构建Cu台阶位促进电催化CO2还原制醇类化学品的研究

doi:10.1016/S1872-2067(23)64508-5

催化学报 ›› 2023, Vol. 52: 187-195.DOI: 10.1016/S1872-2067(23)64508-5

构建Cu台阶位促进电催化CO₂还原制醇类化学品的研究

高晖^a^,^b^,¹, 张恭^a^,^b^,¹, 程东方^a^,^b, 王永涛^a^,^b, 赵静^a^,^b, 李晓芝^a^,^b, 杜晓伟^a^,^b, 赵志坚^a^,^b^,^d^,^e, 王拓^a^,^b^,^c^,^d, 张鹏^a^,^b^,^d^,^e^,^*(), 巩金龙^a^,^b^,^c^,^d

^a天津大学化工学院, 绿色合成与转化教育部重点实验室, 天津300072
^b天津化学化工协同创新中心, 天津300072
^c物质绿色创造与制造海河实验室, 天津300192
^d天津大学国家储能技术产教融合创新平台, 天津300350
^e天津大学-新加坡国立大学福州联合学院, 天津大学国际校区, 福建福州350207

收稿日期:2023-05-27 接受日期:2023-08-16 出版日期:2023-09-18 发布日期:2023-09-25
通讯作者: *电子信箱: p_zhang@tju.edu.cn (张鹏).
作者简介:¹共同第一作者.
基金资助:
国家重点研发计划(2021YFA1501503);国家自然科学基金(22121004);国家自然科学基金(22108197);物质绿色创造与制造海河实验室(CYZC202107);天津市自然科学基金(21JCZXJC00060);高等学校学科创新引智计划(BP0618007);2022年度“天河”青索开放研究基金;科学探索奖

Steering electrochemical carbon dioxide reduction to alcohol production on Cu step sites

Hui Gao^a^,^b^,¹, Gong Zhang^a^,^b^,¹, Dongfang Cheng^a^,^b, Yongtao Wang^a^,^b, Jing Zhao^a^,^b, Xiaozhi Li^a^,^b, Xiaowei Du^a^,^b, Zhi-Jian Zhao^a^,^b^,^d^,^e, Tuo Wang^a^,^b^,^c^,^d, Peng Zhang^a^,^b^,^d^,^e^,^*(), Jinlong Gong^a^,^b^,^c^,^d

^aKey Laboratory for Green Chemical Technology of Ministry of Education, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China
^bCollaborative Innovation Center of Chemical Science and Engineering (Tianjin), Tianjin 300072, China
^cHaihe Laboratory of Sustainable Chemical Transformations, Tianjin 300192, China
^dNational Industry-Education Platform of Energy Storage, Tianjin University, Tianjin 300350, China
^eJoint School of National University of Singapore and Tianjin University, International Campus of Tianjin University, Binhai New City, Fuzhou 350207, Fujian, China

Received:2023-05-27 Accepted:2023-08-16 Online:2023-09-18 Published:2023-09-25
Contact: *E-mail: p_zhang@tju.edu.cn (P. Zhang).
About author:¹Contributed equally to this work.
Supported by:
National Key R&D Program of China(2021YFA1501503);National Natural Science Foundation of China(22121004);National Natural Science Foundation of China(22108197);Haihe Laboratory of Sustainable Chemical Transformations(CYZC202107);Natural Science Foundation of Tianjin City(21JCZXJC00060);Introducing Talents of Discipline to Universities(BP0618007);TianHe Qingsuo Open Research Fund of TSYS in 2022 & NSCC-TJ;Xplorer Prize

摘要/Abstract

摘要：

电催化CO₂制备高附加值的化学品是解决当前碳排放问题的可行技术路线之一. 其中, 合成醇类化合物因具有广泛用途和高价值而备受关注. 在电催化CO₂还原合成多碳醇反应中, 关键中间体*CH₂CHO容易发生热力学有利的脱氧反应而生成C₂H₄, 降低了醇类产物的选择性. 由于电催化CO₂还原是一个表面结构敏感的反应, 因此可以通过设计Cu基催化剂的特定表面结构, 实现对反应路径的有效调节, 从而提升醇类产物的选择性. 本课题组前期通过密度泛函理论(DFT)计算和主成分分析法等对Cu基催化剂的构效关系进行解析, 说明配位不饱和的台阶位点有望高效地促进醇类产物的生成. 本文进一步从实验角度, 证明了配位不饱和的台阶位点是生成醇类产物的活性位点.

本文采用CO分子作为还原剂制备了CuO衍生的金属Cu催化剂(COD-Cu), 利用CO分子对Cu表面的重构作用, 获得了具有丰富台阶位点的Cu催化剂. 而通过H₂还原制备的金属Cu催化剂(HOD-Cu)对照样表面则多为平面位点. X射线衍射和原位拉曼光谱结果表明, CuO前驱体经过CO或H₂还原后被完全还原为金属态, 并且在电化学还原条件下依旧呈现金属态, 排除了催化剂价态对反应的影响. 扫描电镜结果表明, 两种催化剂的形貌没有明显区别, 排除了催化剂形貌对反应的影响. 高分辨透射电镜结果表明, COD-Cu表面因为CO的重构作用, 产生相较于HOD-Cu更多的台阶位点, 这与CO原位红外光谱结果一致(COD-Cu催化剂在2080 cm^-1波数处具有明显的台阶位点CO吸附峰). 电化学CO₂还原活性测试结果表明, COD-Cu表现出更高的醇类产物选择性, 相较于HOD-Cu, 法拉第效率与部分电流密度均提升了5倍以上, 醇类产物的法拉第效率达到40.5%, 部分电流密度达到56.3 mA cm⁻², 产物中醇/烯烃比值为2.2. 这表明台阶位点对调控反应路径促进醇类生成具有重要作用. 结合原位衰减全反射表面增强傅里叶变换红外吸收光谱的阶跃电位和Ar气吹扫实验结果表明, COD-Cu因具有更多的台阶位点而表现出更高的催化CO₂到*CO反应活性, 并有效促进后续的C-C偶联反应. 通过热退火实验制备了具有不同台阶位点含量的COD-Cu催化剂, 其台阶位点的含量与醇类产物的选择性保持良好的线性关系, 进一步验证了台阶位点是促进醇类产物生成活性位点的结论. DFT结果也表明, 台阶位点可以有效的提升关键中间体*CH₂CHO中C-O键强度, 从而抑制C-O键断裂, 促进醇类产物的生成.

综上, 本文提出了一种通过催化剂活性位点设计调控电催化CO₂还原反应路径的有效策略, 为解析催化剂构效关系、明确活性位点提供参考. 得益于催化科学的快速发展，具有高活性的CO₂还原电催化剂不断涌现，未来可在发展活性位点精细化调控方法、开发新型原位瞬态表征技术、创新催化剂失活机制原位研究方法等方面做出更多的努力.

关键词: 电催化, CO₂还原, 铜, 台阶位点, 醇

Abstract:

Electrochemical CO₂ reduction is a sustainable method for producing multicarbon alcohols. However, the selectivity of alcohols is limited owing to the favorable side reaction to convert the key intermediate of *CH₂CHO into ethylene. This study describes the design of a Cu electrocatalyst with abundant step sites to suppress the deoxygenation of *CH₂CHO to ethylene, thereby promoting alcohol production. A Faradic efficiency of 40.5% and partial current density of 56.3 mA/cm² for alcohols are achieved. Moreover, the alcohols/C₂H₄ ratio in the products reaches approximately 2.2. In-situ infrared spectrum characterizations and theoretical calculations reveal that the step sites facilitate C-C coupling and direct the reaction pathway to promote the formation of alcohols by inhibiting the cleavage of the C-O bond in *CH₂CHO. Therefore, the proposed strategy is efficient for designing active sites to steer reaction pathways in CO₂ electroreductions and produce alcohols.

Key words: Electrocatalysis, CO₂ reduction, Copper, Step sites, Alcohol

高晖, 张恭, 程东方, 王永涛, 赵静, 李晓芝, 杜晓伟, 赵志坚, 王拓, 张鹏, 巩金龙. 构建Cu台阶位促进电催化CO₂还原制醇类化学品的研究[J]. 催化学报, 2023, 52: 187-195.

Hui Gao, Gong Zhang, Dongfang Cheng, Yongtao Wang, Jing Zhao, Xiaozhi Li, Xiaowei Du, Zhi-Jian Zhao, Tuo Wang, Peng Zhang, Jinlong Gong. Steering electrochemical carbon dioxide reduction to alcohol production on Cu step sites[J]. Chinese Journal of Catalysis, 2023, 52: 187-195.

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链接本文: https://www.cjcatal.com/CN/10.1016/S1872-2067(23)64508-5

https://www.cjcatal.com/CN/Y2023/V52/I9/187

图/表 4

Fig. 1. Characterization of COD-Cu and HOD-Cu. (a) XRD patterns of CuO, COD-Cu, and HOD-Cu. (b) In-situ Raman spectra of COD-Cu under different potentials. SEM images of HOD-Cu (c) and COD-Cu (d). TEM images of HOD-Cu (e) and COD-Cu (f). (g) ATR-SEFTIRS characterization of COD-Cu under different potentials with peak fitting results.

Fig. 2. Electrochemical CO2RR performance of COD-Cu. (a) Products distributions between -1.4 and -0.8 V in 1.0 mol/L KOH. (b) Faradic efficiency of EtOH and n-PrOH. (c) Partial current density of EtOH and n-PrOH. (d) Alcohols/C2H4 ratio of COD-Cu in the potential range between -1.4 and -0.8 V. (e) Stability test in 1.0 mol/L KOH at -1.1 V. (Color should be used in print).

Fig. 3. In-situ ATR-SEFTIRAS spectroscopic investigations. In-situ ATR-SEFTIRAS spectra of COD-Cu (a) and HOD-Cu (b) under different potentials. (c) Correlation between wavenumbers of *COL with respect to the applied potential for COD-Cu and HOD-Cu. In-situ ATR-SEFTIRAS spectra of COD-Cu (d) and HOD-Cu (e) in Ar gas purge experiment. (f) Relative area of the peak corresponding to *COL as a function of purge duration for COD-Cu and HOD-Cu.

Fig. 4. Correlation between alcohol selectivity and ratio of step sites. (a) Peak fitting results of *COL at -0.4 V for COD-Cu after annealing treatments at different temperatures. (b) Linear relationship between Faradic efficiency of alcohols and step sites ratio. (c) Energy profile to form C2H4 (black line) and EtOH (red line) on Cu (100) without step sites and on Cu (211) with step sites.

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构建Cu台阶位促进电催化CO₂还原制醇类化学品的研究

Steering electrochemical carbon dioxide reduction to alcohol production on Cu step sites

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