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9 protocols using s 4800 scanning electron microscope

1

Characterization of Nanostructured Materials

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The nanostructures of the samples were observed by Hitachi S-4800 scanning electron microscope (SEM) and JEOL JEM-1400 Plus transmission electron microscope (TEM). Thermogravimetric analysis (TGA) was performed by using PerkinElmer PE Pyris1 TGA thermogravimetric analyzer. X-ray photoelectron spectroscopy (XRD) patterns were recorded on a D-MAX 2200 VPC diffractometer using Cu K radiation (40 kV, 26 mA). X-ray photoelectron spectroscopy (XPS) measurements were carried out with a Thermo SCIENTIFIC ESCALAB 250Xi instrument. Raman spectra were tested with HORIBA JY LabRAM HR Evolution. Fourier-transform infrared (FTIR) measurements of the samples were performed with IR spectroscopy (Bruker TENSOR 27), using KBr disk method.
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2

Comprehensive Nanoparticle Characterization Methods

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The nanoparticles are imaged by using a Hitachi S‐4800 scanning electron microscope and a JEOL JEM‐2010 Luminography (Fuji FDL‐5000) Ultramicrotome (CRX) transmission electron microscope. High‐resolution transmission electron microscopy (HRTEM) and energy‐dispersive X‐ray (EDX) analysis were measured by using a JEOL JEM‐2100F microscope. Samples were prepared for TEM by concentrating the nanoparticle mixture through centrifugation (two times, 10 min, 6,000 rpm), followed by resuspension in nanopure water (100 μL) and immobilization of 10 μL portions of the solution on TEM grids (Ted Pella, Inc. Formvar/Carbon 400 mesh, copper coated). UV/Vis spectra were recorded using a UV‐1800 (Shimadzu, UV/Vis spectrophotometer). Gas adsorption isotherms are obtained by using BELSORP‐mini II (BEL Japan, Inc.). The gases used throughout adsorption experiments are highly pure (99.999 %). All samples are activated by thoroughly rinsing, followed by drying under vacuum for 24 h prior to the gas sorption measurements.
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3

Comprehensive Characterization of Nanomaterials

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The morphological characterization of the as-prepared sample was performed with a Hitachi S-4800 scanning electron microscope (SEM) and a JEOL-2100F transmission electron microscope (TEM) at an acceleration voltage of 200 kV. Raman spectra were measured on an HR800 (Horiba Jobin Yvon) with a 514.5 nm laser source. XRD analysis of the sample was done using an XRD Bruker D8-ADVANCE. X-ray photoelectron spectroscopy (XPS) was performed using a Kratos XSAM 800 spectrometer (Manchester, UK). Nitrogen adsorption–desorption isotherms were obtained at 77 K on an Autosorb IQ Quantachrome Analyzer. Before the adsorption measurements, all samples were degassed at 200 °C for more than 6 h under high vacuum. The SSA was calculated by the Brunauer–Emmett–Teller (BET) method. The pore size distribution was analyzed by the nonlocal density functional theory (DFT) method.
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4

Characterization of Crystalline Structures

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The morphology and microstructure of the samples were characterized by a S-4800 scanning electron microscope (SEM) and a JEOL 2010 field-emission transmission electron microscope (TEM). The crystalline structures of the samples were performed on a Rigaku D/Max-2500 X-ray diffractometer with Cu Kα radiation (λ = 0.1542 nm) in the 2θ range from 5° to 90°. Fourier transform infrared (FT-IR) spectra were recorded on a Bruker Optics TENSOR 27 spectrometer using KBr pellets in the wave-number range of 400–4,000 cm−1.
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5

Characterization of Aerogel Morphology

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The morphology of the aerogels was observed by using HITACHI S-4800 scanning electron microscope (SEM) and transmission electron microscope (TEM: JEM-1200EX, JEOL, Japan). X-ray photoelectron spectroscopy (XPS) was carried out in Escalab 250Xi instrument. X-ray diffraction (XRD) measurements were performed in a X-ray diffractometer (X'Pert PRO, PANalytical B.V.) with the use of Cu Kα radiation (λ = 1.5418 Å) at 4° min−1 scanning speed in the 2θ range from 10–90°. Thermogravimetric analysis (TGA) and differential thermal analysis (DTA) were performed on a TA-Q 500 TGA instrument. Samples were pretreated at 100 °C for 30 minutes, and then heated to 1000 °C at a rate of 10 °C min−1 in air. Fourier Transform Infrared Spectroscopy (FT-IR) was recorded on Nicolet 5700 spectrophotometer using KBr pellets containing 1% weight sample in KBr. The nitrogen adsorption–desorption measurements (Quantachrome Instrument Corp) were used to obtain the nitrogen physisorption isotherms at 77 K. Surface areas were evaluated using the Brunauer–Emmett–Teller (BET) method from the adsorption branch of the isotherm. The pore size distributions were calculated according to the Barrett–Joyner–Halenda (BJH) model, and the average pore diameters and cumulative pore volumes were calculated using the desorption branch of the isotherm.
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6

Ultrasound-Assisted Synthesis of Rare-Earth Nanomaterials

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All ILs were purchased from Kekaite Co. (Lanzhou, China). Reagent grade depleted Pr(NO3)3 and 3,3,5,5-tetramethylbenzidine (TMB) were obtained from Macklin Co. Ltd. (Shanghai, China). The trans-resveratrol was purchased from Solarbio Life Science (Beijing, China). All other chemicals, including hydrazine hydrate, ethylenediamine, H2O2 and ethanol, were of analytical grade and used without further purification.
Ultrasound synthesis was assisted by an ultrasonic homogenizer (220 V, 950 W) (Ningbo Scientz Biotechnology Co., Ltd.). Powder X-ray diffraction (XRD) analyses were performed on a Bruker D8 Advance diffractometer with Cu Kα radiation, and scanning electron microscopy (SEM) observations were performed with a Hitachi S-4800 scanning electron microscope, and the morphology and sizes of as-prepared materials were analyzed with JEOL 2100 high resolution transmission electron microscope (HRTEM) (JEOL, Japan). An EMGA-920 Oxygen Elemental Analyzer (HORIBA, Japan) was used to determine the oxygen content. The chemical composition of the products was examined with X-ray photoelectron spectrometer (XPS, ESCALAB 250Xi, ThermoFisher). UV-Visible absorption spectra were recorded on a UV-A390 spectrometer (AOE Instruments, Shanghai, China) with 1.0 cm path length.
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7

Photoelectrochemical Characterization of Modified ITO

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The SEMs were acquired using a Hitachi S-4800 scanning electron microscope (Japan) while TEMs were recorded using a JEM-2100 TEM instrument (JEOL, Japan). The UV-vis absorption spectra were obtained using a UV-3600 UV-vis-NIR spectrophotometer (Shimadzu Co., Kyoto, Japan). Photoelectrochemical measurements were performed with a home-built photoelectrochemical system. A 500 W Xe lamp equipped with a monochromator was used as the irradiation source. The photocurrent was measured on a CHI 630D electrochemical workstation (CH Instruments, Austin, TX). A grating spectrometer Omni-λ1509 (Beijing Zolix Instruments CO., LTD) was used to obtain a continuous wavelength spectrum. All modified processes were performed at 37 °C, and all PEC experiments were carried out at room temperature using a conventional three-electrode system, with a modified ITO electrode as the working electrode, a platinum wire as the counter electrode and a saturated Ag/AgCl electrode as the reference electrode.
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8

Comprehensive Structural Characterization of Products

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The morphology and structure of products were measured with a Hitachi S-4800 scanning electron microscope (SEM) and JEOL JEM-2010 transmission electron microscope (TEM). High-resolution TEM (HRTEM), energy-dispersive X-ray (EDX), high-angle annular dark-field scanning transmission electron microscopy (HAADF-STEM), and elemental mapping measurements were carried out on a FEI Tecnai G2 F20 microscope, which was built as an accessory on the JEOL JEM-2100F. The Fourier transform infrared (FTIR) spectra were obtained with a Nicolet 520 SXFTIR spectrometer. The Brunauer–Emmett–Teller (BET) specific surface area and pore size distribution were examined at 77 K using a Micromeritics ASAP 2050 system. The phase purity and crystallinity of the products were confirmed by X-ray diffraction (XRD) on a Model D/max-rC X-ray diffractometer using Cu Kα radiation source (λ = 1.5406 Å) and operating at 40 kV and 100 mA. X-ray photoelectron spectroscopy (XPS) tests were performed on a Thermo VG Scientific ESCALAB 250 spectrometer with a monochromatic Al Kα X-ray source (1486.6 eV photons). The binding energy was trued with respect to C1s at 284.6 eV.
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9

Characterization of Zr-Phy-DES Material

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FT-IR spectra were recorded on Bruker Tensor 27 IR spectrometer using the KBr pellet method. XPS measurements were carried out on an ESCAL Lab 220i-XL specrometer under a pressure of ∼3 × 10−9 mbar (1 mbar = 100 Pa). XRD measurements were performed on an X-ray diffractometer (D/MAX-RC, Japan) at 40 kV and 200 mA with Cu Kα (λ = 0.154 nm) radiation. TEM images were achieved on a TEM JeoL-1011 with an accelerating voltage of 120 kV. SEM images were obtained on a Hitachi S-4800 Scanning Electron Microscope operated at 15 kV. Elemental mappings of Zr-Phy-DES were recorded using a JEOL-2100F high resolution of transmission electron microscopy (HR-TEM). The content of Zr was detected by ICP-AES (VISTA-MPX). N2 adsorption-desorption isotherms were obtained on the Micromeritics ASAP 2020 V3.00H (USA) surface area analyzer at 77 K at high vacuum. Temperature-programmed desorption of ammonia (NH3-TPD) and temperature-programmed desorption of carbon dioxide (CO2-TPD) were conducted on Micromeritics’ AutoChem 2950 HP Chemisorption Analyzer.
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