Jps 9030

XPS measurements were done on pristine and (dis)charged NaKNi₂TeO₆ electrodes to ascertain the valency state upon alkali-ion extraction and reinsertion in NaK half-cells. Electrochemical measurements were stopped upon charging the electrodes at 4.35 V and discharging other electrodes at 1.3 V in the first cycle. The cells were dismantled, and the electrodes carefully removed inside an argon-filled glove box (with water and oxygen concentration maintained below 1 ppm). The electrodes were washed for five times using 25 mm of super-dehydrated acetonitrile (water concentration of <10 ppm) and dried inside the argon-filled glove box, prior to undertaking XPS analyses at Te 3d and Ni 2p binding energies. A hermetically sealed vessel was used to transfer the electrode samples into the XPS machine (JEOL(JPS-9030) equipped with a Mg Kα source) without exposure to air nor moisture. The electrodes were etched by an Ar-ion beam for 10 s in order to eliminate passivation layer at the surface. The accelerating voltage of Ar-etching was fixed at 600 V. The attained XPS spectra were fitted using Gaussian functions and data processing protocols were performed using COMPRO software.

XPS measurements were performed on pristine Ag2Ni2TeO6, Ag2NiCoTeO6, charged Ag2−xNi2TeO6 and charged Ag2−xNiCoTeO6 electrodes to ascertain the valency state upon silver‐ion extraction. The electrodes were intimately washed with super‐dehydrated acetonitrile and dried inside an argon‐filled glove box, prior to undertaking XPS analyses at Ag3d, Co2p, Te3d, and Ni2p binding energies. A hermetically sealed vessel was used to transfer the electrode samples into the XPS machine (JEOL(JPS‐9030) equipped with both Mg Kα and Al Kα sources). For clarity, XPS analyses at Te3d, Ag3d, and Co2p binding energies were conducted using the Al Kα source, whereas the Mg Kα source was used for analyses at Ni2p binding energies. The electrodes were etched by an Ar‐ion beam for 10 s to eliminate the passivation layer at the surface. The attained XPS spectra were fitted using Gaussian functions, and data processing protocols were performed using COMPRO software.

Scanning Electron Microscopy (SEM, JSM 6060 LA, JEOL, Tokyo, Japan) was used to characterize the morphology of the exfoliated samples. The number of graphene layers was determined by atomic force microscopy (AFM, Bruker, Multimode 8, Karlsruhe, Germany) in tapping mode. Raman spectroscopy analysis was also conducted to investigate the bond quality and confirm the number of graphene layers. The SiO₂ (100 nm)/Si substrates were used for all of the above-mentioned characterizations. The substrates were cleaned with acetone in an ultrasonic bath and subsequently rinsed with isopropanol and blown dry using a nitrogen gun. X-ray photoelectron spectroscopy (XPS, JEOL JPS 9030, Tokyo, Japan) analysis was performed to observe the functional groups and oxygen content of the exfoliated samples. Dynamic light scattering and zeta potential measurements (Zetasizer Nano ZS, Malvern, UK) were used to measure the size distribution and the dispersibility of the exfoliated samples.

The electrodeposited Al–W alloy films were mechanically polished to obtain smooth surfaces. The portion of each Cu substrate on which the alloy film was not deposited was covered with KTC-AC-828T masking resin (Kakoki Trading Co., Japan), after which the films were immersed in 0.56 M (3.5 wt.%) aqueous HNO₃ solution at room temperature.
The films were heat treated in a KBF848N1 electric furnace (Koyo Thermo Systems Co., Japan) in air. The films were heated from room temperature to the desired temperature at a rate of 2 °C min⁻¹, held at that temperature for 10 h, and then cooled slowly over several hours to room temperature.
The surface and cross-sectional morphologies of the alloy films were examined by field-emission scanning electron microscopy (FE-SEM), and the elemental compositions of the films were determined by EDX on a SU6600 field-emission scanning electron microscope (Hitachi, Japan) equipped with a Quantax Xflash 4010 detector (Bruker, USA). To prevent charging effects during the SEM analysis, a thin Au coating was deposited onto the samples by sputtering. The crystal structures of the films were determined by XRD analysis using an X’pert PRO-MPD diffractometer (Malvern Panalytical, UK). The XPS spectra of the film surfaces were measured by JPS-9030 (JEOL, Japan) with Mg Kα (1253.6 eV) X-ray source. The spectra in this paper were calibrated using C1s peak at 285.0 eV.

The presence of Ag nanoparticles in the specimens was characterized using X-ray diffraction (XRD) (XRD-6100, Shimadzu), X-ray photoelectron spectroscopy (XPS; JPS-9030, JEOL), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDX) mapping, high-angle annular dark field (HAADF) images, and secondary electron (SE) images (HF-2200, Hitachi). The morphology of kaolinite specimens were also characterized using TEM, SE, and HAADF images. TEM images were also obtained using a JEM-2100 (JEOL). Before microscopic analyses, the samples were dispersed in ethanol, and the dispersions were cast to a copper grid. The surface area of NS-Kaol was determined from the nitrogen adsorption isotherm (Belsorp MINI, MicrotracBEL) using the Brunauer–Emmett–Teller (BET) method.³⁶