Tga sdta851 analyzer

X-ray diffraction (XRD) was conducted using Cu Kα radiation within the range of 10°–70° (GBC MMA diffractometer, λ = 1.5406 Å). The morphology was investigated with a field emission scanning electron microscope (FESEM, JEOL JSM-7500FA) equipped with energy-dispersive X-ray spectroscopy (EDS). In addition, a 200 kV scanning transmission electron microscope (STEM, JEM-ARM 200F) was used with a double aberration-corrector to acquire selected area electron diffraction (SAED) patterns with an image-forming lens system. The annular bright-field (ABF)-STEM images were collected with a STEM-ABF detector, and the angular range of collected electrons for high-angle annular dark-field (HAADF) images was about 70–250 mrad. The EDS mapping was processed by NSS software. TGA was conducted on a Mettler Toledo TGA/SDTA851 analyzer to measure the thermal decomposition behavior of samples in the temperature range from 50 °C to 900 °C with a heating rate of 5 °C min⁻¹. Time of flight secondary ion mass spectrometry (TOF-SIMS) measurements were carried out in negative mode for S and positive mode for Na based on the relative sensitivity factors (RSF) value. A 30 keV, 3 nA Ga⁺ ion beam was utilized to sputter the cycled S@Mn₁-PNC electrode and produce the secondary ions. The analysis of TOF-SIMS data was performed using TOF-SIMS Explorer (Version: 1.3.1.0).

The structures and morphologies of the as-prepared samples were obtained using a Hitachi H-800 TEM and a LEO 1530 SEM. XRD was performed on a Bruker D8-Advance X-ray powder diffractometer. Specific surface areas were measured at 77 K by BET nitrogen adsorption-desorption (Shimadzu, Micromeritics ASAP 2010 Instrument). To investigate the decomposition process of NiCO₃∙Ni(OH)₂ ∙ xH₂O, the as-obtained hydrothermal samples were analyzed by thermogravimetric analysis (TGA, Mettler Toledo TGA-SDTA851 analyzer) from 25 to 500 °C under an air atmosphere with a heating rate of 5 °C/min. To analyze the content of metallic Ni in Ni-NiO, TGA analysis was carried out on the Ni-NiO-5 min samples by first heating them to 300 °C with a heating rate of 5 °C/min and maintaining them at 300 °C for 30 minutes under Ar protection, which can eliminate the effect of adsorbed water; the samples were then heated to 450 °C in air to investigate the oxidation reaction of metallic Ni. X-ray photoelectron spectroscopy (XPS) was carried out on VG ESCA 2000 with Mg Kα as the X-ray source and the C1s peak at 284.6 eV as an internal standard.