Empyrean diffractometer with cu kα radiation

FT-IR was performed on VERTEX70 (Bruker, Germany). XRD was carried out on an Empyrean diffractometer with Cu-Kα radiation (PANalytical B.V., Holland). ¹H NMR was measured on Bruker 500 M (Bruker, Germany) with (methyl sulfoxide)-d₆ as the solvent and tetramethylsilane (TMS) as the internal standard. Elemental analysis was determined by an Elementar Vario EL III (Elementar, Germany). TGA was carried out on a TGA/DSC3+ thermal analysis system (Mettler toledo, Switzerland). The morphology was obtained by a SU8010 SEM equipped with an EDS detector (HITACHI, Japan). UV–vis absorption spectra were recorded on a U-3900 spectrophotometer (HITACHI, Japan). XPS was carried out on a K-Alpha+ X-ray Photoelectron Spectroscopy (Thermo fisher Scientific, America). ICP-OES analysis was carried out on ICP-OES 730 (Agilent, America). IC analysis was carried out on ICS-1100 (DIONEX, America).

The purity, crystalline nature, and microstructure of the as-synthesized powdery sample were investigated by X-ray diffraction (XRD) and transmission electron microscopy (TEM).
For XRD analysis, an Empyrean diffractometer with Cu_Kα radiation from PANalytical (Almelo, The Netherlands), equipped with a hybrid monochromator for Cu and a PIXcel3D detector, was used. Scans were collected on the mildly ground powder, using Bragg–Brentano geometry between 5–80° diffraction angles, with 0.5° incidence angle, under step scan mode (0.04° scanning step size and 3 s acquisition time per scanning step).
TEM investigation was performed using the Tecnai^TM G2 F30 S-TWIN high-resolution equipment from Thermo Fischer Scientific (former FEI, Hillsboro, OR, USA). Data collection was performed in transmission mode, with point and line resolutions of 2 Å and 1 Å, respectively. Before analysis, small amounts of the as-synthesized powdery sample were dispersed in ethanol under sonication for 15 min, then placed onto the carbon-coated copper grid and dried at RT.