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Method—Setups and Protocols for Operando Batteries Experiments at Variable Temperatures Applied to CaxTiS2 and Na3−xV2(PO4)3

Houdeville, R. G. ; Missyul, A. ; Fuentes, V. ; Moline, M. M.Prieto ; Farre, F. ; Gonzalez, J. B. LU ; Palacin, M. R. and Fauth, Francois (2024) In Journal of the Electrochemical Society 171(2).
Abstract

In this paper, we present two thermalized setups for in situ operando X-ray diffraction data collection in temperature ranging from 0° to 100 °C: a modified Leriche cell and a coin cell chamber. Both setups proved proper thermalization and representative electrochemistry. While the coin cell chamber may only be used in transmission mode, the modified Leriche cell can also be used in reflection mode. Two case studies are presented as example of operation: calcium insertion in TiS2 and sodium (de-)insertion in Na3−xV2(PO4)3. For the former, heating at 60 °C enables faster kinetics to form a solvent co-intercalated phase upon reduction, a process which is reversible upon reoxidation.... (More)

In this paper, we present two thermalized setups for in situ operando X-ray diffraction data collection in temperature ranging from 0° to 100 °C: a modified Leriche cell and a coin cell chamber. Both setups proved proper thermalization and representative electrochemistry. While the coin cell chamber may only be used in transmission mode, the modified Leriche cell can also be used in reflection mode. Two case studies are presented as example of operation: calcium insertion in TiS2 and sodium (de-)insertion in Na3−xV2(PO4)3. For the former, heating at 60 °C enables faster kinetics to form a solvent co-intercalated phase upon reduction, a process which is reversible upon reoxidation. For the later, Na3−xV2(PO4)3 is known to form a low temperature phase at ca 12 °C. Thanks to the thermalized setups, operando X-ray diffraction patterns were collected while cycling on the low temperature phase.

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author
; ; ; ; ; ; and
organization
publishing date
type
Contribution to journal
publication status
published
subject
keywords
batteries, operando, synchrotron, X-ray diffraction
in
Journal of the Electrochemical Society
volume
171
issue
2
article number
020533
publisher
Electrochemical Society
external identifiers
  • scopus:85185540175
ISSN
0013-4651
DOI
10.1149/1945-7111/ad27b5
language
English
LU publication?
yes
id
adff938c-6ff7-434f-a6ea-43f65e515df4
date added to LUP
2024-03-25 11:32:52
date last changed
2024-03-25 11:33:31
@article{adff938c-6ff7-434f-a6ea-43f65e515df4,
  abstract     = {{<p>In this paper, we present two thermalized setups for in situ operando X-ray diffraction data collection in temperature ranging from 0° to 100 °C: a modified Leriche cell and a coin cell chamber. Both setups proved proper thermalization and representative electrochemistry. While the coin cell chamber may only be used in transmission mode, the modified Leriche cell can also be used in reflection mode. Two case studies are presented as example of operation: calcium insertion in TiS<sub>2</sub> and sodium (de-)insertion in Na<sub>3−x</sub>V<sub>2</sub>(PO<sub>4</sub>)<sub>3</sub>. For the former, heating at 60 °C enables faster kinetics to form a solvent co-intercalated phase upon reduction, a process which is reversible upon reoxidation. For the later, Na<sub>3−x</sub>V<sub>2</sub>(PO<sub>4</sub>)<sub>3</sub> is known to form a low temperature phase at ca 12 °C. Thanks to the thermalized setups, operando X-ray diffraction patterns were collected while cycling on the low temperature phase.</p>}},
  author       = {{Houdeville, R. G. and Missyul, A. and Fuentes, V. and Moline, M. M.Prieto and Farre, F. and Gonzalez, J. B. and Palacin, M. R. and Fauth, Francois}},
  issn         = {{0013-4651}},
  keywords     = {{batteries; operando; synchrotron; X-ray diffraction}},
  language     = {{eng}},
  number       = {{2}},
  publisher    = {{Electrochemical Society}},
  series       = {{Journal of the Electrochemical Society}},
  title        = {{Method—Setups and Protocols for Operando Batteries Experiments at Variable Temperatures Applied to Ca<sub>x</sub>TiS<sub>2</sub> and Na<sub>3−x</sub>V<sub>2</sub>(PO<sub>4</sub>)<sub>3</sub>}},
  url          = {{http://dx.doi.org/10.1149/1945-7111/ad27b5}},
  doi          = {{10.1149/1945-7111/ad27b5}},
  volume       = {{171}},
  year         = {{2024}},
}