Tables for
Volume H
Powder diffraction
Edited by C. J. Gilmore, J. A. Kaduk and H. Schenk

International Tables for Crystallography (2018). Vol. H, ch. 2.9, p. 196

Section Electrochemistry using neutron diffraction

W. van Beeka* and P. Pattisona,b

aSwiss–Norwegian Beamlines at ESRF, CS 40220, 38043 Grenoble CEDEX 9, France, and bLaboratory for Quantum Magnetism, Institute of Physics, Ecole Polytechnique Federale de Lausanne, CH-1015 Lausanne, Switzerland
Correspondence e-mail: Electrochemistry using neutron diffraction

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The advantages of high penetration and sensitivity to light elements such as hydrogen, oxygen and lithium make neutron powder diffraction an interesting tool for investigating processes occurring within complex electrochemical systems. Lithium-ion batteries are one of the most widely used portable energy sources. These devices rely on the insertion of lithium ions into both positive and negative electrodes. A proper understanding of the structural processes that occur at the electrodes can only be obtained from in situ diffraction experiments performed during electrochemical charging and discharging. A suitable electrochemical cell for this type of measurement has been reported by Rosciano et al. (2008[link]). The challenge for the design of this type of cell is to enable the neutron-diffraction data to be collected with the minimum of hindrance, while allowing electrochemical characterization to be performed at the same time. In addition, the fact that most separators and polycarbonate-based electrolyte solutions contain large amounts of hydrogen presents problems due to the large incoherent neutron-scattering cross section of hydrogen, which results in a deterioration in the signal-to-background ratio. However, as pointed out by Sharma et al. (2011[link]), designs have been developed that minimize the amount of electrolyte required, and, where possible, deuterated solution can be used. Using a home-made design of a rollover, cylindrical cell that mimicked the geometry of commercial batteries, Sharma et al. (2011[link]) were able to probe structural changes in real time (5 min per pattern) as a function of electrochemical cycling using the Wombat powder diffractometer (ANSTO). Sharma et al. (2015[link]) have since reviewed both synchrotron and neutron electrochemistry cells. Pang & Peterson (2015[link]) provide an overview of all lithium-ion and sodium-ion battery materials studied by neutron powder diffraction in situ since 1998.

Battery materials and fuel cells are extensively used in a vast variety of applications in energy conversion and storage, and there is no doubt that in situ neutron powder diffraction will continue to play an important role in the efforts to further improve the performance of these materials. In Japan, for example, a new neutron-diffraction instrument (SPICA at the J-PARC spallation source) will be used to analyse atomic structures and the behaviour of batteries during their charge cycle. Both at spallation and reactor-based neutron sources, improvements in neutron optics and detector performance have reduced both the volume of sample needed for in situ experiments and the time required to collect each powder pattern.


Pang, W. K. & Peterson, V. K. (2015). A custom battery for operando neutron powder diffraction studies of electrode structure. J. Appl. Cryst. 48, 280–290.Google Scholar
Rosciano, F., Holzapfel, M., Scheifele, W. & Novák, P. (2008). A novel electrochemical cell for in situ neutron diffraction studies of electrode materials for lithium-ion batteries. J. Appl. Cryst. 41, 690–694.Google Scholar
Sharma, N., Du, G., Studer, A. J., Guo, Z. & Peterson, V. K. (2011). In-situ neutron diffraction study of the MoS2 anode using a custom-built Li-ion battery. Solid State Ionics, 199–200, 37–43.Google Scholar
Sharma, N., Pang, W. K., Guo, Z. & Peterson, V. K. (2015). In situ powder diffraction studies of electrode materials in rechargeable batteries. ChemSusChem, 8, 2826–2853.Google Scholar

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