Empyrean X-ray powder diffractometer equipped with a Bragg–Brentano
HD mirror and operated at 45 kV and 40 mA using Cu Kα radiation.
The scans were collected in the 2θ range of 15–90°
(step size, 0.033° and time per step, 3.2 s). Raman spectra were
collected with a Thermo Scientific DXR2 Raman spectrometer equipped
with a 532 nm laser using a spot size of 1.8 μm. The spectra
were acquired in the range of 100–3,500 cm–1 with a spectral resolution of 0.964 cm–1. Five
measurements at different locations of the sample with a measurement
time of 100 s were acquired and averaged. FTIR spectroscopy experiments
were performed on self-supporting pellets using a Bruker Alpha II
spectrometer in transmission mode (12 scans, 2 cm–1 resolution) under a N2 atmosphere. TEM measurements were
acquired with a FEI Talos F200X electron microscope operated at 200
kV. BET (Brunauer–Emmett–Teller) surface areas of the
materials were measured from the N2 physisorption isotherms
recorded at 77 K on an Anton Paar Nova 800 apparatus. The samples
were degassed at 300 °C under vacuum (10–3 mbar) for 3
h prior to measurement.