In Situ Electron Diffraction Tomography Using a Liquid-Electrochemical Transmission Electron Microscopy Cell for Crystal Structure Determination of Cathode Materials for Li-Ion batteries

Olesia M. Karakulina, Arnaud Demortière, Walid Dachraoui, Artem M. Abakumov, Joke Hadermann

Research output: Contribution to journalArticlepeer-review

32 Citations (Scopus)

Abstract

We demonstrate that changes in the unit cell structure of lithium battery cathode materials during electrochemical cycling in liquid electrolyte can be determined for particles of just a few hundred nanometers in size using in situ transmission electron microscopy (TEM). The atomic coordinates, site occupancies (including lithium occupancy), and cell parameters of the materials can all be reliably quantified. This was achieved using electron diffraction tomography (EDT) in a sealed electrochemical cell with conventional liquid electrolyte (LP30) and LiFePO4 crystals, which have a well-documented charged structure to use as reference. In situ EDT in a liquid environment cell provides a viable alternative to in situ X-ray and neutron diffraction experiments due to the more local character of TEM, allowing for single crystal diffraction data to be obtained from multiphased powder samples and from submicrometer-to nanometer-sized particles. EDT is the first in situ TEM technique to provide information at the unit cell level in the liquid environment of a commercial TEM electrochemical cell. Its application to a wide range of electrochemical experiments in liquid environment cells and diverse types of crystalline materials can be envisaged.

Original languageEnglish
Pages (from-to)6286-6291
Number of pages6
JournalNano Letters
Volume18
Issue number10
DOIs
Publication statusPublished - 10 Oct 2018

Keywords

  • electron diffraction tomography
  • in situ electrochemical TEM
  • LiFePO cathode materials
  • Liquid TEM
  • structural determination

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