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26 protocols using k alpha xps spectrometer

1

XPS Characterization of Material Surfaces

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XPS measurements were performed using a K-Alpha+ ​XPS spectrometer (ThermoFisher Scientific, East Grinstead, UK). Data acquisition and processing using the Thermo Avantage software is described elsewhere [34] . All samples were analyzed using a microfocused, monochromated Al Kα X-ray source (400-μm spot size). The K-Alpha+ ​charge compensation system was used during analysis, using electrons of 8-eV energy ​and low-energy argon ions to prevent any localized charge buildup. The spectra were fitted with one or more Voigt profiles (BE uncertainty: ± 0.2 ​eV) and a Shirley background. Scofield sensitivity factors were applied for quantification [35] . All spectra were referenced to the C 1s peak (C–C, C–H) at 285.0-eV binding energy controlled by means of the well-known photoelectron peaks of metallic Cu, Ag, and Au, respectively. The K-Alpha ​+ ​snapmap option was used to image an area of 3 ​× ​3 ​mm with an X-ray spot of 200 ​μm (5 iterations were run to reach a better statistic).
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2

Characterization of Bimetallic Nanoparticles

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We determine the size and morphology of the Co, Pt, and PtCo nanoparticles by a JEOL JEM-2100 transmission electron microscopy (TEM) operated at 200 kV. We use an energy dispersive X-ray spectroscopy (EDX) analyzer attached to the TEM operated in the STEM mode to analyze the compositions of the as-prepared nanoparticles. We record the powder X-ray diffraction (XRD) patterns on a Bruker D8 diffractometer using Cu Kα radiation (λ = 0.154056 nm), and obtain the X-ray photoelectron spectra (XPS) of the components in the nanoparticles using a Thermo Scientific K-Alpha XPS spectrometer.
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3

Comprehensive Membrane Characterization Techniques

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The morphology of membranes was measured by a scanning electron microscope (SEM, SUPRA 55 SAPPHIRE Carl Zeiss, Oberkochen, Germany). The structure of membranes was tested by using a Rigaku Ultima IV X-ray powder diffractometer (XRD) with a Cu Kα target (λ = 1.54056 Å) at a scanning speed of 5° min−1 from 10 to 65° (40 kV and 40 mA). The chemistry of membrane samples was analyzed by a Fourier transform infrared spectrometer (FTIR, Thermo Scientific, Nicolet Magna 550, Waltham, MA, USA) in the scanning range of 400–4000 cm−1 with a resolution frequency of 2 cm−1 for 64 times scan. X-ray photoelectron spectroscopy (XPS) measurements were carried out on a Thermo Scientific K-Alpha XPS spectrometer using Al Kα X-ray source for radiation. The mechanical properties of membranes were characterized by using a CMT6103 electronic universal test machine from MTS at room temperature at a rate of 2 mm min−1. The thermal stability of PVC powder, PVC-P4VP and PVC-P4VP/PA membranes was measured using a thermogravimetric analyzer (TGA, STA449F3, Netzsch, Selb, Germany) with a heating rate of 10 °C min−1 in nitrogen.
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4

Comprehensive Nanostructure Characterization

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The images of transmission electron microscopy (TEM) and high-resolution TEM (HRTEM) were taken using a JEOL JEM-2010F electron microscope operated at 200 kV. High-angle annular dark-field scanning TEM imaging (HAADF-STEM) was performed on an aberration-corrected JEM-ARM 200F operated at 300 kV, which provides a nominal image resolution of 0.07 nm. An energy dispersive X-ray spectroscopy (EDX) analyzer attached to the aberration-corrected JEM-ARM 200F operated in the STEM mode was used to analyze the element distributions of the obtained core-shell nanostructures. Powder X-ray diffraction (XRD) patterns of the samples were recorded by a Bruker D8 diffractometer using Cu Kα radiation (λ = 0.154056 nm), and the X-ray photoelectron spectra (XPS) were collected using a Thermo Scientific K-Alpha XPS spectrometer. The ICP-AES test was conducted on Thermo Scientific 6300 to determine the accurate content of the corresponding component in as-prepared core-shell samples.
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5

Structural and Surface Analysis of Materials

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The powder X-ray diffraction (XRD) measurements were recorded on a Rigaku Dmax/Ultima IV diffractometer with monochromatized Cu Kα radiation (λ = 1.5418 Å). The morphologies were observed by scanning electron microscopy (JSM-6530LV, Rigaku Japan). The surface composition and electronic structure were examined by X-ray photoelectron spectroscopy (XPS) on a ThermoFisher K-Alpha XPS spectrometer equipped with an Al Kα X-ray source.
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6

Comprehensive Physicochemical Characterization

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Bruker‐AXS D8 Advance system with a Cu Kα radiation was conducted on measuring the crystal phase with PXRD in the 2θ range from 10° to 90°. Renishaw inVia confocal Raman microscope provision with an argon ion laser beam was implemented to test Raman spectra. Netzsch Thermo Microbalance TG 209 F1 Libra was employed to observe TGA from ambient temperature to 900 °C with a heating rate of 5 °C min−1 under nitrogen flow. Belsorp max gas sorption analyzer was used to analyze the sorption isotherms at 77 K. K‐Alpha+ XPS spectrometer (Thermo fisher Scientific, USA) was operated using Al Kα radiation to evaluate XPS and the elemental compositions. Moreover, FESEM (TESCAN Maia 3, Czech) and TEM (FEI Talos F200X, USA) with high‐angle annular dark‐field (HAADF) STEM and EDS (JEM2010‐HR, 200 kV) were utilized to study the surface morphology and architecture.
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7

XPS and Raman Analysis of Laser-Induced Carbon Electrodes

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The composition analysis of the laser-induced carbon electrodes was done using X-ray photoelectron spectroscopy (XPS). The measurements were performed using a K-Alpha+ XPS spectrometer (Thermo Fisher Scientific, East Grinstead, UK). For the data acquisition and processing was used a Thermo Avantage software, described elsewhere49 (link). All samples were analyzed using a microfocused, monochromated Al Kα X-ray source (30–400 µm spot size). The spectra were fitted with one or more Voigt profiles (binding energy uncertainty: +/−0.2 eV). The analyzer transmission function, Scofield sensitivity factors50 (link), and effective attenuation lengths (EALs) for photoelectrons were applied for quantification. EALs are calculated using the standard TPP-2M formalism51 (link). All spectra were referenced to the C1s peak of hydrocarbon at 285.0 eV binding energy controlled by means of the well-known photoelectron peaks of metallic Cu, Ag, and Au. Sputter cleaning was performed using an Ar1000+ cluster ion beam at 8 keV and 30° angle of incidence which did not harm the electrodes. Raman spectroscopy was performed with the Raman microscope Bruker Senterra. The power of the laser was 5 mW with a wavelength of 532 nm. The integration time was 60 s with 2 co-additions (2 × 30 s) for each measurement spot.
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8

X-ray Photoelectron Spectroscopy Analysis

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XPS measurements were performed using a K-Alpha+ XPS spectrometer (ThermoFisher Scientific, UK) operating at a base pressure of 1.0 × 10−7 Pa. The data acquisition and processing were performed using the Thermo Avantage software. All samples were analyzed using a microfocused, monochromated Al Kα X-ray radiation (400 µm spot size) with a pass energy of 150 eV for survey and 50 eV for high-resolution core level spectra. The X-ray angle of incidence was 30° and the emission angle was along the surface normal. The K-Alpha charge dual compensation system was employed during analysis, using electrons and low-energy argon ions to prevent any localized build-up of charge. The measured high-resolution spectra were fitted with Voigt profiles. The analyzer transmission function, Scofield sensitivity factors, and effective attenuation length for photoelectrons were applied for quantification. All spectra were referenced to the adventitious C 1s peak at a binding energy (BE) of 285.0 eV. The BE scale was controlled on standards of poly(ethylene terephthalate) and metallic Cu, Ag, and Au.
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9

Characterization of Nanostructured Materials

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All the reagents were purchased from Aldrich and Merck and were used without any purification. Crystalline structures of the samples were evaluated by X-ray diffraction (XRD) analysis on a Bruker D8 Advance Diffractometer with CuKα radiation at 40 kV and 20 mA. Fourier transform infrared (FT-IR) spectra were recorded using KBr pellets with a PerkinElmer 65 spectrophotometer in the range of 400–4000 cm−1. TEM images at an accelerating voltage of 80 KV were taken with a Zeiss-EM10C. Morphology and particle dispersion was investigated by field emission scanning electron microscopy (FESEM) (Cam Scan MV2300). Chemical composition of the prepared nanostructures was measured by EDS (Energy Dispersive X-ray Spectroscopy) performed in SEM. The UV-Vis absorbance spectra were recorded using a double beam UV-visible spectrophotometer (PG Instrument, T80+), equipped with 10 mm quartz cuvettes. The spectra were obtained using a ThermoFisher Scientific K-Alpha XPS spectrometer. Survey spectra were initially obtained at low energy resolution (pass energy −200 eV) followed by the main regions of interest at higher resolution (pass energy −25 eV). A monochromatic Al Kα X-ray was used, with a nominal spot size of 400 μm.
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10

Chemical Bonding Analysis of Drug-Coated PCL Scaffold

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The chemical bonding states and atomic concentrations in the samples before and after the drug coating on the porous PCL scaffold were examined by X-ray Photoelectron Spectroscopy (XPS) (K-Alpha+ XPS Spectrometer, Thermo Scientific, Tokyo, Japan) using a hemispherical electrostatic energy analyzer and an Al Kα X-ray source. The base pressure in the sample chamber was controlled to 10−9 Torr. The measured spectra were displayed as plots of the number of electrons versus the electron binding at a fixed, small energy interval. Peak area and peak height sensitivity factors were used for quantification.
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