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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 649 records · Page 36
All sourcesNASA NTRSDOE OSTI
DOE OSTI2011

Microwave-hydrothermal synthesis of perovskite bismuth ferrite nanoparticles

Highlights: Black-Right-Pointing-Pointer BiFeO{sub 3} (BFO) nanoparticles were grown by hydrothermal microwave method (HTMW). Black-Right-Pointing-Pointer The soaking time is effective in improving phase formation. Black-Right-Pointing-Pointer Rietveld refinement reveals an orthorhombic structure. Black-Right-Pointing-Pointer The observed magnetism of the BFO crystallites is a consequence of particle size. Black-Right-Pointing-Pointer The HTMW is a genuine technique for low temperatures and short times of synthesis. -- Abstract: Hydrothermal microwave method (HTMW) was used to synthesize crystalline bismuth ferrite (BiFeO{sub 3}) nanoparticles (BFO) in the temperature of 180 Degree-Sign C with times ranging from 5 min to 1 h. BFO nanoparticles were characterized by means of X-ray analyses, FT-IR, Raman spectroscopy, TG-DTA and FE-SEM. X-ray diffraction results indicated that longer soaking time was benefit to refraining the formation of any impurity phases and growing BFO crystallites into almost single-phase perovskites. Typical FT-IR spectra for BFO nanoparticles presented well defined bands, indicating a substantial short-range order in the system. TG-DTA analyses confirmed the presence of lattice OH{sup -} groups, commonly found in materials obtained by HTMW process. Compared with the conventional solid-state reaction process, submicron BFO crystallites with better homogeneity could be produced at the temperature as low as 180 Degree-Sign C. These results show that the HTMW synthesis route is rapid, cost effective, and could be used as an alternative to obtain BFO nanoparticles in the temperature of 180 Degree-Sign C for 1 h.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Demonstration of femtosecond X-ray pump X-ray probe diffraction on protein crystals

The development of X-ray free-electron lasers (XFELs) has opened the possibility to investigate the ultrafast dynamics of biomacromolecules using X-ray diffraction. Whereas an increasing number of structures solved by means of serial femtosecond crystallography at XFELs is available, the effect of radiation damage on protein crystals during ultrafast exposures has remained an open question. We used a split-and-delay line based on diffractive X-ray optics at the Linac Coherent Light Source XFEL to investigate the time dependence of X-ray radiation damage to lysozyme crystals. For these tests, crystals were delivered to the X-ray beam using a fixed-target approach. The presented experiments provide probe signals at eight different delay times between 19 and 213 femtoseconds after a single pump event, thereby covering the time-scales relevant for femtosecond serial crystallography. Even though significant impact on the crystals was observed at long time scales after exposure with a single X-ray pulse, the collected diffraction data did not show significant signal reduction that could be assigned to beam damage on the crystals in the sampled time window and resolution range. This observation is in agreement with estimations of the applied radiation dose, which in our experiment was clearly below the values expected to cause damage on the femtosecond time scale. The experiments presented here demonstrate the feasibility of time-resolved pump-multiprobe X-ray diffraction experiments on protein crystals.

43 PARTICLE ACCELERATORS↗
DOE OSTI2020

Nonequilibrium Thermodynamics of Colloidal Gold Nanocrystals Monitored by Ultrafast Electron Diffraction and Optical Scattering Microscopy

Metal nanocrystals exhibit important optoelectronic and photocatalytic functionalities in response to light. These dynamic energy conversion processes have been commonly studied by transient optical probes to date, but an understanding of the atomistic response following photoexcitation has remained elusive. In this paper, we use femtosecond resolution electron diffraction to investigate transient lattice responses in optically excited colloidal gold nanocrystals, revealing the effects of nanocrystal size and surface ligands on the electron–phonon coupling and thermal relaxation dynamics. First, we uncover a strong size effect on the electron–phonon coupling, which arises from reduced dielectric screening at the nanocrystal surfaces and prevails independent of the optical excitation mechanism (i.e., inter- and intraband). Second, we find that surface ligands act as a tuning parameter for hot carrier cooling. Particularly, gold nanocrystals with thiol-based ligands show significantly slower carrier cooling as compared to amine-based ligands under intraband optical excitation due to electronic coupling at the nanocrystal/ligand interfaces. Finally, we spatiotemporally resolve thermal transport and heat dissipation in photoexcited nanocrystal films by combining electron diffraction with stroboscopic elastic scattering microscopy. Taken together, we resolve the distinct thermal relaxation time scales ranging from 1 ps to 100 ns associated with the multiple interfaces through which heat flows at the nanoscale. Our findings provide insights into optimization of gold nanocrystals and their thin films for photocatalysis and thermoelectric applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

Time-resolved scanning electron microscopy with polarization analysis

We demonstrate the feasibility of investigating periodically driven magnetization dynamics in a scanning electron microscope with polarization analysis based on spin-polarized low-energy electron diffraction. With the present setup, analyzing the time structure of the scattering events, we obtain a temporal resolution of 700 ps, which is demonstrated by means of imaging the field-driven 100 MHz gyration of the vortex in a soft-magnetic FeCoSiB square. Owing to the efficient intrinsic timing scheme, high-quality movies, giving two components of the magnetization simultaneously, can be recorded on the time scale of hours.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2018

Free-electron laser data for multiple-particle fluctuation scattering analysis

Fluctuation X-ray scattering (FXS) is an emerging experimental technique in which solution scattering data are collected using X-ray exposures below rotational diffusion times, resulting in angularly anisotropic X-ray snapshots that provide several orders of magnitude more information than traditional solution scattering data. Such experiments can be performed using the ultrashort X-ray pulses provided by a free-electron laser source, allowing one to collect a large number of diffraction patterns in a relatively short time. Here, we describe a test data set for FXS, obtained at the Linac Coherent Light Source, consisting of close to 100 000 multi-particle diffraction patterns originating from approximately 50 to 200 Paramecium Bursaria Chlorella virus particles per snapshot. In addition to the raw data, a selection of high-quality pre-processed diffraction patterns and a reference SAXS profile are provided.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2016

Modeling spatially localized photonic nanojets from phase diffraction gratings

We investigated numerically the specific spatially localized intense optical structure, a photonic nanojet (PNJ), formed in the near-field scattering of optical radiation at phase diffraction gratings. The finite-difference time-domain technique was employed to study the PNJ key parameters (length, width, focal distance, and intensity) produced by diffraction gratings with the saw-tooth, rectangle, and hemispheric line profiles. Our analysis showed that each type of diffraction gratings produces a photonic jet with unique characteristics. Based on the numerical calculations, we demonstrate that the PNJ could be manipulated in a wide range through the variation of period, duty cycle, and shape of diffraction grating rulings.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2011

2-ps Hard X-Ray Streak Camera Measurements at Sector 7 Beamline of the Advanced Photon Source

A hard X-ray streak camera capable of 2-ps time resolution is in operation at the Sector 7 beamline of the Advanced Photon Source. It is used for laser-pump, X-ray probe experiments using the Ti:Sapphire femtosecond laser system installed on the beamline. This streak camera, combined with standardized and prealigned experimental setups, can perform time-resolved liquid-phase absorption spectroscopy, reflectivity, and diffraction experiments.

43 PARTICLE ACCELERATORS↗
DOE OSTI2016

Elucidating microstructure of spinodal copper alloy through annealing

Improvement in the characteristics of a polycrystalline material is done through engineering of microstructures. Spinodal decomposed copper alloy has been annealed at high temperature with systematic variation in time on multiple specimens. Extensive electron backscatter diffraction experiment was carried out to understand the grain boundary characteristics and morphologies of the alloy as a function of annealing time. The logical variation of annealing time strongly influences diffusion induced grain characteristics such as, shape, size, geometry, inclination, density, types, distribution, misorientations and the nature of subsequently induced twinning morphologies. - Highlights: •Spinodal copper alloy is annealed at high temperature by systematic time variation. •EBSD measurements are performed to quantify grain geometries and morphologies. •Annealing time has a strong influence on grain morphologies, twins and misorientations. •Grain morphologies and geometries are correlated with hardness data. •Elucidating microstructure development through grain boundary engineering.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Dynamic x-ray diffraction and nanosecond quantification of kinetics of formation of β -zirconium under shock compression

We report the atomic- and nanosecond-scale quantification of kinetics of a shock-driven phase transition in Zr metal. We uniquely make use of a multiple shock-and-release loading pathway to shock Zr into the β phase and to create a quasisteady pressure and temperature state shortly after. Coupling shock loading with in situ time-resolved synchrotron x-ray diffraction, we probe the structural transformation of Zr in the steady state. Our results provide a quantified expression of kinetics of formation of β-Zr phase under shock loading: transition incubation time, completion time, and crystallization rate.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2012

In-situ synchrotron energy-dispersive x-ray diffraction study of thin Pd foils with Pd:D and Pd:H concentrations up to 1:1

Time resolved, in-situ, energy dispersive x-ray diffraction was performed in an electrolysis cell during electrochemical loading of palladium foil cathodes with hydrogen and deuterium. Concentrations of H:Pd (D:Pd) up to 1:1 in 0.1 M LiOH (LiOD) in H{sub 2}O (D{sub 2}O) electrolyte were obtained, as determined by both the Pd lattice parameter and cathode resistivity. In addition, some indications on the kinetics of loading and deloading of hydrogen from the Pd surface were obtained. The alpha-beta phase transformations were clearly delineated but no new phases at high concentration were determined.

36 MATERIALS SCIENCE↗
DOE OSTI2014

The chemical instability of Na{sub 2}IrO{sub 3} in air

Highlights: • Na{sub 2}IrO{sub 3} decomposes rapidly in laboratory air. • The decomposition requires the simultaneous presence of CO{sub 2} and H{sub 2}O. • Decomposition results in a dramatic change in the magnetic properties. • Second 5 K feature in magnetic susceptibility not previously reported. - Abstract: We report that Na{sub 2}IrO{sub 3}, which has a layered honeycomb iridium oxide sublattice interleaved by Na planes, decomposes in laboratory air while maintaining the same basic crystal structure. The decomposition reaction was monitored by time-dependent powder X-ray diffraction under different ambient atmospheres, through which it was determined that it occurs only in the simultaneous presence of both CO{sub 2} and H{sub 2}O. A hydrated sodium carbonate is the primary decomposition product along with altered Na{sub 2}IrO{sub 3}. The diffraction signature of the altered Na{sub 2}IrO{sub 3} is quite similar to that of the pristine material, which makes the detection of decomposition difficult in a sample handled under ordinary laboratory conditions. The decomposed samples show a significantly decreased magnetic susceptibility and the disappearance of the low temperature antiferromagnetic transition considered to be characteristic of the phase. Samples that have never been exposed to air after synthesis display a previously unreported magnetic transition at 5 K.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Synchronized Stress-strain Measurements in Dynamic Loading at High Pressure using D-DIA

A new data collection protocol for forced oscillation experiments using a multianvil high pressure device is reported. We derive the stress of the sample at high pressure and temperature from synchrotron x-ray diffraction that is synchronized with sample strain measurements from x-ray radiographs. This method yields stress directly from the sample rather than a stress proxy. Furthermore, the diffraction pattern yields useful information concerning time evolution of structurally related phenomena. Here we illustrate some of these possibilities with high pressure experimental data.

99 GENERAL AND MISCELLANEOUS↗
NASA NTRS1993

Diffractive optics fabricated by direct write methods with an electron beam

State-of-the-art diffractive optics are fabricated using e-beam lithography and dry etching techniques to achieve multilevel phase elements with very high diffraction efficiencies. One of the major challenges encountered in fabricating diffractive optics is the small feature size (e.g. for diffractive lenses with small f-number). It is not only the e-beam system which dictates the feature size limitations, but also the alignment systems (mask aligner) and the materials (e-beam and photo resists). In order to allow diffractive optics to be used in new optoelectronic systems, it is necessary not only to fabricate elements with small feature sizes but also to do so in an economical fashion. Since price of a multilevel diffractive optical element is closely related to the e-beam writing time and the number of etching steps, we need to decrease the writing time and etching steps without affecting the quality of the element. To do this one has to utilize the full potentials of the e-beam writing system. In this paper, we will present three diffractive optics fabrication techniques which will reduce the number of process steps, the writing time, and the overall fabrication time for multilevel phase diffractive optics.

Kress, Bernard↗
DOE OSTI2024

Dehydration kinetics of nanoconfined water in beryl probed by high temperature single crystal synchrotron X-ray diffraction

Understanding changes in material properties through external stimuli plays a key role in validating the expected performance of materials and engineering material properties in a controlled manner. Here, we introduce a fundamental protocol to deduce dehydration reactions kinetics of water confined in nanopore channels, with the cyclosilicate beryl as the scaffold of interest, using time-resolved synchrotron X-ray diffraction (SXRD), in the temperature interval of 298–1038 K. The temperature-dependent intensity (I) of the strongest reflection (112) was used as the crystallite variable. An estimation of an isobaric thermal crystallite coefficient, k, analogous with the isobaric thermal expansion coefficient, established the rate of relative crystallization as a function of temperature, $\frac{∂I}{∂T}$. A plot of lnk and $\frac{1}{T}$ gives rise to two kinetic steps, indicating a slow dehydration stage up to ~ 700 K and a fast dehydration stage up to the investigated temperature 1038 K. The crystal structure of beryl determined up to 1038 K, in temperature increment as small as 10 K, indicates the presence of channel ions Na and Fe and a gradual decrease of water upon heating.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2006

Detecting Negative Obstacles by Use of Radar

Robotic land vehicles would be equipped with small radar systems to detect negative obstacles, according to a proposal. The term "negative obstacles" denotes holes, ditches, and any other terrain features characterized by abrupt steep downslopes that could be hazardous for vehicles. Video cameras and other optically based obstacle-avoidance sensors now installed on some robotic vehicles cannot detect obstacles under adverse lighting conditions. Even under favorable lighting conditions, they cannot detect negative obstacles. A radar system according to the proposal would be of the frequency-modulation/ continuous-wave (FM/CW) type. It would be installed on a vehicle, facing forward, possibly with a downward slant of the main lobe(s) of the radar beam(s) (see figure). It would utilize one or more wavelength(s) of the order of centimeters. Because such wavelengths are comparable to the characteristic dimensions of terrain features associated with negative hazards, a significant amount of diffraction would occur at such features. In effect, the diffraction would afford a limited ability to see corners and to see around corners. Hence, the system might utilize diffraction to detect corners associated with negative obstacles. At the time of reporting the information for this article, preliminary analyses of diffraction at simple negative obstacles had been performed, but an explicit description of how the system would utilize diffraction was not available.

Mittskus, Anthony↗
DOE OSTI2026

Resolving Competing Ultraviolet Photoinduced Ring-Opening and Dissociation Pathways in Iodothiophenes by Ultrafast Electron Diffraction

The ultraviolet photochemistry of halothiophenes is thought to proceed via competing pathways, prompt C–X (X = halogen) bond fission, and parent ring opening followed by fragmentation, yet direct structural evidence distinguishing these mechanisms is limited. Here, time-resolved gas-phase ultrafast electron diffraction (UED) has been used to directly follow the structural dynamics of 2- and 3-iodothiophene following photoexcitation at 247 nm. For both isomers, the time-resolved pair distribution functions reveal the appearance of new interatomic distances that cannot be explained by simple C–I bond cleavage and formation of C 4 SH 3 radical cofragments. The signatures, particularly those for 2-iodothiophene, are consistent with a rival ring-opening channel of the intact parent, which evolve on time scales distinct from those associated with the direct C–I bond cleavage. In addition, the extracted kinetics indicate that the ring-opening channel occurs faster in 2-iodothiophene than in the 3-isomer at this excitation wavelength. Furthermore, these measurements provide direct geometric evidence for competing pathways leading to different structures following photodissociation in a model heteroaromatic and further establish UED as a sensitive probe of complex excited-state chemistry.

Bond cleavage↗
DOE OSTI2025

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

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

36 MATERIALS SCIENCE↗