Escalab xi x ray photoelectron spectrometer

The morphology was analyzed by field emission SEM (TESCAN MAIA3LMH) and TEM (Talos F200X). XRD patterns were recorded on a Shimadzu XRD-6100 with Cu Kα radiation. XPS spectra were collected on a Thermo Fisher ESCALAB Xi+ X-ray photoelectron spectrometer. All the XPS data were calibrated by shifting the C 1s peaks to 284.8 eV. The Raman spectra were measured on a Renishaw inVia Qontor Ramna microscope using laser excitation wavelength of 633 nm for copper and copper oxide detection and 532 nm for Ni(OH)_x species detection. The concentration of nitrate in the electrolyte was quantified on a Thermo Scientific Dionex Integrion. The EPR measurements were performed on a JEOL JES-FA200 spectrometer. The ¹H NMR spectra were measured on a AVANCE III HD 600 MHz NMR spectrometer. The mass spectra were collected on a GCMS-QP2020NX Shimadzu instrument. The contents of Ni and Cu elements in the Ni(OH)_x/Cu samples were measured on a NexION 350D inductively coupled plasma mass spectrometer (ICP-MS).

The morphology and size of N,S-CDs were analyzed by transmission electron microscope (HT-7700, Japan) operated at 100 kV. Fourier transform infrared (FT-IR) spectra were obtained on a Thermo Scientific Nicolet iS5 IR spectrometer (USA) ranging from 400 to 4000 cm⁻¹ using attenuated total reflection (ATR) accessory. XPS analysis was measured by Thermo Scientific ESCALAB Xi⁺ X-ray photoelectron spectrometer (USA) using Al Kα as the excitation source (1486.6 eV).

XPS measurements were performed
in an ESCALAB Xi+ X-ray photoelectron
spectrometer (ThermoScientific) employing a monochromated Al Kα
Xray source (hν = 1486.6 eV). High-resolution spectra were collected
using an analysis area of 650 × 650 μm² and
a 20 eV pass energy. The C(1s) level (284.8 eV) was taken as the reference
binding energy. The sample was prepared by suspending an aliquot of
the nontronite sample in ∼1 mL bidistilled water inside the
glovebox, agitated by hand, and then pipetting an aliquot of 0.5 mL
of the suspension onto a carbon sample holder. The suspension was
then dried at 35 °C in an oven in the glovebox. The dried sample
was sealed in an airtight jar, itself sealed in an airtight aluminum
bag. It was then taken out of the glovebox and opened just before
being positioned in the measurement apparatus, where it was immediately
subjected to vacuum conditions. A charge neutralizer was used for
data collection, being monitored using the C(1s) signal corresponding
to adventitious carbon.^{54 (link),55 (link)} C(1s), Fe(2p), O(1s),
Si(2p) spectra were collected and fitted using the Avantage software
(ThermoScientific) via a Lorentzian–Gaussian peak with a default
value of 30% Lorentzian contribution, and a smart background removal
was used for all spectra.

A JEOL 2200FS HRTEM operated at 200 kV, was used to obtain the STEM images. A Cary 50 UV-Vis Spectrophotometer from Agilent Technologies and a JASCO J-815 CD spectropolarimeter were used for UV-Vis spectrum and CD spectrum characterizations, respectively. The XRD data were measured with a Bruker D8 with IµS-XR Source. The zeta potential and titration were conducted with a Malvern Zetasizer Nano ZSP equipped with an Autotitrator. FTIR spectra were measured with a Cary 630 FTIR Spectrometer from Agilent. XPS data were measured by ESCALAB Xi+ X-ray Photoelectron Spectrometer from ThermoFisher Scientific. Solid-state NMR spectra were recorded by a JNM-ECZ600R from JEOL.
UV-titration was conducted by coupling the titration experiments with an Ocean optics USB2000 fiber optic spectrometer. Titration experiments were performed using a commercial, computer-controlled system from Metrohm (Filderstadt, Germany), operated with the custom-designed software Tiamo (v2.2). The setup consists of a titration device (Titrando 809) that regulates two dosing units (Dosino 807) capable of dispensing titrant solution in steps as small as 0.2 µL.
CD titration was conducted by manual addition of concentrated KOH solutions into the cuvettes followed by the measurement of the CD spectrum. The pH was recorded by a Mettler Toledo pH meter. All the pH electrodes were calibrated before use.