K950 carbon evaporator

Elemental analysis for C, H, N and S was performed at the University of Aveiro with a Leco TruSpec 630-200-200 analyzer. PXRD patterns were recorded in transmission mode using a Philips Analytical Empyrean (θ/2θ) diffractometer equipped with a PIXcel1D detector, with automatic data acquisition (X'Pert Data Collector v4.2 software) and monochromatized Cu-Kα radiation (λ = 1.5406 Å). Each sample was mounted between two Mylar foils and then placed in the sample holder. The samples were step-scanned with 0.02º 2θ steps and a counting time of 50 s per step. Scanning electron microscopy (SEM) images were collected using a Hitachi SU-70 microscope operating at 15 kV. Samples were prepared by deposition on aluminium sample holders followed by carbon coating using an Emitech K 950 carbon evaporator. Thermogravimetric analysis (TGA) was performed using a Shimadzu TGA-50 system at a heating rate of 5 ºC min -1 under air. FT-IR spectra were obtained as KBr pellets using a FTIR Mattson-7000 spectrophotometer and recorded in transmission mode from 4000 to 300 cm -1 with a resolution of 4 cm -1 . Raman spectra were recorded on a Bruker RFS100/S FT instrument (Nd:YAG laser, 1064 nm excitation, InGaAs detector). Solid-state 13 C{ 1 H} cross-polarization (CP) magicangle spinning (MAS) NMR spectra were recorded at 100.62 MHz on a Bruker Avance 400 spectrometer using 3.5 µs 1 H 90º pulses, a 2 ms