The morphology of the materials was confirmed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images, which were obtained using a Carl Zeiss SIGMA field-emission scanning electron microscope and a JEOL JEM-F200 microscope, respectively. X-ray diffraction (XRD) patterns were evaluated by the Bruker New D8-Advance, which operated at 40 kV and 40 mA using CuKa radiation (1.5406 Å), to verify the crystalline part of the materials. To identify the components of each sample, X-ray photoelectron spectroscopy (XPS) was conducted using the Thermo Fisher Scientific K-alpha + instrument that set the carbon peak as standard (C 1 s = 284.5 eV). The surface area was measured from the BET nitrogen adsorption/desorption isotherms using a Micromeritics 3Flex analyzer. The pore volume and diameter were calculated by exploring the desorption of the isotherm using the Barrett–Joyner–Halenda (BJH) method. The functional groups and binding of elements were analyzed by Fourier-transform infrared (FT-IR) spectroscopy using a Thermo Scientific (Waltham, MA, USA) Nicolet 6700 spectrometer.
3flex analyzer
Manufactured by Micromeritics
Sourced in United States
The 3Flex is a versatile gas adsorption analyzer that can be used to determine the surface area, pore volume, and pore size distribution of a wide range of materials. The instrument uses advanced data analysis techniques to provide accurate and reliable results.
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Lab products found in correlation
Nicolet is50, by Thermo Fisher Scientific (3 mentions)
K alpha instrument, by Thermo Fisher Scientific (1 mentions)
Jem f200 microscope, by JEOL (1 mentions)
Nicolet 6700 spectrometer, by Thermo Fisher Scientific (1 mentions)
New d8 advance, by Bruker (1 mentions)
K α1 spectrometer, by Thermo Fisher Scientific (1 mentions)
Uv vis, by Thermo Fisher Scientific (1 mentions)
Jsm 7600f, by JEOL (1 mentions)
D max 2400, by Rigaku (1 mentions)
Avance 400 mhz spectrometer, by Bruker (1 mentions)
7900 icp ms, by Agilent Technologies (1 mentions)
Ultima 4 diffractometer, by Rigaku (1 mentions)
S 4800 microscope, by Hitachi (1 mentions)
D8 diffractometer, by Bruker (1 mentions)
Jem arm200f, by JEOL (1 mentions)
Uv vis nir spectrophotometer, by Jasco (1 mentions)
X pert pro powder x ray diffractometer, by Malvern Panalytical (1 mentions)
Nmr system 400 mhz spectrometer, by Agilent Technologies (1 mentions)
Jem 2100f, by JEOL (1 mentions)
S 4300, by Hitachi (1 mentions)
13 protocols using 3flex analyzer
1
Comprehensive Materials Characterization
2
Comprehensive Characterization of ZnO/MgO/Cr2O3 Nanofibers
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The investigation of the binding energy and ionization states of the existing atoms of the ZnO/MgO/Cr2O3 NFs were evaluated by XPS analysis performed on a K-α1 spectrometer (Thermo scientific, K-α1 1066) with an excitation radiation source (A1 Kα1, beam spot size = 300.0 μm, pass energy = 200.0 eV, pressure ∼ 10–8 torr). The photosensitivity and existing functional groups of the synthesized ZnO/MgO/Cr2O3 NFs were evaluated by the application of UV-Vis (Thermo Scientific) and FTIR (Thermo Scientific NICOLET iS50, Madison, WI, USA) spectroscopic analysis. The structural morphology and elemental compositions (shape, size, and structure) of the synthesized ZnO/MgO/Cr2O3 NFs were inspected by FESEM (JEOL, JSM-7600F, Japan) furnished with EDS. The phase crystallinity of the nanomaterial is an important measurable characteristic, and it is able to determine the unit cell dimension. Therefore, the phase crystallinity was studied by powder X-ray diffraction. The N2 adsorption–desorption isotherms were carried out by the 3Flex analyzer (Micromeritics, USA) at 77.0 K. The specific surface area (SBET) was calculated using multi-point adsorption data from the linear segment of the N2 adsorption isotherms using BET theory. Finally, the electrochemical detection was performed by a Keithley electrometer (USA).
3
Fabrication and Characterization of Mesoporous Oxidized Porous Silicon
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A boron-doped
p-type silicon wafer of dimensions 25 × 25 × 0.525 mm, with
a resistivity of 0.01–0.02 Ω cm and orientation (100),
was etched electrochemically in a 1:1 mixture of 48% hydrofluoric
acid and ethanol, following the procedures detailed in the study by
Sailor, Section 2.8.8 A current density
of 120 mA/cm2, applied for 115 s, resulted in a cylindrical
porous layer. This layer had a diameter of 1.5 cm, thickness of approximately
8 μm [measured by scanning electron microscopy (SEM), seeFigure 7 ], and porosity of
approximately 50% (calculated by the spectroscopic liquid infiltration
method8 ).
The freshly etched porous
silicon was then thermally oxidized in
oxygen at 800 °C for 16 h, resulting in a porous silica layer
on top of a crystalline silicon substrate. This process improves stability
because an uncontrolled native oxide layer otherwise forms on the
surface of unoxidized silicon.
Nitrogen isotherm analysis (3Flex
Analyzer, Micromeritics) was
carried out on an oxidized sample, and the surface area per gram was
found by the Brunauer–Emmett–Teller adsorption isotherm
analysis to be 120.4324 m2/g. The Barrett–Joyner–Halenda
adsorption pore size distribution, which is shown in Figure S2 in
theSupporting Informatio n, gave the average
pore diameter as 23 nm. The material, therefore, is classified as
mesoporous by traditional IUPAC definitions (as its pores are between
2 and 50 nm diameter).
p-type silicon wafer of dimensions 25 × 25 × 0.525 mm, with
a resistivity of 0.01–0.02 Ω cm and orientation (100),
was etched electrochemically in a 1:1 mixture of 48% hydrofluoric
acid and ethanol, following the procedures detailed in the study by
Sailor, Section 2.8.8 A current density
of 120 mA/cm2, applied for 115 s, resulted in a cylindrical
porous layer. This layer had a diameter of 1.5 cm, thickness of approximately
8 μm [measured by scanning electron microscopy (SEM), see
approximately 50% (calculated by the spectroscopic liquid infiltration
method8 ).
The freshly etched porous
silicon was then thermally oxidized in
oxygen at 800 °C for 16 h, resulting in a porous silica layer
on top of a crystalline silicon substrate. This process improves stability
because an uncontrolled native oxide layer otherwise forms on the
surface of unoxidized silicon.
Nitrogen isotherm analysis (3Flex
Analyzer, Micromeritics) was
carried out on an oxidized sample, and the surface area per gram was
found by the Brunauer–Emmett–Teller adsorption isotherm
analysis to be 120.4324 m2/g. The Barrett–Joyner–Halenda
adsorption pore size distribution, which is shown in Figure S2 in
the
pore diameter as 23 nm. The material, therefore, is classified as
mesoporous by traditional IUPAC definitions (as its pores are between
2 and 50 nm diameter).
4
Comprehensive Materials Characterization with Advanced Analytical Techniques
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The crystallites of samples were observed by XRD with Rigaku-Dmax 2400 diffractometer. The morphology and composition of samples were checked using SEM and EDX analysis with Quanta 250 instrument. Single-component adsorption isotherms for N2 and CO2 were measured with Micromeritics 3Flex analyzer. FT-IR spectra of samples were detected by the FTIR-850 spectrometer and KBr was dried overnight in an oven prior to analysis. The ICP result of the products was measured by an Agilent 7900 ICP-MS.
Solid-state 27Al and 29Si Magic Angle Spin Nuclear Magnetic Resonance (MAS NMR) spectra were recorded by Bruker Avance 400 MHz spectrometer using a 4 mm diameter zirconia rotor. 27Al MAS NMR measurement was carried at spinning rate of 14 kHz and pulse width of 1.2 μs (45°). 29Si MAS NMR measurement was carried at spinning rate of 12 kHz and pulse width of 1.6 μs (30°). Pyridine infrared (Py-IR) spectra were obtained on a Nicolet iS50 FT-IR Spectrometer, and the details are as follows. Samples were pressed into round disk, vacuum pretreated at 400 °C for 1 h, cooled to room temperature, imported pyridine vapor and adsorbed for 20 min, and then desorption of pyridine was carried out at 150, 300 and 400 °C, respectively. Finally, spectra were recorded after the temperature decreased to room temperature.
Solid-state 27Al and 29Si Magic Angle Spin Nuclear Magnetic Resonance (MAS NMR) spectra were recorded by Bruker Avance 400 MHz spectrometer using a 4 mm diameter zirconia rotor. 27Al MAS NMR measurement was carried at spinning rate of 14 kHz and pulse width of 1.2 μs (45°). 29Si MAS NMR measurement was carried at spinning rate of 12 kHz and pulse width of 1.6 μs (30°). Pyridine infrared (Py-IR) spectra were obtained on a Nicolet iS50 FT-IR Spectrometer, and the details are as follows. Samples were pressed into round disk, vacuum pretreated at 400 °C for 1 h, cooled to room temperature, imported pyridine vapor and adsorbed for 20 min, and then desorption of pyridine was carried out at 150, 300 and 400 °C, respectively. Finally, spectra were recorded after the temperature decreased to room temperature.
5
CO2 Adsorption Study of Adsorbents
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The CO2 adsorption
test of all of the adsorbents was conducted
using a Micromeritics 3Flex Analyzer in the static volumetric mode.
The CO2 adsorption isotherms were collected at 25 and 45
°C at pressures of up to 1 bar in the pressure steps of 50 mbar.
Similarly, N2 adsorption isotherms were collected at 25
°C at pressures of up to 1 bar in the pressure steps of 50 mbar.
A fresh sample of approximately 100 mg was used for each adsorption
run. Prior to the analysis, the adsorbents were degassed at 200 °C
with a ramp rate of 5 °C under a high vacuum for 6 h to remove
any trapped volatile matter carried from their synthesis and water
vapor adsorbed from ambient air. The CO2 and N2 adsorption findings were evaluated using the dry weight of each
adsorbent. In addition, CO2/N2 selectivity was
calculated at 1 bar, and the recyclability of adsorbents was tested
using pressure swing adsorption (PSA) to check the reusability of
the adsorbents and also determine the isosteric heat of adsorption.
test of all of the adsorbents was conducted
using a Micromeritics 3Flex Analyzer in the static volumetric mode.
The CO2 adsorption isotherms were collected at 25 and 45
°C at pressures of up to 1 bar in the pressure steps of 50 mbar.
Similarly, N2 adsorption isotherms were collected at 25
°C at pressures of up to 1 bar in the pressure steps of 50 mbar.
A fresh sample of approximately 100 mg was used for each adsorption
run. Prior to the analysis, the adsorbents were degassed at 200 °C
with a ramp rate of 5 °C under a high vacuum for 6 h to remove
any trapped volatile matter carried from their synthesis and water
vapor adsorbed from ambient air. The CO2 and N2 adsorption findings were evaluated using the dry weight of each
adsorbent. In addition, CO2/N2 selectivity was
calculated at 1 bar, and the recyclability of adsorbents was tested
using pressure swing adsorption (PSA) to check the reusability of
the adsorbents and also determine the isosteric heat of adsorption.
6
Characterization of Nanoparticle Materials
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The phase composition and structure of the obtained NMs were characterized by XRD with Cu Kα radiation (Rigaku Ultima IV diffractometer, Japan). The size of the crystallites was calculated by the Scherrer equation using the main (111) peak. Raman spectrum study was carried out under a 780 nm laser using a 20′ Senterra Raman microscope (Bruker, Germany). Transmission electron microscopy (TEM) images were taken on JEM-2100, 200 kV LaB6 instrument (JEOL, Japan) using a carbon-coated copper grid for samples’ preparation. The surface area and pore characteristics of the samples were measured using 3Flex analyzer (Micromeritics, Germany). Before measurements, 0.5 g of powder of each sample was degassed for 12 h under vacuum (0.05 mbar) at 300 °C. Surface area and pore characteristics were calculated using 3Flex software by the BET and DFT modeling, respectively.
The XPS spectra were recorded using electron spectrometer PHOIBOS 150 MCD-9 (SPECS, Germany), equipped with an X-ray tube (magnesium anode, hν = 1253.6 eV). The vacuum in the spectrometer chamber during the experiment was kept less than 3·10−8 Pa. The source power was 225 W and the spectra were recorded in the constant transmission energy mode (40 eV for full spectra and 10 eV for individual lines). The full spectra were recorded with a step of 1.00 eV and individual lines, with a step of 0.05 eV.
The XPS spectra were recorded using electron spectrometer PHOIBOS 150 MCD-9 (SPECS, Germany), equipped with an X-ray tube (magnesium anode, hν = 1253.6 eV). The vacuum in the spectrometer chamber during the experiment was kept less than 3·10−8 Pa. The source power was 225 W and the spectra were recorded in the constant transmission energy mode (40 eV for full spectra and 10 eV for individual lines). The full spectra were recorded with a step of 1.00 eV and individual lines, with a step of 0.05 eV.
7
Soil Surface Area Characterization
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Nitrogen sorption was used to determine the surface area of the soil samples taken from the field (Table 2 ) and the CWs (Table 3 ). Prior to the analysis, samples were oven dried at 56°C until the mass stabilized. Subsequently, the samples were degassed at 60°C and 0.1 mm Hg, using a Micromeritics Smart VacPrep system (Micromeritics, Norcross, GA, USA). The nitrogen sorption measurements were conducted using a Micromeritics 3Flex analyzer, using the Brunauer-Emmett-Teller (BET) method to calculate the surface area of the soil. The measurements obtained were used to normalize the bacterial count data by surface area.
8
Comprehensive Characterization of Microstructures
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The morphologies of the samples were investigated by using FESEM (Zeiss Supra 4VP) and transmission electron microscopy (TEM, JEOL JEM-ARM200F, with acceleration voltage of 200 keV). The samples for TEM measurements were suspended in ethanol and supported onto a holey carbon film on a Cu gird. FESEM images were taken on a Hitachi S-4800 microscope. The crystalline microstructures of samples were characterized by using XRD diffractometer (Bruker D8 diffractometer) with a Cu Kα radiation source (λ = 0.15406 nm). N2 adsorption-desorption isotherms were recorded on a Micromeritics 3Flex analyzer at the temperature of 77 K. The samples were degassed in a vacuum at 150 °C for 6 h and the Brunauer–Emmett–Teller (BET) method was utilized to calculate the specific surface areas and pore size. The micropore volumes were determined from Dubinin–Radushkevich (DR) equation with both N2 adsorption at 77 K and CO2 adsorption at 273 K. The total pore volume was determined from the N2 adsorbed amount at P/P0 = 0.99 according to the Gurvitch rule. Thermogravimetric analysis (TGA) curves were acquired on a STA 449 C thermobalance with a temperature ramp of 10 °C min−1.
9
Analytical Characterization of DPC-Cx Materials
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Scanning transmission electron microscopy (STEM) analysis was carried out on an FEI-TITAN operated at an accelerating voltage of 300 kV. For sample preparation, powders of the DPC-Cx were dispersed in ethanol with the assistance of sonication for 10 s, and a drop of solution was dropped onto a holey carbon-coated 200 mesh TEM grid. Excess liquid was immediately wicked away with blotting paper and then air dried before exposing the sample to an electron beam and plasma cleaning for 5 s. X-ray diffraction patterns were recorded using a Panalytical X'Pert Pro powder X-ray diffractometer using Cu-Kα radiation. UV-DRS measurements were carried out using a JASCO UV/vis/NIR spectrophotometer. The surface area was obtained using the Brunauer–Emmett–Teller (BET) theory from N2 physisorption data recorded using a Micromeritics 3Flex analyzer. Approximately 100 mg of each sample was degassed at 120 °C for 12 h prior to N2 sorption analysis.
10
Comprehensive Material Characterization
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The NMR spectra were obtained on a Varian NMR System 400 MHz Spectrometer. The SEM analysis was performed on Hitachi S-4300 operated at 16 keV. TEM images was obtained by using a JEOL (JEM-2100F) and operated at the accelerating voltage of the electron beam 200 kV. The N2 adsorption-desorption isotherms were measured using the 3Flex analyzer (Micromeritics, USA) at 77 K. The metal ion concentrations were measured by atomic absorption spectrophotometer (AAS, Hitachi, Z-2300).
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