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7 protocols using escalab mk 2

1

Comprehensive Morphological and Structural Characterization

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The morphology of the samples was characterized by SEM (JSM-7800F, JEOL) and TEM (JEM-2100, JEOL and Tecnai G20, FEI) equipped with an energy dispersive spectrometer. The microstructure analysis of the samples was recorded by XRD (Cu Kα, D/MAX-2400, Rigaku). The texture of the samples was obtained by XPS (ESCALAB MK II, Thermo Fisher Scientific) with C 1s (284.6 eV) calibration. The weight ratio of sulfur in the electrode was measured by TGA (X70 equipment). The weight ratio of Li2S was measured by ionic-coupled plasma optical emission spectroscopy (Optima 2000DV) and calibrated with electrode weight difference before and after loading Li2S. The FTIR spectra were characterized by a Bruker EQUINOX 55 spectrophotometer. Raman spectra were obtained by a Horiba LabRAM HR Evolution Raman microscope. The infrared thermography of the pouch cells was measured by a thermal infrared camera (FLIR, C5).
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2

Comprehensive Characterization of Nanomaterials

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All chemicals and solvents were purchased from Merck (Germany) or Fluka (Switzerland). The fourier-transform infrared spectroscopy (FT-IR) spectra of the samples were recorded with the KBr pellet method by PerkinElmer PE-1600-FTIR spectrometer. A SIGMA VP 500 (Zeiss) microscope equipped with an EDX measurement system was used to record field emission scanning electron microscope (FESEM) imaging and energy-dispersive X-ray spectroscopy (EDX) analysis. Transmission electron microscopy (TEM) images were obtained using a SIGMA VP 500 (Zeiss) microscope. X-ray diffraction (XRD) spectra were carried out using an X-ray diffractometer (PANalytical X'Pert PRO, Netherlands) with Cu Kα radiation (λ = 1.54 Å). An ESCALab MKII (Thermo Fisher Scientific, USA) spectrometer with Al Kα (1.4866 keV) as the X-ray source was used to record X-ray photoelectron spectroscopy (XPS). Zeta potential was measured using a Zetasizer Nano-ZS, Model ZEN3600 (Malvern Instruments Ltd, Malvern, UK).
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3

Multi-Technique Characterization of Materials

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The morphology of as-prepared materials was analyzed by scanning electron microscopy (SEM, JSM-6700F, JEOL, Tokyo, Japan). Transmission electron microscopy (TEM) and energy dispersive spectrum (EDS) mapping images of samples were acquired on a JEM-2100UHR (JEOL, Tokyo, Japan) at an accelerating voltage of 100 kV. X-ray diffraction (XRD) patterns were recorded by PANalytical X’Pert Pro (Panalytical, Almelo, Netherland) with Cu Kα radiation (λ = 1.54178 Å). The surface chemical states of samples were characterized by X-ray photoelectron spectra (XPS) on an ESCALAB MK II (Thermo Scientific, Waltham, MA, USA) with Mg Kα (hυ = 1253.6 eV) as the excitation source. The pore structures were tested by a Multipoint N2 adsorption–desorption experiment on an automatic Micromeritics ASAP 2020 (Micromeritics, Norcross, GA, USA) analyzer at 77 K. The specific surface area was calculated by the BET method and the pore size distribution was generated from the desorption branch of the isotherm by the non-local density functional theory (NLDFT) method.
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4

Characterization of Tungsten Catalysts

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All chemicals and solvents were supplied from Fluka (Switzerland) or Merck (Germany). We used an ESCALab MKII (Thermo Fisher Scientific, USA) spectrometer with Al Kα (1.4866 keV) as the X-ray source to determine X-ray photoelectron spectroscopy (XPS). The 1H NMR and 13CNMR analyses were carried out with a BRUKER DRX-250 AVANCE spectrometer at 250.0 MHz. The optical emission spectrometer inductively coupled plasma (Varian Vista MPX ICP-OES Axial) was used to measure content of W in the catalysts. X-ray diffraction (XRD) spectra were obtained on a Siefert XRD 3003 PTS diffractometer with Cu Kα radiation (λ = 1.54 Å). Thermogravimetric analysis (TGA) was recorded using a TGA Q 50 analyzer under N2 flow at a heating rate of 10 °C min−1. The optical characteristics of samples were measured by Shimadzu UV 2100 151PC UV–Visible spectrophotometer at room temperature. Field emission scanning electron microscope (FE-SEM) imaging and energy-dispersive X-ray spectroscopy (EDX) analysis were carried out on a SIGMA VP 500 (Zeiss) microscope equipped with an EDX measurement system. A Philips EM10C 200 kV microscope was used to record transmission electron microscopy (TEM) images. The fourier-transform infrared spectroscopy (FT-IR) spectra of the samples were recorded with the KBr pellet method by PerkinElmer PE-1600-FTIR spectrometer.
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5

Characterization of Functionalized Electrodes

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The morphology of functionalized electrodes was characterized by SEM (Quanta FEG 200, FEI, USA) using an ETD detector. Atomic force microscopy (AFM) with a 5500 SPM system in tapping mode (Keysight Technologies, USA) was chosen to probe the functionalized graphene surface (i.e., GO, RGO and RGO-A). X-ray photoelectron spectroscopy (XPS) of the modified electrodes was recorded using an X-ray photoelectron spectrometer (ESCALABMKII, Thermo Scientific, USA). The surface hydrophilicity was characterized using a contact angle system (OCA Data Physics, Germany) to measure the WCA of dried electrodes with a droplet (6.0 µL) of Millipore water on top.
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6

Comprehensive Material Characterization

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A N2 adsorption–desorption
test was carried out at 77 K (ASAP2020M, Micromeritics) to investigate
the porosity of samples. The composition and morphology of samples
were analyzed by X-ray diffraction (XRD, X’Pert PRO, PANalytical).
The morphological features were observed by scanning electron microscopy
(SEM, S-4800 Hitachi). The Raman spectrum was obtained by a LabRAM
HR800 Raman Spectrometer at a wavelength of 514 nm. X-ray photoelectron
spectroscopy (XPS, Thermo Fisher ESCALAB MK II, USA) was performed
to determine the composition and the surface elemental conditions
of the sample.
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7

Comprehensive Characterization of FPC Samples

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A field emission scanning electron microscope (FESEM, JSM-7600F, JEOL, Tokyo, Japan) was used for the evaluation of FPCs’ samples’ morphology. The transmission electron microscope (TEM, JEM-2100UHR, JEOL, Tokyo, Japan) was used to characterize the microstructures of the FPCs. To investigate the proportion of FPCs, a thermogravimetric analysis (TGA, TGA/SDTA851, Mettler Toledo, Zurich, Switzerland) was carried out from room temperature to 700 °C at a rate of 10 °C/min under air flow. An X-ray diffractometer (XRD, PANalytical X’Pert Pro, Panalytical, Almelo, The Netherlands) was used to analyze the crystal structures of FPCs, and an X-ray photoelectron spectroscopy (XPS, ESCALAB MK II, Thermo Scientific, Waltham, MA, USA) analysis was conducted to detect the surface chemical state of the samples. The specific surface areas (SBET) and pore size distributions were calculated from the N2 adsorption-desorption isotherms obtained on the automatic analyzer at 77 K (Micromeritics ASAP 2020, Micromeritics, Norcross, GA, USA).
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