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7 protocols using rbd upgraded phi 5000c esca system

1

Comprehensive Material Characterization

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The crystal structures of the samples were identified by powder X-ray diffraction performed using a Philips X’pert pro X-ray diffractometer (Cu-Kα radiation, λ = 1.5418 Å) in the 2θ range from 10° to 70°. The morphologies of the different samples were observed with a scanning electron microscope (SEM, JEOL JSM-6700F) and a transmission electron microscope (TEM, JEOL-2010). The chemical element composition was examined quantitatively by an inductive coupled plasma atomic emission spectrometer (ICP-AES) with an emission spectrometer (Optima 2010 DV, Perkin-Elmer). The specific surface area of the pristine sample was measured by the adsorption–desorption of N2 using an ASAP 2020 instrument. X-ray photoelectron spectroscopy (XPS) was carried out using a Perkin-Elmer RBD upgraded PHI-5000C ESCA system. Curve fitting of the XPS spectra was performed using a CasaXPS program and the binding scale was calibrated from the hydrocarbon contamination using the C 1s peak at 284.8 eV. Differential Scanning Calorimetry (DSC) analysis of the different samples in the delithiated state was carried out on an SDT Q600 from ambient temperature to 400 °C at a rate of 10 °C min−1 under air flow.
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2

Physicochemical Characterization of Nanomaterials

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The following are the details of the instrumentation: Agilent 7800 (Hitachi Ltd., Tokyo, Japan) was used for inductively coupled plasma mass spectrometry; JEM-2100F electron microscopy (JEOL, Tokyo, Japan) for high-resolution transmission electron microscopy (HRTEM); Veeco Nano-Scope Multimode IIIa (Veeco, Plainview, NY, USA) for atomic force microscopy (AFM); JEM Zetasizer Nano-ZS90 (Malvern Instruments, Malvern, UK) for hydrodynamic diameter measurement; Cary 50 spectrophotometer (Varian, Palo Alto, CA, USA) for ultraviolet (UV)–visible absorption spectra measurement; F-182 4500 spectrophotometer (Hitachi) for fluorescence measurement; and RBD-upgraded PHI-5000C ESCA system (Perkin Elmer, Waltham, MA, USA) for X-ray photoelectron spectroscopy (XPS).
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3

Comprehensive Characterization of Solid Samples

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Powder XRD patterns of samples were recorded on a Rigaku Miniflex-600 operating at 40 KV voltage and 15 mA current with Cu Kα radiation (λ = 0.15406 nm). The SEM images were taken using a field-emission SEM (JSM-6701F, JEOL) operated at an accelerating voltage of 5 kV. The morphologies of samples were examined by TEM, using a Hitachi-7700 microscope with an accelerating voltage of 100 kV. The high-resolution TEM, HAADF-STEM, and EELS mapping were carried out by JEOL JEM-ARM200F TEM/STEM with a spherical aberration corrector working at 200 kV. The XPS was carried out on a Perkin-Elmer RBD upgraded PHI-5000C ESCA system. Raman scattering spectra were performed with a Renishaw System 2000 spectrometer using the 514.5 nm line of Ar+ for excitation. Elemental analysis of Co in the solid samples was detected by an Optima 7300 DV ICP-AES. The obtained adsorption–desorption isotherms were performed on a Micromeritics Tristar II 3020 M to evaluate the BET-specific surface area.
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4

Structural Characterization of Materials

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Powder X-ray diffraction (XRD) measurements of the products were performed using a Philips X'Pert Pro Super X-ray diffractometer equipped with graphite monochromatized CuKα radiation (λ = 1.54178 Å). Transmission electron microscopy (TEM), and high-resolution TEM (HRTEM) images were recorded on a JEM-ARF200F transmission electron microscope. The high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM) images were taken on a JEOL JEM-ARF200F atomic resolution analytical microscope. The X-ray photoelectron spectroscopy (XPS) measurements were carried out on a PerkinElmer RBD upgraded PHI-5000C ESCA system. The inductively coupled plasma atomic emission spectroscopy (ICP-AES) measurements were made using a PerkinElmer Optima 8000 ICP-AES/ICP-OES spectrometer.
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5

Comprehensive Morphological and Compositional Characterization of Nanomaterials

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The morphology of the particles was observed by scanning electron microscope (SEM, JSM 6700F, JEOL). Transmission electron microscopic (TEM) images and high-resolution transmission electron microscopic (HRTEM) images were carried out on a JEM-2100F field emission electron microscope at an accelerating voltage of 200 kV. The X-ray powder diffraction (XRD) patterns of the products were performed on a Philips X’Pert Pro Super diffractometer with Cu-Kα radiation (λ = 1.54178 Å). The operation voltage was maintained at 40 kV and current at 200 mA, respectively. The X-ray photoelectron spectroscopy (XPS) was carried out on a PerkinElmer RBD upgraded PHI-5000C ESCA system. A Shimadzu spectrophotometer (Model 2501 PC) was used to record the UV–vis diffuse reflectance spectra of the samples in the region of 200 to 800 nm. The electron paramagnetic resonance (EPR) spectra were recorded on a JEOL JES-FA200 EPR spectrometer (140 K, 9064 MHz, 0.998 mW, X-band).
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6

Comprehensive Characterization of Palladium Catalysts

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X-ray powder diffraction (XRD) patterns of samples were carried out by Philips X'Pert Pro Super diffractometer, which was radiated by graphite monochromatized Cu Kα (λ = 1.54178 Å). The operating voltage was maintained at 40 kV, the current was maintained at 200 mA and analyzed in the range of 10° ≤ 2θ ≤ 70°. Scanning electron microscopy (SEM) images were performed on a field-emission scanning electron microanalyzer (JEOL JSM-6700F, 15 kV). Transmission electron microscopy (TEM) and high-resolution TEM (HRTEM), scanning transmission electron microscopy (STEM) images and energy dispersive X-ray spectroscopy (EDX) analysis were measured on FEI Talos F200X operated at 200 kV. The X-ray photoemission spectroscopy (XPS) was performed on Perkin-Elmer RBD upgraded PHI-5000C ESCA system. JEOL JES-FA200 EPR spectrometer was used here to examine the electron paramagnetic resonance (EPR) spectra with the operating parameters 140 K, 9064 MHz, 0.998 mW, X-band. The actual concentration of Pd was analyzed by inductively coupled plasma-mass (ICP-MS) optical emission spectroscopy on the optima 7300 DV, Perkin-Elmer. The reaction conversion measurements were carried out using gas chromatography (GC) (Agilent 7890B).
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7

XPS Analysis of Jute Fabric

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The XPS experiments of jute fabrics were performed using a RBD upgraded PHI-5000 C ESCA system (Perkin Elmer) with MgK␣ radiation (h = 1253.6 eV). The X-ray anode was run at 250 W, and the high voltage was maintained at 14.0 kV with a detection angle of 54 • . Both the entire spectra (0-1100 eV) and the narrow spectra of carbon with significantly higher resolution were recorded using the RBD 147 interface (RBD Enterprises, USA) and the AugerScan 3.21 software. The binding energies were calibrated with the contaminant carbon (C1s = 284.6 eV). The spectrum analysis including background subtraction, deconvolution, integration, and quantitation was carried out by using the RBD AugerScan 3.21 software.
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