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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 343 records · Page 19
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Lattice Strain Measurement of Core@Shell Electrocatalysts with 4D Scanning Transmission Electron Microscopy Nanobeam Electron Diffraction

Strain engineering enables the direct modification of atomic bonding and is currently an active area of research aimed at improving electrocatalytic activity. However, directly measuring the lattice strain of individual catalyst nanoparticles is challenging, especially at the scale of a single unit cell. In this study, we quantitatively map the strain present in rhodium@platinum (core@shell) nanocube electrocatalysts using conventional aberration-corrected scanning transmission electron microscopy (STEM) and the recently developed technique of 4D-STEM nanobeam electron diffraction. We demonstrate that 4D-STEM combined with data preconditioning allows for quantitative lattice strain mapping with subpicometer precision and without the influence of scan distortions. When combined with multivariate curve resolution, 4D-STEM allows us to distinguish the nanocube core from the shell and to quantify the unit cell size as a function of distance from the core–shell interface. Our results demonstrate that 4D-STEM has significant precision and accuracy advantages in strain metrology of catalyst materials compared to aberration-corrected STEM imaging and is beneficial for extracting information about the evolution of strain in catalyst nanoparticles.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Toroidal plasma enhanced CVD of diamond films

An inductively coupled toroidal plasma source is used as an alternative to microwave plasmas for chemical vapor deposition of diamond films. The source, operating at a frequency of 400 kHz, synthesizes diamond films from a mixture of argon, methane, and hydrogen. The toroidal design has been adapted to create a highly efficient environment for diamond film deposition: high gas temperature and a short distance from the sample to the plasma core. Using a toroidal plasma geometry operating in the medium frequency band allows for efficient (≈90%) coupling of AC line power to the plasma and a scalable path to high-power and large-area operation. In test runs, the source generates a high flux of atomic hydrogen over a large area, which is favorable for diamond film growth. Using a deposition temperature of 900–1050 °C and a source to sample distance of 0.1–2.0 cm, diamond films are deposited onto silicon substrates. The results showed that the deposition rate of the diamond films could be controlled using the sample temperature and source to sample spacing. The results also show the films exhibit good-quality polycrystalline diamond as verified by Raman spectroscopy, x-ray diffraction, and scanning electron microscopy. The scanning electron microscopy and x-ray diffraction results show that the samples exhibit diamond (111) and diamond (022) crystallites. The Raman results show that the sp{sup 3} peak has a narrow spectral width (FWHM 12 ± 0.5 cm{sup −1}) and that negligible amounts of the sp{sup 2} band are present, indicating good-quality diamond films.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Effect of Local Postweld Heat Treatments on Metal Inert Gas-Welded A7N01S-T5 Joints

T6, T7, and retrogression and reaging (RRA) postweld heat treatments (PWHTs) were redefined and deployed to restore MIG-welded A7N01-T5 aluminum alloy joints in train-body structures using an inductive heating device. After the PWHT, the microstructures and mechanical properties of the joints were studied by x-ray diffraction (XRD), electron backscattered diffraction (EBSD), and scanning electron microscopy (SEM). The results showed that the hardness and strength of the joints were improved by the T6 treatment, and the tensile strength of the joints reached 87.39% of the base metal. However, an improvement in the corrosion resistance was not observed. The T7-treated joints enhanced the toughness of the welded joints and improved their corrosion resistance. The RRA-treated joints improved the toughness and corrosion resistance and increased the strength and hardness. The RRA treatment had a more comprehensive effect on the improvement of the welded joint structure and performance and is more suitable for postweld heat treatment of the aluminum alloy welded joints in the body of high-speed trains.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Multibeam Electron Diffraction

One of the primary uses for transmission electron microscopy (TEM) is to measure diffraction pattern images in order to determine a crystal structure and orientation. In nanobeam electron diffraction (NBED), we scan a moderately converged electron probe over the sample to acquire thousands or even millions of sequential diffraction images, a technique that is especially appropriate for polycrystalline samples. However, due to the large Ewald sphere of TEM, excitation of Bragg peaks can be extremely sensitive to sample tilt, varying strongly for even a few degrees of sample tilt for crystalline samples. In this paper, we present multibeam electron diffraction (MBED), where multiple probe-forming apertures are used to create multiple scanning transmission electron microscopy (STEM) probes, all of which interact with the sample simultaneously. We detail designs for MBED experiments, and a method for using a focused ion beam to produce MBED apertures. We show the efficacy of the MBED technique for crystalline orientation mapping using both simulations and proof-of-principle experiments. We also show how the angular information in MBED can be used to perform 3D tomographic reconstruction of samples without needing to tilt or scan the sample multiple times. Finally, we also discuss future opportunities for the MBED method.

47 OTHER INSTRUMENTATION↗
DOE OSTI2015

Synthesis of AlFeCuCrMg{sub x} (x = 0, 0.5, 1, 1.7) alloy powders by mechanical alloying

Novel AlFeCuCrMg{sub x} (x = 0, 0.5, 1, 1.7 mol) high-entropy alloys (HEAs) were synthesized by mechanical alloying. The effect of Mg content on the phase evolution of HEAs was investigated using X-Ray diffractometry (XRD), transmission electron microscopy (TEM) and selected area electron diffraction (SAED) pattern analysis. The particle morphology and composition of HEAs were investigated by scanning electron microscopy (SEM). Thermodynamic parameters were calculated and analyzed to explain the formation of a solid solution. XRD analysis revealed BCC as major phase and FCC as a minor phase in as-milled AlFeCuCr and AlFeCuCrMg{sub 0.5} HEAs. Also, XRD analysis of as-milled AlFeCuCrMg, AlFeCuCrMg{sub 1.7} confirmed the formation of two BCC phases (BCC 1 and BCC 2). TEM–SAED analysis of AlFeCuCrMg{sub x} HEAs concurred with XRD results. Microstructural features and mechanism for solid solution formation have been conferred in detail. Phase formation of the present HEAs has been correlated with calculated thermodynamic parameters. Differential thermal analysis (TGA-DTA) of these alloys confirmed that there is no substantial phase change up to 500 °C. - Highlights: • Novel AlFeCuCrMg{sub x} (x = 0, 0.5, 1, 1.7) HEAs were prepared by mechanical alloying. • Phase evolution and lattice parameter were studied by X-Ray Diffraction. • Crystallite size and lattice microstrain calculated failed to obey the Williamson–Hall method. • Criterions for formation of simple solid solution were compared to the thermodynamic parameters of the present HEAs. • Increase in the Mg concentration in AlMg{sub x}FeCuCr (x = 0, 0.5, 1, 1.7) HEAs supports the formation of BCC phase.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Shape-controlled synthesis and properties of dandelion-like manganese sulfide hollow spheres

Graphical abstract: Dandelion-like MnS hollow spheres assembled with nanorods could be successfully synthesized in large quantities through a simple and convenient hydrothermal synthetic method under mild conditions using soluble hydrated manganese chloride as Mn source, L-cysteine as both a precipitator and complexing reagent. The dandelion-like MnS hollow spheres might have potential applications in microdevices and magnetic cells. Highlights: ► MnS hollow spheres assembled with nanorods could be synthesized. ► The morphologies and sizes of final products could be controlled. ► Possible formation mechanism of MnS hollow spheres is proposed. -- Abstract: Dandelion-like gamma-manganese (II) sulfide (MnS) hollow spheres assembled with nanorods have been prepared via a hydrothermal process in the presence of L-cysteine and polyvinylpyrrolidone (PVP). L-cysteine was employed as not only sulfur source, but also coordinating reagent for the synthesis of dandelion-like MnS hollow spheres. The morphology, structure and properties of as-prepared products have been investigated in detail by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS), selected area electron diffraction (SAED), high-resolution transmission electron microscopy (HRTEM) and photoluminescence spectra (PL). The probable formation mechanism of as-prepared MnS hollow spheres was discussed on the basis of the experimental results. This strategy may provide an effective method for the fabrication of other metal sulfides hollow spheres.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

Preparation of graphene–Ag composites and their application for electrochemical detection of chloride

Highlights: ► Graphene–Ag composites were prepared in situ using ascorbic acid as green reducing agent. ► The morphology of Ag particles was irregular sheet and Ag particles homogeneously distributed on the graphene matrix. ► The surface-enhanced Raman scattering enhancement factor of D band is 5.85 for composites. ► The composites exhibited good sensitivity for the detection of chloride ions. -- Abstract: Graphene–Ag composites were prepared in situ using ascorbic acid as green reducing agent. The composites were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected-area electronic diffraction (SAED), and Raman spectrometer. It was showed that Ag particles homogeneously distributed on the graphene matrix. The morphology of Ag particles was irregular sheet with (1 1 1) basal plane. The surface-enhanced Raman scattering (SERS) enhancement factor of D band is 5.85 for composites. The application of the composites for electrochemical detection of chloride was studied by cyclic voltammetry. The composites exhibited good sensitivity for the detection of chloride ions. The maximum peak current of cyclic voltammetry curve in 5 mM KCl was 0.80 mA. In the range of 500 μM to 50 mM for Cl{sup −}, the current response was proportional and linear to the Cl{sup −} concentration. The sensitivity to the detection for Cl{sup −} was 0.059 (mA/mM) and the detection limit was 61 μM for Cl{sup −}. It indicates graphene–Ag composites would be a competitive material for detection of halide.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Twin boundary-accelerated ferritization of austenitic stainless steels in liquid lead–bismuth eutectic

Exposure of austenitic stainless steels to liquid lead–bismuth eutectic with low concentration of dissolved oxygen typically results in selective leaching of highly-soluble alloying elements and ferritization of the dissolution-affected zone. In this work, focused ion beam, transmission electron backscatter diffraction and scanning transmission electron microscopy were utilized to elucidate early-stage aspects of the dissolution corrosion process of cold-worked austenitic stainless steels exposed to static, oxygen-poor liquid lead–bismuth eutectic at 450 °C for 1000 h. Furthermore, it was found that deformation-induced twin boundaries in the cold-worked steel bulk provide paths of accelerated penetration of the liquid metal into the steel bulk.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

Multimodal Analysis of Spatially Heterogeneous Microstructural Refinement and Softening Mechanisms in Three-Pass Friction Stir Processed Al4Si Alloy

Multiple thermally and thermomechanically induced microstructural refinement mechanisms can be activated in metallic alloys when subjected to solid phase processing methods such as friction stir processing (FSP). In this work, we provide detailed descriptions of the relationship between region-specific microstructural refinement mechanisms and the variation in microhardness, through a systematic and multimodal microstructural characterization of an FSP-processed 75% cold-rolled Al-4 at.% Si model binary alloy. Spatially resolved high-energy synchrotron X-ray diffraction, electron backscattered diffraction, and scanning transmission electron microscopy were used to understand the spatially heterogeneous microstructural evolution due to FSP. Results provide insights into how mechanisms such as static recovery, static recrystallization, dynamic recovery and recrystallization, geometric and continuous dynamic recrystallization, and particle-stimulated static or dynamic grain nucleation may occur heterogeneously in the microstructure as a function of the distance from the stir zone in processed alloys, directly influencing the degree of softening. The systematic analysis of microstructures and hardness in the FSP-processed model binary alloy given in this work highlights the rich microstructural domains that can be uniquely harnessed through solid phase processing of metallic alloys.

Al4Si, Friction Stir Processing, Geometric Dynamic↗
DOE OSTI2014

Diffraction-assisted micropatterning of silicon surfaces by ns-laser irradiation

Single-pulse (532 nm, 8 ns) micropatterning of silicon with nanometric surface modulation is demonstrated by irradiating through a diffracting pinhole. The irradiation results obtained at fluences above the melting threshold are characterized by scanning electron and scanning force microscopy and reveal a good agreement with Fresnel diffraction theory. The physical mechanism is identified and discussed on basis of both thermocapillary and chemicapillary induced material transport during the molten state of the surface.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2011

High rate performances of the cathode material LiNi{sub 1/3}Co{sub 1/3}Mn{sub 1/3}O{sub 2} synthesized using low temperature hydroxide precipitation

Graphical abstract: A low-temperature reaction route is introduced based on hydroxide precipitation method to synthesize a cathode material LiNi{sub 1/3}Co{sub 1/3}Mn{sub 1/3}O{sub 2}. The charge-discharge tests were performed at 1000 mA g{sup -1} between 2.5 and 4.5 V and the discharge capacity is about 160 mAh g{sup -1}. The discharge capacity of the material is strongly impacted by the reaction temperature. The powders sintered at 850 {sup o}C show the best electrochemical performance. Highlights: {yields} A low-temperature reaction route is introduced based on hydroxide precipitation method to synthesize a novel cathode material LiNi{sub 1/3}Co{sub 1/3}Mn{sub 1/3}O{sub 2}. {yields} The charge-discharge tests were performed at higher current as 5 C between 2.5 and 4.5 V. {yields} The discharge capacity of the material is strongly impacted by the reaction temperature. The powders sintered at 850 {sup o}C show the best electrochemical performance. -- Abstract: A low-temperature reaction route is introduced based on hydroxide precipitation method to synthesize the cathode material LiNi{sub 1/3}Co{sub 1/3}Mn{sub 1/3}O{sub 2}. The crystal structure and morphology of the prepared powder have been characterized by X-ray diffraction and Scan electron microscope, respectively. The charge-discharge tests were performed between 2.5 and 4.5 V. The discharge capacity of the material is strongly impacted by the reaction temperature. The powders sintered at 850 {sup o}C show the best electrochemical performance and the initial discharge capacity is about 160 mAh g{sup -1} at 5 C. Powder X-ray diffraction and Scan electron microscope results reveal that the excellent electrochemical performances should be ascribed to the lower precursor reaction temperature, the lower degree of cation mixing and analogous spherical small particles, which can improve the transfer of Li ions and electrons. All these results indicate that this material has potential application in lithium-ion batteries.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Direct imaging of Cl- and Cu-induced short-circuit efficiency changes in CdTe solar cells

To achieve high-efficiency polycrystalline CdTe-based thin-film solar cells, the CdTe absorbers must go through a post-deposition CdCl 2 heat treatment followed by a Cu diffusion step. To better understand the roles of each treatment with regard to improving grains, grain boundaries, and interfaces, CdTe solar cells with and without Cu diffusion and CdCl 2 heat treatments are investigated using cross-sectional electron beam induced current, electron backscatter diffraction, and scanning transmission electron microscope techniques. The evolution of the cross-sectional carrier collection profile due to these treatments that cause an increase in short-circuit current and higher open-circuit voltage are identified. Additionally, an increased carrier collection in grain boundaries after either/both of these treatments is revealed. The increased current at the grain boundaries is shown to be due to the presence of a space charge region with an intrinsic carrier collection profile width of ≈350 nm. Scanning transmission electron microscope electron-energy loss spectroscopy shows a decreased Te and increased Cl concentration in grain boundaries after treatment, which causes the inversion. Furthermore, each treatment improves the overall carrier collection efficiency of the cell separately, and, therefore, the benefits realized by each treatment are shown to be independent of each other.

14 SOLAR ENERGY↗
DOE OSTI2018

The Influence of Microstructure on Oxidation Rate Of V–Cr–Ta–Zr Alloy During Its Chemical-Heat Treatment

Using the methods of scanning (electron backscatter diffraction) and transmission electron microscopy, an investigation of the influence of microstructure of a V–Cr–Ta–Zr alloy on the rate of surface oxide scale formation in the course of its chemical-heat treatment using oxidation in air is performed. It is shown that a preliminary plastic deformation, ensuring a multiple increase in the density of dislocations and misorientation boundaries, results in a 10% thicker surface oxide layer and a respective increase in the concentration of oxygen in the alloy during the final stage of its chemical-heat treatment. The role of this factor in developing the chemical-heat treatment regimes is discussed.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2017

Characterization of Al-Mg Alloy Aged at Low Temperatures

For this research, long-term aged [343 K (70 °C) for 30 months and natural exposure for over 10 years] Al 5456 H116 samples were characterized using electron backscatter diffraction (EBSD), scanning transmission electron microscopy (STEM), state-of-the-art energy-dispersive X-ray spectroscopy (EDS) systems, and small-angle neutron scattering (SANS). ASTM G-67 mass loss tests of the sensitized Al 5456 alloy samples were conducted. Intragranular Mg-rich precipitates, such as Guinier–Preston (GP) zones, were confirmed in Al 5456 H116 aged at 343 K (70 °C) for 30 months, and the volume of these precipitates is 1.39 pct. β' phase is identified at the grain boundary of a navy ship sample, while high-resolution STEM results reveal no intragranular precipitates. Intergranular corrosion (IGC) of Al 5456 was found to be related to the continuity of intergranular precipitates.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Characterization of the effects of different tempers and aging temperatures on the precipitation behavior of Al-Mg (5.25at.%)-Mn alloys

We investigated the effects of different tempers (H131 and H116) and different aging temperatures (50 and 70 °C) on the precipitation behavior of Al-Mg (5.25 at.%)-Mn (Al 5083) alloys aged for a long time (41 and 30 months) using electron backscatter diffraction(EBSD), scanning transmission electron microscopy(STEM), energy-dispersive X-ray spectroscopy(EDS), atom probe tomography (APT), and small angle neutron scattering (SANS). Results for the GP zones and β'' phases were found in Al 5083 H116 aged at 50 °C for 24 months using APT. EDS and SANS revealed that a phase transformation process from GP zones to β'/β phases occurred for precipitates formed in both Al 5083 H131 and H116 aged at 70 °C. The effective diffusion coefficient of Mg in Al 5083 H131 is 1.8 times of that in Al 5083 H116 aged at 70 °C. The precipitation process in Al 5083 H116 aged at 50 °C is much slower than that in the sample aged at 70 °C. Finally, we identified the coarsening process in Al 5083 H131 and H116 aged at 70 °C for > 9 months.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Heterogeneous microstructural evolution during hydrodynamic penetration of a high-velocity copper microparticle impacting copper

Microparticle hydrodynamic penetration (HDP) may be associated with the erosion regime in cold spray processing and other high-velocity impact events. Here, in an experimental approach where we can individually launch particles and study the impact sites, we explore copper microparticles impacted on copper substrates at velocities above 900 m/s where HDP begins. We lift cross-sectional lamellae from the impact sites with a focused-ion beam for further microstructural characterization using electron backscatter diffraction and scanning transmission electron microscopy. Due to the gradients of strain, strain rate, and temperature associated with HDP, heterogeneous microstructures result. The structural evolution processes observed include deformation twinning and multiple dislocation-mediated grain recrystallization mechanisms—geometric dynamic recrystallization (gDRX), discontinuous DRX (dDRX), and meta DRX (mDRX). The higher strains at the interface lead to the most significant structural changes and complex mechanisms. In contrast, there is a gradient to more conventional dislocation plasticity away from the interface (on either the particle or substrate side). Here, these microstructural observations are consistent with the deformation map for copper and extend the observations of impact-induced recrystallization across new regimes of behavior.

Cold spray process↗
DOE OSTI2025

Valence Electron Distributions from Sub-Angstrom Convergent Beam Electron Diffraction

Modern aberration-corrected scanning transmission electron microscopes can acquire four-dimensional data sets (“4D STEM”) by recording convergent beam electron diffraction (CBED) patterns, using precisely positioned, sub-angstrom probes. Here, we demonstrate that these patterns can probe the site symmetry, atomic displacements, and valence electron distributions at individual atomic columns. To this end, 4D STEM CBED patterns were acquired from SrTiO 3 single crystals and compared with patterns calculated using scattering potentials derived from density functional theory. Here, we show that an aspherical valence electron charge build-up at the oxygen sites causes intensity asymmetries in the low-angle scattering portion of the patterns. Using strained SrTiO 3 films containing subtle polar displacements within nanometer-sized domains, it is shown that the high-angle scattering portion in each pattern is sensitive to atomic displacements.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Effect of Bainitic Microstructure on Ballistic Performance of Armour Steel Weld Metal Using Developed High Ni-Coated Electrode

Welding of armour steel has gained significant importance during the past few years as recent civilian and military requirements demand weld metal properties matching with base metal having good ballistic performance along with high strength and toughness at − 40 °C as per specification. The challenge of armour steel welding therefore lies in controlling the weld metal composition which is strongly dependent on welding electrode/consumables, resulting in desired weld microstructure consisting of lower bainite along with retained austenite. The performance of butt-welded armour steel joints produced by the developed electrodes was evaluated using tensile testing, ballistic testing, impact toughness at room temperature and subzero temperature. Microstructures of weld metals are exclusively characterized by x-ray diffraction technique, scanning electron microscope and transmission electron microscopy with selected area diffraction pattern. Experimental results show that weld metal with relatively lower carbon, higher manganese and lower nickel content was attributed to lower bainite with film type of retained austenite may be considered as a most covetable microstructure for armour steel weld metal.

36 MATERIALS SCIENCE↗