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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 55 records · Page 3
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Evidence of Room Temperature Ferromagnetism in Zn{sub 1−x}Sn{sub x}S Thin Films

Tin (Sn)-doped zinc sulfide (Zn{sub 1−x}Sn{sub x}S) thin films at different tin (Sn) concentrations (= 0.00, 0.02, 0.05, and 0.08) were coated onto Corning 7059 glass substrates using the electron beam evaporation technique. The films were subjected to different characterization techniques to study the physical properties of the thin films. The structural properties of the films were studied using a powder X-ray diffractometer (XRD), and it was found that the films were cubic in structure without any impurity phases. The crystallite size increased with an increase of Sn concentration, and the mean crystallite size was 21 nm. The chemical composition and surface morphology of the films were studied using scanning electron microscopy (FE-SEM) with energy-dispersive analysis of X-rays (EDAX). Optical properties such as transmittance and absorbance were recorded using a diffuse reflectance spectroscope (UV–vis–NIR). All the films exhibited high optical transmittance of 85% in the visible region of the solar spectrum. The band gap of the films was calculated using Tauc’s relation, and it was found that it increased from 3.53 to 3.57 eV with an increase in the Sn doping concentration from x = 0.02 to x = 0.08. The room temperature photoluminescence studies of the films were recorded using a fluorescence spectrophotometer, and it was found that the films exhibited a prominent emission peak at 420 nm. The magnetic properties of the films and glass substrates at room temperature were studied using a vibrating sample magnetometer. From this, it was found that the films were weakly ferromagnetic at room temperature and the strength of magnetization increased with an increase of doping concentration from x = 0.02 to x = 0.05 and decreased at higher doping concentrations (x = 0.08). The films showed high magnetization at x = 0.05. The films at x = 0.05 exhibited the magnetization (M{sub s}), retentivity (M{sub r}), and coercive fields (H{sub c}) 18 × 10{sup − 6} emu/cm{sup 3}, 1.6 × 10{sup − 6} emu/cm{sup 3}, and 91.80 Oe, respectively.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2013

Simple polyol route to synthesize heptanoic acid coated magnetite (Fe{sub 3}O{sub 4}) nanoparticles

Highlights: ► Heptanoic acid@Fe{sub 3}O{sub 4} nanocomposite has been prepared via simple polyol. ► Heptanoic acid used as both surfactant and solvents. ► Magneto polymer composite with adjustable Ea has a potential usage as functional composites. - Abstract: Magnetite (Fe{sub 3}O{sub 4}) nanoparticles were prepared via polyol method by using FeCl{sub 2} as only source of iron. As-prepared samples were characterized by powder X-ray diffractometer (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), thermal gravimetric analyzer (TGA) and vibrating sample magnetometer (VSM). Crystalline phase was identified as Fe{sub 3}O{sub 4} and the crystallite sizes were calculated as 19.1 ± 1.1 and 22 ± 1.3 nm for uncalcinated and calcinated products from X-ray line profile fitting. The capping of heptanoic acid around Fe{sub 3}O{sub 4} nanoparticles was confirmed by FT-IR spectroscopy, the interaction being via bridging oxygen's of the carboxylate and the nanoparticle surface and also by TG analysis. VSM measurements showed that both samples exhibited typical superparamagnetic behavior at room temperature with different Ms values. The ε′ decreases with increasing frequency for both composites and permeability has almost same values for all temperatures at higher frequencies. As synthesized and calcinated samples conductivity increase linearly with the temperature.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Machine Learning Based System for Automated Estimation of Crystal Unit Cell Parameters from X-ray Diffraction Powder Patterns (MLCell) v0.1

This software uses machine learning models to perform inference on X-ray diffraction powder patterns, output from a diffractometer, to estimate all 6 unit cell parameters of crystalline lattices. Novel aspects of this software originated from the incorporation of concepts from crystallography to an ML-based approach; The resulting method achieves new performance capabilities without significant loss of accuracy and with less computationally intensive models.

Oklejas, Vanessa↗
DOE OSTI2014

One-step synthesis of homogeneous BaFe{sub 12}O{sub 19}/Y{sub 3}Fe{sub 5}O{sub 12} composite powders

Highlights: • A simple one-step sol–gel method was used to synthesize composite magnets. • The composite powders show good homogeneity and exchange coupling. • The M{sub r}/M{sub s} value increases with the BaM concentration. - Abstract: BaFe{sub 12}O{sub 19}/Y{sub 3}Fe{sub 5}O{sub 12} (BaM/YIG) composite powders were synthesized via a simple one-step sol–gel method. The phase composition and morphology of the as-synthesized composite powders were characterized using an X-ray diffractometer and a scanning electron microscopy equipped with energy dispersive X-ray spectroscopy. The magnetic properties of the composite powders were investigated by a vibrating sample magnetometer. Compared with the composite powders prepared by the conventional physical mixing method, the BaM/YIG composite powders show better homogeneity and exchange coupling.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Effect of hydrothermal condition on the formation of multi-component oxides of Ni-based metallic glass under high temperature water near the critical point

The specific feature of multi-component oxides synthesized by hydrothermal process under high temperature (633 K) and highly pressurized water (18.9 MPa) near critical point. Effects of hydrothermal processing duration times 24 hours and 72 hours, respectively, on the oxide formation of the Ni{sub 59}Zr{sub 20}Ti{sub 16}Si{sub 2}Sn{sub 3} metallic glass synthesized by powder metallurgy process were characterized by X-ray diffractometer, differential scanning calorimeter along with the particle size, morphology and crystalline phase of the oxides. The crystallization of the needle-shape NiTiO{sub 3}, ZrTiO{sub 4} and ZrSnO{sub 4} ternary oxide phases observed on the surface of metallic glass at below glass transition temperature and the morphology of oxide phases changed to plate-shape around 2 μm in diameter by the increase processing time. This hydrothermal processing in subcritical water provides accelerated dense metal oxide crystals due to the reaction medium being at higher pressure than conventional oxidation processing.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Dielectrical properties of PANI/TiO{sub 2} nanocomposites

Conducting polyaniline/titanium dioxide (PANI/TiO{sub 2}) composites have been succesfully synthesized by insitu polymerization technique. The PANI/TiO{sub 2} nanocomposites of different compositions were prepared by varying weight percentage of TiO{sub 2} nanoparticles such as 10 wt%, 20 wt%, 30 wt%, 40 wt% and 50 wt% into the fixed amount of the aniline monomer. The prepared powder samples were characterized by X-ray diffractometer (XRD) and Scanning electron microscope (SEM). The intensity of diffraction peaks for PANI/TiO{sub 2} composites is lower than that for TiO{sub 2}. SEM pictures show that the nanocomposite were prepared in the form of long PANi chains decorated with TiO{sub 2} nanoparticles. The dielectric properties and AC conductivity were studied in the frequency range1K Hz–10M Hz. At higher frequencies, the composites exhibit almost zero dielectric loss and maximum value of σ{sub ac} is found for a concentration of 20 wt% TiO{sub 2} in polyaniline. The interface between polyaniline and TiO{sub 2} plays an important role in yielding a large dielectric constant in nanocomposites.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Influence of compositional variation on electrical properties of PANI/SnO{sub 2} nanocomposites

Conducting polyaniline/tin oxide (PANI/SnO{sub 2}) nanocomposites have been successfully synthesized by in-situ polymerization technique. The PANI/SnO{sub 2} nanocomposites of different compositions were prepared by varying weight percentage of SnO{sub 2} nanoparticles such as 10 wt%, 20 wt%, 30 wt%, 40 wt% and 50 wt% into the fixed amount of the aniline monomer. The prepared powder samples were characterized by X-ray diffractometer (XRD), Fourier Transform Infrared spectroscopy (FT-IR) and Scanning electron microscope (SEM). The intensity of diffraction peaks for PANI/SnO{sub 2} composites is increases with increasing SnO{sub 2} wt%. SEM observation showed that the prepared SnO{sub 2} nanoparticles were uniformly dispersed and highly stabilized throughout the macromolecular chain that formed a uniform metal-polymer nanocomposite material. AC electrical conductivity and dielectric properties were studied in the frequency range of 1 KHz -1 MHz. At higher frequencies, the composites exhibit almost zero dielectric loss and maximum value of AC electrical conductivity (σ{sub ac}) of 0.21 S/m is found for a concentration of 30 wt% of SnO{sub 2} in polyaniline.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2025

What Is the Limit of Quantification for the Minor Phase in Time-of-Flight Neutron Diffraction? A Case Study on Fe and Ni Powder Mixtures at VULCAN

A phase present in small quantities within materials may not simply serve as a secondary component; it can play a crucial role in determining the integrity, properties, and performance of the material. These minor but important phases usually draw attention in material design and processing for fundamental understanding as well as material quality control. Accurately quantifying a minor phase amid a majority phase, especially at extremely low fractions, remains a challenging task. Time-of-flight neutron diffraction, coupled with advanced pattern analysis techniques like Rietveld refinement, is a powerful tool for crystal structure identification and phase quantification. The deep penetrating capability of neutrons enables the detection and quantification of trace phases within materials. In this study, the quantification limits of time-of-flight neutron diffraction were explored using the VULCAN diffractometer at the Spallation Neutron Source, using Fe–Ni powder mixtures as a sample system. By comparing the refinement results to the known weighed values, it was determined that the reliable quantification of a minor Ni phase is achievable down to about 0.1 wt% while a Ni fraction as low as 0.02 wt% is difficult to trace. Effective control of the refinement parameters, especially the profile function parameters, are found to significantly influence the convergence of fittings and the accuracy of phase quantification.

Rietveld refinement↗
DOE OSTI2018

Mössbauer Studies and the Microwave Properties of Al{sup 3+}- and In{sup 3+}-Substituted Barium Hexaferrites

The correlation of the chemical composition, the structure, and the microwave characteristic of solid solutions of the BaFe{sub 12–x}D{sub x}O{sub 19} (0.1 ≤ x ≤ 1.2) barium hexaferrite substituted with diamagnetic Al{sup 3+} and In{sup 3+} ions has been studied. The precise data on the crystal structure have been obtained by powder neutron diffraction using a high-resolution Fourier diffractometer (Dubna, JINR). The data on the distribution of the diamagnetic substituting ions in the hexaferrite structure have been obtained by Mössbauer spectroscopy. The microwave properties (the transmittance and the reflectance) have been studied in the frequency range 20–65 GHz and in external magnetic fields to 8 kOe. It is found that the transmission spectra are characterized by a peak that corresponds to the resonant frequency of the electromagnetic energy absorption, which is due to the ferromagnetic resonance phenomenon. The correlation of the chemical composition, the features of the ion distribution in the structure, and the electromagnetic properties has been revealed. It is shown that external magnetic fields shift the absorption peak of electromagnetic radiation to higher frequencies due to an increase in the magnetocrystal anisotropy. The results enable the conclusion that the features of the intrasublattice interactions and the electromagnetic properties should be explained using the phenomenological Goodenough–Kanamori model.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2025

Position-Dependent Neutron Time-of-Flight Deviation at VULCAN Diffractometer

In neutron diffraction, it is critical to precisely measure the lattice spacing, as it is an indicator of a material’s physical characteristics, such as lattice strain, thermal expansion, and phase structures. In time-of-flight (TOF) measurements, the lattice spacing is determined by the recorded TOF from a well-calibrated instrument. However, changes in neutron time-of-flight are sensitive to many factors, such as the alignment of instrument optics, temperature, sample positions, sample dimensions, internal strains, and chemical or physical heterogeneities at the grain level. At VULCAN (SNS, ORNL), which is a high-flux engineering neutron diffractometer, we used a 1-mm-diameter diamond powder sample to scan for changes in TOF by measuring d-spacing values at different sample positions under several configurations. The 2D map of the TOF deviation or d-spacing deviation, in terms of lattice shift/lattice strain, is reported. The change in TOF is dependent on the scanned location in the beam as well as on detector locations. The results are informative for experimental planning, data interpretation, and future instrument design.

36 MATERIALS SCIENCE↗
DOE OSTI2015

High-resolution neutron diffraction study of microstructural changes in nanocrystalline ball-milled niobium carbide NbC{sub 0.93}

High resolution neutron diffraction was applied for elucidating of the microstructural evolution of nanocrystalline niobium carbide NbC{sub 0.93} powders subjected to high-energy ball milling. The diffraction patterns were collected with the high resolution Fourier diffractometer HRFD by using the reverse time-of-flight (RTOF) mode of data acquisition. The traditional single diffraction line analysis, the Rietveld method and more advanced Whole Powder Pattern Modeling technique were applied for the data analysis. The comparison of these techniques was performed. It is established that short-time milling produces a non-uniform powder, in which two distinct fractions with differing microstructure can be identified. Part of the material is in fact milled efficiently, with a reduction in grain size, an increase in the quantity of defects, and a corresponding tendency to decarburize reaching a composition NbC{sub 0.80} after 15 h of milling. The rest of the powder is less efficiently processed and preserves its composition and lower defect content. Larger milling times should have homogenized the system by increasing the efficiently milled fraction, but the material is unable to reach a uniform and homogeneous state. It is definitely shown that RTOF neutron diffraction patterns can provide the very accurate data for microstructure analysis of nanocrystalline powders. - Highlights: • The NbC{sub 0.93} powder was processed by high-energy ball milling. • The microstrain and dislocation density increase with milling time increase. • The corresponding decrease in crystallite size with milling time was observed. • The material exhibits the presence of two fractions after ball milling. • The RTOF neutron diffraction data are suitable for accurate microstructure analysis.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Temperature dependent DC electrical conductivity studies of ZnO nanoparticle thick films prepared by simple solution combustion method

ZnO nanoparticles of different size were prepared by varying the molar ratio of glycine and zinc nitrate hexahydrate as fuel and oxidizer (F/O = 0.8, 1.11, 1.7) by simple solution combustion method. Powder samples were characterized by UV-Visible spectrophotometer, X-ray diffractometer, Scanning electron microscope (SEM). DC electrical conductivity measurements at room temperature and in the temperature range of 313-673K were carried out for the prepared thick films and it was found to increase with increase of temperature which confirms the semiconducting nature of the samples. Activation energies were calculated and it was found that, F/O molar ratio 1.7 has low E{sub AL} (Low temperature activation energy) and high E{sub AH} (High temperature activation energy) compared to other samples.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Effect of Sc{sup 3+} on structural and magnetic properties of Mn-Zn nano ferrites

In the present investigation, for the first time, we report on the effect of Sc{sup 3+} on the structural and magnetic properties of Mn{sub 0.5}Zn{sub 0.5}Sc{sub y}Fe{sub 2-y}O{sub 4} (y = 0.01, 0.03 and 0.05) nanoferrites synthesized by solution combustion method using the mixture of fuels. As synthesized powders were characterized for the detailed structural analysis by X-ray diffractometer (XRD), Fourier transmission infrared spectroscopy (FTIR) and room temperature magnetic properties by using vibrating sample magnetometer (VSM). The results of XRD and FTIR confirm that the formation of nano crystalline, single-phased Mn-Zn ferrite with cubic spinel structure belongs to Fd-3m space group. The room temperature magnetic studies shows that, the saturation magnetization (M{sub S}), remanence magnetization (M{sub R}) and magnetic moment (η{sub B}), magnetic particle size (D{sub m}) have found to increase with Sc{sup 3+} ion concentration up to x = 0.3 and then decrease. The values of αY-K and the magnetic particle size (D{sub m}) are found to be in the range of 68-75° and 10-19 nm respectively, with Sc{sup 3+} concentration.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2021

The First Neptunium Dioxide Neutron Diffraction Experiment at HFIR

Here we present the first neutron diffraction experiment of a 50 mg sample of neptunium(IV) dioxide (NpO 2 ) powder at the High Flux Isotope Reactor (HFIR) using the wide-angle neutron diffractometer (WAND 2 ) HB-2C. We also provide a brief literature survey to pinpoint gaps in the crystal, electronic, and magnetic structure of NpO 2 to determine the optimum experiment to be pursued in the next HFIR user proposal cycle. Characterizing actinide materials with neutron diffraction, inelastic scattering, neutron imaging, polarized neutron studies, and small-angle neutron scattering techniques will increase our understanding of 5f electron behavior and elucidate atomic and magnetic structural properties. This strategy will help fill gaps in the literature and provide theoretical physicists with the data needed to build physical and chemical models to guide and validate computational methods. These methods may be used for predicting structural and chemical features of actinide-based materials. This proof-of-principle effort begins to uncover how to advance actinide science and technology at Oak Ridge National Laboratory (ORNL) using neutron capabilities. This effort has already sparked collaborative discussions between researchers outside the Radioisotope Science and Technology Division, including theoretical physicists from the Nuclear Nonproliferation Division and beamline scientists in the Neutron Scattering Division. We intend to continue pursuing neutron experiments and develop a scientific strategy focused on studying transuranium elements (e.g., Np, Pu, Am, and Cm) using the advanced neutron capabilities at ORNL.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2016

Dispersion of Nano-Sized Oxide Particles in Ni-based Alloy

High temperature materials with a good resistance to oxidation or corrosion are crucial for the Generation IV nuclear system such as VHTR (Very High Temperature Reactor). While several commercial Ni-based high temperature alloys have been among the candidate ones for the IHX (intermediate heat exchanger) or HGD (hot gas duct) of VHTR, they disclose their insufficiency for the application to the anticipated outlet temperature range such as 900 deg. C or above. Unless the operating temperature is significantly lowered and the performance of the system drops in consequence, a breakthrough in the candidate materials for the key components shall be necessary for the realization of the system. Feasibility for the oxide dispersion strengthening (ODS) of Ni-based alloys was studied by fabrication of alloy 617-base ODS alloy. Alloy 617 powders were mechanically alloyed (MA) with 0.3 wt% Y{sub 2}O{sub 3} powders of around 30 nm in diameter using a horizontal ball mill (ZoZ CM 08). After degassing and canning procedure, MA powders were hot extruded. Extruded alloy samples were tensile tested at high temperatures as well as at room temperature. Also high temperature creep rupture tests were conducted at 950 deg. C in air under 20 and 25 MPa, respectively. The behavior of oxide particles within the Ni-based alloy matrix was investigated by mechanical alloying of Ni- Cr-Fe ternary alloy powders and pure Ni powders with oxide particles, respectively. Oxide such as Y{sub 2}O{sub 3}, Cr{sub 2}O{sub 3}, HfO{sub 2}, ZrO{sub 2}, TiO{sub 2}, La{sub 2}O{sub 3} were chosen from the thermodynamic point of view as the first stable candidates from more than twenty oxides, nitrides and carbides. The behavior of oxide particle within the MA powder matrix along with the temperature was characterized by using high temperature XRD (X-ray Diffractometer) and (HR)TEM (High Resolution Transmission Electron Microscope). Creep rupture tests of the ODS alloy samples at 950 deg. C showed one order of magnitude lower creep rates than those of the corresponding alloy. (authors)

36 MATERIALS SCIENCE↗
DOE OSTI2025

Fast and Accurate Pixel Calibration of Tof Neutron Diffractometers with Machine Learning

At a spallation neutron source, neutron pulses of varying energies are generated, and the detection of neutrons by instrument detectors is recorded as time-of-flight from the emission of the neutron pulse to its arrival at specific detector pixels with high time resolution. The flight path of neutrons from the moderator to the sample and then to the detector must be precisely calibrated at the detector-pixel level using standard powders, so the neutron events from all pixels can be time-focused to produce high-resolution diffraction patterns. Modern time-of-flight neutron diffractometers at spallation neutron sources are equipped with two-dimensional detectors with millimeter-scale pixelations. The number of pixels in a diffraction instrument can reach millions, which makes a single-pixel-level calibration process time-consuming or even impossible with conventional refinement or fitting approaches. Here we present a machine-learning-aided calibration process using a train-and-predict approach, in which machine learning models are trained on the relationship between an individual pixel time-of-flight diffraction pattern and its diffraction constant. These models use a portion of the available pixels for training, and a good model then predicts the diffraction constants precisely and rapidly for large sets of pixel diffraction patterns.

detector pixel calibration↗
DOE OSTI2020

Pressure-induced phase transition in barium hydride studied with neutron scattering

Barium hydride can undergo a structural phase transition from an orthorhombic phase to a hexagonal phase induced by high temperature or high pressure. This transition causes an immediate increase in the hydrogen diffusion rates by over an order of magnitude, and therefore, understanding the origin and details of such transition is of great interest not only for fundamental reasons but also for improving materials for future applications. In this work, the pressure evolution of the crystal structure was characterized using neutron powder diffraction up to a maximum pressure of 11.3 GPa. The pressure dependence of the unit cell volumes, lattice parameters, atomic sites, and compressibilities were determined for both phases. A structural phase transition occurred over a wide pressure range of P = 1.3 GPa–4.9 GPa. The transition to the higher density hexagonal phase reduced the volume per formula unit of BaD 2 by 13.6%, hence increasing the volumetric storage density. In addition, we investigated the hydrogen diffusion process using high pressure quasi-elastic neutron scattering up to 7.1 GPa. Our results show that the hydrogen mobility increases with pressure in the hexagonal phase. This work sheds light on the structural and dynamical aspects of barium hydride caused by the application of high pressure. Finally, the results may aid in the development of advanced metal hydride systems with increased hydrogen dynamics.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Ternary germanides RERhGe{sub 2} (RE = Y, Gd-Ho) – New representatives of the YIrGe{sub 2} type

The YIrGe{sub 2} type ternary germanides RERhGe{sub 2} (RE = Y, Gd-Ho) were synthesized from the elements by arc-melting and characterized by powder X-ray diffraction. The structure of DyRhGe{sub 2} was refined from single crystal X-ray diffractometer data: Immm, a = 426.49(9), b = 885.0(2), c = 1577.4(3) pm, wR2 = 0.0533, 637 F{sup 2} values, 30 variables (300 K data). The structure contains two crystallographically independent dysprosium atoms in pentagonal prismatic and hexagonal prismatic coordination. The three-dimensional [RhGe{sub 2}] polyanion is stabilized through covalent Rh–Ge (243–261 pm) and Ge–Ge (245–251 pm) bonding. The close structural relationship with the slightly rhodium-poorer germanides RE{sub 5}Rh{sub 4}Ge{sub 10} (≡ RERh{sub 0.8}Ge{sub 2}) is discussed. Temperature-dependent magnetic susceptibility measurements reveal Pauli paramagnetism for YRhGe{sub 2} and Curie-Weiss paramagnetism for RERhGe{sub 2} with RE = Gd, Tb, Dy and Ho. These germanides order antiferromagnetically at T{sub N} = 7.2(5), 10.6(5), 8.1(5), and 6.4(5) K, respectively. - Graphical abstract: The germanides RERhGe{sub 2} (RE = Y, Gd-Ho) are new representatives of the YIrGe{sub 2} type.

36 MATERIALS SCIENCE↗