Operando X-ray diffraction in transmission geometry « at home » from tape casted electrodes to all-solid-state battery

Beam Effects in Synchrotron Radiation Operando Characterization of Battery Materials: X-Ray Diffraction and Absorption Study of LiNi0.33Mn0.33Co0.33O2 and LiFePO4 Electrodes

“…Experiments were conducted in three types of electrochemical cells, enabling operando testing: Leriche, 37 LeRiChe’S v2 38 (both with 200 μm thick Be windows), and modified 2032 coin cells with 75 μm thick Kapton windows. 36 Cells were assembled in an Ar-filled glovebox and cycled with a BioLogic VSP potentiostat in galvanostatic mode with a potential limitation (GCPL).…”

“…In addition, they offer the possibility of contrasting the effects between two chemistries that exhibit distinct intercalation mechanisms and voltage profiles. The study spans across diverse experimental conditions involving different electrochemical cell types (coin cells, 36 Leriche 37 and LeRiChe’S v2 cells 38 ), combined X-ray absorption spectroscopy (XAS), and powder X-ray diffraction (PXRD) techniques and seeks to correlate beam effects with factors such as energy, photon flux, exposure time, and other parameters associated with radiation dosage.…”

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

“…For the electrochemical tests, the working electrodes consisted of a loose powder mixture made by manual grinding with mortar and pestle. In the case of TiS 2 (Aldrich, 99.995%), the as received powder was mixed with carbon black (Super P, Timcal) and polyvinylidene fluoride binder (PVDF) from Sigma-Aldrich (Mw ∼534,000 g.mol −1 ) in weight ratios of 84:10:6 while for the case of NVP, carbon coated powder 7 was mixed with 10% of carbon black (weight) and no binder was used. Typically, approx.…”

“…4 For example, the so called Leriche 5 cell was inspired from the Swagelok cells commonly used for laboratory battery testing. 6 A new version of this cell has been developed at Laboratoire de Réactivité et Chimie des Solides (LRCS) Amiens (LeRiChe'S v.2 cell 7 ) which in its design resembles the AMPIX cell 8 developed at Argonne National Laboratory and widely used in U.S. As alternative interesting design, one can mention Sottman's cell 9 which has been used for operando X-ray diffraction and absorption spectroscopy at the Swiss Norwegian beamline of ESRF (European Synchrotron Radiation Facility). An exhaustive list of electrochemical cell designs to be used for operando experiments at synchrotrons can also be found in Ref.…”

Synchrotron radiation based operando characterization of battery materials

“…cylindrical or radially symmetric cells for tomographic imaging). Customized cell setups were common in the early days of operando studies and new improved designs are being continuously developed 8 considering adaptability to somewhat different concepts ( e.g. all solid state cells).…”