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

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.