Abstract
In operando powder diffraction remains one of the most powerful tools for non-destructive investigation of battery electrode materials. While in operando X-ray, especially synchrotron radiation, powder diffraction is by now a routine experimental technique, in operando neutron powder diffraction is still less established. We present a new electrochemical cell for in operando neutron powder diffraction, which is, first and foremost, easy to use, but can also cycle electrode materials under electrochemical conditions close to those achieved using standard laboratory cells. The cell has been designed in multiple sizes, and high-quality electrochemical and neutron powder diffraction data is presented for sample sizes as low as 48 mg total active material. The cell handles lithium-ion and sodium-ion materials equally well, with no difference in how the cell is prepared and assembled. The cell is intended to be used as sample environment at powder diffractometers at the neutron facilities MLZ, ORNL and ACNS.
| Original language | English |
|---|---|
| Article number | e202200046 |
| Journal | Chemistry-Methods |
| Volume | 2 |
| Issue number | 10 |
| DOIs | |
| State | Published - Oct 2022 |
Funding
We would like to thank workshop technician Lars Brændegaard Hansen at the Department of Physics, Chemistry and Pharmacy, University of Southern Denmark. He has played a vital role in both constructing and designing the cell. We also thank Mickey Sejerup Pedersen for supplying NaFeMnO. D.R.S. acknowledges the funding from the project “Operando Neutron Diffraction of Cathode Materials for Rechargeable Li‐ion Batteries” with project number 87686 by Nordforsk under the Nordic Council of Ministers. A.Ø.D. and D.B.R. acknowledge the Danish Ministry of Higher Education and Science for funding via the SMART Lighthouse project. M.H. acknowledges the funding from the project 05K16VK2/05K19VK3 “Energy research with Neutrons (ErwiN)” by the German Federal Ministry of Education and Research (BMBF). D.R.S, A.Ø.D. and D.R.B. thank Danscatt for funding travel costs related to the neutron diffraction experiments. We thank ANSTO for beamtime at Wombat (proposal number P8958). We also thank T. Darwish and N. Yepuri from the National Deuteration Facility for synthesizing deuterated ethylene carbonate (proposal number CB8567). We acknowledge the beamtime at D20, ILL (proposal 5‐23‐740. Data reference: doi:10.5291/ILL‐DATA.5‐23‐740). This research used resources at the High Flux Isotope Reactor and Spallation Neutron Source, DOE Office of Science User Facilities operated by the Oak Ridge National Laboratory. x 1/3 2/3 2 We would like to thank workshop technician Lars Brændegaard Hansen at the Department of Physics, Chemistry and Pharmacy, University of Southern Denmark. He has played a vital role in both constructing and designing the cell. We also thank Mickey Sejerup Pedersen for supplying NaxFe1/3Mn2/3O2. D.R.S. acknowledges the funding from the project “Operando Neutron Diffraction of Cathode Materials for Rechargeable Li-ion Batteries” with project number 87686 by Nordforsk under the Nordic Council of Ministers. A.Ø.D. and D.B.R. acknowledge the Danish Ministry of Higher Education and Science for funding via the SMART Lighthouse project. M.H. acknowledges the funding from the project 05K16VK2/05K19VK3 “Energy research with Neutrons (ErwiN)” by the German Federal Ministry of Education and Research (BMBF). D.R.S, A.Ø.D. and D.R.B. thank Danscatt for funding travel costs related to the neutron diffraction experiments. We thank ANSTO for beamtime at Wombat (proposal number P8958). We also thank T. Darwish and N. Yepuri from the National Deuteration Facility for synthesizing deuterated ethylene carbonate (proposal number CB8567). We acknowledge the beamtime at D20, ILL (proposal 5-23-740. Data reference: doi:10.5291/ILL-DATA.5-23-740). This research used resources at the High Flux Isotope Reactor and Spallation Neutron Source, DOE Office of Science User Facilities operated by the Oak Ridge National Laboratory.
| Funders | Funder number |
|---|---|
| High Flux Isotope Reactor and Spallation Neutron Source | |
| Office of Science | |
| Oak Ridge National Laboratory | |
| Bundesministerium für Bildung und Forschung | 5-23-740, P8958, :10.5291/ILL-DATA.5-23-740, CB8567 |
| Nordisk Ministerråd | |
| Syddansk Universitet | 87686 |
| Ministry of Science and Higher Education of the Russian Federation |
Keywords
- Li-ion battery
- Na-ion battery
- in operando
- materials science
- neutron diffraction
