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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 1,099 records · Page 61
All sourcesNASA NTRSDOE OSTI
DOE OSTI2017

Substrate preparation effects on defect density in molecular beam epitaxial growth of CdTe on CdTe (100) and (211)B

Recent studies have demonstrated that growth of CdTe on CdTe (100) and (211)B substrates via molecular beam epitaxy (MBE) results in planar defect densities 2 and 3 orders of magnitude higher than growth on InSb (100) substrates, respectively. To understand this shortcoming, MBE growth on CdTe substrates with a variety of substrate preparation methods is studied by scanning electron microscopy, secondary ion mass spectrometry, x-ray photoelectron spectroscopy, cross sectional transmission electron microscopy, and atom probe tomography (APT). Prior to growth, carbon is shown to remain on substrate surfaces even after atomic hydrogen cleaning. APT revealed that following the growth of films, trace amounts of carbon remained at the substrate/film interface. This residual carbon may lead to structural degradation, which was determined as the main cause of higher defect density.

14 SOLAR ENERGY↗
DOE OSTI2024

Identifying point defects and ordering in the high-entropy layered oxide Li 1.5 MO 3-δ (M=Mn, Al, Fe, Co, Ni) for energy storage applications

High-entropy layered oxides (HELOs) represent a very promising class of next-generation battery cathodes, combining the well-studied properties of layered cathode materials such as LiCoO 2 with the chemical tunability and stability of high-entropy materials. HELO materials often form particles with complex defects and domain structures, complicating accurate characterization of structure and cation mixing. Understanding disorder and order in HELO materials is necessary for understanding their performance and utility as cathodes. Here we demonstrate the characterization of the HELO Li 1.5 MO 3-δ (M = Mn, Al, Fe, Co, Ni), wherein X-ray powder diffraction, transmission electron microscopy imaging, and electron diffraction patterns are analyzed to reveal the presence of ordering in the HELO, with imaging and diffraction simulation employed to compare experimental results to atomic modeling. Finally, without rigorous characterization at the atomic scale, important features such as defect ordering can be easily overlooked and therefore remain unconsidered when interpreting experimental results.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Dramatic influence of Dy{sup 3+} doping on strain and domain structure in lead-free piezoelectric 0.935(Na{sub 1/2}Bi{sub 1/2})TiO{sub 3}−0.065BaTiO{sub 3} ceramics

An electric-field induced giant strain response and doping level dependent domain structural variations have been studied in the dysprosium (Dy{sup 3+})-modified 0.935(Na{sub 1/2}Bi{sub 1/2})TiO{sub 3}-0.065BaTiO{sub 3}(xDy : NBBT) ceramics with the doping levels of 0%, 0.5%, 1%, and 2%. X-ray diffraction and Raman spectroscopy analyses not only demonstrates the change in ionic configurations induced by Dy{sup 3+} doping, but also shows the local crystal symmetry for x ≥ 0.5% doping levels to deviate from the idealized cubic structure. Piezoresponse force microscopy measurement exhibits the presence of an intermediate phase with orthorhombic symmetry at the critical Dy{sup 3+} doping level of 2%. Moreover, at this doping level, a giant recoverable nonlinear strain of ∼0.44% can be observed with high normalized strain (S{sub max}/E{sub max}) of 728 pm/V. At the same applied field, the strain exhibits a 175% increase than that of NBBT ceramic. Such a large strain stems from the varying coherence lengths of polar nanoregions (PNRs) and an unusual reversible 90° domain switching caused by the symmetry conforming property of point defects, where the restoring force is provided by unswitchable defects. The mechanism reveals a new possibility to achieve large electric-field strain effect for a wide range of ferroelectric systems, which can lead to applications in novel “on-off” actuators.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Study of the specific features of single-crystal boron microstructure

A complex study of the structure of β-boron single crystal grown by the floating-zone method, with sizes significantly exceeding the analogs known in the literature, has been performed. The study includes X-ray diffraction analysis and X-ray diffractometry (measurement of pole figures and rocking curves), performed on both laboratory and synchrotron sources; atomic-resolution scanning transmission electron microscopy with spherical aberration correction; and energy-dispersive microanalysis. X-ray diffraction analysis using synchrotron radiation has been used to refine the β-boron structure and find impurity Si atoms. The relative variations in the unit-cell parameters a and c for the crystal bulk are found to be δa/a ≈ 0.4 and δc/c ≈ 0.1%. X-ray diffractometry has revealed that the single-crystal growth axis coincides with the [22̄013] crystallographic axis and makes an angle of 21.12° with the [0001] threefold axis. Electron microscopy data have confirmed that the sample under study is a β-boron crystal, which may contain 0.3–0.4 at % Si as an impurity. Planar defects (stacking faults and dislocations) are found. The results of additional measurements of the temperature dependence of the thermal conductivity of the crystal in the range of 50–300 K are indicative of its high structural quality.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Reduction of phosphorus diffusion in germanium by fluorine implantation

The control of phosphorus (P) diffusion in germanium (Ge) is essential for the realisation of ultrashallow n-type junctions in Ge. This work reports a detailed study of the effect of fluorine (F) co-implantation on P diffusion in Ge. P and F profiles were characterized by secondary ion mass spectroscopy. The ion implantation damage was investigated using cross sectional transmission electron microscopy. It is shown that F co-implantation reduces the implanted P profile width and reduces both intrinsic and extrinsic P diffusion in Ge. A defect mediated mechanism for the strong influence of F co-implantation on P diffusion in Ge is proposed and invokes the formation of F{sub n}V{sub m} clusters in the F-amorphized Ge layer. A fraction of these F{sub n}V{sub m} clusters decorate the interstitial type end-of-range defects in the re-grown Ge layer and the rest react during re-growth with interstitial germanium atoms diffusing back from the amorphous crystalline interface. The Ge vacancies are then annihilated and mobile interstitial F is released and out diffuses from the surface. This results in a re-grown Ge layer which has a low vacancy concentration and in which the P diffusion rate is reduced. These results open the way to the realization of enhanced Ge n-type devices.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Characterisation of reduced graphene oxides prepared from natural flaky, lump and amorphous graphites

Highlights: • Natural flaky, lumpy and amorphous graphites were used to synthesis rGO. • Investigation the effect of the crystal morphology on the oxidation process of GrO and characteristics of prepared rGO. • Low graphitisation degree, big specific surface area and small lateral size were beneficial to the oxidation of graphite. - Abstract: The characterisation of reduced graphene oxides (rGOs) prepared from natural flaky, lumpy, and amorphous graphites using Hummers method was investigated. The prepared graphite oxides (GrOs) and rGOs were characterised by X-ray diffraction, Fourier transform infrared spectroscopy, Raman spectroscopy, UV–vis spectroscopy, atomic force microscopy and electrochemical performance. The results showed that amorphous graphite was much easier to oxidise than lumpy and flaky graphites and was preferable for preparing single or double layer graphene because low graphitisation degree, high defect degree, high specific surface area and small crystal size were beneficial for (1) the oxidants to attack the exposed carbon atoms, (2) the intercalation of oxidants, and (3) the diffusion of oxidants between graphitic layers. In addition, rGO synthesised from amorphous graphite had the most defects and the smallest size of the in-plane sp{sup 2} domains compared to those obtained from the other two nature graphites.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Impact of metal diffusion, lattice distortions, native defects, and ambient on dielectric breakdown in Ni–Ga 2 O 3 Schottky diodes

Ga 2 O 3 unipolar devices are of high interest due to their ~8 MV/cm predicted breakdown fields, which have not yet been achieved due to premature device failure. Pre- and post-failure defect analysis of Ni–Ga 2 O 3 Schottky diodes in ultrahigh vacuum (UHV) and air were performed using depth-resolved cathodoluminescence, high angle annular dark field scanning transmission electron microscopy, and energy dispersive x-ray analysis to understand the physical mechanisms that precede premature breakdown. The breakdown voltage in UHV was dramatically reduced by nearly 40% compared with the breakdown in air. This reduction in the breakdown voltage correlated with post-breakdown differences in Ni distribution, indicating that the coordination and bonding of Ni contribute strongly to electrical behavior in Ni–Ga 2 O 3 Schottky diodes. Breakdown studies in UHV revealed that Ni diffuses away more from the metal–semiconductor interface than with air breakdown, where Ni localizes more near the interface, indicative of the preferential formation of a Ni oxide under O-poor conditions. These measurements also identified the formation of divacancy-interstitial complexes and their characteristic luminescence signature ~150 nm from the interface, the densities of which correlated with breakdown fields. These findings show that electric-field-induced degradation occurs via the rearrangement of native point defects, which act as an additional precursor to device failure. Macroscopically, they show the impact of both vacuum conditions and metal reactivity on Ga 2 O 3 device fabrication.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Methoxy Formation Induced Defects on MoS 2

Here, we find that exposure of the MoS 2 basal plane to methanol leads to the formation of adsorbed methoxy and coincides with sulfur vacancy generation. The conversion of methanol to methoxy on MoS 2 is temperature dependent. Density functional theory simulations and experiment indicate that the methoxy moieties are bound to molybdenum, not sulfur, while some adsorbed methanol is readily desorbed near or slightly above room temperature. Our calculations also suggest that the dissociation of methanol via O–H bond scission occurs at the defect site (sulfur vacancy), followed subsequently by formation of a weakly bound H 2 S species that promptly desorbs from the surface with creation of new sulfur vacancy. Photoluminescence and scanning tunneling microscopy show clear evidence of the sulfur vacancy creation on the MoS 2 surface, after exposure to methanol.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

In Operando Visualization of the Electrochemical Formation of Liquid Polybromide Microdroplets

Zinc–bromine flow batteries are promising for stationary energy storage, and bromine-complexing agents have been used to form phase-separated liquid polybromide products. However, an understanding of the dynamics of polybromide nucleation is limited due to the beam sensitivity and complexity of polybromides. Here we report an in operando platform composed of dark-field light microscopy and a transparent electrochemical cell to reveal the dynamics of polybromide formation in their native environment. Using our platform, we confirm and reveal the liquid nature, chemical composition, pinning effect (strong interaction with Pt), residual effect (residual charge products on the surface), self-discharging, and over-oxidation of the polybromide products. Overall, the results provide insights into the role of complexing agents and guide the future design of zinc–bromine flow batteries. Furthermore, our in operando platform can potentially be used to study sensitive species and phases in other electrochemical reactions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Laser-interference pulse number dependence of surface chemistry and sub-surface microstructure of AA2024-T3 alloy

The laser-based treatment of a metal surface is an intrinsically non-chemical technique that can alter both the topology and chemistry of surfaces. A laser-based treatment for coating and joining applications can offer alternative surface preparations to the chemically-based surface preparation techniques, which are subject to severe environmental protection and hazardous-waste management considerations. In this study, the surface chemistry and sub-surface microstructural changes are investigated for a novel surface processing method using laser interferometry produced by two beams of a pulsed Nd:YAG laser. The two-beam laser-interference allowed the structuring of the surface at length scales much less than that of the laser beam spot. Surface chemistry changes in the oxide layer of AA 2024-T3 aluminum alloy rolled sheet due to laser processing were investigated using x-ray photoelectron spectroscopy (XPS). Near surface microstructural changes have been investigated with scanning electron microscopy and energy dispersive x-ray spectroscopy (SEM/EDS), and scanning transmission electron microscopy (STEM) as a function of number of interfering laser shots. SEM microstructure pictures of the top surface shows the minimization of surface defects, as all of the sharp features from a rolled sheet surface were smoothed by laser-structuring. STEM images indicate that the laser-interference processing reduced the formation of CuMn-rich precipitates over a 500–800 nm depth from the top surface. XPS data indicated that the Al oxide layer is modified compared to that of the baseline specimen and that the oxide thickness increases with the number of shots per spot. Finally, the additional thicker oxide on Al alloys is expected to increase the corrosion resistance of the coated Al 2024.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Laser-Induced Enhancement of Acoustic Mode Quality Factor Revealed by Correlated Single-Particle Optical and Electron Microscopy

Acoustic modes in plasmonic nanostructures provide fundamental insights into their optomechanical behavior at the nanoscale, enabling emerging applications in plasmon-enhanced optomechanics, ultrasensitive sensing, and nanoscale energy transduction. Here we explore the modulation of acoustic phonon dynamics in lithographically fabricated gold nanodisks via laser-induced photothermal annealing. Using a correlated approach that utilizes both single-particle transient extinction spectroscopy and advanced electron microscopy, we directly link nanoscale structural transformations to changes in mechanical properties as probed through the coherence of the excited acoustic modes. Specifically, ultrafast pump–probe microscopy reveals an enhancement in the acoustic mode quality factor of annealed gold nanodisks, indicative of reduced damping and improved vibrational coherence. Structural characterization via scanning electron microscopy and electron backscatter diffraction confirms that photoinduced annealing results in smoother surface morphology and overall enhanced crystallinity. The improved crystalline order reduces defect and crystal boundary scattering, which we suggest as the reason underlying the lower quality factor before annealing. Furthermore, these findings demonstrate that targeted structural engineering at the nanoscale offers a powerful strategy for optimizing the optomechanical performance of plasmonic nanostructures, with broad implications for the design of next-generation nanophotonic and optomechanical systems.

Annealing (metallurgy)↗
DOE OSTI2014

Investigation of Metal Free Naphthalocyanine Vapor Deposited on Au(111)

Naphthalocyanines (Ncs) are promising candidates for future components in electronic devices and applications. To maximize the efficiency of Nc devices, it is critical to understand their structural and electronic properties and how these are impacted by deposition methods. The formation of a metal free naphthalocyanine (H2Nc) self-assembled monolayer on a Au(111) crystal was investigated by scanning tunneling microscopy under ultra-high-vacuum conditions at room temperature. A rigorous purification and processing procedure was developed to produce high purity, low defect, and well-ordered monolayers. High-resolution STM images reveal epitaxial growth of H2Nc on Au(111) with the observed structure having a molecular spacing of 1.6 ± 0.05 nm, with molecules orientated slightly off (roughly 2.5°) the low density packing direction of Au(111). A commensurate structure having 4 molecules per unit cell and unit cell parameters of A = 3.25 ± 0.05 nm, B = 3.17 ± 0.05 nm, and α = 87.5 ± 2° is proposed. Orbital-mediated tunneling spectroscopy was used to examine the electronic properties of individual molecules within the thin film. The first ionization potential and electron affinity of H2Nc adsorbed on Au(111) were measured to be -0.68 ± 0.03 and 1.12 ± 0.02 eV, relative to the Fermi energy.

Environmental Molecular Sciences Laboratory↗
DOE OSTI2022

Compositionally complex doping for zero-strain zero-cobalt layered cathodes

We report the high volatility of the price of cobalt and the geopolitical limitations of cobalt mining have made the elimination of Co a pressing need for the automotive industry. Owing to their high energy density and low-cost advantages, high-Ni and low-Co or Co-free (zero-Co) layered cathodes have become the most promising cathodes for next-generation lithium-ion batteries. However, current high-Ni cathode materials, without exception, suffer severely from their intrinsic thermal and chemo-mechanical instabilities and insufficient cycle life. Here, in this paper, by using a new compositionally complex (high-entropy) doping strategy, we successfully fabricate a high-Ni, zero-Co layered cathode that has extremely high thermal and cycling stability. Combining X-ray diffraction, transmission electron microscopy and nanotomography, we find that the cathode exhibits nearly zero volumetric change over a wide electrochemical window, resulting in greatly reduced lattice defects and local strain-induced cracks. In-situ heating experiments reveal that the thermal stability of the new cathode is significantly improved, reaching the level of the ultra-stable NMC-532. Owing to the considerably increased thermal stability and the zero volumetric change, it exhibits greatly improved capacity retention. This work, by resolving the long-standing safety and stability concerns for high-Ni, zero-Co cathode materials, offers a commercially viable cathode for safe, long-life lithium-ion batteries and a universal strategy for suppressing strain and phase transformation in intercalation electrodes.

25 ENERGY STORAGE↗
DOE OSTI2017

Effects of Bi Addition on the Microstructure and Mechanical Properties of Nanocrystalline Ag Coatings

Here in this study we investigated the effects of Bi addition on the microstructure and mechanical properties of an electrodeposited nanocrystalline Ag coating. Microstructural features were investigated with transmission electron microscopy (TEM). The results indicate that the addition of Bi introduced nanometer-scale Ag-Bi solid solution particles and more internal defects to the initial Ag microstructures. The anisotropic elastic-plastic properties of the Ag nanocrystalline coating with and without Bi addition were examined with nanoindentation experiments in conjunction with the recently-developed inverse method. The results indicate that the as-deposited nanocrystalline Ag coating contained high mechanical anisotropy. With the addition of 1 atomic percent (at%) Bi, the anisotropy within Ag-Bi coating was very small, and yield strength of the nanocrystalline Ag-Bi alloy in both longitudinal and transverse directions were improved by over 100% compared to that of Ag. On the other hand, the strain-hardening exponent of Ag-Bi was reduced to 0.055 from the original 0.16 of the Ag coating. Furthermore, the addition of Bi only slightly increased the electrical resistivity of the Ag-Bi coating in comparison to Ag. Lastly, results of our study indicate that Bi addition is a promising method for improving the mechanical and physical performances of Ag coating for electrical contacts.

36 MATERIALS SCIENCE↗
NASA NTRS2002

Enlargement of Step-Free SiC Surfaces by Homoepitaxial Web-Growth of Thin SiC Cantilevers

Lateral homoepitaxial growth of thin cantilevers emanating from mesa patterns that were reactive ion etched into on-axis commercial SiC substrates prior to growth is reported. The thin cantilevers form after pure stepflow growth removes almost all atomic steps from the top surface of a mesa, after which additional adatoms collected by the large step-free surface migrate to the mesa sidewall where they rapidly incorporate into the crystal near the top of the mesa sidewall. The lateral propagation of the step-free cantilevered surface is significantly affected by pregrowth mesa shape and orientation, with the highest lateral expansion rates observed at the inside concave comers of V-shaped pregrowth mesas with arms lengthwise oriented along the {1100} direction. Complete spanning of the interiors of V's and other mesa shapes with concave comers by webbed cantilevers was accomplished. Optical microscopy, synchrotron white beam x-ray topography and atomic force microscopy analysis of webbed regions formed over a micropipe and closed-core screw dislocations show that c-axis propagation of these defects is terminated by the webbing. Despite the nonoptimized process employed in this initial study, webbed surfaces as large as 1.4 x 10(exp -3) square centimeters, more than four times the pregrowth mesa area, were grown. However, the largest webbed surfaces were not completely free of bilayer steps, due to unintentional growth of 3C-SiC that occurred in the nonoptimized process. Further process optimization should enable larger step-free webs to be realized.

Neudeck, Philip G.↗
DOE OSTI2016

New insights on the formation of supersaturated Cu-Nb solid solution prepared by mechanical alloying

The deformation-driven alloying mechanisms in the immiscible Cu-Nb system during mechanical alloying (MA) process have been studied by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high-resolution TEM (HRTEM) observations. It is found that the dominating alloying mechanism changes at the different stages of milling. Initially, the alloying process is mainly governed by interfaces and dislocations, which supply fast diffusion channels between phases. In the intermediate stage, Nb particles with sizes below 8 nm undergo a bcc to fcc allotropic transformation, and the interdiffusion between fcc-Nb and fcc-Cu is promoted due to the similarity of lattice structures. Further milling generates disclination defects, which contribute to the formation of fragments or subgrains with sizes below 5 nm. The introduction of such defects and fragments benefits the formation of a complete Cu-Nb solid solution. The formation kinetics of solid solution is analyzed by Johnson-Mehl-Avrami equation, which suggests that the speed of the diffusion of Nb atoms into Cu is very slow. - Highlights: •The bcc to fcc transformation in Nb nanoparticles promotes diffusion process. •The formation of fragments with sizes below 5 nm is attributed to the disclination defects. •Defect-assisted diffusion is responsible for the alloying process.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Shear-band thickness and shear-band cavities in a Zr-based metallic glass

Strain localization into shear bands in metallic glasses is typically described as a mechanism that occurs at the nano-scale, leaving behind a shear defect with a thickness of 10–20 nm. Here we sample the structure of a single system-spanning shear band that has carried all plastic flow with high-angle annular dark field scanning transmission electron microscopy (HAADF-STEM) and high-energy x-ray tomography (XRT). It is found that the shear-band thickness and the density change relative to the matrix sensitively depend on position along the shear band. A wide distribution of shear-band thickness (10 nm–210 nm) and density change (–1% to –12%) is revealed. There is no obvious correlation between shear-band thickness and density change, but larger thicknesses correspond typically to higher density changes. More than 100 micron-size shear-band cavities were identified on the shear-band plane, and their three-dimensional arrangement suggests a strongly fluctuating local curvature of the shear plane. As a result, these findings urge for a more complex view of a shear band than a simple nano-scale planar defect.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Crystal defects in solar cells produced by the method of thermomigration

The results of studying the crystal structure of regions in silicon, recrystallized during the course of thermomigration of the liquid Si–Al zone in the volume of the silicon substrate, are reported (similar regions doped with an acceptor impurity are used to obtain high-voltage solar cells). X-ray methods (including measurements of both diffraction-reflection curves and topograms) and also high-resolution electron microscopy indicate that single-crystal regions in the form of a series of thin strips or rectangular grids are formed as a result of the thermomigration of liquid zones. Dislocation half-loops are detected in the surface layers of the front and back surfaces of the substrate. (311)-type defects are observed in the recrystallized regions.

14 SOLAR ENERGY↗