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Title: Multielectrode electrochemical cell for in situ structural characterization of amorphous thin-film catalysts using high-energy X-ray scattering

Journal Article · · Journal of Applied Crystallography (Online)
ORCiD logo [1];  [2];  [2];  [2];  [3];  [4];  [1]; ORCiD logo [1]; ORCiD logo [5];  [6]; ORCiD logo [6]; ORCiD logo [4];  [7]
  1. Brookhaven National Laboratory (BNL), Upton, NY (United States). National Synchrotron Light Source II (NSLS-II)
  2. Brookhaven National Laboratory (BNL), Upton, NY (United States). Center for Functional Nanomaterials (CFN)
  3. Brookhaven National Laboratory (BNL), Upton, NY (United States). Chemistry Department
  4. Stony Brook University, NY (United States)
  5. Argonne National Laboratory (ANL), Argonne, IL (United States). Advanced Photon Source (APS)
  6. Yale University, New Haven, CT (United States)
  7. Brookhaven National Laboratory (BNL), Upton, NY (United States). Center for Functional Nanomaterials (CFN); Stony Brook University, NY (United States)
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A multielectrode-based electrochemical cell allows the structural characterization of an amorphous thin-film water oxidation catalyst under various electrochemical potentials using high-energy X-ray scattering and atomic pair distribution function (PDF) techniques. A multielectrode with five electrodes provides a sufficiently low background signal to enable high-energy X-ray scattering (HEXS) measurements and amplifies the extremely low HEXS signals from samples for high-resolution PDF analysis of in situ data from thin-film catalysts. Glassy carbon (GC) creates a relatively low intensity HEXS pattern and is used as a working electrode. Instead of a three-dimensional (3D) porous electrode architecture, the flat geometry of the electrode enables various deposition techniques to be used for the preparation of a highly conductive metal oxide layer. PDF analysis demonstrates high spatial resolution for a 230 nm thick amorphous iridium oxide film deposited on two roughened 60 µm thick GC electrodes. The PDF analysis resolves the domain size and distinguishes changes in fine structure which are directly correlated with the structure and function of the catalysts. In conclusion, the results bring the opportunity to analyze the structure of nanometre-scale amorphous thin-film catalysts in an electrolyte-compatible and compact 3D-printed electrochemical cell in a three-electrode configuration.

Research Organization:
Brookhaven National Laboratory (BNL), Upton, NY (United States)
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES). Scientific User Facilities (SUF); USDOE Office of Science (SC), Basic Energy Sciences (BES). Chemical Sciences, Geosciences & Biosciences Division (CSGB)
Grant/Contract Number:
SC0012704; AC02-06CH11357; FG02-07ER15909
OSTI ID:
2280504
Report Number(s):
BNL-225140-2023-JAAM
Journal Information:
Journal of Applied Crystallography (Online), Vol. 56, Issue 5; ISSN 1600-5767
Publisher:
International Union of CrystallographyCopyright Statement
Country of Publication:
United States
Language:
English

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Related Subjects

36 MATERIALS SCIENCE
multielectrode cells
pair distribution function
high-energy X-ray scattering
thin films
oxygen evolution catalysts
in situ studies
operando studies
electrochemistry