Hydrogel samples that were either freshly prepared or swollen in the cup model setting for 24 h in biological fluids were lyophilized for 24 h. The resulting pieces were mounted onto an SEM holder using carbon tape and coated with a (5 nm) layer of carbon using a Safematic CCU-010 coater. Scanning electron microscope (SEM) imaging was performed on a Quanta 650 SEM (FEI, Thermo Fisher Scientific) at an accelerating voltage of 10 kV.
Quanta 650 sem
Manufactured by Thermo Fisher Scientific
Sourced in Germany
The Quanta 650 SEM is a scanning electron microscope (SEM) manufactured by Thermo Fisher Scientific. It is designed to provide high-resolution imaging and analysis of a wide range of sample types. The Quanta 650 SEM utilizes an electron beam to scan the surface of a sample, generating detailed information about its topography and composition.
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Lab products found in correlation
Hepes buffer, by Merck Group (1 mentions)
X pert pro mpd diffractometer, by Malvern Panalytical (1 mentions)
Alpha 300r, by WITec (1 mentions)
Crx 6.5 k, by Keysight (1 mentions)
Dimension icon, by Bruker (1 mentions)
D8 advance, by Bruker (1 mentions)
S 5500 sem, by Hitachi (1 mentions)
Asap 2020 instrument, by Micromeritics (1 mentions)
Magellan 400 sem, by Thermo Fisher Scientific (1 mentions)
E4980al, by Keysight (1 mentions)
Cary 5000, by Agilent Technologies (1 mentions)
Leo 912ab tem, by Zeiss (1 mentions)
Axis ultra xps spectrometer, by Shimadzu (1 mentions)
13 protocols using quanta 650 sem
1
Hydrogel Structural Analysis via SEM
2
SEM Sample Preparation Protocol
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Prior to SEM, paraformaldehyde fixed samples were pretreated with the following solutions: 50 mM NaN3 for 1 h followed by 2% tannic acid for 1 h, 1% osmium tetroxide for 2 h, 1% thiocarbohydrazide for 30 min, and 1% osmium tetroxide overnight. The samples were washed using 10 mM HEPES buffer (pH 7.4) between steps (all Sigma-Aldrich). The samples were then dehydrated in a graded series of aqueous ethanol solutions (50−100%) and oven-dried (2 h at 40 °C) to remove residual moisture. The dried samples were mounted over SEM stubs with double-sided conductivity tape and a thin layer of gold palladium was applied before capturing images using a Quanta 650 SEM (FEI, The Netherlands).
3
Structural Characterization of Synthesized HES
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The crystal structure of synthesized
HES was examined by powder X-ray diffraction (p-XRD)
using a Panalytical X’Pert Pro MPD diffractometer with Cu Kα
radiation (λ = 0.15418 nm). The morphology and elemental distribution
of the HES was investigated by FEI Quanta 650 SEM operating at 20
kV and 200 keV FEI Talos F200A for TEM. Thermogravimetric analysis
(TGA) was conducted under N2 atmosphere from room temperature
to 600 °C at a heating rate of 15 °C min–1 using a TGA STAR equipment (MettlerToledo). Detailed experimental
results for both X-ray photoelectron spectroscopy (XPS) and electrochemical
analysis are described in theSupporting Information .
HES was examined by powder X-ray diffraction (p-XRD)
using a Panalytical X’Pert Pro MPD diffractometer with Cu Kα
radiation (λ = 0.15418 nm). The morphology and elemental distribution
of the HES was investigated by FEI Quanta 650 SEM operating at 20
kV and 200 keV FEI Talos F200A for TEM. Thermogravimetric analysis
(TGA) was conducted under N2 atmosphere from room temperature
to 600 °C at a heating rate of 15 °C min–1 using a TGA STAR equipment (MettlerToledo). Detailed experimental
results for both X-ray photoelectron spectroscopy (XPS) and electrochemical
analysis are described in the
4
Multilayer GeSe Photodetector Fabrication
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Device Fabrication: Multilayer GeSe was exfoliated from the commercial bulk crystals (2D semiconductors) and transferred to a silicon substrate (300 nm SiO2 on the surface) assisted by scotch tape. Then the electrode patterns were fabricated by an electron‐beam lithography system (FEI Quanta 650 SEM and Raith Elphy Plus) and Cr/Au (10/50 nm) metals were deposited by the thermal evaporation (Nexdap, Angstrom Engineering). In order to remove the residual contamination and enhance the metal–semiconductor contact, the fabricated device was subsequently annealed at 300 °C for 1 h in a gas flow of Ar/H2 (100/5 sccm).
Device Characterizations and Measurements: The morphology and thickness were determined by an optical microscope (BX51, Olympus) and atomic force microscope (Dimension Icon, Bruker). Temperature and polarization‐dependent Raman spectra were performed by a confocal Raman system (Alpha 300R, WITec) with 532 nm laser source. The electrical tests were realized by a semiconductor system (B1500A, Keysight), and the device is in a probe station (CRX‐6.5 K, Lake Shore). For photodetection test, a fixed wavelength of 532 nm laser with tunable power intensity was used as light source.
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Device Fabrication: Multilayer GeSe was exfoliated from the commercial bulk crystals (2D semiconductors) and transferred to a silicon substrate (300 nm SiO2 on the surface) assisted by scotch tape. Then the electrode patterns were fabricated by an electron‐beam lithography system (FEI Quanta 650 SEM and Raith Elphy Plus) and Cr/Au (10/50 nm) metals were deposited by the thermal evaporation (Nexdap, Angstrom Engineering). In order to remove the residual contamination and enhance the metal–semiconductor contact, the fabricated device was subsequently annealed at 300 °C for 1 h in a gas flow of Ar/H2 (100/5 sccm).
Device Characterizations and Measurements: The morphology and thickness were determined by an optical microscope (BX51, Olympus) and atomic force microscope (Dimension Icon, Bruker). Temperature and polarization‐dependent Raman spectra were performed by a confocal Raman system (Alpha 300R, WITec) with 532 nm laser source. The electrical tests were realized by a semiconductor system (B1500A, Keysight), and the device is in a probe station (CRX‐6.5 K, Lake Shore). For photodetection test, a fixed wavelength of 532 nm laser with tunable power intensity was used as light source.
5
Fabrication and Characterization of AgCrS2 Nanosheets
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AgCrS2 nanosheets were transferred to the silica substrate. Then, the Au/AgCrS2/Au devices were fabricated by electron-beam lithography (EBL, FEI Quanta 650 SEM & Raith Elphy Plus) and thermal evaporation coating (Angstrom Engineering, Nexdep). The ionic conductivity of AgCrS2 nanosheets is obtained by fitting the electrochemical impedance spectra (Autolab PGSTAT 302 N) of the Au/AgCrS2/Ag devices at room temperature. The testing frequency range is 1 Hz to 1 MHz. To avoid electromagnetic interference the whole process was operated in a Faraday cage.
6
Fabrication and Characterization of Photodetector and FET Devices
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The laser direct writing (MicroWriter ML Baby‐plus, Durham) and electron beam lithography (FEI Quanta 650 SEM and Raith Elphy Plus) were used to construct the device of two‐probe electrodes (photodetector) and three‐probe electrodes (FET device), separately; and Cr (10 nm) and Au (80 nm) were thermally deposited on the sample as electrodes (Nexdep, Angstrom Engineering). Annealing the device at 200 °C under high purity Ar gas was applied to enhance the electrode–sample contact. A semiconductor analyzer (B1500A, Agilent) with a 365, 532, and 808 nm laser and a probe station (CRX‐6.5K, Lake Shore) were used to measure the electric and photoelectric performances.
7
Characterization of Sulfur Samples
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The content of sulfur was analysed using a thermogravimetric analyser (Diamond PE) under an Ar atmosphere at a heating rate of 10°C min−1 from room temperature to 600°C, with a gas flow-rate of 40 ml min−1. Scanning electron microscope (SEM) observation was carried out on a FEI Quanta 650 SEM operated at 20 kV. Scanning transmission electron microscopy (STEM) was conducted with a Hitachi S-5500 SEM, and energy-dispersive X-ray spectroscopy was applied for collecting elemental signals and mapping. Transmission electron microscopy (TEM) and high-resolution TEM images were recorded with a JEOL-2100 instrument. Powder X-ray diffraction (XRD) was conducted on a Bruker D8 Advance X-ray diffractometer using Cu Kα radiation at a scanning rate of 4° min−1 in the 2θ range from 10° to 70°. Specific surface area, pore volume and pore-size distribution were determined by the Brunauer–Emmett–Teller (BET) method on a Micromeritics ASAP 2020 instrument.
8
SEM and EDX analysis of carbon disks
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For SEM analysis, the carbon disks were then mounted on conventional aluminum stubs and coated with 10 nm carbon using a CCU-010 coater (Safematic, Switzerland). SEM imaging (secondary and backscattered electrons) and EDX analysis was performed on a Quanta 650 SEM (FEI, Thermo Fisher Scientific) at 10 kV. EDX Data was evaluated using Pathfinder 2.4 (Thermo Fisher Scientific). Large field of view stitch images of entire thin sections (secondary and backscattered electrons) were created on a Magellan 400 SEM (FEI, Thermo Fisher Scientific).
9
Characterization of PVDF-HFP/EMIM:TFSI/HMDA Ionic Elastomer
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To characterize the mechanical performance of PVDF-HFP/EMIM:TFSI/HMDA ionic elastomer films, the solution of ionic elastomer was drop casted onto glass slides and cured at room temperature for 12 hours to obtain sample sheets (15 × 4 × 0.08 mm3). The mechanical testing was performed by a ZwickRoell zwickiLine Z0.5 instrument. All the tensile experiments were performed at room temperature (25°C) with a strain rate of 20 mm/min for both stretching and relaxing steps. The scanning electron microscopy (SEM) images were taken by an FEI Quanta 650 SEM.
To characterize the capacitance of the EDL, ionic elastomer films were prepared with the dimension of 20 × 30 × 0.15 mm3. Then, the films were sandwiched between two Ag nanoparticle paste electrodes, with an area of 10 × 10 mm2. The capacitance was measured with a Keysight E4980AL inductance capacitance and resistance (LCR) meter. For the testing of sheet resistance strain of electrodes, electrodes were stretched to varied strains with a customized stretcher, and the resistance values were measured with a customized four-probe platform. To characterize the robustness of electrodes, an electrode was stretched to 50 for 500 times, during which the resistances were measured with the electrometer. The microscope images of ionic elastomer and electrodes were taken with a ZEISS microscope (Axioscope 5).
To characterize the capacitance of the EDL, ionic elastomer films were prepared with the dimension of 20 × 30 × 0.15 mm3. Then, the films were sandwiched between two Ag nanoparticle paste electrodes, with an area of 10 × 10 mm2. The capacitance was measured with a Keysight E4980AL inductance capacitance and resistance (LCR) meter. For the testing of sheet resistance strain of electrodes, electrodes were stretched to varied strains with a customized stretcher, and the resistance values were measured with a customized four-probe platform. To characterize the robustness of electrodes, an electrode was stretched to 50 for 500 times, during which the resistances were measured with the electrometer. The microscope images of ionic elastomer and electrodes were taken with a ZEISS microscope (Axioscope 5).
10
Morphological and Adsorption Analysis
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The morphology investigation was performed with a scanning electron microscope (FEI Quanta 650 SEM operated at 20 kV) and an energy-dispersive X-ray (EDX) spectrometer to detect the elemental signals. TEM images were collected with a TEM field emission from JEOL 2010F powered at 200 kV. The adsorption of the host toward the polysulfide (Na2S6 was chosen as a representative) was measured with a UV–vis spectrometer (Cary 5000) with baseline correction (Varian).
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