Here, bare Cu grid (used in TEM measurement) and NMMF@C-modified Cu grid were used as matrix for Li deposition. The plated Li amount was 0.5 mAh cm−2 at the current density of 0.5 mA cm−2. Once the samples were washed using dioxolane and dried, it was transferred into the cryo-TEM holder in an Ar-filled glove box. Using a sealed container, the cryo-TEM holder was quickly inserted into FEI Talos-S, and then, liquid nitrogen was poured into the cryo-TEM holder until the sample temperature dropped below −170°C. All cryo-TEM images were taken at cryogenic temperatures (−170°C).
Talos s
Manufactured by Thermo Fisher Scientific
The Talos-S is a scanning electron microscope (SEM) designed for materials characterization. It provides high-resolution imaging and analytical capabilities for a wide range of samples. The Talos-S is equipped with advanced electron optics and detection systems to deliver detailed information about the structure and composition of materials.
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Lab products found in correlation
S 4800, by Hitachi (1 mentions)
Nanonova 450, by Thermo Fisher Scientific (1 mentions)
Lab ram high resolution spectrometer, by Horiba (1 mentions)
Su8220, by Thermo Fisher Scientific (1 mentions)
Asap 2460, by M&M Mass Spec Consulting (1 mentions)
Axis ultra dld, by Shimadzu (1 mentions)
Elan drc e, by PerkinElmer (1 mentions)
5 protocols using talos s
1
Cryogenic Li deposition on Cu grid
2
Ex situ characterization of cycled Na-ion electrodes
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All the samples were characterized by scanning electron microscopy (SEM, Hitachi S-4800), transmission electron microscopy (TEM, JEOLJEM-2100), inductively coupled plasma-mass spectrometry (ICP-MS, Thermo X2), X-ray diffraction (XRD, Bruker D8 Discovers X-ray analytical systems with Cu Kα radiation), energy dispersive X-ray (EDX, an EDX detector system attached to FEI Talos-S), and X-ray photoelectron spectroscopy (XPS, ESCALAB 250Xi).
The cycled electrode samples for ex situ XPS and XRD characterization were obtained by disassembling the cycled half-cells using Na metal anode in Ar-filled glovebox (H2O < 0.1 ppm, O2 < 0.1 ppm). The electrodes were rinsed using dimethyl carbonate (DMC, 99%, Sigma Aldrich) repeatedly, then dried in glovebox to remove the solvents. For ex situ XPS measurements, the dried electrodes were first placed into a vacuum transfer vessel in glovebox and then transferred into the XPS ultrahigh vacuum chamber. For ex situ XRD measurements, the dried electrodes were transferred from glovebox and then tested in air.
The cycled electrode samples for ex situ XPS and XRD characterization were obtained by disassembling the cycled half-cells using Na metal anode in Ar-filled glovebox (H2O < 0.1 ppm, O2 < 0.1 ppm). The electrodes were rinsed using dimethyl carbonate (DMC, 99%, Sigma Aldrich) repeatedly, then dried in glovebox to remove the solvents. For ex situ XPS measurements, the dried electrodes were first placed into a vacuum transfer vessel in glovebox and then transferred into the XPS ultrahigh vacuum chamber. For ex situ XRD measurements, the dried electrodes were transferred from glovebox and then tested in air.
3
Nanodiamond Film Morphology Characterization
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FESEM (FEI Nano Nova 450) was used to observe the morphologies of the samples at a low voltage of 5 or 3 kV. To protect the microstructure of the NCD films from damage during TEM sample preparation, small fragments of film were scraped down from the silicon substrate and loaded on copper mesh. The submicroscopic structures or ultrastructures of the samples were characterized by using HRTEM (FEI Talos-s, 200 kV accelerator voltage) and aberration‐corrected scanning transmission electron microscopy (Titan G2 80-200 ChemiSTEM). EDS and EELS were used to recognize the composition information of the samples. Raman spectra were taken to evaluate the structure and components of the films. A Labram high-resolution spectrometer (Horiba Jobin-Yvon) interfaced with an Olympus microscope (objective 50×) was used to acquire the Raman spectra for four different sites, and the spectra were collected in the range of 500 to 3,500 cm−1. Some of the spectra had been deconvoluted well into Gaussian lines.
4
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).
5
Structural and Compositional Analysis of Electrode Materials
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Powder XRD analysis [X’Pert Pro diffractometer using CuKα radiation (λ = 0.15418 nm)] of different samples was carried out to investigate the crystalline phase of the synthesized samples. The morphology and microstructure of these samples including NMMF, NMMF@C, and the behavior of lithium deposition were observed by FESEM (Nova NanoSEM450). Elemental analysis was conducted on an EDX spectrometer attached to FESEM. XPS analysis was performed using Al Kα (1486.6 eV) monochromatic x-ray source (AXIS Ultra DLD, Kratos). The concentration of metal ions was measured using ICP-MS with PerkinElmer ELAN DRC-e. In addition, the microstructures of samples, deposited Li metal, and SEI were carried out using TEM (FEI Talos-S), and cryo-TEM characterizations were carried out using Gatan 698 cryo-transfer holder.
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