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Title: A high pressure x-ray photoelectron spectroscopy experimental method for characterization of solid-liquid interfaces demonstrated with a Li-ion battery system

We report a methodology for a direct investigation of the solid/liquid interface using high pressure x-ray photoelectron spectroscopy (HPXPS). The technique was demonstrated with an electrochemical system represented by a Li-ion battery using a silicon electrode and a liquid electrolyte of LiClO{sub 4} in propylene carbonate (PC) cycled versus metallic lithium. For the first time the presence of a liquid electrolyte was realized using a transfer procedure where the sample was introduced into a 2 mbar N{sub 2} environment in the analysis chamber without an intermediate ultrahigh vacuum (UHV) step in the load lock. The procedure was characterized in detail concerning lateral drop gradients as well as stability of measurement conditions over time. The X-ray photoelectron spectroscopy (XPS) measurements demonstrate that the solid substrate and the liquid electrolyte can be observed simultaneously. The results show that the solid electrolyte interphase (SEI) composition for the wet electrode is stable within the probing time and generally agrees well with traditional UHV studies. Since the methodology can easily be adjusted to various high pressure photoelectron spectroscopy systems, extending the approach towards operando solid/liquid interface studies using liquid electrolytes seems now feasible.
Authors:
; ; ;  [1] ;  [2] ;  [3] ; ; ;  [4]
  1. Department of Chemistry–Ångström Laboratory, Uppsala University, Box 538, SE-751 21 Uppsala (Sweden)
  2. Department of Chemistry–Ångström Laboratory, Uppsala University, Box 523, SE-751 20 Uppsala (Sweden)
  3. VG Scienta AB, Box 15120, SE-750 15 Uppsala (Sweden)
  4. Department of Physics and Astronomy, Uppsala University, Box 516, SE-751 20 Uppsala (Sweden)
Publication Date:
OSTI Identifier:
22392462
Resource Type:
Journal Article
Resource Relation:
Journal Name: Review of Scientific Instruments; Journal Volume: 86; Journal Issue: 4; Other Information: (c) 2015 Author(s); Country of input: International Atomic Energy Agency (IAEA)
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; 46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND TECHNOLOGY; INTERFACES; LIQUIDS; LITHIUM IONS; LITHIUM PERCHLORATES; SOLID ELECTROLYTES; SUBSTRATES; X-RAY PHOTOELECTRON SPECTROSCOPY