Abstract
Utilizing CO2 as a carbon feedstock for producing fuels and useful chemicals is attractive due to the advantages of being abundant, nontoxic, and economical. Electrochemical CO2 reduction (CO2RR) provides an avenue to close the anthropogenic carbon cycle. However, the reaction process of multi-electronic products of CO2RR is quite complex. It is hard to yield a target product with high selectivity, high current density, low overpotential, and good stability simultaneously. In recent years, in situ/operando characterization techniques have played important roles in the catalysis field via establishing the structure—reactivity/selectivity relationships of catalysts and thereby obtaining information about mechanisms. As a result, it is necessary to apply in situ/operando characterization technologies to clarify the reaction pathway of CO2RR. In this mini-review, we discuss recent progress on the in situ/operando characterizations for electrochemical CO2RR, including microscopies, infrared spectroscopy, Raman spectroscopy, X-ray photoelectron spectroscopy, and X-ray absorption fine spectroscopy. Moreover, the capabilities of these in situ/operando characterizations and the remaining challenges are also discussed.
Similar content being viewed by others
References
Shindell D, Smith CJ. Nature, 2019, 573: 408–411
Lu L, Sun X, Ma J, Zhu Q, Wu C, Yang D, Han B. Sci China Chem, 2018, 61: 228–235
Jiang X, Nie X, Guo X, Song C, Chen JG. Chem Rev, 2020, 120: 7984–8034
Yang D, Zhu Q, Han B. Innovation, 2020, 1: 100016
Xu L, Ma X, Wu L, Tan X, Song X, Zhu Q, Chen C, Qian Q, Liu Z, Sun X, Liu S, Han B. Angew Chem Int Ed, 2022, 61: e202210375
He M, Sun Y, Han B. Angew Chem Int Ed, 2022, 61: e202112835
Tan X, Guo W, Liu S, Jia S, Xu L, Feng J, Yan X, Chen C, Zhu Q, Sun X, Han B. Chem Sci, 2022, 13: 11918–11925
Zhang L, Dang Y, Zhou X, Gao P, Petrus van Bavel A, Wang H, Li S, Shi L, Yang Y, Vovk EI, Gao Y, Sun Y. Innovation, 2021, 2: 100170
Song X, Guo W, Ma X, Xu L, Tan X, Wu L, Jia S, Wu T, Ma J, Zhang F, Jia J, Sun X, Han B. Green Chem, 2022, 24: 1488–1493
Ma X, Xu L, Liu S, Zhang L, Tan X, Wu L, Feng J, Liu Z, Sun X, Han B. Chem Catal, 2022, 2: 3207–3224
Huang JE, Li F, Ozden A, Sedighian Rasouli A, García de Arquer FP, Liu S, Zhang S, Luo M, Wang X, Lum Y, Xu Y, Bertens K, Miao RK, Dinh CT, Sinton D, Sargent EH. Science, 2021, 372: 1074–1078
Jiao X, Zheng K, Chen Q, Li X, Li Y, Shao W, Xu J, Zhu J, Pan Y, Sun Y, Xie Y. Angew Chem Int Ed, 2020, 59: 15497–15501
Ren X, Liu S, Li H, Ding J, Liu L, Kuang Z, Li L, Yang H, Bai F, Huang Y, Zhang T, Liu B. Sci China Chem, 2020, 63: 1727–1733
Gao D, Wei P, Li H, Lin L, Wang G, Bao X. Acta Physico Chim Sin, 2021, 37: 2009021
Wang H, Wu Y, Zhao Y, Liu Z. Acta Physico Chim Sin, 2021, 37: 2010022
Zhong D, Zhao ZJ, Zhao Q, Cheng D, Liu B, Zhang G, Deng W, Dong H, Zhang L, Li J, Li J, Gong J. Angew Chem Int Ed, 2021, 60: 4879–4885
Tan X, Sun X, Han B. Natl Sci Rev, 2022, 9: nwab022
Jin S, Hao Z, Zhang K, Yan Z, Chen J. Angew Chem Int Ed, 2021, 60: 20627–20648
Xiong L, Zhang X, Chen L, Deng Z, Han S, Chen Y, Zhong J, Sun H, Lian Y, Yang B, Yuan X, Yu H, Liu Y, Yang X, Guo J, Rümmeli MH, Jiao Y, Peng Y. Adv Mater, 2021, 33: 2101741
Zhao Y, Zu X, Chen R, Li X, Jiang Y, Wang Z, Wang S, Wu Y, Sun Y, Xie Y. J Am Chem Soc, 2022, 144: 10446–10454
Li P, Bi J, Liu J, Zhu Q, Chen C, Sun X, Zhang J, Han B. Nat Commun, 2022, 13: 1965
Wu Y, Chen C, Yan X, Sun X, Zhu Q, Li P, Li Y, Liu S, Ma J, Huang Y, Han B. Angew Chem Int Ed, 2021, 60: 20803–20810
Wu Y, Cao S, Hou J, Li Z, Zhang B, Zhai P, Zhang Y, Sun L. Adv Energy Mater, 2020, 10: 2000588
Zhang E, Wang T, Yu K, Liu J, Chen W, Li A, Rong H, Lin R, Ji S, Zheng X, Wang Y, Zheng L, Chen C, Wang D, Zhang J, Li Y. J Am Chem Soc, 2019, 141: 16569–16573
Liang S, Huang L, Gao Y, Wang Q, Liu B. Adv Sci, 2021, 8: 2102886
Li M, Garg S, Chang X, Ge L, Li L, Konarova M, Rufford TE, Rudolph V, Wang G. Small Methods, 2020, 4: 2000033
Xie W, Li H, Cui G, Li J, Song Y, Li S, Zhang X, Lee JY, Shao M, Wei M. Angew Chem Int Ed, 2021, 60: 7382–7388
Yi L, Chen J, Shao P, Huang J, Peng X, Li J, Wang G, Zhang C, Wen Z. Angew Chem Int Ed, 2020, 59: 20112–20119
Peng H, Tang MT, Liu X, Lamoureux PS, Bajdich M, Abild-Pedersen F. Energy Environ Sci, 2021, 14: 473–482
Li X, Wang S, Li L, Sun Y, Xie Y. J Am Chem Soc, 2020, 142: 9657–9581
Jiao X, Hu Z, Li L, Wu Y, Zheng K, Sun Y, Xie Y. Sci China Chem, 2022, 65: 428–440
Zou Y, Wang S. Adv Sci, 2021, 8: 2003579
Cao X, Tan D, Wulan B, Hui KS, Hui KN, Zhang J. Small Methods, 2021, 5: 2100700
Vavra J, Shen TH, Stoian D, Tileli V, Buonsanti R. Angew Chem Int Ed, 2021, 60: 1347–1354
Bañares MA. Catal Today, 2005, 100: 71–77
Yang Y, Xiong Y, Zeng R, Lu X, Krumov M, Huang X, Xu W, Wang H, DiSalvo FJ, Brock JD, Muller DA, Abruña HD. ACS Catal, 2021, 11: 1136–1178
Handoko AD, Wei F, Jenndy F, Yeo BS, Seh ZW. Nat Catal, 2018, 1: 922–934
Li J, Gong J. Energy Environ Sci, 2020, 13: 3748–3779
Grosse P, Gao D, Scholten F, Sinev I, Mistry H, Roldan Cuenya B. Angew Chem Int Ed, 2018, 57: 6192–6197
Phan TH, Banjac K, Cometto FP, Dattila F, García-Muelas R, Raaijman SJ, Ye C, Koper MTM, López N, Lingenfelder M. Nano Lett, 2021, 21: 2059–2065
Wang X, Klingan K, Klingenhof M, Möller T, Ferreira de Araújo J, Martens I, Bagger A, Jiang S, Rossmeisl J, Dau H, Strasser P. Nat Commun, 2021, 12: 794
Jacobse L, Huang YF, Koper MTM, Rost MJ. Nat Mater, 2018, 17: 277–282
Pfisterer JHK, Liang Y, Schneider O, Bandarenka AS. Nature, 2017, 549: 74–77
Wang X, Cai ZF, Wang YQ, Feng YC, Yan HJ, Wang D, Wan LJ. Angew Chem Int Ed, 2020, 59: 16098–16103
Gao D, Zhang Y, Zhou Z, Cai F, Zhao X, Huang W, Li Y, Zhu J, Liu P, Yang F, Wang G, Bao X. J Am Chem Soc, 2017, 139: 5652–5655
Beermann V, Holtz ME, Padgett E, de Araujo JF, Muller DA, Strasser P. Energy Environ Sci, 2019, 12: 2476–2485
Arán-Ais RM, Rizo R, Grosse P, Algara-Siller G, Dembélé K, Plodinec M, Lunkenbein T, Chee SW, Cuenya BR. Nat Commun, 2020, 11: 3489
Simon GH, Kley CS, Roldan Cuenya B. Angew Chem Int Ed, 2021, 60: 2561–2568
Dang S, Qin B, Yang Y, Wang H, Cai J, Han Y, Li S, Gao P, Sun Y. Sci Adv, 2020, 6: eaaz2060
Zhang CC, Shi J, Hartlaub S, Palamara JP, Petrovic I, Yilmaz B. Catal Commun, 2021, 150: 106273
Wei X, Yin Z, Lyu K, Li Z, Gong J, Wang G, Xiao L, Lu J, Zhuang L. ACS Catal, 2020, 10: 4103–4111
Zhang G, Zhao ZJ, Cheng D, Li H, Yu J, Wang Q, Gao H, Guo J, Wang H, Ozin GA, Wang T, Gong J. Nat Commun, 2021, 12: 5745
Pérez-Gallent E, Figueiredo MC, Calle-Vallejo F, Koper MTM. Angew Chem Int Ed, 2017, 56: 3621–3624
Ma W, Xie S, Liu T, Fan Q, Ye J, Sun F, Jiang Z, Zhang Q, Cheng J, Wang Y. Nat Catal, 2020, 3: 478–487
Zhu S, Jiang B, Cai WB, Shao M. J Am Chem Soc, 2017, 139: 15664–15667
Chen S, Li WH, Jiang W, Yang J, Zhu J, Wang L, Ou H, Zhuang Z, Chen M, Sun X, Wang D, Li Y. Angew Chem Int Ed, 2022, 61: e202114450
Wang J, Tan HY, Zhu Y, Chu H, Chen HM. Angew Chem Int Ed, 2021, 60: 17254–17267
Zhou X, Shan J, Chen L, Xia BY, Ling T, Duan J, Jiao Y, Zheng Y, Qiao SZ. J Am Chem Soc, 2022, 144: 2079–2084
Ko YJ, Kim JY, Lee WH, Kim MG, Seong TY, Park J, Jeong YJ, Min BK, Lee WS, Lee DK, Oh HS. Nat Commun, 2022, 13: 2205
Dutta A, Montiel IZ, Kiran K, Rieder A, Grozovski V, Gut L, Broekmann P. ACS Catal, 2021, 11: 4988–5003
Chernyshova IV, Somasundaran P, Ponnurangam S. Proc Natl Acad Sci USA, 2018, 115: E9261–E9270
Gao J, Zhang H, Guo X, Luo J, Zakeeruddin SM, Ren D, Grätzel M. J Am Chem Soc, 2019, 141: 18704–18714
Zhan C, Dattila F, Rettenmaier C, Bergmann A, Kühl S, García-Muelas R, López N, Cuenya BR. ACS Catal, 2021, 11: 7694–7701
Guo W, Tan X, Bi J, Xu L, Yang D, Chen C, Zhu Q, Ma J, Tayal A, Ma J, Huang Y, Sun X, Liu S, Han B. J Am Chem Soc, 2021, 143: 6877–6885
Chen C, Sun X, Yan X, Wu Y, Liu M, Liu S, Zhao Z, Han B. Green Chem, 2020, 22: 1572–1576
Su X, Jiang Z, Zhou J, Liu H, Zhou D, Shang H, Ni X, Peng Z, Yang F, Chen W, Qi Z, Wang D, Wang Y. Nat Commun, 2022, 13: 1322
Karapinar D, Huan NT, Ranjbar Sahraie N, Li J, Wakerley D, Touati N, Zanna S, Taverna D, Galvão Tizei LH, Zitolo A, Jaouen F, Mougel V, Fontecave M. Angew Chem Int Ed, 2019, 58: 15098–15103
Weng Z, Wu Y, Wang M, Jiang J, Yang K, Huo S, Wang XF, Ma Q, Brudvig GW, Batista VS, Liang Y, Feng Z, Wang H. Nat Commun, 2018, 9: 415
Yang HB, Hung SF, Liu S, Yuan K, Miao S, Zhang L, Huang X, Wang HY, Cai W, Chen R, Gao J, Yang X, Chen W, Huang Y, Chen HM, Li CM, Zhang T, Liu B. Nat Energy, 2018, 3: 140–147
Gu J, Hsu CS, Bai L, Chen HM, Hu X. Science, 2019, 364: 1091–1094
Zheng Y, Vasileff A, Zhou X, Jiao Y, Jaroniec M, Qiao SZ. J Am Chem Soc, 2019, 141: 7646–7659
Acknowledgements
This work was supported by National Natural Science Foundation of China (22002172, 22121002), Beijing Natural Science Foundation (J210020), National Key Research and Development Program of China (2020YFA0710203), Chinese Academy of Sciences (QYZDY-SSW-SLH013) and Photon Science Center for Carbon Neutrality.
Author information
Authors and Affiliations
Corresponding authors
Ethics declarations
Conflict of interest The authors declare no conflict of interest.
Rights and permissions
About this article
Cite this article
Song, X., Xu, L., Sun, X. et al. In situ/operando characterization techniques for electrochemical CO2 reduction. Sci. China Chem. 66, 315–323 (2023). https://doi.org/10.1007/s11426-021-1463-6
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s11426-021-1463-6