Development of a versatile electrochemical cell for in situ grazing-incidence X-ray diffraction during non-aqueous electrochemical nitrogen reduction

Blair, Sarah J.; Nielander, Adam C.; Stone, Kevin H.; Kreider, Melissa E.; Niemann, Valerie A.; Benedek, Peter; McShane, Eric J.; Gallo, Alessandro; Jaramillo, Thomas F.

doi:10.1107/S1600577523006331

Development of a versatile electrochemical cell for in situ grazing-incidence X-ray diffraction during non-aqueous electrochemical nitrogen reduction

Journal Article · Fri Aug 18 00:00:00 EDT 2023 · Journal of Synchrotron Radiation (Online)

DOI:https://doi.org/10.1107/S1600577523006331· OSTI ID:1995923

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In situ techniques are essential to understanding the behavior of electrocatalysts under operating conditions. When employed, in situ synchrotron grazing-incidence X-ray diffraction (GI-XRD) can provide time-resolved structural information of materials formed at the electrode surface. In situ cells, however, often require epoxy resins to secure electrodes, do not enable electrolyte flow, or exhibit limited chemical compatibility, hindering the study of non-aqueous electrochemical systems. Here, a versatile electrochemical cell for air-free in situ synchrotron GI-XRD during non-aqueous Li-mediated electrochemical N ₂ reduction (Li-N ₂ R) has been designed. This cell not only fulfills the stringent material requirements necessary to study this system but is also readily extendable to other electrochemical systems. Under conditions relevant to non-aqueous Li-N ₂ R, the formation of Li metal, LiOH and Li ₂ O as well as a peak consistent with the α-phase of Li ₃ N was observed, thus demonstrating the functionality of this cell toward developing a mechanistic understanding of complicated electrochemical systems.

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Research Organization:: SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States)

Sponsoring Organization:: National Science Foundation (NSF); USDOE; USDOE Office of Science (SC), Basic Energy Sciences (BES). Chemical Sciences, Geosciences & Biosciences Division (CSGB); Villum Foundation

Grant/Contract Number:: AC02-76SF00515

OSTI ID:: 1995923

Alternate ID(s):: OSTI ID: 2000060

Journal Information:: Journal of Synchrotron Radiation (Online), Journal Name: Journal of Synchrotron Radiation (Online) Journal Issue: 5 Vol. 30; ISSN 1600-5775; ISSN JSYRES

Publisher:: International Union of Crystallography (IUCr)Copyright Statement

Country of Publication:: Denmark

Language:: English

References (28)

Reversible Lithium-Ion Insertion in Molybdenum Oxide Nanoparticles Lee, Se-Hee; Kim, Yong-Hyun; Deshpande, Rohit Advanced Materials, Vol. 20, Issue 19 https://doi.org/10.1002/adma.200800999	journal	October 2008
Lithium-mediated electrochemical reduction of high pressure N2 to NH3 Tsuneto, Akira; Kudo, Akihiko; Sakata, Tadayoshi Journal of Electroanalytical Chemistry, Vol. 367, Issue 1-2 https://doi.org/10.1016/0022-0728(93)03025-K	journal	March 1994
Reversible Nitrogen Fixation Based on a Rechargeable Lithium-Nitrogen Battery for Energy Storage Ma, Jin-Ling; Bao, Di; Shi, Miao-Miao Chem, Vol. 2, Issue 4 https://doi.org/10.1016/j.chempr.2017.03.016	journal	April 2017
Understanding Continuous Lithium-Mediated Electrochemical Nitrogen Reduction Lazouski, Nikifar; Schiffer, Zachary J.; Williams, Kindle Joule, Vol. 3, Issue 4 https://doi.org/10.1016/j.joule.2019.02.003	journal	April 2019
A Roadmap to the Ammonia Economy MacFarlane, Douglas R.; Cherepanov, Pavel V.; Choi, Jaecheol Joule, Vol. 4, Issue 6 https://doi.org/10.1016/j.joule.2020.04.004	journal	June 2020
Organic solvent resistant poly(ether-ether-ketone) nanofiltration membranes da Silva Burgal, João; Peeva, Ludmila G.; Kumbharkar, Santosh Journal of Membrane Science, Vol. 479 https://doi.org/10.1016/j.memsci.2014.12.035	journal	April 2015
In Situ Study of Silicon Electrode Lithiation with X-ray Reflectivity Cao, Chuntian; Steinrück, Hans-Georg; Shyam, Badri Nano Letters, Vol. 16, Issue 12 https://doi.org/10.1021/acs.nanolett.6b02926	journal	November 2016
Ammonia as a Renewable Energy Transportation Media Giddey, S.; Badwal, S. P. S.; Munnings, C. ACS Sustainable Chemistry & Engineering, Vol. 5, Issue 11 https://doi.org/10.1021/acssuschemeng.7b02219	journal	October 2017
Lithium Metal-Gas Reactions. Markowitz, M. M.; Boryta, D. A. Journal of Chemical & Engineering Data, Vol. 7, Issue 4 https://doi.org/10.1021/je60015a047	journal	October 1962
How a century of ammonia synthesis changed the world Erisman, Jan Willem; Sutton, Mark A.; Galloway, James Nature Geoscience, Vol. 1, Issue 10 https://doi.org/10.1038/ngeo325	journal	September 2008
In situ/operando synchrotron-based X-ray techniques for lithium-ion battery research Bak, Seong-Min; Shadike, Zulipiya; Lin, Ruoqian NPG Asia Materials, Vol. 10, Issue 7 https://doi.org/10.1038/s41427-018-0056-z	journal	July 2018
On the crystallography and reversibility of lithium electrodeposits at ultrahigh capacity Zhao, Qing; Deng, Yue; Utomo, Nyalaliska W. Nature Communications, Vol. 12, Issue 1 https://doi.org/10.1038/s41467-021-26143-9	journal	October 2021
Revealing solid electrolyte interphase formation through interface-sensitive Operando X-ray absorption spectroscopy Swallow, Jack E. N.; Fraser, Michael W.; Kneusels, Nis-Julian H. Nature Communications, Vol. 13, Issue 1 https://doi.org/10.1038/s41467-022-33691-1	journal	October 2022
Glassy Li metal anode for high-performance rechargeable Li batteries Wang, Xuefeng; Pawar, Gorakh; Li, Yejing Nature Materials, Vol. 19, Issue 12 https://doi.org/10.1038/s41563-020-0729-1	journal	July 2020
Challenges and prospects in the catalysis of electroreduction of nitrogen to ammonia Suryanto, Bryan H. R.; Du, Hoang-Long; Wang, Dabin Nature Catalysis, Vol. 2, Issue 4 https://doi.org/10.1038/s41929-019-0252-4	journal	March 2019
Electrochemical flow cell enabling operando probing of electrocatalyst surfaces by X-ray spectroscopy and diffraction Farmand, Maryam; Landers, Alan T.; Lin, John C. Physical Chemistry Chemical Physics, Vol. 21, Issue 10 https://doi.org/10.1039/C8CP07423B	journal	January 2019
Combined, time-resolved, in situ neutron reflectometry and X-ray diffraction analysis of dynamic SEI formation during electrochemical N₂ reduction Blair, Sarah J.; Doucet, Mathieu; Niemann, Valerie A. Energy & Environmental Science, Vol. 16, Issue 8 https://doi.org/10.1039/D2EE03694K	journal	January 2023
The effect of deposition parameters on radiofrequency sputtered molybdenum thin films Khatri, H.; Marsillac, S. Journal of Physics: Condensed Matter, Vol. 20, Issue 5 https://doi.org/10.1088/0953-8984/20/05/055206	journal	January 2008
Observation of the effect of refraction on x rays diffracted in a grazing-incidence asymmetric Bragg geometry Toney, Michael F.; Brennan, Sean Physical Review B, Vol. 39, Issue 11 https://doi.org/10.1103/PhysRevB.39.7963	journal	April 1989
A radially accessible tubular in situ X-ray cell for spatially resolved operando scattering and spectroscopic studies of electrochemical energy storage devices Liu, Hao; Allan, Phoebe K.; Borkiewicz, Olaf J. Journal of Applied Crystallography, Vol. 49, Issue 5 https://doi.org/10.1107/S1600576716012632	journal	September 2016
An electrochemical cell for operando bench-top X-ray diffraction Sottmann, Jonas; Pralong, Valérie; Barrier, Nicolas Journal of Applied Crystallography, Vol. 52, Issue 2 https://doi.org/10.1107/S1600576719000773	journal	February 2019
A refraction correction for buried interfaces applied to in situ grazing-incidence X-ray diffraction studies on Pd electrodes Landers, Alan T.; Koshy, David M.; Lee, Soo Hong Journal of Synchrotron Radiation, Vol. 28, Issue 3 https://doi.org/10.1107/S1600577521001557	journal	March 2021
Crystallinity and dielectric properties of PEEK, poly(ether ether ketone) Giants, T. W. IEEE Transactions on Dielectrics and Electrical Insulation, Vol. 1, Issue 6 https://doi.org/10.1109/94.368664	journal	January 1994
Study of the reactions of Li with tetrahydrofuran and propylene carbonate by photoemission spectroscopy Zhuang, G. R.; Wang, K.; Chen, Y. Journal of Vacuum Science & Technology A: Vacuum, Surfaces, and Films, Vol. 16, Issue 5 https://doi.org/10.1116/1.581475	journal	September 1998
Is lithium the key for nitrogen electroreduction? Westhead, Olivia; Jervis, Rhodri; Stephens, Ifan E. L. Science, Vol. 372, Issue 6547 https://doi.org/10.1126/science.abi8329	journal	June 2021
Identification of Surface Films Formed on Lithium in Dimethoxyethane and Tetrahydrofuran Solutions Aurbach, D. Journal of The Electrochemical Society, Vol. 135, Issue 8 https://doi.org/10.1149/1.2096170	journal	January 1988
Reactions of Tetrahydrofuran and Lithium Hexafluoroarsenate with Lithium Koch, V. R. Journal of The Electrochemical Society, Vol. 126, Issue 2 https://doi.org/10.1149/1.2129002	journal	February 1979
Soft X-Ray Irradiation Effects of Li2O2, Li2CO3 and Li2O Revealed by Absorption Spectroscopy Qiao, Ruimin; Chuang, Yi-De; Yan, Shishen PLoS ONE, Vol. 7, Issue 11 https://doi.org/10.1371/journal.pone.0049182	journal	November 2012

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Related Subjects

73 NUCLEAR PHYSICS AND RADIATION PHYSICS
electrocatalysis
electrochemical cell design
grazing incidence
in situ
non-aqueous Li-mediated electrochemical nitrogen reduction
solid electrolyte interphase
synchrotron X-ray diffraction

Development of a versatile electrochemical cell for in situ grazing-incidence X-ray diffraction during non-aqueous electrochemical nitrogen reduction

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