2-Cu and BC-Cu. (g) HER on CeO2, CeO2-Cu and BC-Cu. (h) Reaction paths and free energy diagrams of CO2 reduction to CH4 on CeO2, CeO2-Cu and BC-Cu. (i) Differential charge density distributions of *CHO adsorbed BC-Cu. COHP analysis of CeO2 (j), BC-Cu (k) and CeO2-Cu (l).

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硼掺杂调控界面水取向强化CO₂电还原制甲烷

Boron-incorporation-mediated interfacial water orientation for boosting CO₂ electroreduction to CH₄

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