SEM images were obtained using a field emission scanning electron microscope (ULTRA55, ZEISS) operated at 3.0 kV. TEM images were captured using a transmission electron microscope (JEM2100, TOSHIBA). The specific surface area and pore size distribution were determined by Quadrasorb evoTM (Quantachrome). Before the adsorption, the samples were degassed at 120 °C for 8 h. The specific surface areas were calculated by the multipoint Brunauer–Emmett–Teller (BET) method and the pore size distribution was calculated by the discrete Fourier transform (DFT) method. The total pore volume was estimated from the N2 amount adsorbed at a relative pressure of P/P0 = 0.99. The small-angle X-ray scattering (SAXS) measurements used 13.5 keV radiation (λ = 0.918 Å). Raman spectra measurements were performed using the RenishawinVia + Reflex Raman spectrometer at a 514 nm excitation wavelength with a frequency range of 1000–2000 cm−1. The infrared spectrum was obtained by the Thermo Scientific Nicolect IS10 Fourier transform infrared spectrometer. The X-ray diffraction (XRD) measurements were taken with a Rigaku D/max B diffractometer using Cu KR radiation (40 kV, 20 mA).
D max b diffractometer
Manufactured by Rigaku
Sourced in Japan
The D/Max-B diffractometer is a versatile X-ray diffraction instrument manufactured by Rigaku. It is designed to perform qualitative and quantitative analysis of crystalline materials. The core function of the D/Max-B is to detect and measure the diffraction patterns of X-rays interacting with the sample, providing information about the crystal structure, phase composition, and other physical properties of the material.
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5 protocols using d max b diffractometer
1
Comprehensive Characterization of Nanomaterials
2
Structural Analysis of Honeycomb Fibers
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The X-ray diffraction pattern (XRD) of the honeycomb fiber was obtained by using a Rigaku D/MAX-B diffractometer equipped with Cu Kα radiation at λ = 0.154 nm. The diffract spectra of the fibers were recorded within a 2θ range from 0° to 60° with each point recorded in a step of 0.5° and a count time of 60 s. The prepared fibers were subjected to attenuated total reflection Fourier transform infrared (ATR FTIR) analysis with a resolution of 2 cm−1 with using a Nicolet-Nexus 670 FTIR spectrometer (Nicolet Instrument Corporation, Madison, WI, USA) within the range of 600–4000 cm−1.
3
Characterization of Felt Samples
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The bulk densities of the samples were calculated from their dimensions (measured using a Vernier caliper, sensitivity ±0.01 mm) and their weight (measured using a digital balance, sensitivity ±0.1 mg). The X-ray diffraction (XRD) spectra were collected with a D/Max- B diffractometer (Rigaku Co., Tokyo, Japan) operating at 40 kV and 30 mA with Cu Kα radiation. A digital microscope (Olympus-DSX 1000, Olympus Corp., Shinjuku City, Tokyo, Japan) was used to study the fracture surface. The scanning electron microscopy (SEM) micrographs were taken using a Supra 40 FE-SEM (Carl Zeiss NTS GmbH, Oberkochen, Germany) on the fracture surfaces after coating the samples with a thin Pt-Pd film by sputtering. The thermal diffusivities of the different felt samples were measured using the Laser Flash Analyzer, LFA 467-HyperFlash (NETZSCH-Gerätebau GmbH, Selb, Germany) in an N2 environment. Disk-shaped samples were made to fit in the measurement slits having a diameter = 12.7 mm, the thickness of the samples was recorded, and the parallel surfaces were coated with a thin graphite film to avoid reflection of the laser energy from the surfaces.
4
Synthesis and Characterization of Hf-Co Nanoparticles
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The aligned Hf-Co nanoparticles and the Hf-Co:Fe-Co nanocomposites were produced using a cluster-deposition method described elsewhere (also see the supplementary information S1 )22 21 . Some of the nanoparticles were deposited on carbon-coated copper grids with low coverage densities to measure the average particle size and size distribution using a FEI Tecnai Osiris (Scanning) transmission electron microscope. For the SQUID (superconducting quantum interference device) and PPMS (physical property measurement system) measurements, thin films of dense-packed nanoparticles and nanocomposites were fabricated on single-crystalline Si (001) substrates and the error in evaluating the coercivity and magnetization from the hysteresis loops is within 2%. The mass (or nominal thickness) of the films was measured using a quartz-crystal thickness monitor. The thickness of the films reported in this study was always in the range of 110 - 280 nm. The nanoparticle/nanocomposite thin films were capped with a thin SiO2 cap layer immediately after deposition by using a radio-frequency magnetron sputtering gun located in the deposition chamber. X-ray diffraction measurement of Hf-Co nanoparticles deposited on Si (001) substrate was carried out using a Rigaku D/Max-B diffractometer with a Co Kα wavelength of about 1.7889 Å.
5
Epitaxial Magnetic Oxide Heterostructures
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The h-RFeO3 (001)/Fe3O4 (111)/Al2O3 (001) films were grown using pulsed laser depositions. [16, 18] The Fe3O4 (111) thin films (5-30 nm) were deposited epitaxially on Al2O3 (001) substrates, as described in our previous work. [16] The h-RFeO3 thin films (5-30 nm) were deposited epitaxially on top of the Fe3O4 (111) thin films, in a 5 mTorr Ar environment at 750 °C with a laser fluence of ~1 J cm -2 , and a repetition rate of 2 Hz. [9, 14, 19, 20] The epitaxial relations between different layers in the films were studied with in-situ reflection high energy electron diffraction (RHEED) and ex-situ X-ray diffractions (XRD). The -2 scans of X-ray diffraction were carried out using a Rigaku D/Max-B diffractometer, with a cobalt K-𝛼 source (𝜆 = 1.79 Å). The rocking curve (ω scan), φ scan, and reciprocal space mapping were studied using a Rigaku Smartlab diffractometer, with a copper K-𝛼 source (𝜆 = 1.54 Å). The surface morphology of the films was studied using the atomic force microscopy (AFM) with a Bruker Dimension ICON. The magnetic properties of the h-RFeO3 (001)/Fe3O4 (111)/Al2O3 (001) films were studied using a superconducting quantum interference device (SQUID) magnetometer.
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