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

Autor: Blair SJ; Chemical Engineering, Stanford University, 443 Via Ortega, Stanford, CA 94305, USA., Nielander AC; SUNCAT Center for Interface Science and Catalysis, SLAC National Accelerator Laboratory, 2575 Sand Hill Rd, Menlo Park, CA 94025, USA., Stone KH; Stanford Synchrotron Radiation Lightsource, SLAC National Accelerator Laboratory, 2575 Sand Hill Rd, Menlo Park, CA 94025, USA., Kreider ME; Chemical Engineering, Stanford University, 443 Via Ortega, Stanford, CA 94305, USA., Niemann VA; Chemical Engineering, Stanford University, 443 Via Ortega, Stanford, CA 94305, USA., Benedek P; Chemical Engineering, Stanford University, 443 Via Ortega, Stanford, CA 94305, USA., McShane EJ; Chemical Engineering, Stanford University, 443 Via Ortega, Stanford, CA 94305, USA., Gallo A; SUNCAT Center for Interface Science and Catalysis, SLAC National Accelerator Laboratory, 2575 Sand Hill Rd, Menlo Park, CA 94025, USA., Jaramillo TF; Chemical Engineering, Stanford University, 443 Via Ortega, Stanford, CA 94305, USA.
Jazyk: angličtina
Zdroj: Journal of synchrotron radiation [J Synchrotron Radiat] 2023 Sep 01; Vol. 30 (Pt 5), pp. 917-922. Date of Electronic Publication: 2023 Aug 18.
DOI: 10.1107/S1600577523006331
Abstrakt: 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.
(open access.)
Databáze: MEDLINE
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