We used X-ray diffractometry (XRD) for structural analysis with a Brucker D4 Endeavor X-ray diffractometer coupled with CuKα radiation (Bruker D4 Endeavor, Bruker, Billerica, MA, USA). The measurements were performed at room temperature with a time step of 30 s within the range of Bragg’s angle 2 θ from 20° to 80°, with an angle step of 0.036°. The XRD utilized a Cu anode with a wavelength of 0.154 nm.
D4 endeavor
Manufactured by Bruker
Sourced in United States, Germany
The D4 Endeavor is an X-ray diffractometer designed for powder diffraction analysis. It is capable of collecting high-quality X-ray diffraction data for phase identification, structure determination, and quantitative analysis of polycrystalline materials.
Automatically generated - may contain errors
Lab products found in correlation
Diffrac eva v4, by Bruker (1 mentions)
760d electrochemical workstation, by CH Instruments (1 mentions)
Quanta 200, by Thermo Fisher Scientific (1 mentions)
Nova nanosem 200, by Thermo Fisher Scientific (1 mentions)
Cary 500 spectrometer, by Agilent Technologies (1 mentions)
Jem f200, by JEOL (1 mentions)
Labram hr evolution, by Horiba (1 mentions)
Discovery dsc, by TA Instruments (1 mentions)
N n dimethylacetamide, by Merck Group (1 mentions)
Jem 2100, by JEOL (1 mentions)
Tristar 2 3020, by Micromeritics (1 mentions)
Spectrum two, by PerkinElmer (1 mentions)
11 protocols using d4 endeavor
1
Structural Analysis of Materials by XRD
2
X-ray Diffraction of Crystalline Materials
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X-ray diffraction (XRD) was performed using a D4 Endeavor diffractometer (Bruker AXS GmbH, Karlsruhe, Germany) at room temperature. A quartz monochromator Cu Ka1 radiation source (λ = 0.1541 nm) and a Sol-X energy dispersive detector were used. The angular range (2ϑ) was in the range from 10° to 70°, with a step size of 0.02° and collection time of 4 s.
3
Cold Gas Spraying of Sputtering Target
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Example 3
Commercial Mo, Al and Ti powders suitable for cold gas spraying were sprayed by means of cold gas spraying onto an Al tube as support material. The powders were conveyed from separate containers. The chemical composition was set via the transport rates of the individual powders. The microstructure of the resulting sputtering target containing 20 at % of Al and 5 at % of Ti is shown in cross section (scanning electron micrograph) in
4
Crystallography Analysis of Composite Membranes
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The crystallography pattern of composite membranes was obtained using a diffractometer D4 Endeavor (Bruker, Billerica, MA, USA) with Cu Kα radiation (λ = 1.5406 A) in a continuous scan mode and an energy dispersive detector from Sol-XE (Bruker, Karlsruhe, Germany). A filament current of 30 mA and an acceleration voltage of 45 kV were applied. Diffraction angles were between 5° and 80°, while the scan step was 0.02°. By using JCPDS standard cards, the type of formed minerals was evaluated.
5
XRPD Analysis for Crystallinity Screening
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XRPD was used to test all samples for potential crystallinity. The XRPD data were collected with a D4 Endeavor (Bruker Corporation, United States) at room temperature. X-rays were generated from a copper source (Cu Kα 35 KV × 50 mA). A VÅNTEC detector collected scattered light in a range between 4 and 30° (step size 0.016°, integration time 1 s). Approximately 15–25 mg of the powder samples were transferred to quartz specimen holders and levelled using a glass slide. Crystallinity in the powders was assessed qualitatively from the collected powder diffraction patterns.
6
XRD Analysis of Edible Oleogels
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XRD analysis was performed using a Bruker D4 Endeavor (Karlsruhe, Germany). EC powder and oleogels were gently spread onto the sample holder and tested in that form. The pellets of BW and CRW were firstly melted in a water bath and then poured into a Plexiglass mould and allowed to cool down. Raw ingredients (EC powder, BW and CRW) and oleogels were examined at intervals of 0.02° with a 2θ range from 5 to 40° at room temperature. The diffractometer was equipped with a Cu-Kα radiation source operated at 40 kV and a current of 35 mA at 1.5 Å wavelength. The diffractograms were analysed in the DIFFRAC EVA V4.2 software (Bruker AXS Materials Research Software, Karlsruhe, Germany).
7
X-ray Diffraction Analysis of Crystal Structure
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Crystal structure was determined using the X-ray diffraction (XRD) diffractometer D4 ENDEAVOR (Bruker, Karlsruhe, Germany). Diffraction angle was chosen in the range of 2θ from 10° to 80°, with increments of 0.02° for 2θ and 0.75 s of measurement time per step. Analysis of the measured data was performed with X’Pert HighScore (PANalytical B.V., version 3.0.5) software. Phase quantifications and associated crystal structure analyses were carried out by Rietveld refinement using (Version 4.2.2) software. The errors of each fit were calculated individually and are reported in Table 1 , Table 2 and Table 3 .
8
Comprehensive Analytical Characterization of Sample
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A FEI Quanta 200 scanning electron microscope (SEM) with an attached energy-dispersive X-ray spectrometer (EDS) was used to check the morphologies and to do the elemental analysis of the samples. The crystal structure of the sample was obtained through X-ray diffraction (XRD) analysis using a Bruker D4 endeavor. A thermo-scientific K-alpha system was used to conduct high-resolution X-ray photoelectron spectroscopy (XPS). The machine consisted of an Al Kα monochromated X-ray source through which the samples were scanned. The sample scanning was done with a dwell time of 50 ms−1 and pass energy of 50 eV. Electrochemical measurements were conducted using a CHI 760D electrochemical workstation (CH instruments).
9
Characterization of Cobalt Oxysulfide Micro-Cages
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An FEI Nova NanoSEM 200 was used to investigate the micro-cage structure of cobalt oxysulfide. The crystal lattices and chemical composition of the material were studied under a JEOL JEM-F200 transmission electron microscopy (TEM) with an energy-dispersive X-ray spectroscopy (EDS) detector equipped (accelerating voltage of 200 kV). X-ray diffraction (XRD) measurements were conducted on a Bruker D4 ENDEAVOR with a monochromatic Cu Kα radiation source (λ = 0.154 nm) equipped. X-ray photoelectron spectroscopy (XPS) was performed on a Krato AXIS Supra XPS (dual Al/Ag monochromatic X-ray source equipped) using Al Kα X-rays at 1486.7 eV. The measured XPS spectra were analyzed using CasaXPS (version 2.3.24). The material optical absorption property was investigated using a Cary 500 spectrometer, in which the UV-Vis-NIR spectra were measured on a drop-casted material sample upon a glass substrate. A HORIBA LabRAM HR Evolution was utilized to study the Raman spectra of cobalt oxysulfide with the excitation wavelength of 532 nm.
10
Characterization of Pharmaceutical Samples
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Powder X-ray diffraction (PXRD) was performed by preparing the samples using a flat plate diffraction patterns collected on a D4 Endeavor (Bruker Corporation, Billerica, Massachusetts, USA). The scan was carried out between 2° and 55° 2θ using CuKα radiation with a secondary graphite monochromator.
Differential scanning calorimetry (DSC) was performed in dry nitrogen gas using a Discovery DSC (TA Instruments -A division of Waters Ltd, Herts, UK). The DSC was calibrated using indium at heating rate of 10°C/min. The samples (2.5 -3 mg) were analysed in a T-zero standard pan at heating rate of 10°C/min over the range from 30°C to 100°C. Due to sample limitations only one measurement was made.
Headspace gas chromatography (HS-GC) was performed using a 6892N Network GC system coupled to a 7694 HS sampler (Agilent Technologies, CA, US). Around 20 mg of each sample was dissolved in N,N-dimethylacetamide (≥99%) purchased from Sigma Aldrich (Dorset, UK). A liquid-vapour equilibrium was established by heating the solution in a sealed vial and an aliquot of the headspace vapour was analysed by capillary GC. Quantification of each volatile impurity was achieved by comparison of the chromatographic peak areas of external reference standards with the peak areas of the test sample solutions.
Differential scanning calorimetry (DSC) was performed in dry nitrogen gas using a Discovery DSC (TA Instruments -A division of Waters Ltd, Herts, UK). The DSC was calibrated using indium at heating rate of 10°C/min. The samples (2.5 -3 mg) were analysed in a T-zero standard pan at heating rate of 10°C/min over the range from 30°C to 100°C. Due to sample limitations only one measurement was made.
Headspace gas chromatography (HS-GC) was performed using a 6892N Network GC system coupled to a 7694 HS sampler (Agilent Technologies, CA, US). Around 20 mg of each sample was dissolved in N,N-dimethylacetamide (≥99%) purchased from Sigma Aldrich (Dorset, UK). A liquid-vapour equilibrium was established by heating the solution in a sealed vial and an aliquot of the headspace vapour was analysed by capillary GC. Quantification of each volatile impurity was achieved by comparison of the chromatographic peak areas of external reference standards with the peak areas of the test sample solutions.
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