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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 397 records · Page 22
All sourcesNASA NTRSDOE OSTI
DOE OSTI2016

Imaging in real and reciprocal space at the Diamond beamline I13

The Diamond Imaging and Coherence beamline I13 consists of two independent branchlines for imaging in real and reciprocal space. Different microscopies are available providing a range of spatial resolution from 5µm to potentially 5nm. The beamline operates in the energy range of 6-35keV covering different scientific areas such as biomedicine, materials science and geophysics. Several original devices have been developed at the beamline, such as the EXCALIBUR photon counting detector and the combined robot arms for coherent X-ray diffraction.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2011

Phase relations in a barium-rich high-temperature region (25-45 mol% CuO, 900-1100 deg. C) of the BaO-CuO{sub x} system

The phase relations have been studied in the BaO-CuO{sub x} system in the range of 25.0-45.0 mol% CuO at 900-1100 deg. C at P(O{sub 2})=21 kPa (air) by visual polythermal analysis (VPA), powder X-ray diffraction (XRD), electron diffraction (ED) with simultaneous energy-dispersive X-ray (EDX) elemental analysis in a transmission electron microscope (TEM), and iodometric chemical analysis. The discrete deviations 2.02 (101:50), 2.04 (102:50), 2.10 (105:50) of Ba/Cu (Ba:Cu) composition from the stoichiometric ratio 2:1 have been found for the known Ba{sub 2}CuO{sub 3+{delta}} oxides in the subsolidus region 900-970 deg. C. Unit cell parameters of the 101:50 orthorhombic oxide, 102:50 tetragonal one, 105:50 orthorhombic one are, respectively, a=4.049, b=3.899, c=13.034 A; a=3.985, c=12.968 A; a=4.087, b=3.897 and c=12.950 A. ED patterns of the 101:50, 102:50, 105:50 oxides show characteristic supercell reflections with the respective vector 1/60[5 4 0], {approx}2/11<1 1 0> and 1/6[2 0 0]. Oxides of the 2:1, 7:4, 5:3 and 23:20 compositions have been found in the crystallization region 970-1050 deg. C. Unit cell parameters of the 2:1 orthorhombic oxide are a=4.095, b=3.795, c=13.165 A. Interplanar spacings and X-ray characteristic peak intensities of the 7:4, 5:3 and 23:20 oxides are given. Oxides 2:1 and 7:4 melt pseudocongruently at 1020 and 1005 deg. C, oxides 5:3 and 23:20 melt incongruently at 995 and 980 deg. C, respectively. A diagram of the phase relations in the studied region of the BaO-CuO{sub x} system has been constructed, whose structure is considered as the total projection of phase states of the system existing for different x. - Graphical Abstract: A diagram of phase relations in the BaO-CuO{sub x} system in the range of 30.0-45.0 mol% CuO at 900-1050 deg. C at P(O{sub 2})=21 kPa (air) constructed on the data obtained by visual polythermal analysis (the liquidus line), XRD and ED with elemental analysis. Highlights: > A combination of physical-chemical and structural methods was used. > New discrete oxides have been found. > The diagram reflects the total projection of phase states at different x.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2011

Synthesis of Cu Nanowires with Polycarbonate Template

Copper nanowires were fabricated into arrays of pores on ion-track etched polycarbonate membrane, using electrodeposition technique. We coated Au thin film layer on one side of membrane in order to have electrical contact. X-ray diffraction analysis shows that the Au layer has a strong (111) texture. The pores which have cylindrical shape with 6 micron length and 30 nm diameter were filled by copper atoms, fabricating Cu nanowires. Energy Disperse Spectrometry (EDS) indicated the picks of copper which filled the pores of substrate. The morphology and structure of Cu nanowires were characterized by SEM, TEM and XRD, respectively. The results show that although all the nanowires do not have uniform diameter, but all of them are continuous along the length.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2019

Laguerre–Gauss and Hermite–Gauss soft X-ray states generated using diffractive optics

Light’s capacity to carry angular momentum is integral to our knowledge of physics and ability to probe matter. In addition to spin, photons can occupy free-space orbital angular momentum eigenstates. Visible light orbital angular momentum is used in quantum information experiments, super-resolution microscopy, optical tweezers and angular momentum transfer to atoms in optical lattices. Soft X-ray orbital angular momentum applications, slowed by the lack of suitable optics and the rarity of coherent X-ray sources, could enable the direct alteration of atomic states through orbital angular momentum exchange, and methods to study the electronic properties of quantum materials. We have made soft X-ray diffractive optics that generate single Laguerre–Gauss modes, observed carrying up to 30$\hbar$ angular momentum per photon, or their superpositions. We also present Hermite–Gauss diffractive optics and a soft X-ray orbital angular momentum analyser. Finally, these tools could enable both the manipulation and finer characterization of topologically complex electronic matter, such as magnetic skyrmions.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2018

Glancing-incidence focussed ion beam milling: A coherent X-ray diffraction study of 3D nano-scale lattice strains and crystal defects

Here, this study presents a detailed examination of the lattice distortions introduced by glancing incidence Focussed Ion Beam (FIB) milling. Using non-destructive multi-reflection Bragg coherent X-ray diffraction we probe damage formation in an initially pristine gold micro-crystal following several stages of FIB milling. These experiments allow access to the full lattice strain tensor in the micro-crystal with ~25 nm 3D spatial resolution, enabling a nano-scale analysis of residual lattice strains and defects formed. Our results show that 30 keV glancing incidence milling produces fewer large defects than normal incidence milling at the same energy. However the resulting residual lattice strains have similar magnitude and extend up to ~50 nm into the sample. At the edges of the milled surface, where the ion-beam tails impact the sample at near-normal incidence, large dislocation loops with a range of Burgers vectors are formed. Further glancing incidence FIB polishing with 5 keV ion energy removes these dislocation loops and reduces the lattice strains caused by higher energy FIB milling. However, even at the lower ion energy, damage-induced lattice strains are present within a ~20 nm thick surface layer. These results highlight the need for careful consideration and management of FIB damage. They also show that low-energy FIB-milling is an effective tool for removing FIB-milling induced lattice strains. This is important for the preparation of micro-mechanical test specimens and strain microscopy samples.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2025

Reuniting crystallography with real space: Ab initio structure elucidation with 4D-STEM

Structure elucidation via single-crystal methods has historically lacked experimental access to real-space information, instead relying exclusively on diffraction-space measurements of Bragg reflections. Here we exploit the dual-space imaging power of 4D scanning transmission electron microscopy to meaningfully integrate real-space information into the crystallographic workflow. We show that virtual apertures assembled by segmentation of high-angle annular dark-field images enable i) pixel-by-pixel separation of coherent Bragg signal from clusters of closely spaced nanocrystals and ii) selective extraction of integrated intensities from thinner subregions of individual specimens, facilitating retroactive tuning of multiple scattering artifacts. This strategy empowers us to simply pick and choose whichever nanoscale regions of interest generate the highest-quality diffraction patterns, allowing us to solve several independent structures of the metal-organic framework UiO-66 from specimens whose agglomerated morphology proved intractable for conventional microcrystal electron diffraction. Our method is compatible with both rotational and serial approaches to data processing, ultimately divulging the first scanning nanobeam electron diffraction structures determined by direct methods at subangstrom resolution.

Saha, Ambarneil↗
DOE OSTI2011

Characterization of Large Grain Nb Ingot Microstructure Using EBSP Mapping and Laue Camera Methods

Large grain/single crystal Nb is currently being examined for fabricating superconducting radiofrequency (SRF) cavities as an alternative to using rolled sheet. Three ingot slices from different suppliers have been characterized and are compared. It is desirable to know the grain orientations of an ingot slice before fabrication. Characterization of an ingot slice has been done using electron backscattered pattern (EBSP) orientation imaging microscopy (OIM), which requires cutting out pieces from the slice, a destructive technique. Use of a Laue camera allows nondestructive characterization of grain orientations. The OIM method was used to examine ingot slices from CBMM and Ningxia, while the Laue method was used to examine a Heraeus ingot slice. The three ingot slices are compared in terms of their crystal orientations and grain boundary misorientations, indicating no obvious commonalities. The Laue method has practical advantages over OIM for evaluating ingot slices during the manufacturing process.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Hybrid molecular beam epitaxy of germanium-based oxides

Abstract Germanium-based oxides such as rutile GeO 2 are garnering attention owing to their wide band gaps and the prospects of ambipolar doping for application in high-power devices. Here, we present the use of germanium tetraisopropoxide (GTIP), a metal-organic chemical precursor, as a source of germanium for the demonstration of hybrid molecular beam epitaxy for germanium-containing compounds. We use Sn 1- x Ge x O 2 and SrSn 1- x Ge x O 3 as model systems to demonstrate our synthesis method. A combination of high-resolution X-ray diffraction, scanning transmission electron microscopy, and X-ray photoelectron spectroscopy confirms the successful growth of epitaxial rutile Sn 1- x Ge x O 2 on TiO 2 (001) substrates up to x = 0.54 and coherent perovskite SrSn 1- x Ge x O 3 on GdScO 3 (110) substrates up to x = 0.16. Characterization and first-principles calculations corroborate that germanium occupies the tin site, as opposed to the strontium site. These findings confirm the viability of the GTIP precursor for the growth of germanium-containing oxides by hybrid molecular beam epitaxy, thus providing a promising route to high-quality perovskite germanate films.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Electrical Properties of Barium and Zirconium Modified NBT Ferroelectric Ceramics

Recently a new wave of interest has risen on relaxor ferroelectrics with complex perovskite structure due to their wide use in fabrication of multilayer ceramic capacitors, electrostrictive actuators, and electromechanical transducers. The polycrystalline 0.93(Bi{sub 0.5}Na{sub 0.5})Ba{sub 0.07}Z{sub 0.04}T{sub 0.96}O{sub 3}(0.07BNBZT) ceramic material, which is in the vicinity of the morphotropic phase boundary (MPB) has been prepared by using high temperature solid state reaction method. The tolerance factor has been estimated and found to be 0.815. XRD analysis revealed a rhombohedral perovskite type structure. SEM micrographs showed highly dense grains with rectangular shape. The average grain size is found to be 1.51{mu}m. Dielectric studies in the material ha indicated relaxor behaviour with diffuse phase transition. High value of {epsilon}{sub m}>1958 is found at 1kHz, Tm (phase transition temperature) 335 deg. C, The diffuseness parameter was established to be 1.60 revealing the relaxor behaviour. Further, to confirm the relaxor behaviour in the material, Vogel-Fulcher (V-F) relation has been used. Estimated V-F parameters are found to be T{sub f} = 138 deg. C, E{sub a} = 0.080 eV and {nu}{sub o} = 2.32x10{sup 8} Hz. Cole-Cole analysis has shown a non-Debye type relaxation in the system. Conductivity studies in the material obeyed the Jonscher's power law in frequency range of (45Hz-5MHz) and temperature range of (35 deg. C - 600 deg. C). The electric conduction in the system may be due to hopping/mobility/ transportation of charge carriers.

36 MATERIALS SCIENCE↗
NASA NTRS2024

Ternary Feldspar Within Felste Clasts From Apollo Impact Melt Breccia 72255

Granitic clasts with unique ternary feldspar compositions have been identified within samples of the layered impact melt breccia from Apollo 17 Station 2 Boulder 1 (72215, 72235, 72255 and 72275), and in a felsite clast from station 3 (73215). These “ternary” compositions seemingly plot within the miscibility gap of the albite-anorthite-orthoclase (Ab-An-Or) system. Feldspars with these compositions have not been identified in terrestrial samples, and equilibrium feldspar compositions from laboratory experiments indicate they would not be thermodynamically stable. Thus, the physiochemical processes involved in forming these unique ternary feldspars remain poorly understood. To better constrain the formation of ternary feldspar within lunar breccias, we have undertaken a coordinated scanning electron microscope (SEM)-based coupled electron backscatter diffraction (EBSD) and energy dispersive spectrometry (EDS), electron microprobe analyzer (EPMA) wavelength dispersive spectrometry, and transmission electron microscopy (TEM) study. The goals of this study are twofold: 1) confirm whether ternary feldspar is present as coherent, single-crystals or sub-microscopic intergrowths of normal compositions, and 2) better constrain the formation conditions of clasts containing ternary feldspar.

T. M. Erickson↗
DOE OSTI2022

3D Bragg Coherent Diffraction Imaging of Extended Nanowires: Defect Formation in Highly Strained InGaAs Quantum Wells

InGaAs quantum wells embedded in GaAs nanowires can serve as compact near-infrared emitters for direct integration onto Si complementary metal oxide semiconductor technology. While the core–shell geometry in principle allows for a greater tuning of composition and emission, especially farther into the infrared, the practical limits of elastic strain accommodation in quantum wells on multifaceted nanowires have not been established. One barrier to progress is the difficulty of directly comparing the emission characteristics and the precise microstructure of a single nanowire. Here, in this study, we report an approach to correlating quantum well morphology, strain, defects, and emission to understand the limits of elastic strain accommodation in nanowire quantum wells specific to their geometry. We realize full 3D Bragg coherent diffraction imaging (BCDI) of intact quantum wells on vertically oriented epitaxial nanowires, which enables direct correlation with single-nanowire photoluminescence. By growing In 0.2 Ga 0.8 As quantum wells of distinct thicknesses on different facets of the same nanowire, we identified the critical thickness at which defects are nucleated. A correlation with a traditional transmission electron microscopy analysis confirms that BCDI can image the extended structure of defects. Finite element simulations of electron and hole states explain the emission characteristics arising from strained and partially relaxed regions. This approach, imaging the 3D strain and microstructure of intact nanowire core–shell structures with application-relevant dimensions, can aid the development of predictive models that enable the design of new compact infrared emitters.

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

Three dimensions, two microscopes, one code: Automatic differentiation for x-ray nanotomography beyond the depth of focus limit

Conventional tomographic reconstruction algorithms assume that one has obtained pure projection images, involving no within-specimen diffraction effects nor multiple scattering. Advances in x-ray nanotomography are leading toward the violation of these assumptions, by combining the high penetration power of x-rays, which enables thick specimens to be imaged, with improved spatial resolution that decreases the depth of focus of the imaging system. We describe a reconstruction method where multiple scattering and diffraction effects in thick samples are modeled by multislice propagation and the 3D object function is retrieved through iterative optimization. We show that the same proposed method works for both full-field microscopy and for coherent scanning techniques like ptychography. Our implementation uses the optimization toolbox and the automatic differentiation capability of the open-source deep learning package TensorFlow, demonstrating a straightforward way to solve optimization problems in computational imaging with flexibility and portability.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2018

Structural Changes as a Function of Thickness in [(SnSe) 1+δ ] m TiSe 2 Heterostructures

Single- and few-layer metal chalcogenide compounds are of significant interest due to structural changes and emergent electronic properties on reducing dimensionality from three to two dimensions. To explore dimensionality effects in SnSe, a series of [(SnSe) 1+δ ] m TiSe 2 intergrowth structures with increasing SnSe layer thickness (m = 1-4) were prepared from designed thin-film precursors. In-plane diffraction patterns indicated that significant structural changes occurred in the basal plane of the SnSe constituent as m is increased. Scanning transmission electron microscopy cross-sectional images of the m = 1 compound indicate long-range coherence between layers, whereas the m >/= 2 compounds show extensive rotational disorder between the constituent layers. For m >/= 2, the images of the SnSe constituent contain a variety of stacking sequences of SnSe bilayers. Density functional theory calculations suggest that the formation energy is similar for several different SnSe stacking sequences. The compounds show unexpected transport properties as m is increased, including the first p-type behavior observed in (MSe)m(TiSe 2 ) n compounds. The resistivity of the m >/- 2 compounds is larger than for m = 1, with m = 2 being the largest. At room temperature, the Hall coefficient is positive for m = 1 and negative for m = 2-4. The Hall coefficient of the m = 2 compound changes sign as temperature is decreased. The room-temperature Seebeck coefficient, however, switches from negative to positive at m = 3. These properties are incompatible with single band transport indicating that the compounds are not simple composites.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Studies on Stuctural and Electrical Properties of (1-X)Ba(Fe{sub 0.5}Nb{sub 0.5})O{sub 3}-xSrTiO{sub 3}, with X = 0, 0.05 Ceramics

A polycrystalline ceramics of (1-x)Ba(Fe{sub 0.5}Nb{sub 0.5})O{sub 3}-xSrTiO{sub 3}, with x = 0, 0.05 was synthesized by high temperature solid-state reaction technique. X-ray diffraction analysis of the powders suggests the formation of a single-phase material with monoclinic structure. SEM images exhibit the uniform distribution of grains of the sample. Sintered pellets were investigated for its dielectric ({epsilon} and tan{delta}) properties in the temperature range of 30 deg. C - 270 deg. C and in the frequency range of 100Hz-5MHz suggest that the compound do not have dielectric anomaly in the studied frequency and temperature ranges.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Adaptively coupled phase retrieval in multi-peak Bragg coherent diffraction imaging

Recent advances in Bragg coherent diffraction imaging (BCDI) experimental techniques permit routine measurement of multiple Bragg peaks from a single crystalline grain. The resulting images contain the full lattice distortion vector field which can be differentiated to provide lattice strain and rotation. With the advent of fourth-generation synchrotron light sources, such multi-peak datasets are produced at high rates, facilitating the need for rapid phase retrieval of the multiple peaks and subsequent image analysis. Here we describe and demonstrate a new implementation of a coupled phase retrieval technique for multi-peak BCDI which simultaneously treats each Bragg peak of the dataset and produces a three-dimensional image of the crystal's morphology and lattice distortion field. In addition, this method uses the redundant information contained in the various Bragg diffraction patterns to detect and suppress spurious signal appearing on the detector in a subset of the measurements. Compared with manual data editing, adaptive coupling produces a more consistent phase profile in reciprocal space and sharper surfaces in direct space, with no significant difference in computational cost. These improvements reduce the need for manual preprocessing and enable robust high-throughput analysis of multi-peak BCDI data, supporting near-real-time strain microscopy at modern synchrotron facilities.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Soft X-Ray Microscopy at HZB: Zone Plate Development and Imaging Using the Third Order of Diffraction

The Helmholtz-Zentrum Berlin (HZB) operates a transmission x-ray microscope (TXM) in the soft x-ray photon energy range with an energy resolution up to E/{Delta}E = 10{sup 4}. An approach to achieve ultrahigh spatial resolution with conventional, standard zone plate optics is to employ higher orders of diffraction of the zone plate objective. In this paper, we demonstrate that 11-nm lines and spaces of a multilayer test structure are clearly resolved by the x-ray microscope using the third order of diffraction of a zone plate objective with 20-nm outermost zone width. The disadvantage of high-order imaging is an about one order of magnitude lower diffraction efficiency of the used zone plates employed in the third order compared to the first order of diffraction. In addition, the measured background signal in the TXM images is no longer negligible. Therefore, we worked on the fabrication of zone plates with sub-20-nm outermost zone width to increase the spatial resolution in the first order of diffraction. A new high-resolution 100-keV e-beam lithography system from VISTEC, which was recently installed at the Helmholtz-Zentrum Berlin, makes these developments possible. Initial results on zone plates with an outermost zone width down to 15 nm exposed with the new e-beam system are presented. Furthermore, the contrast transfer function of the transmission x-ray microscope operating in partial coherence mode is measured by using the first and third diffraction order of the zone plate objective.

43 PARTICLE ACCELERATORS↗
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 OSTI2023

Spin-mediated shear oscillators in a van der Waals antiferromagnet

Understanding how microscopic spin configuration gives rise to exotic properties at the macroscopic length scale has long been pursued in magnetic materials. One seminal example is the Einstein-de Haas effect in ferromagnets, in which angular momentum of spins can be converted into mechanical rotation of an entire object. However, for antiferromagnets without net magnetic moment, how spin ordering couples to macroscopic movement remains elusive. Here we observed a seesaw-like rotation of reciprocal lattice peaks of an antiferromagnetic nanolayer film, whose gigahertz structural resonance exhibits more than an order-of-magnitude amplification after cooling below the Neel temperature. Using a suite of ultrafast diffraction and microscopy techniques, we directly visualize this spin-driven rotation in reciprocal space at the nanoscale. This motion corresponds to interlayer shear in real space, in which individual micro-patches of the film behave as coherent oscillators that are phase-locked and shear along the same in-plane axis. Using time-resolved optical polarimetry, we further show that the enhanced mechanical response strongly correlates with ultrafast demagnetization, which releases elastic energy stored in local strain gradients to drive the oscillators. Finally, our work not only offers the first microscopic view of spin-mediated mechanical motion of an antiferromagnet but it also identifies a new route towards realizing high-frequency resonators up to the millimetre band, so the capability of controlling magnetic states on the ultrafast timescale can be readily transferred to engineering the mechanical properties of nanodevices.

36 MATERIALS SCIENCE↗