The crystallographic phase of the as-synthesized samples was determined with a Panalytical X-Pert X-ray diffractometer (XRD) with a scanning rate of 2.5° per min. The morphology and elemental compositions of the prepared photocatalysts were observed by a scanning electron microscope (SEM) equipped with an energy dispersive X-ray (EDX) spectrometer and transmission electron microscopy (TEM, JEM-2010). X-ray photoelectron spectroscopy (XPS) was performed on an ESCALAB250 instrument (Thermo VG Corp.) The UV-vis spectra were carried out on a spectrometer (Shimadzu UV-3600). The photoluminescence (PL) spectra of the samples were recorded on an Edinburgh Instruments FLS 920 spectrometer at an excitation wavelength of 350 nm.
X pert x ray diffractometer
Manufactured by Malvern Panalytical
Sourced in Netherlands
The X'Pert X-ray diffractometer is a laboratory instrument designed for the analysis of crystalline materials. It utilizes X-ray radiation to determine the atomic and molecular structure of a sample by measuring the diffraction pattern that occurs when the X-rays interact with the crystalline structure. The core function of the X'Pert X-ray diffractometer is to provide detailed information about the composition, structure, and properties of a wide range of materials.
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Lab products found in correlation
Talos f200x tem, by Thermo Fisher Scientific (3 mentions)
Jem 2100f, by JEOL (2 mentions)
Escalab 250xi, by Thermo Fisher Scientific (2 mentions)
Fls920 spectrometer, by Edinburgh Instruments (1 mentions)
Uv 3600, by Shimadzu (1 mentions)
Asap 2020 surface area analyzer, by Micromeritics (1 mentions)
Cary 50 bio uv visible spectrophotometer, by Agilent Technologies (1 mentions)
Mpms 5xl squid magnetometer, by Quantum Design (1 mentions)
Ea 1112 chns o microanalyser, by Thermo Fisher Scientific (1 mentions)
Cary 50 bio uv visible spectrometer, by Agilent Technologies (1 mentions)
Supernova diffractometer, by Agilent Technologies (1 mentions)
5400 esca, by Physical Electronics (1 mentions)
Via raman microscope, by Renishaw (1 mentions)
Asap 2020, by Micromeritics (1 mentions)
Inspect f, by Philips (1 mentions)
Jcm 5000 sem, by JEOL (1 mentions)
Nicolet iz10 spectrometer, by Thermo Fisher Scientific (1 mentions)
Avatar360 ftir spectrometer, by Thermo Fisher Scientific (1 mentions)
Sdt q600, by TA Instruments (1 mentions)
Tg 209 f3 tarsus, by Netzsch (1 mentions)
29 protocols using x pert x ray diffractometer
1
Comprehensive Materials Characterization Techniques
2
Characterization of Zeolite Crystals
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Zeolite crystal sizes were determined with a Carl Zeiss Ltd 40VP Supra Scanning Electron Microscope (SEM). The particle sizes of samples X1, B1 and B2 were also verified by dynamic light scattering (DLS) using a Zetasizer Nano ZS instrument with a 173° backscattering angle geometry. Semi-quantitative chemical analysis was performed on uncoated sample pellets by energy-dispersive X-ray spectroscopy (EDS) using an Apollo 40 SDD detector (EDAX Inc.). The average of five measurements was used in the determinations. X-ray diffraction (XRD) patterns were collected with a PANalytical X'Pert X-ray diffractometer (XRD) employing Cu Kα radiation (40 kV and 30 mA) and a PIXcell detector. Nitrogen adsorption isotherms of the zeolite samples prior to silver ion-exchange were recorded on a Micromeritics ASAP 2020 surface area analyzer at -196 °C. Samples were degassed at 300 °C overnight prior to analysis. BET areas were calculated using the BET equation, whereas external surface areas (SEXT) and micropore volumes (V) were determined by the t-plot method. BJH pore-size distributions were determined from the desorption branch of the isotherms.
3
Comprehensive Physicochemical Characterization
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Elemental analyses (C, H, N, S) and FT-IR (as KBr disks, between 400 cm -1 and 4000 cm -1 ) were recorded on a FLASH EA 1112 CHNS-O microanalyser and a Thermo NicolletAvatar 360 FT-IR spectrometer, respectively. UV-visible spectra between 220 nm and 800 nm were recorded on a Varian Cary 50 bio UV-Visible Spectrophotometer with samples dissolved in ethanol. Magnetic susceptibility measurements on polycrystalline samples were performed on a Quantum Design MPMS5XL SQUID magnetometer. X-ray powder diffraction patterns were recorded on a PANanalytical X′pert X-ray diffractometer with Cu Kα radiation, 1.54184 Å, at room temperature.
4
Characterization of Organic Compounds via Spectroscopic Techniques
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Elemental analyses (of C, H, N, S) and Fourier Transform Infrared (FT-IR) spectra (as KBr disks, between 400 cm−1 and 4000 cm−1) were acquired using a FLASH EA 1112 CHNS-O microanalyzer and a Thermo NicolletAvatar 360 FT-IR spectrometer (Thermo Fisher Scientific, Waltham, MA, USA), respectively.
UV-visible spectra between 220 nm and 800 nm were recorded on a Varian Cary 50 bio UV-visible Spectrometer with samples dissolved in ethanol.
X-ray powder diffraction patterns were recorded on a PANanalytical X’pert X-ray diffractometer with 1.54184 Å Cu-Kα radiation, at room temperature. Single-crystal X-ray diffraction data were collected with an Agilent SuperNova diffractometer with a micro-focus X-ray at the same radiation wavelength. The structure was solved by direct methods with SHELXS-2016 [68 (link)].
UV-visible spectra between 220 nm and 800 nm were recorded on a Varian Cary 50 bio UV-visible Spectrometer with samples dissolved in ethanol.
X-ray powder diffraction patterns were recorded on a PANanalytical X’pert X-ray diffractometer with 1.54184 Å Cu-Kα radiation, at room temperature. Single-crystal X-ray diffraction data were collected with an Agilent SuperNova diffractometer with a micro-focus X-ray at the same radiation wavelength. The structure was solved by direct methods with SHELXS-2016 [68 (link)].
5
Quantifying Crystalline Phases in Si-XLPE Films
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WAXS was used to identify and globally quantify the crystalline phase of the Si-XLPE films. The experiments were conducted with a PANalytical X’Pert X-ray diffractometer (PANalytical, Almelo, The Netherlands). The incident beam was composed of monochromatic Co Kα radiation with wavelength Å. The measurements were conducted with a angle ranging from 10° to 50°. As an example, Figure 2 reports the raw X-ray diffractogram obtained for the unaged Si-XLPE film.
As shown inFigure 2 , all the diffractograms (in green colour) were mathematically deconvolved into two components: crystalline peaks (in blue colour) and amorphous halos (in red colour), using the Fityk commercial software [50 (link)]. In fact, these diffractograms exhibited six main crystalline peaks located at angles of , 27°, 36°, 42°, 43°, and 47° that were respectively assigned to the diffraction planes (110), (200), (120), (111), (201), and (211) of the PE orthorhombic lattice [51 (link)]. In addition, they contained two amorphous halos typically ranging between and 27°, and between and 45°.
The global crystallinity ratio of the Si-XLPE films was determined as follows:
where and are the total areas under the crystalline peaks and the amorphous halos, respectively.
As shown in
The global crystallinity ratio of the Si-XLPE films was determined as follows:
where and are the total areas under the crystalline peaks and the amorphous halos, respectively.
6
Comprehensive Materials Characterization
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The products were characterized using a PANalytical X' Pert X-ray diffractometer (Holland), a field emission scanning electron microscope (SEM, S-4800, equipped with EDS), and a transmission electron microscope (TEM, JEM-2010F). X-ray photoelectron spectroscopy (XPS, Thermo VG Scientific).
7
Comprehensive Material Characterization Protocol
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The X-ray diffraction (XRD) patterns of the samples were examined on a Panalytical X' Pert X-ray diffractometer (Holland). Raman spectra were obtained by a Via Raman microscope (Renishaw, England). The microstructure and porous morphology of the samples were examined using scanning electron microscopy (SEM, FEI, Holand) and high-resolution transmission electron microscopy (HRTEM, JEOL JEM-2100F, Japan). The N2 adsorption-desorption isotherm measurements of the samples were performed using a Micromeritics ASAP 2020 (America) analyzer. The specific surface area was determined using the Brunauer-Emmett-Teller (BET) method, where the samples were degassed under vacuum at 160 °C for 4 h before the measurement. The chemical compositions of the carbon materials were quantitatively analyzed by X-ray photoelectron spectroscopy (XPS, Physical Electronics 5400 ESCA).
8
Extensive Characterization of Ceramic Materials
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Phase analysis for all samples was performed using a Panalytical X'Pert X-ray diffractometer. High resolution XRD patterns for lattice parameter determination were obtained using a Stoe Cu-PSD (position sensitive detector).
Ceramics for SEM were first thermally etched at 90 % of the sinter temperature for 30 minutes. The calcined powders and sintered, thermally etched ceramics were affixed to carbon pads, sputtered with gold, and imaged using a Phillips Inspect F. Energy dispersive Xray analysis was performed using an EDAX EDS detector.
Infrared spectroscopy was performed using a Perkin Elmer Frontier FTIR and GoldenGate Diamond ATR between 4000-400 cm -1 . Samples for FTIR were dried at 180 °C for 24 h before testing to remove surface H2O and CO2. Measurements were taken with the CO2/H2O suppression off, which resulted in some noise in the data (2500-1250 cm -1 ).
Raman spectroscopy was performed using a Renishaw inVia Raman microscope with a 514 nm green laser operated at 20 mW.
Gold paste electrodes were applied to sintered ceramics for electrical testing. Bulk capacitance and tan h (the dissipation factor expressed as the ratio of equivalent series resistance to capacitive resistance) were measured using an LCR meter (Model 4284A, Hewlett Packard, HP). Measurements were taken at the following fixed frequencies: 100 kHz, 250 kHz and 1 MHz at temperatures between 25 and 250 °C.
Ceramics for SEM were first thermally etched at 90 % of the sinter temperature for 30 minutes. The calcined powders and sintered, thermally etched ceramics were affixed to carbon pads, sputtered with gold, and imaged using a Phillips Inspect F. Energy dispersive Xray analysis was performed using an EDAX EDS detector.
Infrared spectroscopy was performed using a Perkin Elmer Frontier FTIR and GoldenGate Diamond ATR between 4000-400 cm -1 . Samples for FTIR were dried at 180 °C for 24 h before testing to remove surface H2O and CO2. Measurements were taken with the CO2/H2O suppression off, which resulted in some noise in the data (2500-1250 cm -1 ).
Raman spectroscopy was performed using a Renishaw inVia Raman microscope with a 514 nm green laser operated at 20 mW.
Gold paste electrodes were applied to sintered ceramics for electrical testing. Bulk capacitance and tan h (the dissipation factor expressed as the ratio of equivalent series resistance to capacitive resistance) were measured using an LCR meter (Model 4284A, Hewlett Packard, HP). Measurements were taken at the following fixed frequencies: 100 kHz, 250 kHz and 1 MHz at temperatures between 25 and 250 °C.
9
Synthesis and Characterization of SRO/STO Superlattices
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The SRO/STO superlattices were synthesized with six‐ and y‐u.c. of the SRO and STO layers, that is, [6|y] superlattice, at 750 °C in 100 mTorr of oxygen partial pressure using pulsed laser epitaxy. To enhance the Raman cross‐section of inelastic light scattering, the SRO/STO superlattices were used with 50 repetitions. Stoichiometric SRO and STO targets were ablated using a KrF laser (248 nm, IPEX868, Lightmachinery) with a laser fluence of 1.5 J cm−2 and a repetition rate of 5 Hz. X‐ray θ–2θ, off‐axis, and reciprocal space map measurements were performed using a high‐resolution PANalytical X'Pert X‐ray diffractometer. X‐ray rocking curve measurements show the excellent crystallinity of the superlattices even after 50 repetitions (Figure S2 , Supporting Information).
10
Film Morphology Characterization Techniques
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Film morphology was characterized through XRD, TEM, and STEM coupled with EDS-mapping. XRD scans of θ–2θ were conducted using a Panalytical X'Pert X-ray diffractometer wit Cu Kα radiation. Bright field TEM, STEM, SAED patterns and EDS-mapping was performed in a FEI Talos F200X TEM. Samples for electron microscopy were prepared, for both cross-section and plan-view, via a standard grinding procedure which entails manual grinding, polishing, dimpling, and a final ion milling step to achieve electron transparency (PIPS 691 precision ion polishing system, 5 keV for cross-section and 4–4.5 keV for plan-view sample).
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