Crystalline phases of material were identified from X-ray diffraction patterns obtained using Bruker D8 Advance X-ray Diffractometer with Cu Kα emitted radiations (V = 40 kV, I = 30 mA, P = 1200 W and λ = 1.548 Å). Thermogravimetric analysis (TGA) profiles of samples were obtained using Discovery TGA 5500 by TA Instruments. Morphology and elemental analysis were obtained by using scanning electron microscope images and energy dispersive X-ray spectrometry from TESCAN VEGA3 scanning electron microscope (HV = 20 kV, beam intensity = 11) equipped with EDS Detector by Oxford Instruments. Types of bonding present on molecular level were analysed by Fourier transform infrared spectrum obtained by CARY 630 FTIR Spectrometer. N2 adsorption/desorption isotherms of as-synthesized samples were acquired from Quantachrome NovaWin instrument. The Brunauer–Emmet–Teller (BET) method was employed to calculate surface area while the Barret–Joyner–Halinda (BJH) method was employed to calculate pore size distribution.
Eds detector
Manufactured by Oxford Instruments
Sourced in United Kingdom, Japan
The EDS (Energy Dispersive Spectroscopy) detector is a core component of analytical equipment used in materials science, life sciences, and other research fields. It is designed to detect and analyze the characteristic X-rays emitted by a sample when it is exposed to a focused electron beam, allowing for the identification and quantification of the elements present in the sample.
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Lab products found in correlation
D8 advanced diffractometer, by Bruker (3 mentions)
Mira3 fe sem microscope, by TESCAN (3 mentions)
Em10c 100 kv series microscope, by Zeiss (3 mentions)
Optima 7300dv icp oes analyzer, by PerkinElmer (2 mentions)
Nicolet nexus 670 ft ir, by Bruker (2 mentions)
X pert pro, by Malvern Panalytical (2 mentions)
Cary 630 ftir spectrometer, by Agilent Technologies (1 mentions)
D8 advance x ray diffractometer, by Bruker (1 mentions)
Discovery tga 5500, by TA Instruments (1 mentions)
Stem su8230, by Hitachi (1 mentions)
Cpd300, by Leica (1 mentions)
Desk 5 tsc sputter coater, by Denton (1 mentions)
Jsm 7200f, by JEOL (1 mentions)
Ultracut uct microtome, by Leica (1 mentions)
Su3500, by Hitachi (1 mentions)
H 9500, by Hitachi (1 mentions)
Inca software, by Oxford Instruments (1 mentions)
Tecnai20f, by Thermo Fisher Scientific (1 mentions)
Carbon coated copper tem grid, by Agar Scientific (1 mentions)
Axs xflash detector 4010, by Bruker (1 mentions)
25 protocols using eds detector
1
Comprehensive Materials Characterization
2
Dental Material Microstructural Analysis
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Two dentin specimens from each tooth, which represents 10 specimens from each tested material, were prepared for SEM and EDX analyses. The same specimens were used for both analyses. The samples were dried in a graded ethanol series (50–100%), and then sputter-coated with gold. SEM was performed under high-vacuum conditions (Hitachi SU8230 STEM). Two photomicrographs were captured for each section to observe details at the tooth-restoration interface (the intimate adaptation of the adhesive-resin layer to the dentine, the hybrid layer) and the materials’ structures. The photomicrographs were analyzed by a single examiner (LB) using a blinded protocol, and measurements of the hybrid layers and resinous tags penetrating the dentin were performed using ImageJ software. EDX was performed using a Hitachi SU8230 STEM under the following conditions: 30 kV acceleration voltage, 10 µA extraction current, 15 mm working distance, Oxford Instruments EDS detector placed inside the sample chamber, and AZtec Software. Measurements were performed at the same magnifications of similar surfaces (three ROIs) for all samples: the healthy tooth, the added restorative material, and the transition material between the healthy tooth and the restorative material. Ten measurements for each material were averaged to provide a single mean value for each parameter for each specimen.
3
Electron Microscopy of Mineral Samples
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The samples were rehydrated with water in an oven at 60 °C, fixed in 2.5% glutaraldehyde for two days, washed in sodium cacodylate buffer, and then passed through 30%, 50%, 70%, 90%, and 100% ethanol solutions. The samples were then dried in a Leica CPD300 critical point dryer (Leica Microsystems, Wetzlar, Germany) supplied with liquid CO2. The dried samples were mounted on aluminum stubs with double-sided adhesive carbon tapes and coated with platinum using a Desk V TSC sputter coater (Denton Vacuum, Moorestown, NJ, USA) supplied with argon gas. The samples were imaged using a JSM-7200F field-emission SEM (JEOL Ltd., Tokyo, Japan). Mineral elements were mapped and analyzed using an EDS detector (Oxford Instruments, Oxford, UK) attached to the SEM.
4
Characterization of Membrane Samples
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The membrane samples (2 × 5 mm) wrapped with epoxy resin were smoothed and wrapped with conductive tape for SEM analysis. After sputtering with Pt, the cross-sectional images and elemental distribution of the samples were obtained using a Hitachi SU3500 device equipped with an EDS detector (Oxford Instruments) at an accelerating voltage of 15.0 kV. For TEM analysis, the membrane samples were stained with a 0.5 M Pb(OAc)2 aqueous solution, washed with water, and dried. The stained membranes were embedded in epoxy resin, sectioned to 50 nm thickness with Leica microtome Ultracut UCT, and then placed on a copper grid. The TEM images were captured using the Hitachi H-9500 at an accelerating voltage of 200 kV.
5
SEM Analysis of Material Composition
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Few micrograms of the samples were analysed using a JEOL JSM-6610LV Scanning Electron Microscope with an Oxford Instrument EDS detector. All samples were uncoated. Images were acquired between 3 and 5 kV, with a spot intensity of 53, in secondary electron detector mode (SED). Elemental composition analyses were conducted at 20 kV with a spot intensity of 53 using the backscatter electron detector (BSE). The dimensions of the acquisition areas were adjusted based on features visible on the uncoated surface in BSE mode. Elemental composition was based on the acquired sum spectrum.
Spectra interpretation and image management were completed using Inca software (Oxford Instruments, UK).
Spectra interpretation and image management were completed using Inca software (Oxford Instruments, UK).
6
Characterizing Gold-Polymer Nanohybrids via TEM
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Transmission electron microscopy
(TEM) was used to determine the morphology of the gold-polymer nanohybrids.
Bright field TEM and high angle annular dark field scanning TEM (HAADF-STEM)
images of the particles were acquired using a Tecnai20F (FEI) microscope
equipped with a Gatan CCD camera (model 694) and an energy-dispersive
X-ray spectroscopy (EDS) detector (Oxford Instrument) operated at
an accelerating voltage of 200 kV. Samples were dissolved in Milli-Q
water (1 mg mL–1). The samples were then left at
the desired temperature (10 or 45 °C) for 30 min before being
drop-deposited on 200 mesh carbon-coated copper TEM grids (Agar Scientific)
prior to analysis.
EDS analysis was used to quantify the chemical
composition of the gold-polymer nanohybrids. X-ray counts were recorded
during a 1 min period at 10 kV and analyzed using INCA Energy 3000
software (Oxford Instruments).
(TEM) was used to determine the morphology of the gold-polymer nanohybrids.
Bright field TEM and high angle annular dark field scanning TEM (HAADF-STEM)
images of the particles were acquired using a Tecnai20F (FEI) microscope
equipped with a Gatan CCD camera (model 694) and an energy-dispersive
X-ray spectroscopy (EDS) detector (Oxford Instrument) operated at
an accelerating voltage of 200 kV. Samples were dissolved in Milli-Q
water (1 mg mL–1). The samples were then left at
the desired temperature (10 or 45 °C) for 30 min before being
drop-deposited on 200 mesh carbon-coated copper TEM grids (Agar Scientific)
prior to analysis.
EDS analysis was used to quantify the chemical
composition of the gold-polymer nanohybrids. X-ray counts were recorded
during a 1 min period at 10 kV and analyzed using INCA Energy 3000
software (Oxford Instruments).
7
Scanning Electron Microscopy for Material Analysis
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FESEM images were recorded with an FESEM Zeiss Merlin instrument, equipped with an EDS detector (Oxford Instruments, Abingdon-on-Thames, UK).
8
Structural and Elemental Analysis of Wood Carbon Monolith
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Texture properties of the fresh and spent wood carbon monolith are determined by obtaining N2 and CO2 adsorption–desorption isotherms obtained at 77 K and 298 K by using a Micromeritics model ASAP 2020 instrument. SEM observation is carried out by using a JEOL JSM-7800F instrument (20 kV and 10 mm working distance) instrument equipped with a Bruker AXS XFlash Detector 4010 (MA, USA). EDS detector from Oxford Instrument is further equipped on the SEM instrument to perform the samples’ elemental composition and surface mapping analysis. TEM was performed at room temperature on a JEOL JEM-2100 microscope equipped with a LaB6 gun operated at 200 kV. Eurofins Biofuel & Energy Testing Sweden AB (https://www.eurofins.com/ ) conducted ultimate elemental analysis and the corresponding ash content and composition analysis of the wood carbon monolith sample. Raman spectra were obtained by using a Tyrode I Raman microscope equipped with a 532-nm wavelength diode laser. For a more detailed understanding of the matter, kindly refer to section 2 in the Supplementary Information.
9
Comprehensive Characterization of LiFePO4-PANI
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The LiFePO4–PANI was characterized by X-ray powder diffraction (PXRD), using an X’Pert3 PANalytical diffractometer with a scan rate of 0.02 °/s, by Cu–Kα radiation (λ = 1.5406 Å, 45 kV, 20 mA). X’pert Highscore software (PANalytical. B. V, Lelyweg, the Netherlands) was used for the identification of the phases. The morphologies of the samples were determined by S-4800 series field-emission high-resolution scanning electron microscope (SEM) (Hitachi, Tokyo, Japan), equipped with an EDS detector (Oxford Instruments, Abingdon, UK). The powder samples were mounted in the sample holder and sputtered with a thin layer of Pt/Pd. Fourier transform infrared spectroscopy (FTIR) was done on a Spectrum 100 spectrometer (Perkin Elmer), in the wavelength range of 4000–400 cm−1, with a resolution of 1 cm−1. Thermogravimetric analysis (TGA) (LABSYS evo STA 1150, SETARAM Instrumentation, Caluire-et-Cuire, France) was carried out on 20 mg of specimen, from room temperature to 800 °C, with a heating rate of 2 °C/min.
10
Multi-Technique Characterization of Materials
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X-ray diffraction (XRD) pattern was carried out on a Rigaku D/Max-2500 diffractometer equipped with a Cu Kα1 radiation (λ = 1.54 Å). Scanning electron microscopic images (SEM) were collected on a JEOL scanning electron microscope (S-4800, Japan). Transmission electron microscopic images (TEM) were obtained by a JEM-2100F microscope (JEOL, Japan) equipped with an EDS detector (Oxford Instrument, UK). X-ray photoelectron spectroscopy (XPS) was performed on an ESCALab220i-XL electron spectrometer (VG Scientific, UK) with a monochromatic Al Kα source. The gas products for CO2 reduction were measured on a gas chromatography (GC, Agilent Technologies 7890B). The liquid products were analyzed with a Bruker AVANCE 600 using dimethyl sulphoxide (DMSO) as an internal standard.
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