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147 protocols using axis ultra dld spectrometer

1

Comprehensive Material Characterization Protocol

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The morphology of samples was characterized by transmission electron microscope (JEM-2100F, JEOL, Tokyo, Japan). Field-emission scanning electron microscope (FE-SEM) analysis was performed on JSM-6700F at an acceleration voltage of 10.0 kV. X-ray photoelectron spectroscopic (XPS) measurements were performed on a Kratos AXIS Ultra DLD spectrometer with a monochromatic AlKa X-ray source. Thermal gravimetic analysis (TGA) was conducted in oxygen atmosphere at a heating rate of 5 °C min−1 from 25 °C to 800 °C. X-ray photoelectron spectroscopy (XPS) analysis was conducted using a Kratos AXIS Ultra DLD spectrometer with a monochromatic AlKa X-ray source. Conductivity was measured by a four-point probe method in the van der Pauw configuration with an Accent HL5500 system. N2 adsorption/desorption isotherms were determined by an Auto sorb IQ instrument. The Brunauer-Emmett-Teller (BET) method was carried out to calculate the surface areas.
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2

Comprehensive Characterization of Prepared Samples

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The morphologies and structures of the as-prepared samples were characterized by using scanning electron microscopy (SEM, Zelss Sigma300) at 3 kV and transmission electron microscopy (TEM, FEI Talos-F200s) at a voltage of 200 kV. The crystalline structure and chemical states of the samples were verified by powder X-ray diffraction (XRD, D/max-2500 diffractometer, Rigaku, Japan), energy-dispersive spectroscopy (EDS), and X-ray photoelectron spectroscopy (XPS, Kratos Axis Ultra DLD spectrometer). Surface area allowing Brunauer-Emmett-Teller (BET) isotherms was carried out by monitoring N2 adsorption/desorption using a NOVA 2000 surface area analyzer (Quantachrome) at 77 K.
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3

XPS Analysis of Beam-Induced Charging

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First,
1 mL of each sample was spread on an HF etched, p-doped, 1 inch silicon
wafer and then spin-coated at 3000 rpm for 60 s. XPS measurements
were performed on a Kratos AXIS-Ultra DLD spectrometer, using a monochromatic
Al Kα source at low power, 15–75 W, and detection pass
energies of 20–80 eV. The pressure in the analysis chamber
was kept below 1 × 10–9 Torr. An electron flood
gun (eFG) was used to address the beam-induced charging effects and
stabilize the surface potential. Then, the energy scale was corrected
for surface charging effects by setting the C 1s peak to 285.0 eV,
which was used as a convenient reference with no attempt to get an
absolute scaling.56 (link) The beam-induced damage
effects were thoroughly investigated by performing repeated scans
on a given spot in comparison to rapid scans at fresh spots. The stoichiometry
changes upon long exposures are an example of exploiting these “damage”
effects to learn about the diffusion of the Ca ions (Ca2+) under externally applied fields, as described in the main text.
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4

Surface Wettability and Composition Analysis

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Surface wettability was evaluated by measuring static water contact angle (WCA) (FTA-125, First Ten Angstroms, Newark, CA, USA). WCAs of at least six 5 μL droplets were measured for each sample. The surface chemical compositions of the substrates were characterized by X-ray photoelectron spectroscopy (XPS) analysis (AXIS Ultra DLD spectrometer, Kratos Analytical Inc., Manchester, UK) with a monochromated Al K—source at a power of 45 W. Each atom specimen was analyzed at the emission angle of 0° as measured from the surface normal. Data were processed using CasaXPS processing software (version 2.3.15, Casa Software Ltd., Teignmouth, UK). Binding energies were referenced to the aliphatic hydrocarbon peak at 285.0 eV.
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5

Spectroscopic Characterization of Colloidal Nanoplatelets

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The absorption spectra
from colloidal suspensions of nanoplatelets were acquired on Cary300
spectrophotometer. The photoluminescence spectra were collected instead
on a Cary Eclipse spectrofluorometer. Low magnification transmission
electron microscopy (TEM) and selected-area electron diffraction (SAED)
images were acquired on a JEOL JEM-1011 microscope equipped with a
thermionic gun at an accelerating voltage of 100 kV. The samples were
prepared by depositing a diluted suspension of nanoparticles on a
200-mesh carbon-coated copper grids. Energy dispersive X-ray spectroscopy
(EDS) measurements were performed at 25 kV on a JEOL JSM-6490LA scanning
electron microscope (SEM). X-ray photoelectron spectroscopy XPS measurements
were performed with a Kratos Axis Ultra DLD spectrometer. For XPS
analysis, high-resolution spectra were acquired at a pass energy of
10 eV using a monochromatic Al Kα source (15 kV, 20 mA). The
thickness of iridescent areas of the nanoplatelet films was quantified
using a ZETA-20 true color 3D optical profilometer, after the sample
surface was softly scratched with a tip of a pair of plastic tweezers.
All the crystal structure models presented in this work have been
built using VESTA, ver. 3.4.6.83 (link)
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6

Comprehensive Structural Characterization

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Powder XRD measurements were taken on a Rigaku model Ultima IV diffractometer with Cu-Kα X-ray source. SEM images were collected on a FEI Nova Nano 230 scanning electron microscope. TEM equipped with EDS and SAED was conducted on a Tecnai G2 F20 electron microscope. XPS was measured by a Kratos Axis Ultra DLD spectrometer. Inductively coupled plasma atomic emission spectrometer (ICP-AES) was performed on PerkinElmer Optima 83000. X-ray absorption fine structure spectra (Ni K-edge/Yb L-edge) were collected at BL14W beamline in Shanghai Synchrotron Radiation Facility (SSRF). The storage rings of SSRF were operated with a stable current of 200 mA at 3.5 GeV. With Si(111) double-crystal monochromator, the data collection was taken in Transmission mode using Lytle detector under ambient conditions.
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7

Characterization of Ti3C2Tx/Ag Morphology

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The morphology of Ti3C2Tx/Ag was obtained using TEM (JEOL‐2010F). XRD experiments were conducted on specimens using an X‐ray diffractometer (Bruker D8 Advance, Bruker AXS) operating at 40 kV and 40 mA. Nickel‐filtered Cu Kα radiation (λ = 0.154 nm) was used in the incident beam. The water contact angle was measured by an optical contact angle measuring device (POWEREACH JC2000). An XPS analysis was carried out with a Kratos Axis Ultra DLD spectrometer using monochromatic Al Kα X‐rays at a base pressure of 1 × 10−7 Pa. Survey scans were conducted between 1100 and 0 eV and revealed the overall elemental compositions of the sample; additionally, regional scans for specific elements were performed. The peak energies were calibrated by placing the major C 1s peak at 284.6 eV.
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8

Characterization of Filtration Performance

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SEM images were examined by a Hitachi Regulus 8100 SEM working at an acceleration voltage of 5 kV. Fourier-transform infrared (FTIR) spectra were collected with a VERTEX80v spectrometer (Bruker Optik GmbH, Germany). X-ray photoelectron spectrometer (XPS) spectra were recorded on an AXIS UltraDLD spectrometer (Kratos, UK). The element content data of samples were collected with an elemental analyzer (2400 Ⅱ, Perkin Elmer, USA). A T200-Auto 3 Plus contact angle analyzer (BiolinScientific, Germany) was used to conduct the water contact angle test, in which a drop of distilled water (4 μL) from a micro syringe was automatically dispensed on the surface of sample. A digital air permeability tester (YG461E, Wenzhou Fangyuan Instrument Co., Ltd, China) (Fig. S2) was used to evaluate the air permeability. An Automated Filter Tester 8130 (TSI Inc., USA) (Fig. S3) was used to measure the filtration efficiency and pressure drop with a flow rate of 85 L min−1, and sodium chloride (NaCl) monodisperse aerosols with a mass median diameter of 0.26 μm were used as the model particles.
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9

Structural and Chemical Analysis

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The SEM measurements were performed on a scanning electron microscope (FESEM, JSM-7610F, 10 kV). The TEM and HR-TEM measurements were taken with a JEOL JEM-F200 microscope. The samples were prepared by dropping ethanol dispersion of samples onto carbon-coated copper TEM grids using pipettes and dried under ambient condition. The X-ray photoelectron spectroscopy (XPS) measurements were conducted on a Kratos Axis Ultra DLD spectrometer. The electron paramagnetic resonance (EPR) spectroscopy was probed by a Bruker E580 spectrometer at room temperature (295 K).
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10

Comprehensive Characterization of N-CQDs

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A FEI TF-20 instrument operating at 200 kV (FEI, Hillsboro, TX, USA) was used to obtain high resolution transmission microscopy (HRTEM) information. FTIR spectra were collected from 20 scans with a resolution of 4 cm−1 by a Magna-IR560 unit (Nicolet Co., Madison, WI, USA). UV-vis. spectroscopy was performed on a UV-2550 spectrophotometer (Shimadzu, Kyoto, Japan) though a quartz cell with a 1 cm optical path. An LS-55 fluorescence spectrometer (PerkinElmer, Waltham, MA, USA) recorded the fluorescence. X-ray photoelectron spectroscopy (XPS) data for the N-CQDs powder deposited on copper substrates were measured by an AXIS Ultra DLD spectrometer (Kratos, Manchester, UK) with a monochromatized Al Kα X-ray source (1486.6 eV) for determining the composition and chemical bonding configurations.
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