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8 protocols using phi 1600 esca

1

Characterization of Annealed Products by Advanced Techniques

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Crystallographic properties of the annealed products were determined by XRD (Rigaku D/Max‐2500) with filtered Cu Kα radiation (λ = 1.5418 Å) in the 2θ range of 10°–90°. Morphological and microstructural studies were scrutinized by field‐emission scanning electron microscopy (FE‐SEM, JEOL JSM7500F) and TEM (TECNAI G2 20). Elemental analyses were ascertained by SEM‐ and TEM‐energy dispersive X‐ray spectrometer (EDS) mapping. Nitrogen adsorption–desorption isotherms obtained on a Micromeritics ASAP 2460 instrument (MicroActive) at 77 K were applied to evaluate the porosity and specific surface area. Raman spectra were gathered on a confocal Raman microscope (Thermo‐Fisher Scientific) using an argon‐ion laser (λ = 532 nm) in ambient air. The chemical content was ascertained by ICP atomic emission spectroscopy (ICP‐AES, Varian 725‐ES). X‐ray photoelectron spectrometry (XPS, Perkin Elmer PHI 1600 ESCA) was applied to investigate the valence states of the elements during cycling.
When it comes to in operando XRD characterizations, a particular mold battery was assembled employing beryllium foil as the testing window to allow X‐ray passage and carbon paper as the current collector, thus monitoring in situ reaction during cycling. Each scan was recorded in 0.02° incremental steps between 2θ = 12° and 42°. The charge/discharge test was conducted at 0.1 C.
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2

Structural Characterization of TQBQ-COF Material

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The structure of the resultant TQBQ-COF material was examined by solid-state 13C NMR with Inova 400 MHz Spectrometer (Varian Inc., USA), and Fourier transform infrared spectroscopy (FTIR, Bruker 5700 TENSOR П) in range of 400–4000 cm−1. Powder XRD (Rigaku MiniFlex600 × -ray generator, Cu Kα radiation, λ = 1.54178 Å), high-resolution transmission electron microscopy (HRTEM) and the selected area electron diffraction (SAED) pattern (Taols F200X G2) were applied to investigate the crystallinity and the microstructure of the TQBQ-COF powder. The elemental distributions of the TQBQ-COF material and the relevant electrodes before and after discharge/charge were characterized by scanning electron microscopy-Energy dispersive spectrum mapping (SEM-EDS), elemental analysis (EA, vario EL CUBE), and X-ray photoelectron spectroscopy (XPS, Perkin Elmer PHI 1600 ESCA), respectively. The morphologies of the TQBQ-COF material and the relevant electrodes were observed by scanning electron microscopy (SEM, JEOL JSM7500F), transmission electron microscopy (TEM, Taols F200X G2), and N2 adsorption/desorption measurement (BEL Sorp mini). Moreover, Raman (DXR Microscope, Thermo Fisher Scientific with excitation at 532 nm) and TG-DSC analyzer (NETZSCH, STA 449 F3) were separately carried out to examine the structure and the stability of TQBQ-COF material, respectively.
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3

Comprehensive Characterization of Zinc Electrodes

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The morphology of the prepared G&B‐S@Zn and bare Zn electrodes were characterized by SEM (FEI XL30 Sirion) at an accelerating voltage of 10 kV. The morphology of Zn deposition and after cycling were also obtained. EDS elemental maps were used to define the distribution of elements. The microstructures of the products were determined by TEM (FEI Tecnai G2 F30). AFM (Bruker Multimode 8 with a Nanoscope V controller) was used to further understand the morphology of the G&B‐S@Zn and bare Zn. Bruker Alpha FT‐IR spectrometer (ATR‐Ge, 1000–4000 cm−1) were recorded on FT‐IR spectra. XPS measurements characterized the chemical composition of the G&B‐S@Zn sample on a spectrometer (PerkinElmer PHI 1600 ESCA) with Al Kα radiation (hv = 1486.6 eV). XRD (Bruker D8 Advance) with CuKα radiation range 5°–70°. The contact angle test (OCA20, Dataphysics, Germany) was characterized the wettability between the electrolyte and the G&B‐S interfacial layer. In situ DEMS (Hidden HPR‐40) was used to monitor the hydrogen evolution rate (RH) during the plating/stripping of symmetric cells. In situ XRD test was used to investigate the Zn deposition process. QCM‐D (Biolin Scientific) was employed to characterize the mechanical properties of the G&B‐S film.
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4

Characterization of CaVO Nanoribbons and Cathodes

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The morphologies of CaVO nanoribbons and cathodes were characterized via field-emission scanning electron microscopy (SEM, JEOL JSM7500F, 5 kV and Phenom XL, 15 kV). The SEM–energy dispersive spectroscopy (EDS) of the samples are collected with Phenom XL at an acceleration voltage of 15 kV. The microstructure was characterized by TEM (FEI Talos F200X and FEI Talos F200X G2) equipped with EDS mapping at an acceleration voltage of 200 kV. The crystalline structure of samples was determined by XRD (Rigaku SmartLab) with Cu Kα radiation (λ = 0.15405 nm). TGA (Netzsch STA 449 F3 Jupiter analyzer) was carried out in an Ar flow from room temperature to 600 °C at a heating rate of 10 °C min−1. In situ XRD experiments were performed using home-made cells that were designed with Be window for X-ray penetration. XPS (PerkinElmer PHI 1600 ESCA) was used to characterize the composition and surface oxidation state of the electrodes. V K-edge XANES spectra were collected at the beamline 14W1 in Shanghai Synchrotron Radiation Facility. The solid state 1H nuclear magnetic resonance (1H NMR) was taken from a 400 MHz superconducting NMR spectrometer (AVANCE ||| 400).
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5

Printed Catalyst Characterization Methods

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The morphology of the printed catalyst
was observed by scanning electron microscopy (SEM, S8100, Hitachi,
Japan). Porosity and specific area were measured by mercury intrusion
porosimetry (MIP, AutoPore Iv-9510, Micromeritics, USA). X-ray diffraction
(D8-focus, Bruker, German) was used to determine the crystalline composition
of the printed catalyst. X-ray photoelectron spectroscopy (XPS, PHI1600
ESCA, PerkinElmer, USA) was used to analyze the element valence change
during the growth of HKUST-1. The rheology of the Cu/Fe inks was measured
using a rotary rheometer (DHR-2, TA Instruments, USA) in oscillation
mode (strain, 1%; frequency, 10 Hz).
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6

Structural Analysis of V2O5/CNTs Composite

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Scanning electron microscopy (SEM, Supra-55, Zeiss, Oberkochen, Germany) and transmission electron microscopy (TEM, JEOL2100F, JEOL, Tokyo, Japan) were used to investigate the morphology of the samples. The chemical components of the V2O5/CNTs film were confirmed with X-ray photoelectron spectroscopy (XPS, PHI 1600 ESCA, PerkinElmer, Waltham, MA, USA). The structure of the V2O5 nanowires and V2O5/CNTs film was characterized using X-ray diffraction (XRD, Rigaku D/Max-3A, Rigaku Corporation, Tokyo, Japan). Raman spectra were recorded by a spectrophotometer (Thermo-Fisher Scientific, Waltham, MA, USA).
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7

Comprehensive Nanomaterial Characterization

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The morphology of NVO was characterized by SEM (JEOL JSM-7500F) and TEM (JEOL-2100 F, 200 kV) with energy dispersive spectroscopy (EDS) for elemental analysis. XRD tests were performed on Rigaku Ultima IV with Cu Kα radiation. FTIR and XPS spectra were collected through Bruker Tensor II and PerkinElmer PHI 1600 ESCA, respectively. The solid state 1H NMR spectra were taken from a 300 MHz superconducting NMR spectrometer (Varian Infinitplus-300). ICP-AES results were obtained from PerkinElmer Optima 8300. CV curves were measured by an electrochemical workstation (CHI 660E) with a voltage window of 0.3–1.25 V at different scan rates from 0.1 to 0.5 mV s−1. Galvanostatic charge/discharge tests were performed on a battery test system (LAND CT2001A) with a voltage range from 0.3 to 1.25 V.
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8

Characterization of Zinc Electrode Surfaces

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A scanning electron microscope (FFG-SEM, Zeiss-Leo Gemini 1530, Carl Zeiss NTS GmbH, Oberkochen, Germany) was employed to characterize the surface morphologies of zinc electrodes at different stages of the experiment process. Elemental mappings were performed using energy dispersive X-ray spectroscopy with a Bruker XFlash 6 detector (Bruker, Karlsruhe, Germany). X-ray diffraction (XRD) was carried out on a Panalytical X’pert Pro diffractometer device (Panalytical, Almelo, Netherlands) operating with Co Kα radiation in reflection mode. The X-ray photoelectron spectroscopy (XPS) analysis was performed in a PHI 1600 ESCA (PerkinElmer, Waltham, MA, USA) spectrometer with a monochromatic Al-Kα source. The binding energies were calibrated using the C 1s peak at 284.8 eV.
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