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22 protocols using labram hr evolution raman microscope

1

Comprehensive Characterization of 3D-MoSx Films

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Surface morphology analysis and cross-section imaging of the PS/FTO electrodes, MoSx, 3D-MoSx and 3D-MoS2 films were performed by a field emission scanning electron microscopy (FE-SEM, Hitachi S4800, Japan) operated at 5 kV. For the SEM cross-section imaging, the back side of the 3D-MoSx and 3D-MoS2 deposited FTO electrodes were cut by a diamond tip glass cutter following a line going through the middle of the piece. The electrode was then broken into two pieces by applying pressure along the cutting line. SEM images were then collected in different positions on the freshly-exposed edge. Raman spectra were collected by using a LabRAM HR Evolution Raman Microscope (Horiba). Excitation was made by a green 532 nm laser with low power of 0.1 mW to avoid the MoSx-to-MoS2 crystallization.21 (link) Size distribution of spherical PS particles have been analyzed employing dynamic laser scattering method using a Horiba SZ-100. Samples were diluted to the concentration of 1 mg mL−1 and measured 3 times using 173° back-scatter (NIBS standard), the DLS signals were collected in 120 seconds for each measurement. The water contact angle measurement was assayed using H2SO4 0.5 M solution on a Kruss DSA25 drop shape analyzer.
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2

Raman and PL Spectroscopy Characterization

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Raman and PL spectroscopy were carried out using a Horiba Jobin Yvon LabRAM HR-Evolution Raman microscope. The excitation light is a 532 nm laser, with an estimated laser spot size of 1 μm and the laser power of 1 mW.
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3

Cryogenic Raman Spectroscopy with Magnetic Field

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Raman measurements were performed using a 632.81 nm excitation laser with a full-width-half maximum (FWHM) of 0.85 cm−1. The laser power was kept below ~100 μW to avoid local heating and damage to the samples. The laser beam was focused onto the sample via a ×40 microscope objective to a spot size of about 3 μm in diameter. The Raman signal was collected in the back-scattering geometry and measured with a Horiba LabRAM HR Evolution Raman microscope (1800 grooves/mm grating). All measurements were taken in a closed-cycle helium cryostat from 11 to 300 K with a base pressure lower than 7 × 10−7 Torr. An out-of-plane magnetic field ranging from 0 to 7 T was applied.
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4

Thermogravimetric and Spectroscopic Analysis of Metal Complexes

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The thermogravimetric analyses (TGAs) of the metal complexes were carried out with a Perkin–Elmer Pyris 1 TGA apparatus at a heating rate of 5 °C/min for CuL14 and MnL14, and 2.5 °C/min for FeL14 in a temperature range of 25 to 800 °C under an O2 atmosphere at a flow rate of 20 mL/min. Spectrum evaluations were performed using the Pyris version 11.1.1.0492 software package.
The infrared spectra were recorded in the spectral range between 4000 and 250 cm−1 in KBr pellets with a Perkin–Elmer FTIR/FIRS Spectrometer Frontier instrument. A total of 32 scans were performed. Raman spectra were obtained using a HORIBA LabRam HR Evolution Raman microscope at room temperature. A He–Ne laser was employed with an energy of 633 nm from 20 mW to 100 mW and a slit of 100 µm. The X-ray photoelectron spectra (XPS) were obtained on a Perkin–Elmer PHI 5100 model with a Mg Kα source under a vacuum of 4 × 10−9 torr. All the spectra were corrected to alkyl type carbon C1s (285.0 eV) and fitted by applying a Tougard baseline and a Gaussian–Lorentzian function to each peak.
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5

In situ SERS Measurements of Electrochemical Reactions

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The measurements were carried out using a Horiba LabRAM HR Evolution Raman microscope with a common objective (10×) in a modified flow cell, and the 785-nm laser was chosen. The Ag/AgCl electrode and Ni foam were used as the reference electrode and counter electrode. The electrolyte for both the cathode and the anode was 1 M KOH. The different potentials were applied during the In situ SERS measurements, and a 15-minute electrolysis was performed at each potential before the signals were collected.
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6

Characterizing Graphene Surfaces with c-AFM

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The c-AFM measurements were carried out in an Asylum Research Cypher AFM with conductive probes in ambient conditions (temperature ∼26°C, relative humidity ∼50%). A constant voltage bias was applied between the sample and the probe. The typical spring constant and resonance frequency of the conductive probe coated with Ti/Ir (ASYELEC.01-R2, Asylum Research) are 2.8 N/m and 75 kHz, respectively. To exclude the possibility of an extra moiré pattern in top multilayer graphene created during the transfer process, we also carried out c-AFM measurements on suspended graphene near the graphite edge without the bottom graphite substrate (Fig. S3). In our c-AFM experiments, measurements were intentionally conducted in the inner regions of graphene far away from the graphite edge, where the strain induced by the SiO2/Si substrate was minimized (Fig. S4). The Raman spectra were obtained using a Horiba LabRAM HR Evolution Raman microscope with a 532 nm He-Ne laser as the excitation source.
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7

Multi-Technique Nanomaterial Characterization

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OM and FL images were acquired with an optical microscope (DM4000 M, Leica). Raman and PL spectra, line scans and mapping images were obtained with a Horiba Jobin Yvon LabRAM HR-Evolution Raman microscope under 532 nm laser irradiation. AFM characterizations were performed on Multimode 8 (Bruker). TEM, HAADF, and SAED measurements were performed using a transmission electron microscope (Talos F200X, Thermo Fisher) operated at 200 kV. XPS spectra were acquired using an Axis Ultra spectrometer (ESCALAB 250Xi, Thermo Fisher).
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8

Characterization of MoS2 Thin Films

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Surface coverage and thickness were measured using peak-force tapping mode in a Bruker Icon AFM using scanasyst AFM tips with a nominal tip radius of ∼2 nm and a spring constant of 0.4 N/m. Raman and PL measurements were performed using a HORIBA LabRAM HR Evolution Raman microscope with laser wavelengths of 532 nm. Raman spectra were collected with 1800 grooves per mm grating, while PL measurements were conducted with 300 grooves per mm grating. The Raman and PL maps were acquired over a 5 × 5 µm2 area. X-ray diffraction characterization of MoS2 films was carried out with a PANalytical MRD diffractometer with a 5-axis cradle. X-rays were generated in a standard Cu anode X-ray tube operated at 40 kV accelerating voltage and 45 mA filament current. Cu K line was filtered by a mirror with 1/4° slit and Ni filter on the primary beam side. On the diffracted beam side, an 0.27° parallel plate collimator with 0.04 rad Soller slits with PIXcell detector in open detector mode was employed. Samples' surface was ~2–4° away from the X-ray incidence plane such that diffraction caused by the (h k i 0) planes, to determine the in-plane epitaxial relation of the film with respect to a substrate, could be measured35 (link).
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9

In Situ Raman Analysis of CO2 Electrochemical Conversion

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A flow cell with a quartz window by GaossUnion (Tianjin) Photoelectric Technology Company was used to carry out in situ Raman measurements using a Horiba LabRAM HR Evolution Raman microscope (Fig. S25). A 785 nm laser was used and signals were recorded using a 20 s integration and by averaging two scans. The gas diffusion electrode sprayed with the catalyst was used as working electrode and a graphite rod and a Hg/HgO electrode were used as counter and reference electrodes, respectively. The counter electrode was separated from the working electrode by anion exchange membrane. The 5 M KOH aqueous solution was used as electrolyte and were recirculated by pump with flow rates of 20 mL min−1. Meanwhile, CO2 gas was continuously supplied to the gas chamber with a flow rate of 40 mL min−1.
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10

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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