Alpha 300 confocal raman spectrometer

The powder X-ray diffraction (XRD) were obtained using Rigaku X-ray diffractometer with X-ray source of wavelength λ = 0.15406 nm at 40 kV voltage and 30 mA current. The XRD data were recorded in the range of 2θ values from 5° to 90° in step size of 0.016°. The Raman spectra were recorded with WITec alpha 300 Confocal Raman spectrometer using Nd:YAG laser as excitation source of wavelength 532 nm. The morphology of the synthesized sample was studied using field emission scanning electron microscopy (FESEM, FEI Quanta 200) and transmission electron microscopy (TEM, Technai G-20). The sample preparation for TEM was done by ultrasonicating the sample in ethanol and drop casted over carbon coated 200 mesh copper grid. Thermo gravimetric analysis (TGA) of the synthesized sample was carried out using SDTQ600 TA instruments from room temperature to 1000 °C with a heating rate of 20 °C min⁻¹ in zero air atmosphere. The oxidation state of the elements of the sample was confirmed by X-ray photoelectron spectroscopy carried out using SPECS instrument and PHOIBOS 100MCD as the analyzer.