The morphology and phase components were examined by XRD (Cu Kα, λ = 1.5406 Å), SEM (HITACHI SU8220), TEM (FEI Talos F200X; Tecnai G2 F30), AC-TEM (FEI Themis Z). XPS (Thermo ESCALAB 250) characterization was carried out to decouple the electronic structure information. Raman mapping and operando Raman spectroscopy (HORIBA LabRAM HR Evolution) were conducted to understand the bonding types and underlying charge-storage mechanisms. The laser excitation wavelength is 532 nm, and a laser power of 1–3.2 mW is used to obtain high signal-to-noise spectra without affecting the microstructure. To avoid laser damage, a series of pre-experiments had been done before the operando measurement: the sample was dried thoroughly in a vacuum drying oven at 60 °C for eliminating any impurities; ex-situ experiments are carried out for comparison; a pre-measurement was done at a low laser power (less than 0.5 mW), then the power was gradually increased to improve the resolution of typical peaks without altering the local chemical environment. AFM (Bruker, Dimension Icon) characterization was adopted to investigate the surface roughness and wrinkled structure. For fine structure analysis, sXAS spectra were collected in Beamline 7.3.1 of Advanced Light Source (ALS), Lawrence Berkeley National Laboratory (LBNL), and Beamline BL14W1 of Shanghai Synchrotron Radiation Facility (SSRF).
Su8220
Manufactured by Thermo Fisher Scientific
Sourced in United States
The SU8220 is a high-resolution analytical scanning electron microscope (SEM) designed for a wide range of applications. It features a stable electron column, advanced imaging capabilities, and versatile sample handling options.
Automatically generated - may contain errors
Lab products found in correlation
Escalab 250, by Thermo Fisher Scientific (3 mentions)
Themis z, by Thermo Fisher Scientific (1 mentions)
Talos f200x, by Thermo Fisher Scientific (1 mentions)
Labram hr evolution, by Horiba (1 mentions)
Talos s, by Thermo Fisher Scientific (1 mentions)
Asap 2460, by M&M Mass Spec Consulting (1 mentions)
Tecnai g2 f20, by Thermo Fisher Scientific (1 mentions)
Fei quanta 200 fesem, by Thermo Fisher Scientific (1 mentions)
Hrtem, by Thermo Fisher Scientific (1 mentions)
5 protocols using su8220
1
Comprehensive Materials Characterization Protocol
2
Adsorbent Material Characterization
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The phase of the adsorbent was confirmed by X-ray diffraction (XRD, X′ Pert PRO) with Cu Kα radiation, the test conditions were: scanning angle range 5–90°, scanning speed 5 (°) min−1, accelerating voltage 45 kV, applied current 40 mA. The morphology of the material was tested by Scanning Electron Microscope (SEM, SU8220) and Transmission Electron Microscope (TEM, FEI Talos-S). The specific surface area and pore size distribution of the adsorbent were measured by BET analysis (ASAP2460).
3
Comprehensive Characterization of As-Obtained Samples
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The crystal structure of the as-obtained samples was characterized with a D8 Advance X-ray powder diffractometer (Cu Kα radiation with a step of 0.02° per second in the 2θ ranging from 10–80°). Raman spectra were obtained under visible light with wavelength 100–2000 cm−1 on in Via Reflex. The morphology and energy dispersive X-ray spectroscopy (EDS) mappings were characterized by a SU8220 field-emission scanning electron microscope (FESEM) equipped with an energy-dispersive spectrophotometer at an accelerating voltage of 5 kV. Transition electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) images and SAED patterns were acquired on Tecnai G2 F20 (FEI) microscope. The surface compositions were analyzed using X-ray photoelectron spectrometer (XPS) on AXIS ULTRA (Kratos Analytical Ltd). Brunauer–Emmett–Teller specific surface area and the pore size distribution were acquired by N2 adsorption/desorption isotherms measurement on ASAP 2460. Thermogravimetric analysis (TGA) curves were tested using TGA/DSC 3+ in air atmosphere from 25 to 800 °C with a heating rate of 10 °C min−1, respectively.
4
Morphological Analysis via FESEM
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An Hitachi SU8220 (FEI Quanta 200 FESEM, FEI Company, Hillsboro, OR, USA) was used to conduct FESEM at a magnification of 500× to study the film’s morphology.
5
Comprehensive Structural Characterization of Materials
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FT-IR spectra were recorded with a Thermo Fisher 6700 spectrometer by using the KBr pellet method. XRD patterns were obtained with a Rigaku D/Max 2400 diffractometer by using Cu Kα radiation operated at 45 kV and 200 mA. Nitrogen sorption/desorption isotherms were characterized at 77 K with a Micromeritics ASAP 2020 analyzer. Prior to the gas adsorption, powders were outgassed at 120 °C for 8 h under a vacuum of 10−6 Torr. To further characterize the structure, the as-prepared samples were observed and characterized using the SEM (Hitachi, SU8220) and HR-TEM (FEI, Eindhoven, The Netherlands). In addition, XPS measurements were measured using an ESCALAB 250 analyzer with an Al Kα X-ray source and a base pressure of 1 × 10−9 mbar.
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