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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 433 records · Page 24
All sourcesNASA NTRSDOE OSTI
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↗
DOE OSTI2015

Interface-structure of the Si/SiC heterojunction grown on 6H-SiC

The Si/SiC heterojunctions were prepared on 6H-SiC (0001) C-face by low-pressure chemical vapour deposition at 850 ∼ 1050 °C. Transmission electron microscopy and selected area electron diffraction were employed to investigate the interface-structure of Si/SiC heterojunctions. The Si/6H-SiC heterostructure of large lattice-mismatch follows domain matching epitaxy mode, which releases most of the lattice-mismatch strain, and the coherent Si epilayers can be grown on 6H-SiC. Si(1-11)/6H-SiC(0001) heterostructure is obtained at 900 °C, and the in-plane orientation relationship of Si/6H-SiC heterostructure is (1–11)[1-1-2]{sub Si}//(0001)[-2110]{sub 6H-SiC}. The Si(1-11)/6H-SiC(0001) interface has the same 4:5 Si-to-SiC matching mode with a residual lattice-mismatch of 0.26% along both the Si[1-1-2] and Si[110] orientations. When the growth temperature increases up to 1000 °C, the 〈220〉 preferential orientation of the Si film appears. SAED patterns at the Si/6H-SiC interface show that the in-plane orientation relationship is (-220)[001]{sub Si}//(0001)[2-1-10]{sub 6H-SiC}. Along Si[110] orientation, the Si-to-SiC matching mode is still 4:5; along the vertical orientation Si[001], the Si-to-SiC mode change to approximate 1:2 and the residual mismatch is 1.84% correspondingly. The number of the atoms in one matching-period decreases with increasing residual lattice-mismatch in domain matching epitaxy and vice versa. The Si film grows epitaxially but with misfit dislocations at the interface between the Si film and the 6H-SiC substrate. And the misfit dislocation density of the Si(1-11)/6H-SiC(0001) and Si(-220)/6H-SiC(0001) obtained by experimental observations is as low as 0.487 × 10{sup 14 }cm{sup −2} and 1.217 × 10{sup 14 }cm{sup −2}, respectively, which is much smaller than the theoretical calculation results.

36 MATERIALS SCIENCE↗
DOE OSTI2011

A very promising piezoelectric property of Ta{sub 2}O{sub 5} thin films. I: Monoclinic-trigonal phase transition

Ceramic thin films of tantalum oxide of a new trigonal structure (a=12.713(7) A, {alpha}=28.201(0){sup o}, space-group R3) were produced by thermal treatments of amorphous deposits on (001)Si wafers, either by electrostatic spray deposition or by injection metal-organic chemical vapor decomposition. This trigonal phase comes from the transformation of a monoclinic phase 11L- or 25L-Ta{sub 2}O{sub 5}. The transformation is reversible under oxygen atmosphere and, from results of TEM investigations, occurs mainly via atomic motions along the z unique axis of the monoclinic structure parallel to the polar three-fold axis of the trigonal structure. The non-centrosymmetry and direction of polar axis of the trigonal phase, identified by high resolution TEM imaging, indicate a possibility of very high electric dipole moments linked to a strong piezoelectricity. From results of XPS analyses of both monoclinic and trigonal structures, the binding energies remain similar to those of Ta{sub 2}O{sub 5}. As the formation of the trigonal structure gives rise to an important volume expansion, stresses induced in ceramic thin films are likely influencing both properties of birefringence and piezoelectricity which are presented in a separated article (part II). It is mentioned that the formation of trigonal phase does not occur in bulk Ta{sub 2}O{sub 5} samples, for which an incommensurate phase transition has been observed in a previous work. - Graphical abstract: (a) {theta}/2{theta} X-ray pattern of the tantalum oxide layer prepared by i-MOCVD, cooled down at 5 deg. C min{sup -1} after a thermal treatment at 850 deg. C under N{sub 2} for 1 h. (b) Rhombohedral cell of the Ta{sub 2}O{sub 5} trigonal structure of R3 space-group decorated with its 10 Ta sites. Highlights: > We examine crystallographic properties of a new Ta{sub 2}O{sub 5} trigonal phase. > Its formation occurs only in thin films. > It comes from a reversible transition with a monoclinic phase. > A possibility of strong piezoelectricity is deduced from the present study.

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

Epitaxial europium oxide on Ni(100) with single-crystal quality

High quality epitaxy of EuO on Ni(100) is developed in an in situ scanning tunneling microscopy (STM) and low-energy electron diffraction (LEED) study. A careful selection of the initial growth parameters is decisive to obtain a surface oxide suitable for the subsequent epitaxy of single phase EuO(100). After the creation of a three layer thick coalesced oxide film for the subsequent growth a distillation technique is applied. Appropriate annealing of films with up to 100 nm thickness generates sufficient conductivity for STM and electron spectroscopies. Oxygen vacancies are directly imaged by STM. They are of decisive importance for the metal-to-insulator transition around the temperature of the ferromagnetic-to-paramagnetic transition. A fast relaxation of the initial biaxial strain observed by LEED leaves little hope for an increase of the Curie temperature through epitaxial compression. Ex situ x-ray adsorption spectroscopy and magneto-optical Kerr effect microscopy measurements of thicker films are consistent with the stoichiometric single phase EuO with bulk properties.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Excess Conductivity Investigation of Y{sub 3}Ba{sub 5}Cu{sub 8}O{sub 18±δ} Superconductors Prepared by Various Parameters of Planetary Ball Milling Technique

Superconducting samples of type Y{sub 3}Ba{sub 5}Cu{sub 8}O{sub 18±δ} were elaborated by using a planetary high-energy ball milling (HEBM) technique with various parameters. Phases, microstructure, and superconductivity have been examined using X-ray powder diffraction (XRD), scanning electron microscopy (SEM), and electrical resistivity measurements. SEM investigation shows the occurrence of nanoentities embedded into the superconducting matrix for samples prepared by a ball milling technique. The main objective of this study is to investigate the influence of ball milling parameters on the fluctuation-induced conductivity (FIC). The electrical resistivity versus temperature, ρ(T), above T{sub c} was analyzed using Lawrence–Doniach (LD) and Aslamazov–Larkin (AL) models. Different fluctuation regimes indicated by short-wave fluctuation (SWF) and three-dimensional (3D), two-dimensional (2D), one-dimensional (1D), and critical region (CR) fluctuations were identified. The coherence length at zero temperature, the effective layer thickness, the critical magnetic fields, and the critical current densities are determined. The superconducting parameters strongly depend on the planetary ball milling technique, and the results are explained in relevancy to the microstructure. It was found that the achievement of a microstructure with well-dispersed nanoentities is an effective way for introducing pinning centers for enhancing critical current density and flux pinning capability of bulk Y-358.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2017

Manipulating the polar mismatch at the LaNi O 3 / SrTi O 3 (111) interface

Heteroepitaxial growth of transition-metal oxide films on the open (111) surface of SrTi O 3 results in significant restructuring due to the polar mismatch. Monitoring the structure and composition on an atomic scale of LaNi O 3 / SrTi O 3 (111) interface as a function of processing conditions has enabled the avoidance of the expected polar catastrophe. Using atomically resolved transmission electron microscopy and spectroscopy as well as low-energy electron diffraction, the structure of the thin film, from interface to the surface, has been studied. Here, we show that the proper processing can lead to a structure that is ordered, coherent with the substrate without intermediate structural phase. Using angle-resolved x-ray photoemission spectroscopy we show that the oxygen content of thin films increases with the film thickness, which indicates that the polar mismatch is avoided by the presence of oxygen vacancies.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Revealing the nanostructure of calcium phosphate coatings using HRTEM/FIB techniques

Herein, we report on the micro- and nanostructure of the calcium phosphate coating produced by pulsed laser deposition (PLD), using focused ion beam (FIB) lamella sample preparation and transmission electron microscopy (TEM) as the characterization technique. The initial selected area electron diffraction (SAED) data demonstrated the presence of hydroxyapatite (HA) over any other possible calcium phosphate crystalline structure and the polycrystalline nature of the coating. Moreover, the SAED analyses showed clear textured ring patterns coherent with the presence of a preferred orientation in the HA nano-crystal growth. The SAED data also indicated that the coating appears to be textured in the 〈002〉 crystalline direction. Dark-field images obtained using 002 as the working reflection showed a clear oriented crystal growth in columns, from bottom to top. These columns have a peculiar arrangement of nano-crystals since, in some cases, the preferred orientation appears to start at a certain distance from the substrate. Direct d-spacing measurements on high-resolution TEM images provided further proof of the presence of an HA nano-crystal structure. The reported data may be of interest in the future to adjust the microstructure of the HA coatings. - Highlights: •The FIB lift-out technique allows a very site-specific sample preparation method for HRTEM analysis. •It also permits a fast assessment of the HA coating thickness and elemental composition (EDS). •The coatings exhibit a nano-crystalline nature, with a texturing effect along the 002 planes. •PLD is suitable for the production of crystalline c-axis oriented hydroxyapatite coatings. •The crystalline HA phase in the PLD coating is very similar to the present in bone.

36 MATERIALS SCIENCE↗
DOE OSTI2011

The role of kinetics on the Mn-induced reconstructions of the GaAs(001) surface

A combined scanning tunneling microscopy and low-energy electron diffraction investigation of the Mn/GaAs(001) interface formation is reported. The interface, grown on a (2 x 4) reconstructed substrate produced by molecular beam epitaxy, was studied as a function of Mn evaporation with thickness ranging from 1/8 ML to 1 ML. The interaction of Mn atoms with the semiconductor surface is strong and leads to surface reconstructions involving a rearrangement of the two outmost atomic layers of the substrate. For Mn thickness lower than 1/2 ML, the surface is characterized by a (2 x 1) periodicity. Conversely, when the Mn deposition is increased to 1/2 ML the surface reconstruction is strongly dependent on the preparation procedure. If Mn deposition is performed on the substrate at 390 deg. C, a fully ordered surface characterized by a clear (2 x 2) reconstruction is obtained, whereas, annealing the sample after Mn deposition, gives a disordered surface with a (2 x 1) symmetry. An intermediate phase between (2 x 1) and (2 x 2) is found for Mn depositions in between 1/4 and 1/2 ML. No further structural evolution was observed for both preparation methods above 1/2 ML coverage.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Current Status of Single Particle Imaging with X-ray Lasers

The advent of ultrafast X-ray free-electron lasers (XFELs) opens the tantalizing possibility of the atomic-resolution imaging of reproducible objects such as viruses, nanoparticles, single molecules, clusters, and perhaps biological cells, achieving a resolution for single particle imaging better than a few tens of nanometers. Improving upon this is a significant challenge which has been the focus of a global single particle imaging (SPI) initiative launched in December 2014 at the Linac Coherent Light Source (LCLS), SLAC National Accelerator Laboratory, USA. A roadmap was outlined, and significant multi-disciplinary effort has since been devoted to work on the technical challenges of SPI such as radiation damage, beam characterization, beamline instrumentation and optics, sample preparation and delivery and algorithm development at multiple institutions involved in the SPI initiative. Currently, the SPI initiative has achieved 3D imaging of rice dwarf virus (RDV) and coliphage PR772 viruses at ~10 nm resolution by using soft X-ray FEL pulses at the Atomic Molecular and Optical (AMO) instrument of LCLS. Meanwhile, diffraction patterns with signal above noise up to the corner of the detector with a resolution of ~6 Ångström (Å) were also recorded with hard X-rays at the Coherent X-ray Imaging (CXI) instrument, also at LCLS. Achieving atomic resolution is truly a grand challenge and there is still a long way to go in light of recent developments in electron microscopy. However, the potential for studying dynamics at physiological conditions and capturing ultrafast biological, chemical and physical processes represents a tremendous potential application, attracting continued interest in pursuing further method development. In this paper, we give a brief introduction of SPI developments and look ahead to further method development.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Correlation between cation order/disorder and the electrocaloric effect in the MLCCs of complex perovskite ferroelectrics

The physical properties (dielectric, ferroelectric, piezoelectric, etc.) of complex perovskite ferroelectrics depend on the degree of order/disorder and the scale of the ordered domains. In this study, the electrocaloric (EC) properties of three representative complex perovskite ferroelectrics, Pb(Mg 1/3 Nb 2/3 )O 3 -8PbTiO 3 (PMN-8PT), 1mol% Sm-doped Pb(Mg 1/3 Nb 2/3 )O 3 -8PbTiO 3 (1S-PMN-8PT) and Pb(Sc 1/2 Ta 1/2 )O 3 (PST) are evaluated. Multi-layer ceramic capacitors (MLCCs) with identical structural configurations were fabricated for these three compounds, and their EC properties were characterized by direct measurement using a thermocouple. The EC temperature change of PMN-8PT, 1S-PMN-8PT and PST MLCCs under 20 V μm –1 at room temperature were found to be 1.42 K, 1.54 K, and 3.10 K, respectively. X-ray diffraction and high-resolution transmission electron microscopy data suggests that the high EC performance of PST is related to the ordering of B-site cations (Sc 3+ and Ta 5+ ) with the ordering parameter S = 0.82 and a long coherence length of ~100 nm, such that the sample transitioned from a relaxor ferroelectric to a normal ferroelectric. Furthermore, these results provide pathway towards design of high performance EC materials required for solid state refrigeration and air-conditioning technologies.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Ethanol Sensitivity of Cu{sub 1-x}Sn{sub x}O(x = 0.00, 0.03, and 0.05) Nanoflakes

Cu{sub 1-x}Sn{sub x}O(x = 0.00, 0.03, and 0.05) nanoflakes were synthesized by a simple wet chemical method and X-Ray diffraction (XRD) result confirms the monoclinic structure of CuO with no secondary phases due to Sn doping. The scanning electron microscopic images indicate the formation of nanoflakes. The fundamental Raman modes were observed at 273, 318, 610, and 1084 cm{sup -1} for undoped CuO sample and theses modes were slightly shifted towards lower frequency side for Sn-doped samples, which indicates the inclusion of Sn in CuO. In addition, XRD and Raman studies infer the decrease of crystallinity in doped samples, which is reflected in the sensitivity towards ethanol. The ethanol sensitivity (resistivity measurement) increases with ethanol gas concentration and decreases with Sn-doping in CuO nanoflakes.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Morphology, structure, and chemistry of nanoclusters in a mechanically alloyed nanostructured ferritic steel

Nanostructured ferritic steels have excellent high temperature creep properties and radiation tolerance due to the presence of a high density of Ti-Y-O-enriched nanoclusters. The morphology of the nanoclusters is found to be consistent with a truncated rhombic dodecahedron defined by the {l_brace}100{r_brace} and {l_brace}110{r_brace} planes in the Fe matrix. The derived symmetry and the compositional information indicate that the nanoclusters are inconsistent with the cubic Y2Ti2O7 or the polymorphs of Y2TiO5 phase. Possible structural models are discussed.

36 MATERIALS SCIENCE↗