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8 protocols using sta 449 f3 jupiter analyzer

1

Comprehensive Material Characterization

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Powder X-ray diffraction patterns were collected on a Rigaku MiniFlex600 X-ray diffractometer with Cu radiation. The X-ray diffraction data was refined by the RIETAN-2,000 Rietveld refinement program42 . SEM images were taken with a JEOL JSM-7500F microscope (operating voltage, 5 kV) equipped with an EDS analyzer. TEM and high-resolution TEM imaging was obtained on Philips Tecnai G2 F20 (acceleration voltage, 200 kV). Chemical composition was determined by EDS and atomic absorption spectrometry (AAS, Hitachi 180-90 spectrophotometer). Surface areas were calculated from the N2 adsorption/desorption isotherms at 77 K on BELsorp-Mini. Thermogravimetric analysis was carried out on a Netzsch STA 449 F3 Jupiter analyzer. XPS was performed by a Perkin Elmer PHI 1,600 ESCA system. The X-ray absorption near-edge structure spectra were collected on BL14W1 beamline of Shanghai Synchrotron Radiation Facility (SSRF) and analysed with software of Ifeffit Athena.
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2

Thermal Decomposition Analysis of Samples

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The thermal decomposition of the produced
samples was analyzed using a Netzsch STA 449 F3 Jupiter analyzer.
The freeze-dried samples (5 mg each) were heated in 85 μL aluminum
oxide crucibles (Netzsch) from 40 to 900 °C with a heating rate
of 10 K min–1 in a stream of 50 mL/min air and 20
mL/min nitrogen (70 mL/min gas flow consisting of 15 vol % oxygen).
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3

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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4

Multimodal Characterization of Materials

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Powder XRD patterns were collected on a Rigaku X-ray diffractometer (MiniFlex600) with Cu Kα radiation. SEM images were obtained on Field-emission JEOL JSM-7500F microscope. TEM and HRTEM images were taken on Philips Tecnai G2 F20. ABF-STEM was performed on Titan Cubed Themis G2 300 (FEI) at an acceleration voltage of 200 kV. The XAS data were collected on BL14W1 beamline of Shanghai Synchrotron Radiation Facility and analyzed with software of Ifeffit Athena62 . ICP-AES measurements were conducted on a PerkinElmer Optima 8300. XPS was tested on a Perkin Elmer PHI 1600 ESCA system. Raman spectra were obtained on confocal Thermo-Fisher Scientific DXR microscope using 532 nm excitation. TGA was measured by a Netzsch STA 449 F3 Jupiter analyzer.
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5

Spectroscopic Characterization of Vanadium Complexes

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Carbon, hydrogen, and nitrogen percentages were determined on a Perkin Elmer - CHN 2400 Elemental Analyzer, while the vanadium content was obtained by gravimetric analysis. An FTIR MB-BOMEN spectrophotometer was used to register the infrared spectra (4000–400 cm−1) from KBr pellets. A Netzsch STA449 F3 Jupiter analyzer equipped with a silicon carbide furnace and dinitrogen as carrier gas was the instrument used for collecting thermogravimetric (TGA) data. A sample (ca. 4 mg) was heated in an aluminum pan in the range of 25 to 800 °C at 10 °C min−1. X-band (9.5 GHz) EPR spectra were recorded at 77 K from solutions in water and DMEM using a Bruker ELEXSYS E-500 spectrometer. 51V NMR spectra were obtained from a Bruker 400 MHz Avance III spectrometer (9.4 T) equipped with a multinuclear direct detection probe (5 mm), using calibrated 90 ° pulses, 2048 scans, a recycling delay of 0.100 s, acquisition times of 0.218 s and a spectral width of 714 ppm. The 51V nucleus was detected at 105.2 MHz, and VOCl3 (neat, capillary) was used as a reference (0.00 ppm). Spectral intensities were normalized on each experiment by comparison with the reference signal.
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6

Thermal Characterization of Materials

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The qualitative characterization of the both obtained materials have been determined by thermogravimetric analysis (TGA) using a Jupiter STA 449 F3 analyzer (Netzsch, Selb, Germany). Samples weighing approximately 10 mg were placed onto thermobalance and heated from 30 to 1000 °C at a heating rate of 10 °C/min in a nitrogen atmosphere. Additionally, DTG curve was plotted to better visualize the thermal decomposition process.
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7

Characterization of Hybrid Materials

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Dispersive and microstructural properties were evaluated using scanning electron microscopy (SEM) and recorded using an EVO40 microscope (Zeiss, Jena, Germany).
The particle size range was determined using a Mastersizer 2000 instrument (Malvern Instruments Ltd., Malvern, UK) by laser diffraction technique. Additionally, Zetasizer Nano ZS (Malvern Instruments Ltd.) was used to determine the particle size distributions, based on the noninvasive backscattering (NIBS) method.
The efficiency of obtaining hybrid materials was confirmed using Fourier transform infrared spectroscopy (FTIR). For this purpose, the Vertex 70 spectrometer (Bruker Optik GmbH, Ettlingen, Germany) was used. The designed hybrid materials and pure components were analyzed in the form of potassium bromide tablets. The FTIR analysis was performed at a wavenumber range of 4000–400 cm−1.
The thermogravimetric analysis (TGA) of the samples was determined using a Jupiter STA449F3 analyzer (Netzsch GmbH, Selb, Germany). Measurements were conducted at a heating rate of 10 °C/min over the temperature range of 25–600 °C under nitrogen flow (10 mL/min).
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8

Thermal Characterization of Chitinous Scaffold

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Qualitative characterization of the isolated chitinous scaffold was performed by thermogravimetric analysis (TGA) using a Jupiter STA 449 F3 analyzer (Netzsch, Selb, Germany). Specimens (~10 mg) were inserted on a thermobalance and heated from 30 to 1000 °C at a heating rate of 10 °C/min in a nitrogen atmosphere. Additionally, a DTG curve was plotted to better visualize the process of thermal decomposition.
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