Understanding fundamentals of electrochemical reactions with tender X-rays: A new lab-based operando X-ray photoelectron spectroscopy method for probing liquid/solid and gas/solid interfaces across a variety of electrochemical systems

doi:10.1016/S1872-2067(22)64092-0

Abstract

Abstract:

Electrocatalysis is key to improving energy efficiency, reducing carbon emissions, and providing a sustainable way of meeting global energy needs. Therefore, elucidating electrochemical reaction mechanisms at the electrolyte/electrode interfaces is essential for developing advanced renewable energy technologies. However, the direct probing of real-time interfacial changes, i.e., the surface intermediates, chemical environment, and electronic structure, under operating conditions is challenging and necessitates the use of in situ methods. Herein, we present a new lab-based instrument commissioned to perform in situ chemical analysis at liquid/solid interfaces using ambient pressure X-ray photoelectron spectroscopy (APXPS). This setup takes advantage of a chromium source of tender X-rays and is designed to study liquid/solid interfaces by the “dip and pull” method. Each of the main components was carefully described, and the results of performance tests are presented. Using a three-electrode setup, the system can probe the intermediate species and potential shifts across the liquid electrolyte/solid electrode interface. In addition, we demonstrate how this system allows the study of interfacial changes at gas/solid interfaces using a case study: a sodium-oxygen model battery. However, the use of APXPS in electrochemical studies is still in the early stages, so we summarize the current challenges and some developmental frontiers. Despite the challenges, we expect that joint efforts to improve instruments and the electrochemical setup will enable us to obtain a better understanding of the composition-reactivity relationship at electrochemical interfaces under realistic reaction conditions.

Key words: Tender X-rays, Ambient pressure X-ray photoelectron spectroscopy, Electrocatalysis, Liquid/solid interface, Gas/solid interface

Chiyan Liu, Qiao Dong, Yong Han, Yijing Zang, Hui Zhang, Xiaoming Xie, Yi Yu, Zhi Liu. Understanding fundamentals of electrochemical reactions with tender X-rays: A new lab-based operando X-ray photoelectron spectroscopy method for probing liquid/solid and gas/solid interfaces across a variety of electrochemical systems[J]. Chinese Journal of Catalysis, 2022, 43(11): 2858-2870.

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URL: https://www.cjcatal.com/EN/10.1016/S1872-2067(22)64092-0

https://www.cjcatal.com/EN/Y2022/V43/I11/2858

Figures/Tables 7

Fig. 1. Schematic of a three-electrode “dip and pull” cell where a working electrode is in contact with a thin film of liquid electrolyte at equilibrium with water vapor for in situ APXPS measurement.

Fig. 2. Configuration of the laboratory-based APXPS instrument. (a) The system consists of three parts: a Cr-Kα X-ray source, analysis chamber, and HiPP-2 electron energy analyzer. (b) The X-ray beam is perpendicular to the optical axis of the electron analyzer, and the sample can be rotated to vary the incident angle of the X-ray source, which is separated from the analysis chamber by a Be window. (c) Photograph of the APXPS system. (d) Three-electrode setup in 1 mol L-1 KF electrolyte.

Fig. 3. Au 4f spectra obtained under PE = 100, 200 and 500 eV with slit sizes of 0.5, 1.5, and 4.0 mm. CPS is the abbreviation of counts per second.

Fig. 4. System performance with varying photoemission geometry. (a) Au 3d5/2 spectra taken at different angles between the sample surface and the light source. (b) Au 3d5/2 peak intensities and X-ray footprint widths as a function of the sample angle.

Fig. 5. (a) Au 3d5/2 spectra collected at different Ar pressures. (b) Au 3d5/2 peak intensity plotted as a function of Ar pressure.

Fig. 6. O 1s (a), Pt 4f (b), and Pt 3d5/2 (c) spectra of the WE in water vapor at 17 Torr using the operando “dip and pull” method and collected at ?0.065, 0.435, 0.635, 0.935 and 1.235 V vs. the standard hydrogen electrode (SHE). (d) Voltammogram of the dipped three-electrode setup (a Pt metal foil WE, Ag/AgCl RE, and Pt CE) in 1 mol L-1 KF electrolyte. (e) O 1s BE of liquid water vs. the WE potential.

Fig. 7. (a) Schematic of the structure (left) and photograph (right) of the Na-O2 battery during measurements in the analysis chamber. P is the potentiostat. (b) Discharge-charge curve of the solid-state Na-O2 cell in the APXPS analysis chamber (at 4 Torr O2 + 11 Torr water vapor atmosphere at room temperature). (c) Na 1s and O 1s spectra of the cathode of the Na-O2 battery during discharge and charge processes.

References

[1]	M. Armand, J. M. Tarascon, Nature, 2008, 451, 652-657.
[2]	M. P. Mercer, H. E. Hoster, Nano Energy, 2016, 29, 394-413.
[3]	A. Knop-Gericke, V. Pfeifer, J.-J. Velasco-Velez, T. Jones, R. Arrigo, M. Hävecker, R. Schlögl, J. Electron Spectrosc. Relat. Phenom., 2017, 221, 10-17.
[4]	V. Pfeifer, T. E. Jones, J. J. Velasco Vélez, R. Arrigo, S. Piccinin, M. Hävecker, A. Knop-Gericke, R. Schlögl, Chem. Sci., 2017, 8, 2143-2149.
[5]	L. J. Frevel, R. Mom, J.-J. Velasco-Vélez, M. Plodinec, A. Knop-Gericke, R. Schlögl, T. E. Jones, J. Phys. Chem. C, 2019, 123, 9146-9152.
[6]	H. Siegbahn, J. Phys. Chem., 1985, 89, 897-909.
[7]	M. Salmeron, R. Schlögl, Surf. Sci. Rep., 2008, 63, 169-199.
[8]	C. Arble, M. Jia, J. T. Newberg, Surf. Sci. Rep., 2018, 73, 37-57.
[9]	D. E. Starr, Z. Liu, M. Havecker, A. Knop-Gericke, H. Bluhm, Chem. Soc. Rev., 2013, 42, 5833-5857.
[10]	Y. Han, H. Zhang, Y. Yu, Z. Liu, ACS Catal., 2021, 11, 1464-1484.
[11]	H. Siegbahn, M. Lundholm, J. Electron Spectrosc. Relat. Phenom., 1982, 28, 135-138.
[12]	I. Doron-Mor, A. Hatzor, A. Vaskevich, T. van der Boom-Moav, A. Shanzer, I. Rubinstein, H. Cohen, Nature, 2000, 406, 382-385.
[13]	G. Ertas, S. Suzer, in: Surface Chemistry in Biomedical and Environmental Science, J. P. Blitz, V. M. Gun'ko, ed., Springer Netherlands, Dordrecht, 2006, 45-58.
[14]	C. Zhang, M. E. Grass, A. H. McDaniel, S. C. DeCaluwe, F. E. Gabaly, Z. Liu, K. F. McCarty, R. L. Farrow, M. A. Linne, Z. Hussain, G. S. Jackson, H. Bluhm, B. W. Eichhorn, Nat. Mater., 2010, 9, 944-949.
[15]	J. Schnadt, J. Knudsen, N. Johansson, J. Phys.-Condens. Matter, 2020, 32, 413003.
[16]	J. J. Velasco-Velez, V. Pfeifer, M. Hävecker, R. S. Weatherup, R. Arrigo, C.-H. Chuang, E. Stotz, G. Weinberg, M. Salmeron, R. Schlögl, A. Knop-Gericke, Angew. Chem. Int. Ed., 2015, 54, 14554-14558.
[17]	R. Mom, L. Frevel, J.-J. Velasco-Vélez, M. Plodinec, A. Knop-Gericke, R. Schlögl, J. Am. Chem. Soc., 2019, 141, 6537-6544.
[18]	L. J. Falling, R. V. Mom, L. E. Sandoval Diaz, S. Nakhaie, E. Stotz, D. Ivanov, M. Hävecker, T. Lunkenbein, A. Knop-Gericke, R. Schlögl, J.-J. Velasco-Vélez, ACS Appl. Mater. Interfaces, 2020, 12, 37680-37692.
[19]	S. Axnanda, E. J. Crumlin, B. Mao, S. Rani, R. Chang, P. G. Karlsson, M. O. M. Edwards, M. Lundqvist, R. Moberg, P. Ross, Z. Hussain, Z. Liu, Sci. Rep., 2015, 5, 9788.
[20]	T. Masuda, H. Yoshikawa, H. Noguchi, T. Kawasaki, M. Kobata, K. Kobayashi, K. Uosaki, Appl. Phys. Lett., 2013, 103, 111605.
[21]	Y. Takagi, H. Wang, Y. Uemura, E. Ikenaga, O. Sekizawa, T. Uruga, H. Ohashi, Y. Senba, H. Yumoto, H. Yamazaki, S. Goto, M. Tada, Y. Iwasawa, T. Yokoyama, Appl. Phys. Lett., 2014, 105, 131602.
[22]	Y. T. Law, S. Zafeiratos, S. G. Neophytides, A. Orfanidi, D. Costa, T. Dintzer, R. Arrigo, A. Knop-Gericke, R. Schlögl, E. R. Savinova, Chem. Sci., 2015, 6, 5635-5642.
[23]	M. Favaro, B. Jeong, P. N. Ross, J. Yano, Z. Hussain, Z. Liu, E. J. Crumlin, Nat. Commun., 2016, 7, 12695.
[24]	F. J. Dyson, Imagined Worlds, Harvard University Press, Cambridge, 1997.
[25]	R. Schlögl, Angew. Chem. Int. Ed., 2015, 54, 3465-3520.
[26]	K. F. Kalz, R. Kraehnert, M. Dvoyashkin, R. Dittmeyer, R. Gläser, U. Krewer, K. Reuter, J.-D. Grunwaldt, ChemCatChem, 2017, 9, 17-29.
[27]	J.-J. Velasco-Velez, L. J. Falling, D. Bernsmeier, M. J. Sear, P. C. J. Clark, T.-S. Chan, E. Stotz, M. Hävecker, R. Kraehnert, A. Knop-Gericke, C.-H. Chuang, D. E. Starr, M. Favaro, R. V. Mom, J. Phys. D-Appl. Phys., 2021, 54, 124003.
[28]	C. A. Campos-Roldán, R. G. González-Huerta, N. Alonso-Vante, J. Electrochem. Soc., 2018, 165, J3001-J3007.
[29]	A. J. Bard, L. R. Faulkner, Electrochemical Methods: Fundamentals and Applications, 2nd ed., John Wiley & Sons, New York, 2003.
[30]	M. Kobata, I. Pis, H. Nohira, H. Iwai, K. Kobayashi, Surf. Interface Anal., 2011, 43, 1632-1635.
[31]	K. Kobayashi, M. Kobata, H. Iwai, J. Electron Spectrosc. Relat. Phenom., 2013, 190, 210-221.
[32]	D. F. Ogletree, H. Bluhm, G. Lebedev, C. S. Fadley, Z. Hussain, M. Salmeron, Rev. Sci. Instrum., 2002, 73, 3872-3877.
[33]	J. A. Whaley, A. H. McDaniel, F. El Gabaly, R. L. Farrow, M. E. Grass, Z. Hussain, Z. Liu, M. A. Linne, H. Bluhm, K. F. McCarty, Rev. Sci. Instrum., 2010, 81, 086104.
[34]	M. O. M. Edwards, P. G. Karlsson, S. K. Eriksson, M. Hahlin, H. Siegbahn, H. Rensmo, J. M. Kahk, I. J. Villar-Garcia, D. J. Payne, J. Åhlund, Nucl. Instrum. Methods Phys. Res., Sect. A, 2015, 785, 191-196.
[35]	Z. Novotny, D. Aegerter, N. Comini, B. Tobler, L. Artiglia, U. Maier, T. Moehl, E. Fabbri, T. Huthwelker, T. J. Schmidt, M. Ammann, J. A. van Bokhoven, J. Raabe, J. Osterwalder, Rev. Sci. Instrum., 2020, 91, 023103.
[36]	J. J. Olivero, R. L. Longbothum, J. Quant. Spectrosc. Radiat. Transfer, 1977, 17, 233-236.
[37]	J. L. Campbell, T. Papp, At. Data Nucl. Data Tables, 2001, 77, 1-56.
[38]	S. Mähl, M. Neumann, S. Dieckhoff, V. Schlett, A. Baalmann, J. Electron Spectrosc. Relat. Phenom., 1997, 85, 197-203.
[39]	A. Regoutz, M. Mascheck, T. Wiell, S. K. Eriksson, C. Liljenberg, K. Tetzner, B. A. D. Williamson, D. O. Scanlon, P. Palmgren, Rev. Sci. Instrum., 2018, 89, 073105.
[40]	Y. Takata, M. Yabashi, K. Tamasaku, Y. Nishino, D. Miwa, T. Ishikawa, E. Ikenaga, K. Horiba, S. Shin, M. Arita, K. Shimada, H. Namatame, M. Taniguchi, H. Nohira, T. Hattori, S. Södergren, B. Wannberg, K. Kobayashi, Nucl. Instrum. Methods Phys. Res., Sect. A, 2005, 547, 50-55.
[41]	V. N. Strocov, J. Synchrotron Radiat., 2013, 20, 517-521.
[42]	M. E. Grass, P. G. Karlsson, F. Aksoy, M. Lundqvist, B. Wannberg, B. S. Mun, Z,. Hussain,; Z. Liu, Rev. Sci. Instrum., 2010, 81, 053106.
[43]	J. Cai, Q. Dong, Y. Han, B.-H. Mao, H. Zhang, P. G. Karlsson, J. Åhlund, R.-Z. Tai, Y. Yu, Z. Liu, Nucl. Sci. Tech., 2019, 30, 81.
[44]	R. Rizo, E. Sitta, E. Herrero, V. Climent, J. M. Feliu, Electrochim. Acta, 2015, 162, 138-145.
[45]	M. Favaro, C. Valero-Vidal, J. Eichhorn, F. M. Toma, P. N. Ross, J. Yano, Z. Liu, E. J. Crumlin, J. Mater. Chem. A, 2017, 5, 11634-11643.
[46]	C. Jiang, B. Mao, F. Diao, Q. Li, Z. Wen, P. Si, H. Zhang, Z. Liu, J. Phys. D-Appl. Phys., 2021, 54, 174005.
[47]	A. Barrie, F. J. Street, J. Electron Spectrosc. Relat. Phenom., 1975, 7, 1-31.
[48]	N. Zhao, C. Li, X. Guo, Phys. Chem. Chem. Phys., 2014, 16, 15646-15652.
[49]	B. Mao, Y. Dai, J. Cai, Q. Li, C. Jiang, Y. Li, J. Xie, Z. Liu, Top. Catal., 2018, 61, 2123-2128.
[50]	J. G. Vos, A. Venugopal, W. A. Smith, M. T. M. Koper, J. Electrochem. Soc., 2020, 167, 046505.
[51]	K. A. Stoerzinger, M. Favaro, P. N. Ross, Z. Hussain, Z. Liu, J. Yano, E. J. Crumlin, Top. Catal., 2018, 61, 2152-2160.
[52]	C. Wang, C. Meng, S. Li, G. Zhang, Y. Ning, Q. Fu, J. Am. Chem. Soc., 2021, 143, 17843-17850.
[53]	C. Wang, Y. Ning, H. Huang, S. Li, C. Xiao, Q. Chen, L. Peng, S. Guo, Y. Li, C. Liu, Z.-S. Wu, X. Li, L. Chen, C. Gao, C. Wu, Q. Fu, Natl. Sci. Rev., 2021, 8, nwaa289.
[54]	Z. Nagy, H. You, J. Electroanal. Chem., 1995, 381, 275-279.