Supra 40

The samples were characterized by different analytic techniques. XRD was performed on a Philips X'Pert Pro Super X-ray diffractometer equipped with graphite-monochromatized Cu Ka radiation (λ = 1.54178 Å). Scanning electron microscope (SEM, Zeiss Supra 40) and JEOL 2010F(s) TEM were applied to investigate the size and morphology. The HRTEM images, EELS, SAED, and EDX elemental mappings were taken on JEMARM 200F Atomic Resolution Analytical Microscope with an acceleration voltage of 200 kV. XPS was performed by an X-ray photoelectron spectrometer (ESCALab MKII) with an excitation source of mg Kα radiation (1253.6 eV). ICP data were obtained by an Optima 7300 DV instrument. Ultraviolet photoelectron spectroscopy was carried out at the BL11U beamline of National Synchrotron Radiation Laboratory in Hefei, China. The X-ray absorption spectra of Ni and S K-edges were obtained at the beamline 4B7A station of Beijing Synchrotron Radiation Facility (China).

XRD was performed on a Japan Rigaku DMax-γA X-ray diffractometer with Cu Kα radiation (λ = 1.54178 Å). The morphology of the samples was investigated by SEM (Zersss Supra 40) and TEM (JEOL 2010F(s)). The STEM and HRTEM images, SAED and EDX elemental mapping were taken on JEMARM 200 F Atomic Resolution Analytical Microscope with an acceleration voltage of 200 kV. SEM-EDX was determined by GeminiSEM 500 with an Oxford Aztec series X-ray energy spectrum. Raman spectra was measured on a Raman microscope (HORIBA) with a 785 nm excitation laser. ICP-AES data were obtained by an Optima 7300 DV instrument. N₂ adsorption/desorption isotherms were recorded on an ASAP 2020 accelerated surface area and a porosimetry instrument (Mictromeritics), equipped with an automated surface area, at 77 K by using Barrett−Emmett−Teller calculations. XPS was taken on an X-ray photoelectron spectrometer (ESCALab MKII) with an X-ray source (Mg Kα hυ = 1253.6 eV).