Powder X-ray diffraction (PXRD) data were collected on each sample after furnace annealing and after consolidation in the SPS. Samples were ground into a fine powder by mortar and pestle in an Ar drybox and plated with ethanol to obtain a uniform, thin spread onto a zero background holder on a Bruker D8 Advance Eco Diffractometer (BRUKER AXS, Inc., 5465 East Cheryl Parkway, Madison, WI, USA) operated at 40 kV and 25 mA utilizing Ni filtered Cu Kα radiation with the knife-edge attachment. Data were collected from 20° to 80° 2θ with a step size of 0.19° at 1.5 s. Data were converted from .raw to .gsas using powdll and analyzed via Rietveld refinement using General Structure Analysis System, GSAS-II [19 (link),20 ]. The GSAS-II instrument parameter file used in refinement was generated from a similarly-prepared LaB6 standard. Lattice parameters of the RE phases were obtained from refinement of a 14-1-11 phase modelled from published Crystallographic Information File (CIF) of Yb14ZnSb11.
D8 advance eco diffractometer
Manufactured by Bruker
Sourced in United States
The D8 Advance Eco diffractometer is a compact and cost-effective X-ray diffraction (XRD) instrument designed for phase identification and characterization of solid materials. It features a sealed X-ray tube, a theta-theta goniometer, and a fast 1D detector. The D8 Advance Eco provides reliable and reproducible data for a wide range of applications in research and industry.
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Lab products found in correlation
7 protocols using d8 advance eco diffractometer
1
PXRD Analysis of Annealed and Consolidated Samples
2
Structural Analysis of Material Phases
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An in-house Bruker D8 Advance Eco diffractometer
(using Cu Kα radiation) was used to gather X-ray
powder diffraction (XRPD) data in order to follow the reactions between
heating steps. Data for detailed structural analysis were collected
on beamline I1122 (link) at the Diamond Light
Source using 30 min scans with 0.82 Å X-rays (calibrated precisely
using a Si standard at the start of each beam time session) with the
high-resolution multi-analyzer crystal (MAC) detector. A position-sensitive
detector (PSD) was also used on beamline I11 to gather full diffraction
patterns at 190 temperatures while cooling from 600 to 300 K in approximately
1 h. Neutron powder diffraction (NPD) was carried out on the WISH
instrument23 (link) at the ISIS Facility, where
approximately 0.8 g of each material was loaded into vanadium cans,
and data were obtained at various temperatures between 7 and 543 K
using a cryofurnace to cool down and warm up the samples. The XRPD
and NPD data were analyzed by Rietveld refinement using the TOPAS
Academic V5 software.24 (link)
(using Cu Kα radiation) was used to gather X-ray
powder diffraction (XRPD) data in order to follow the reactions between
heating steps. Data for detailed structural analysis were collected
on beamline I1122 (link) at the Diamond Light
Source using 30 min scans with 0.82 Å X-rays (calibrated precisely
using a Si standard at the start of each beam time session) with the
high-resolution multi-analyzer crystal (MAC) detector. A position-sensitive
detector (PSD) was also used on beamline I11 to gather full diffraction
patterns at 190 temperatures while cooling from 600 to 300 K in approximately
1 h. Neutron powder diffraction (NPD) was carried out on the WISH
instrument23 (link) at the ISIS Facility, where
approximately 0.8 g of each material was loaded into vanadium cans,
and data were obtained at various temperatures between 7 and 543 K
using a cryofurnace to cool down and warm up the samples. The XRPD
and NPD data were analyzed by Rietveld refinement using the TOPAS
Academic V5 software.24 (link)
3
Comprehensive Perovskite Material Characterization
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XRD data were recorded using a Bruker D8 ADVANCE ECO diffractometer (Cu Kα radiation, λ = 0.15418 nm). The absorbance spectra of the perovskite films were recorded using a microspectrometer (SD1200-LS-HA, StreamOptics Co.) with a detection wavelength range of 400–1000 nm. The PL spectra were recorded using a spectrometer (tecSpec MMS) with a detection wavelength range of 400–1100 nm. A 405 nm laser was used as the excitation source. The temperature-dependent PL was obtained with VPF-100 liquid nitrogen cooled cryostat (Janis Research). The electrical characteristics were measured using a Keithley 2400 SourceMeter. The EL spectra, radiance, and EQE were recorded and calculated using a spectrometer (USB2000+, Ocean Optics) and ISM-Nit software (Isuzu Optics Corp.). The spectrometer was calibrated with a spectroradiometer (specbos 1211, JETI). Conventional transmission electron microscopy (TEM) observations were carried out using a JEOL JEM-2100 microscope.
4
Sintered Pellet Characterization by PXRD
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Pieces of the sintered
pellets obtained from SPS were ground into fine powders using an agate
mortar and pestle for additional PXRD analysis. One pellet was also
measured to check for the possibility of a preferred orientation.
A Bruker D8 Advance Eco diffractometer with Cu Kα radiation
was used to collect PXRD data. The diffractometer operated at 40 kV
and 25 mA from 2θ range 20–80° with step size 0.015°
and a scan rate of 1 s per step. Samples were determined to be single-phase
Eu11–xNaxZn4Sn2As12 via Rietveld refinement
employing the crystallographic information file (CIF) with the TOPAS5
software (provided in Supporting Information,Figures S2 and S3, Table S2 ).34
pellets obtained from SPS were ground into fine powders using an agate
mortar and pestle for additional PXRD analysis. One pellet was also
measured to check for the possibility of a preferred orientation.
A Bruker D8 Advance Eco diffractometer with Cu Kα radiation
was used to collect PXRD data. The diffractometer operated at 40 kV
and 25 mA from 2θ range 20–80° with step size 0.015°
and a scan rate of 1 s per step. Samples were determined to be single-phase
Eu11–xNaxZn4Sn2As12 via Rietveld refinement
employing the crystallographic information file (CIF) with the TOPAS5
software (provided in Supporting Information,
5
Structural Characterization of Solid Products
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Laboratory PXRD data on the solid products
were collected using a Bruker D8 Advance Eco diffractometer (Cu Kα
radiation). For detailed structural refinement, data were collected
on beamline I1131 (link) at the Diamond Light
Source using 1.5 min scans with a MYTHEN position sensitive detector
(PSD), using Si-calibrated 0.82 Å X-rays. The PSD was also used
to gather diffraction patterns at 82 temperatures over a range of
100–300 K and 211 temperatures over a range of 303–1173
K. PND measurements at ambient temperature were made using the GEM32 (link) instrument at the ISIS Pulsed Neutron and Muon
Facility, Rutherford Appleton Laboratory, UK. A sample of approximately
1.5 g was loaded into a 6 mm-diameter vanadium can and sealed using
an indium gasket. Diffraction data were collected for an integrated
proton charge to the ISIS target of 350 μAhr (microamp hours),
equivalent to approximately 2 h exposure in the neutron beam. Refinements
of the structural models against the diffraction data were carried
out using TOPAS Academic V6 software.33 (link)
were collected using a Bruker D8 Advance Eco diffractometer (Cu Kα
radiation). For detailed structural refinement, data were collected
on beamline I1131 (link) at the Diamond Light
Source using 1.5 min scans with a MYTHEN position sensitive detector
(PSD), using Si-calibrated 0.82 Å X-rays. The PSD was also used
to gather diffraction patterns at 82 temperatures over a range of
100–300 K and 211 temperatures over a range of 303–1173
K. PND measurements at ambient temperature were made using the GEM32 (link) instrument at the ISIS Pulsed Neutron and Muon
Facility, Rutherford Appleton Laboratory, UK. A sample of approximately
1.5 g was loaded into a 6 mm-diameter vanadium can and sealed using
an indium gasket. Diffraction data were collected for an integrated
proton charge to the ISIS target of 350 μAhr (microamp hours),
equivalent to approximately 2 h exposure in the neutron beam. Refinements
of the structural models against the diffraction data were carried
out using TOPAS Academic V6 software.33 (link)
6
Structural Analysis of Single-Gelator and Binary Gels
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To compare the
crystal structures of single gelators and their gels with binary BA
systems, X-ray diffraction (XRD) patterns of these gels were studied.
A dab of sample was placed onto the standard PMMA sample holders.
The measurement on binary systems was conducted under the same condition
as single nBA gelators and gels:38 (link),39 (link) a Bruker D8 ADVANCE ECO diffractometer in the Bragg–Brentano
geometry equipped with a Cu X-ray source (Kα1 = 1.54060
Å and Kα2 = 1.54439 Å) and LYNXEYE-XE-T
position-sensitive detector was operated at room temperature. A knife-edge
was embedded to reduce the background due to the scattering of the
primary beam. The diffraction patterns were recorded from 0.6 to 50°
(2θ) with a step size of 0.01° and measuring time of 0.5
s per step.
crystal structures of single gelators and their gels with binary BA
systems, X-ray diffraction (XRD) patterns of these gels were studied.
A dab of sample was placed onto the standard PMMA sample holders.
The measurement on binary systems was conducted under the same condition
as single nBA gelators and gels:38 (link),39 (link) a Bruker D8 ADVANCE ECO diffractometer in the Bragg–Brentano
geometry equipped with a Cu X-ray source (Kα1 = 1.54060
Å and Kα2 = 1.54439 Å) and LYNXEYE-XE-T
position-sensitive detector was operated at room temperature. A knife-edge
was embedded to reduce the background due to the scattering of the
primary beam. The diffraction patterns were recorded from 0.6 to 50°
(2θ) with a step size of 0.01° and measuring time of 0.5
s per step.
7
Comprehensive Characterization of Microcrystalline Samples
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Powder X-ray diffraction data were collected on a Bruker D8 Advance Eco diffractometer equipped with a Cu Kα radiation source (λ = 1.541874 Å), in the Debye-Scherrer geometry. The microcrystalline samples were sealed in glass capillaries and measured in the 5-50°2θ range at room temperature. The reference powder patterns from SC-XRD measurements were generated using Mercury CSD 4.3.1 software. 29 Elemental analyses of CHN were performed on an ELEMENTAR Vario Micro Cube CHNS analyser. IR spectra were collected on a Bruker Alpha II spectrometer with a diamond ATR add-on. The thermogravimetric data were collected using a Netzsch TG 209 F1 Libra apparatus. The water sorption/desorption processes were characterized by the dynamic vapor sorption method using the SMS DVS Resolution apparatus. The isotherm was measured in a 0-90% relative humidity range at a temperature of 25 °C. Every measurement step was performed until a stable Dalton Transactions Paper mass was achieved. Magnetic susceptibility measurements were on a Quantum Design MPMS-3 Evercool magnetometer in magnetic fields up to 70 kOe. The experimental data were corrected for diamagnetism of the sample and the sample holder. The magnetic data were fitted using the PHI programme. 31
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