The crystal phase and crystallinity of samples were studied by the X-ray diffraction (XRD) method (Rigaku SmartLab 3 diffractometer (Tokyo, Japan) of the engineering center of the Saint Petersburg State Technological Institute (Technical University)) using Cu-Kα irradiation (λ = 1.54 Å). Samples were scanned along 2θ in the range of 10–70° at 0.5 degrees/min. For XRD analysis, samples were dried at 120 °C for 4 h. For SEM analysis, the samples were dried in vacuo for 2 h and examined using a Tescan VEGA 3 scanning electron microscope (Brno, Czech Republic). The particle size and zeta potential in colloidal solutions were measured using a Photocor EPM/Photocor Compact Z (Moscow, Russia). The surface area, pore volume, and pore size distribution were investigated using Quantachrome Nova 1200e (Boynton Beach, FL, USA) by nitrogen adsorption at 77 K, and analyzed using the BET and BJH equations. Prior to analysis, all samples were degassed at 110 °C for 4 h.
Smartlab 3 diffractometer
Manufactured by Rigaku
Sourced in Japan
The SmartLab 3 is a high-performance X-ray diffractometer designed for advanced materials analysis. It features a modular architecture that allows for customization to meet specific research needs. The SmartLab 3 is capable of performing a wide range of X-ray diffraction measurements, including powder, thin-film, and single-crystal analysis.
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Lab products found in correlation
2 protocols using smartlab 3 diffractometer
1
Comprehensive Characterization of Crystalline Materials
2
Structural and Thermal Characterization of Sintered Pellets
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The crystal structures
of the sintered pellets were examined using X-ray powder diffraction
(Rigaku Smart Lab 3 diffractometer) with Cu Kα radiation. Data
were collected over a 2θ range of 10–120° with a
step size of 0.02° and a step time of 2°/min. Le Bail fittings
were performed using the FullProf program included in the WinPLOTR
software.48 (link),62 (link),63 (link) The shape
of the diffraction peaks was modeled using a pseudo-Voigt profile
function. Zero-point shifts, asymmetry parameters, and lattice parameters
were systematically refined, and the background contribution was manually
estimated. Observations of microstructural aspects of the sintered
samples were performed on the fractured cross section and polished
surface using a Hitachi SU-4800 scanning electron microscope (SEM)
and a mini-SEM (TM3000, Hitachi) both equipped with an energy-dispersive
spectrometer (EDS).
The thermal diffusivity α and heat
capacity Cp were measured using LFA-467
Hyperflash (Netzsch) under a flowing argon atmosphere (50 mL/min).
The thermal conductivity κ was derived as a product of the sample’s
density (measured by Archimedes’ method), thermal diffusivity,
and heat capacity Cp. The measurements
of electrical resistivity ρ and Seebeck coefficient S were performed simultaneously using a commercial instrument
Ulvac ZEM-2 under partial helium pressure.
of the sintered pellets were examined using X-ray powder diffraction
(Rigaku Smart Lab 3 diffractometer) with Cu Kα radiation. Data
were collected over a 2θ range of 10–120° with a
step size of 0.02° and a step time of 2°/min. Le Bail fittings
were performed using the FullProf program included in the WinPLOTR
software.48 (link),62 (link),63 (link) The shape
of the diffraction peaks was modeled using a pseudo-Voigt profile
function. Zero-point shifts, asymmetry parameters, and lattice parameters
were systematically refined, and the background contribution was manually
estimated. Observations of microstructural aspects of the sintered
samples were performed on the fractured cross section and polished
surface using a Hitachi SU-4800 scanning electron microscope (SEM)
and a mini-SEM (TM3000, Hitachi) both equipped with an energy-dispersive
spectrometer (EDS).
The thermal diffusivity α and heat
capacity Cp were measured using LFA-467
Hyperflash (Netzsch) under a flowing argon atmosphere (50 mL/min).
The thermal conductivity κ was derived as a product of the sample’s
density (measured by Archimedes’ method), thermal diffusivity,
and heat capacity Cp. The measurements
of electrical resistivity ρ and Seebeck coefficient S were performed simultaneously using a commercial instrument
Ulvac ZEM-2 under partial helium pressure.
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