determined by inductively coupled plasma mass spectrometry (ICP-MS)
(Shimadzu ICPMS-2030), and water content was estimated using thermogravimetric
analysis (TGA) (NETZSCH STA 449 F3 Jupiter) under Ar at a heating
rate of 5 °C min–1. Scanning electron microscopy
(SEM) was carried out on a Zeiss Merlin microscope. Synchrotron X-ray
diffraction (XRD) measurements were performed on I11 beamline of the
Diamond Light Source operating with an X-ray wavelength of 0.826872
Å. The position-sensitive detector was used to collect diffraction
patterns over the temperature range 30–450 °C with a hot-air
blower. Ex situ X-ray powder diffraction measurements
of the electrode materials were performed using a Rigaku Smartlab
diffractometer (Cu Kα). All Rietveld and Pawley refinements
were carried out using the TOPAS-Academic software.29