The materials were suspended in EtOH (0.1–0.5 mg/mL final concentration) and probe sonicated. About 3 μL of the suspension was deposited on a silicon wafer substrate and dried at 60 °C for 12 h. Images were collected in high vacuum with a Zeiss Sigma VP Field Emission SEM, using an in-lens detector at 5.0 keV beam energy. The elemental composition of a sample was determined using characteristic X-ray spectrum of the specimen being examined. The EDS analysis was performed in a ‘‘spot mode’’ in which the beam (set at 10 keV) was localized on a single area manually chosen within the field of view. The location was represented on the provided SEM images by a ‘‘+’’. Data was elaborated by means of Bruker Esprit 1.9.
Esprit 1
Manufactured by Bruker
The Esprit 1.9 is a high-performance electron microscopy (EM) analysis software developed by Bruker. It provides advanced image processing and analysis capabilities for a wide range of EM applications, including scanning electron microscopy (SEM) and transmission electron microscopy (TEM).
Automatically generated - may contain errors
Lab products found in correlation
Sigma vp field emission sem, by Zeiss (1 mentions)
Jsm 6510, by JEOL (1 mentions)
Quantax 400, by Bruker (1 mentions)
Jem arm 200f neoarm, by JEOL (1 mentions)
Talos f200x, by Thermo Fisher Scientific (1 mentions)
Mls 1200 mega, by Milestone (1 mentions)
Tecnai osiris, by Thermo Fisher Scientific (1 mentions)
7700 series, by Agilent Technologies (1 mentions)
8454 uv vis spectrophotometer, by Agilent Technologies (1 mentions)
Av 400 mhz spectrometer, by Bruker (1 mentions)
Tecnai osiris microscope, by Thermo Fisher Scientific (1 mentions)
8 protocols using esprit 1
1
SEM Imaging and Elemental Analysis
2
Surface Composition Analysis via EDS
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EDS measurements were carried out to obtain quantitative information on the surface composition. During these measurements, the spectrum of the characteristic X-rays induced by the high-energy electron beam is detected. The acceleration voltage applied in our EDS measurements (20 kV) gives an informal depth of about 4–5 μm in pure carbon [18 (link)]. The spectra were evaluated with Bruker ESPRIT 1.9 software, which uses the standardless P/B-ZAF (peak to background ZAF) method.
Besides the EDS measurements, back-scattered electron (BSE) images were also taken of the surface of the samples. In these images, areas with higher average atomic numbers appear brighter than those with lower ones.
Besides the EDS measurements, back-scattered electron (BSE) images were also taken of the surface of the samples. In these images, areas with higher average atomic numbers appear brighter than those with lower ones.
3
Nanomaterial Characterization by TEM/STEM
4
Nanoparticle Composition Analysis by EDX
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To analyze the nanoparticles composition energy dispersive X-ray (EDX) spectroscopy studies on the nanoparticles were performed using a JEOL JSM6510 scanning electron microscope (SEM) equipped with an energy dispersive X-ray detector (Bruker Quantax 400). The obtained spectra were quantified by using the software Esprit 1.9 (Bruker). The determined compositions of the nanoparticles are summarized in Table S2 in the ESI.†
5
Characterizing PtCo Cathode Nanostructure
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To prepare cross sections of the BOT and EOT cathodes for STEM
analysis,
portions of the MEA were embedded in epoxy resin and then cut by diamond-knife
ultramicrotomy, with a target thickness of ∼75 nm. High-angle
annular dark-field scanning transmission electron microscopy (HAADF-STEM)
and energy-dispersive X-ray spectrum (EDS) images were recorded using
a Talos F200X transmission electron microscope (TEM) (Thermo Fisher
Scientific) operated at 200 kV and equipped with Super-X EDS system
with 4 SDD windowless detectors. The Co composition for each MEA cathode
was obtained from EDS elemental maps (21 nm pixel resolution, 10.9
μm field of view) which was processed with the Esprit 1.9 software
(Bruker). HAADF images and EDS maps of individual PtCo particles were
recorded using a JEM-ARM200F “NEOARM” analytical electron
microscope (JEOL Ltd.) operated at 80 kV and equipped with dual SDD
windowless detectors each with a 100 mm2 active area.
analysis,
portions of the MEA were embedded in epoxy resin and then cut by diamond-knife
ultramicrotomy, with a target thickness of ∼75 nm. High-angle
annular dark-field scanning transmission electron microscopy (HAADF-STEM)
and energy-dispersive X-ray spectrum (EDS) images were recorded using
a Talos F200X transmission electron microscope (TEM) (Thermo Fisher
Scientific) operated at 200 kV and equipped with Super-X EDS system
with 4 SDD windowless detectors. The Co composition for each MEA cathode
was obtained from EDS elemental maps (21 nm pixel resolution, 10.9
μm field of view) which was processed with the Esprit 1.9 software
(Bruker). HAADF images and EDS maps of individual PtCo particles were
recorded using a JEM-ARM200F “NEOARM” analytical electron
microscope (JEOL Ltd.) operated at 80 kV and equipped with dual SDD
windowless detectors each with a 100 mm2 active area.
6
Scanning Electron Microscopy and ICP-AES Analysis
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Scanning electron
microscopy (SEM) experiments were performed using an ESEM instrument
Quanta 250 FEG (FEI, Hillsboro, OR) equipped with an energy-dispersive
spectrometer for X-ray microanalysis (Bruker Nano GmbH, Berlin, Germany).
The energy-dispersive X-ray spectrometer is equipped with a QUANTAX
XFlash 6 | 30 detector with energy resolution ≤126 eV full
width at half maximum (FWHM) at Mnkα. The spectra were collected
and analyzed using ESPRIT 1.9 software (Bruker Nano GmbH). ICP-AES
analyses were performed with an ULTIMA 2 instrument JOBIN YVON in
the radial configuration, with a JY 2501 monochromator calibrated
against carbon lines. The optical path was continuously purged with
nitrogen (2 L/min). The samples of the functionalized frameworks were
dissolved in 2 mL of a mixture of HNO3 65% and H2O2 30% and then heated by microwave irradiation (Milestone,
MLS-1200 MEGA, equipped with TFM inner vessels). Calibration was performed
with standard solutions, 10% of HNO3 on six different metal
concentration levels, ranging from 0.5 to 100 mg/L. No significant
spectral interferences were detected. Data were acquired by considering
the following emission lines: Fe 238.204 nm, Co 228.616 nm, and Mo
202.030 nm. Data acquisition and processing were performed using the
ICP JY v 5.4.2 software (Jobin Yvon).
microscopy (SEM) experiments were performed using an ESEM instrument
Quanta 250 FEG (FEI, Hillsboro, OR) equipped with an energy-dispersive
spectrometer for X-ray microanalysis (Bruker Nano GmbH, Berlin, Germany).
The energy-dispersive X-ray spectrometer is equipped with a QUANTAX
XFlash 6 | 30 detector with energy resolution ≤126 eV full
width at half maximum (FWHM) at Mnkα. The spectra were collected
and analyzed using ESPRIT 1.9 software (Bruker Nano GmbH). ICP-AES
analyses were performed with an ULTIMA 2 instrument JOBIN YVON in
the radial configuration, with a JY 2501 monochromator calibrated
against carbon lines. The optical path was continuously purged with
nitrogen (2 L/min). The samples of the functionalized frameworks were
dissolved in 2 mL of a mixture of HNO3 65% and H2O2 30% and then heated by microwave irradiation (Milestone,
MLS-1200 MEGA, equipped with TFM inner vessels). Calibration was performed
with standard solutions, 10% of HNO3 on six different metal
concentration levels, ranging from 0.5 to 100 mg/L. No significant
spectral interferences were detected. Data were acquired by considering
the following emission lines: Fe 238.204 nm, Co 228.616 nm, and Mo
202.030 nm. Data acquisition and processing were performed using the
ICP JY v 5.4.2 software (Jobin Yvon).
7
Characterization of Cu3Ag7/CF Electrocatalyst
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The morphology features of samples were assessed by using scanning electron microscopy (FEI XL30, 15 kV), as well as transmission electron microscopy (TEM), selective area electron diffraction (SAED, 40 μm aperture), and scanning transmission electron microscopy (STEM) with an FEI Tecnai Osiris (200 kV). Samples for TEM were prepared by suspending dry Cu3Ag7/CF electrocatalyst on carbon-coated 200-mesh copper TEM grids (Ted Pella 01894-F). STEM−energy-dispersive X-ray spectroscopy (EDX) maps were collected using Bruker Esprit 1.9 software and averaged over 8 scans. X-ray diffraction (XRD) patterns were collected on a Philips X’Pert Pro PW3040/00 (PAN analytical) instrument. The scan range was set from 20° to 90° (in 2θ) with a Cu-tube operated at 45 kV and 40 mA. The evolved H2 through the electrolysis process was quantified by gas chromatography (GC, SRI 8610C) equipped with a Molecular Sieve 13 packed column, a HayesSep D packed column, and a thermal conductivity detector, and Ar was used as the carrier gas. The Cu and Ag quantities of the sample were analyzed via inductively coupled plasma mass spectrometry (ICP-MS, Agilent 7700 series) in 2% nitric acid. 1H NMR spectra were recorded in the designated solvents on a Bruker AV 400 MHz spectrometer. UV–vis absorption spectra were collected on an Agilent 8454 UV–Vis Spectrophotometer.
8
Scanning Electron Microscopy of Granules
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For the chemical analysis of granules, 200 nm-thin sections, collected on carbon/formvar coated copper grids, were observed in scanning/transmission electron microscopy (STEM) mode and analyzed by STEM (HAADF) detector, on a Tecnai OSIRIS microscope (FEI) operated at 200 kV. The chemical composition of regions of interest was then analyzed by EDS using the ESPRIT 1.9 software (Bruker).
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