The fabricated samples were characterized by X-ray diffraction (XRD, SmartLab, Rigaku Co., Ltd., Japan) with Cu Kα (λ = 1.5418 Å) radiation operating at 45 kV and 200 mA and by Raman spectroscopy (inVia Raman Microscope, Renishaw Co. Ltd., UK) with a solid-state laser operating at 532 nm to examine the structural features. N2 adsorption/desorption isotherms were recorded on a BELSORP mini II analyzer (MicrotracBEL Corp.) at 77 K in liquid nitrogen to characterize the surface area and pore structure of the adsorbents. The specific surface area (SSA) was determined by the Brunauer–Emmett–Teller (BET) method, and the pore size distribution was calculated from the Barrett–Joyner–Halenda analysis. Morphologies were observed by field-emission scanning electron microscopy (FE-SEM, S-4800, HITACHI High Technologies Co., Ltd., Japan) at an accelerating voltage of 10 kV and by transmission electron microscopy (TEM, JEM-2500SE, JEOL, Japan) at an accelerating voltage of 200 kV. Energy-dispersive X-ray spectroscopy (EDS) and elemental mapping images were obtained on an FE-SEM system equipped with an EDS system (EMAX Energy, Horiba Ltd., Japan). X-ray photoelectron spectroscopy (XPS) was carried out on a PHI 5000 VersaProbe II (ULVAC-PHI, Inc., Japan) with Mg Kα radiation to examine the surface chemistry of materials.
Phi 5000 versa probe 2
Manufactured by Physical Electronics
Sourced in Japan, United States, France
The PHI 5000 Versa Probe II is a high-performance X-ray photoelectron spectroscopy (XPS) system designed for surface analysis. It provides a comprehensive set of capabilities for the characterization of various materials, including thin films, surfaces, and interfaces. The system features a focused monochromatic X-ray source, a versatile sample handling system, and a high-performance electron energy analyzer to deliver accurate and reliable data on the chemical composition and electronic structure of the analyzed samples.
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Lab products found in correlation
Jsm 6610lv scanning electron microscope, by JEOL (5 mentions)
Ultima 4 x ray diffractometer, by Rigaku (5 mentions)
Smartlab, by Rigaku (4 mentions)
Jsm 7800f, by JEOL (3 mentions)
Spm 9700, by Shimadzu (3 mentions)
Asap 2020, by Micromeritics (3 mentions)
Nicolet 6700, by Thermo Fisher Scientific (3 mentions)
Amx 500, by Bruker (2 mentions)
Ifs 48, by Bruker (2 mentions)
D2 phaser, by Bruker (2 mentions)
Aa 7000, by Shimadzu (2 mentions)
Jsm 7401f, by JEOL (2 mentions)
Dimension fastscan, by Bruker (2 mentions)
Labram hr800, by Horiba (2 mentions)
S 4800, by Hitachi (2 mentions)
Spectrum two pe, by PerkinElmer (2 mentions)
Single reflection diamond znse, by PerkinElmer (2 mentions)
Alkα x ray radiation source, by Physical Electronics (2 mentions)
Belsorp mini 2 analyzer, by Microtrac (1 mentions)
Jem 2500se, by JEOL (1 mentions)
87 protocols using phi 5000 versa probe 2
1
Comprehensive Structural Characterization of Fabricated Samples
2
Comprehensive Characterization of Samples
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The properties of the samples were characterized using several techniques. The surface morphology of the samples was observed using field emission scanning electron microscopy (FESEM, Hitachi S-4800, Hitachi, Krefeld, Germany). The surface structure of the samples were probed by N2 adsorption/desorption isotherms measured at −196 °C, carried out using an ASAP 2020 (Micromeritics, Norcross, GA, USA) accelerated surface and porosimetry analysis system. X-ray photoelectron spectroscopy (XPS) was a technique which analyzed the elements constituting the sample surface, its composition, and chemical bonding state by irradiating X-rays on the sample surface, and measuring the kinetic energy of the photoelectrons emitted from the sample surface. The XPS spectra of all samples were obtained using a spectrophotometer (PHI 5000 VersaProbe II, ULVAC-PHI, Kanagawa, Japan), where the scanning X-ray monochromator (Al Anode, hν = 1401 eV) was used and the information on elements within a few nanometers of the sample surface could be obtained. For calibration purposes, the C1s electron binding energy that corresponds to graphitic carbon was set at 284.6 eV. A nonlinear least squares curve-fitting program (XPSPEAK software, version 4.1, The Chinese University of Hong Kong, Hong Kong, China) was used for deconvolution of the XPS spectra.
3
Comprehensive Characterization of CoMoS Catalysts
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Example 3
Characterization of the Activated CoMoS Catalysts
Textural properties of the catalysts were evaluated via N2 adsorption-desorption isotherm analysis at 77 k using a Micromeretics ASAP 2020. The catalysts (approximately 0.1 g each) were initially degassed under flowing argon at 523 k for 2.5 h. The BET method was used to calculate the surface area, whereas absorption branch of BJH method was applied to calculate the pore size and pore volume of the catalysts.
FTIR spectra of the catalysts were recorded on a Nicolet 6700 FTIR spectrometer with a wavelength range of 400-4000 cm−1. The FTIR sample pellets were prepared using a mixture of the respective catalyst and KBr at a weight ratio of 1:100.
Catalyst crystallinity and the distribution of CoMo on the silica support were determined by scanning the catalysts' X-ray diffraction pattern between 20 to 80° 2θ at 40 kV and 40 mA using a Rigaku Ultima IV X-ray diffractometer.
Surface morphology of the catalysts was imaged using a JEOL JSM-6610LV scanning electron microscope. Element mapping with the corresponding EDX spectrum were recorded using an energy dispersive X-ray spectrometer.
The degree of Mo sulfidation of the catalysts due to different activation conditions were determined by X-ray photoelectron spectroscopy (XPS) using a PHI 5000 Versa Probe II, ULVAC-PHI Inc. spectroscope.
4
Spectroscopic Characterization of Samples
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FT-IR spectrum was recorded on Bruker IFS 48 (Bruker, Ettlingen, Germany) using Thermo Scientific iD5 Diamond ATR accessory (Thermo Fisher Scientific, Waltham, MA, USA). 1H NMR spectra were measured on Bruker AMX 500 spectrometer (1H, 500.14 MHz) in D2O:DMSO (3:2 v/v) mixture at RT. XPS measurements were carried out using a PHI 5000 Versa Probe II (ULVAC-PHI, Chigasaki, Japan) spectrometer with a monochromatic Al Kα radiation source (E = 1486.6 eV). A dual-beam charge compensation was used to avoid possible charging of samples. High resolution spectra were recorded with the analyzer pass energy set to 46.95 eV. All binding energies were corrected to C–C line at 284.8 eV. Deconvolution of obtained spectra was done with PHI MultiPak software. The spectrum background subtraction was done using the Shirley method.
5
XPS Analysis of Photocatalytic Reduction
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The XPS analysis was performed using a ULVAC-PHI PHI 5000 VersaProbe II under Al Kα radiation (hν = 1486.6 eV, 15 kV, 25 W). The peak positions were calibrated by the W4f7/2 (35.60 eV) of W6+ atoms in POMs, and the baseline was subtracted by the Shirley method. The curve fitting was performed with the spin–orbit separation ΔEP(W4f5/2–W4f7/2) of 2.1 eV and the intensity ratio I(W4f5/2)/I(W4f7/2) of 0.75.16 (link) The ratio of Lorentzian to Gaussian varied in the range of 50 ± 5%. The sample was prepared as follows: hydrogen gas was bubbled into the aqueous solution (20 mL) containing I (0.05 mM) and IIox (0.25 mM) for 10 min. The UV-vis spectrum of the resulting solution was measured after ca. 1 h incubation at 323 K, showing that the yield of IIred reached to >99%. The resulting solution was dried in vacuo to give a dark blue powder, which was used for the measurement.
6
X-ray Photoelectron Spectroscopy Analysis
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X-ray photoelectron spectroscopy (XPS) measurements were performed using a PHI 5000 Versa Probe II (ULVAC-PHI, Chigasaki, Japan) spectrometer equipped with an Al Kα radiation source (E = 1486.6 eV). The operating pressure in the analytical chamber was less than 3 × 10−7 Pa. High resolution spectra were recorded with the analyzer pass energy set to 49.95 eV. A dual-beam charge neutralizer was used to compensate the charge-up effect. All binding energies were corrected to C–C line at 284.8 eV. The spectrum background subtraction was done using the Shirley method. Data analysis software from PHI MultiPak was used to calculate elemental compositions from the peak areas.
7
X-ray Photoelectron Spectroscopy Analysis of Ti64(Sr+Ag) and SBA2-Ag Surfaces
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The chemical composition of the surfaces of Ti64(Sr+Ag) and SBA2-Ag samples was also analyzed by X-ray photoelectron spectroscopy (XPS; XPS, PHI 5000 Versaprobe II, ULVAC-PHI, Inc., Kanagawa, Japan) using an Al–Ka radiation line as the X-ray source. The take-off angle was set at 45° so that the system is able to detect photoelectrons to a depth of 1–5 nm from the surface. The binding energy of the obtained spectra was calibrated by reference to 284.6 eV of the C1s peak, which is attributed to the CH2 groups. The peak profile analysis of the Ag region was performed by using the National Institute of Standards and Technology (NIST) database: Ag+-20667-12-3; Ag0 7440-22-4. The peak profile analysis of the Ag region obtained on a metal Ag foil is reported as a reference.
8
Comprehensive Characterization of Carbon Dots
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Fourier transform infrared (FT-IR) spectra were acquired on a TENSOR27 FTIR spectrometer (Bruker, Germany) in the wavenumber range from 4000 cm−1 to 400 cm−1. The ultraviolet-visible (UV-vis) spectrogram was conducted on a UV-2550 spectrophotometer (Shimadzu, Japan). The fluorescence spectra were obtained by G9800A Cary Eclipse fluorescence spectrophotometer (Agilent, USA). X-ray photoelectron spectroscopy (XPS) characterization was performed with PHI5000 VersaProbe-II with monochromatized Al Kα radiation (ULVAC-PHI, Japan). The size and the morphology of carbon dots were analyzed under a TecnaiG2 F30 S-Twin (FEI, USA) transmission electron microscope. The pH was adjusted with HCl or NaOH solutions and monitored by employing a digital pH-meter (PHS-3, Shanghai, China).
9
Characterization of Cesium-Manganese Oxide Powders
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Phase of the obtained powders were characterized by powder X-ray diffractometer (XRD: D2 Phaser, Bruker with Cu Kα). To calculate the change in the interlayer distance, powder X-ray diffraction patterns of the samples were additionally collected with an addition of KCl as an internal standard. The patterns were then used to calculate interlayer distances by Le Bail method using a TOPAS software. Scanning electron microscope (SEM: FEI quanta 450) and transmission electron microscope (TEM: JEOL2100plus, operated at 200 keV) were used to investigate the sample morphology, composition, and elemental distribution. The Cs : Mn mole ratio was determined by Inductively coupled plasma-optical emission spectrometry (ICP-OES). BELSORP-mini II surface area and pore size analyzer, Bel-Japan, was used to study the Brunauer–Emmett–Teller (BET) surface areas. The chemical composition of the prepared samples was confirmed by X-ray photoelectron spectroscopy (XPS: PHI5000 VersaProbe II, ULVAC-PHI) with a monochromatic Al Kα excitation source (1486.6 eV).
10
XPS Analysis of Freeze-Dried Samples
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XPS
spectra were recorded on each freeze-dried sample using a PHI 5000
VersaProbe II (ULVAC-PHI, Inc., Chigasaki, Japan) and monochromatic
Al-Kα radiation (hϖ = 1486.6 eV) with a 128-channel hemispheric
analyzer, FAT mode. The acquisition conditions were as follows: high
resolution (C 1s, N 1s, P 2p regions): step 0.0500 eV; time per step
50 ms; X-ray source with beam ⌀ 200 μm, 50 W, 15 kV;
45° angle, Pass Energy 23,500 eV; 20 min/region; charge compensation
with Ar + and e–. The fitting was done using the model Gauss–Lorentz,
Shirley background, with the software Multipak 9.9.0 (ULVAC-PHI, Inc.).
spectra were recorded on each freeze-dried sample using a PHI 5000
VersaProbe II (ULVAC-PHI, Inc., Chigasaki, Japan) and monochromatic
Al-Kα radiation (hϖ = 1486.6 eV) with a 128-channel hemispheric
analyzer, FAT mode. The acquisition conditions were as follows: high
resolution (C 1s, N 1s, P 2p regions): step 0.0500 eV; time per step
50 ms; X-ray source with beam ⌀ 200 μm, 50 W, 15 kV;
45° angle, Pass Energy 23,500 eV; 20 min/region; charge compensation
with Ar + and e–. The fitting was done using the model Gauss–Lorentz,
Shirley background, with the software Multipak 9.9.0 (ULVAC-PHI, Inc.).
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