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Results for “Single Particle X-ray Diffractive Imaging”

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 91 records · Page 5
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

Femtosecond X-ray Fourier holography imaging of free-flying nanoparticles

Ultrafast X-ray imaging on individual fragile specimens such as aerosols, metastable particles, superfluid quantum systems and live biospecimens provides high-resolution information that is inaccessible with conventional imaging techniques. Coherent X-ray diffractive imaging, however, suffers from intrinsic loss of phase, and therefore structure recovery is often complicated and not always uniquely defined. Here in this paper, we introduce the method of in-flight holography, where we use nanoclusters as reference X-ray scatterers to encode relative phase information into diffraction patterns of a virus. The resulting hologram contains an unambiguous three-dimensional map of a virus and two nanoclusters with the highest lateral resolution so far achieved via single shot X-ray holography. Our approach unlocks the benefits of holography for ultrafast X-ray imaging of nanoscale, non-periodic systems and paves the way to direct observation of complex electron dynamics down to the attosecond timescale.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2021

The role of precursor decomposition in the formation of samarium doped ceria nanoparticles via solid-state microwave synthesis

The impact on the final morphology of ceria (CeO 2 ) nanoparticles made from different precursors (commercial: cerium acetate/nitrate) and in house: cerium tri(methylsilyl)amide (Ce-TMSA)) via a microwave solid state reaction has been determined. In all instances, powder X-ray diffraction indicated that the cubic fluorite CeO 2 phase (PDF# 04–004-9150, with the space group Fm-3 m) had formed. Scanning electron microscopy (SEM) images revealed spherical nanoparticles were produced from the Ce-TMSA precursor. The commercial acetate and nitrate precursors produced particles with irregular morphology. The roles of the precursor decomposition and binding energy in the synthesis of the nanocrystals with various morphologies, as well as a possible growth mechanism, were evaluated based on experimental and computational data. The formation of spherical shaped nanoparticles was determined to be due to the preferential single-step decomposition of the Ce-TMSA as well as the low activation energy to overcome decomposition. Due to the complicated decomposition of the commercial precursors and high activation energy the resulting particles adopted an irregular morphology. Highly uniform samarium doped ceria (Sm x Ce 1-x O 2-δ ) nanospheres were also synthesized from Ce-TMSA and samarium tri(methylsilyl)amide (Sm-TMSA). The effects of reaction time and temperature, on the final morphology were observed through SEM. The rapid single-step decomposition of TMSA-based precursors as observed through thermogravimetric analysis (TGA) and confirmed through the calculation of potential energy surfaces and binding energies from density functional theory (DFT) calculations, indicated that nanoparticle formation follows LaMer’s classical nucleation theory.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Experimental demonstration of coupled multi-peak Bragg coherent diffraction imaging with genetic algorithms

Bragg coherent diffraction imaging has the potential to provide significant insight into the structure-properties relationship for crystalline materials by imaging, with nanoscale resolution, three-dimensional strain fields within individual grains and nanoparticles. The capability of present-day synchrotrons to locate and measure a multiplicity of Bragg reflections from a single grain makes it possible to recover the full strain tensor with nanometer resolution. Recent methods for coupling reconstructions from several peaks to determine the strain tensor have been developed and applied to synthetic data, but have not been applied to experimental data. Here, using a coupled genetic reconstruction algorithm, we reconstruct an experimental data set and demonstrate improvements in the ability to resolve vector-valued displacement fields internal to the particle as compared to what is achieved with a noncoupled approach. The coupled approach developed in this work was also validated on simulated data sets. In both simulated and experimental data, reconstructions from our coupled Bragg peak algorithm show improvements over the noncoupled independent reconstruction method of 5% in terms of accuracy and 53% in terms of consistency.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Thermal annealing dynamics of carbon-coated LiFePO{sub 4} nanoparticles studied by in-situ analysis

The thermal behavior of core-shell carbon-coated lithium iron phosphate (LiFePO{sub 4}-C) nanoparticles made by flame spray pyrolysis (FSP) during annealing was investigated by in-situ transmission electron microscopy (TEM), in-situ X-ray powder diffraction (XRD) as well as ex-situ diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS). Crystallization of the initially glassy LiFePO{sub 4}-C nanoparticles starts at quite low temperatures (T=400 °C), forming single crystals inside the confinement of the carbon shell. Upon increasing the temperature to T≥700 °C, LiFePO{sub 4} starts to diffuse through the carbon shell resulting in cavities inside the mostly intact carbon shell. By increasing the temperature further to T≥800 °C, the initial core-shell morphology converts into open carbon shells (flakes and cenospheres) and bulky LiFePO{sub 4} particles (diameter in the range 300–400 nm), in agreement with ex-situ experiments. - Graphical abstract: TEM images of a typical sample area recorded at room temperature and after heating in-situ heating reveal the growth of particles and the formation of empty carbon cages. - Highlights: • LiFePO{sub 4} coated by a carbon shell is produced by flame spray pyrolysis. • The amorphous LiFePO{sub 4} starts to crystallize at 400 °C as revealed by in-situ XRD. • Crystal growth was visualized by TEM heating experiments. • The formation of empty carbon cages starts at 700 °C.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2017

Preference of multi-walled carbon nanotube (MWCNT) to single-walled carbon nanotube (SWCNT) and activated carbon for preparing silica nanohybrid pickering emulsion for chemical enhanced oil recovery (C-EOR)

The aim of this research was to determine the best nano hybrid that can be used as a Pickering emulsion Chemical Enhanced Oil Recovery (C-EOR). Therefore, we have prepared different carbon structures nano hybrids with SiO{sub 2} nano particles with different weight percent using sol-gel method. The as-prepared nano materials were characterized with X-Ray Diffraction (XRD), Field Emission Scanning Electron Microscopy (FE-SEM) and Thermal Gravimetric Analysis (TGA). Pickering emulsions of these nanohybrids were prepared at pH=7 in ambient temperature and with distilled water. Stability of the mentioned Pickering emulsions was controlled for one month. Emulsion phase morphology was investigated using optical microscopic imaging. Evaluation results demonstrated that the best sample is the 70% MWCNT/SiO{sub 2} nanohybrid. Stability of the selected nanohybrid (70% MWCNT/SiO{sub 2} nanohybrid) was investigated by alteration of salinity, pH and temperature. Results showed that the mentioned Pickering emulsion has very good stability at 0.1%, 1% salinity, moderate and high temperature (25 °C and 90 °C) and neutral and alkaline pH (7, 10) that is suitable for the oil reservoirs conditions. The effect of the related nano fluid on the wettability of carbonate rock was investigated by measuring the contact angle and interfacial tension. Results show that the nanofluid could significantly change the wettability of the carbonate rock from oil wet to water wet and can decrease the interfacial tension. Therefore, the 70% MWCNT/SiO{sub 2} nanohybrid Pickering emulsion can be used for Chemical Enhanced Oil Recovery (C-EOR).

36 MATERIALS SCIENCE↗
DOE OSTI2020

Refinement for single-nanoparticle structure determination from low-quality single-shot coherent diffraction data

With the emergence of X-ray free-electron lasers, it is possible to investigate the structure of nanoscale samples by employing coherent diffractive imaging in the X-ray spectral regime. In this work, we developed a refinement method for structure reconstruction applicable to low-quality coherent diffraction data. The method is based on the gradient search method and considers the missing region of a diffraction pattern and the small number of detected photons. We introduced an initial estimate of the structure in the method to improve the convergence. The present method is applied to an experimental diffraction pattern of an Xe cluster obtained in an X-ray scattering experiment at the SPring-8 Angstrom Compact free-electron LAser (SACLA) facility. It is found that the electron density is successfully reconstructed from the diffraction pattern with a large missing region, with a good initial estimate of the structure. The diffraction pattern calculated from the reconstructed electron density reproduced the observed diffraction pattern well, including the characteristic intensity modulation in each ring. Our refinement method enables structure reconstruction from diffraction patterns under difficulties such as missing areas and low diffraction intensity, and it is potentially applicable to the structure determination of samples that have low scattering power.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2016

Enhancing scattering images for orientation recovery with diffusion map

We explore the possibility for orientation recovery in single-molecule coherent diffractive imaging with diffusion map. This algorithm approximates the Laplace-Beltrami operator, which we diagonalize with a metric that corresponds to the mapping of Euler angles onto scattering images. While suitable for images of objects with specific properties we show why this approach fails for realistic molecules. Here, we introduce a modification of the form factor in the scattering images which facilitates the orientation recovery and should be suitable for all recovery algorithms based on the distance of individual images. (C) 2016 Optical Society of America

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2018

Modifying High-Voltage Olivine-Type LiMnPO 4 Cathode via Mg Substitution in High-Orientation Crystal

The LiMnPO4 material with Mg2+ ion substitution in transition metal site is successfully obtained by a facile solvothermal method combining with the subsequent spray drying and pyrolysis. The TEM image shows the controlled crystalline orientation of the primary Mg-doped LiMnPO4 particle, and the three-dimensional (3D) hierarchical micronano structure and the electronic structure of the Mg-doped material are investigated by the reconstructed nanotomography and X-ray absorption spectroscopy, respectively. The uniformity of Mg2+ ions substitution at the secondary particle level is confirmed by the transmission X-ray microscopy combined with X-ray absorption near edge structure. The prepared material exhibits an excellent electrochemical performance with the capacity of 156 mAh/g at the rate of 0.1 C, and good capacity retention of 100% after 400 cycles at the rate of 1 C. The in operando synchrotron X-ray diffraction data indicate that the performance improvement of the Mg-doped materials is attributed to the changed electrochemical reaction mechanism from the typical two-phase reaction for pristine LiMnPO4 material to the two-phase reaction combined with the single-phase (solid-solution) reaction process. These findings provide a new approach and understanding on developing high-energy cathode materials for lithium-ion batteries.

high orientation↗
DOE OSTI2016

Dynamic deformation and fracture of single crystal silicon: Fracture modes, damage laws, and anisotropy

Impact fracture of single-crystal Si is critical to long-term reliability of electronic devices and solar cells for its wide use as components or substrates in semiconductor industry. Single-crystal Si is loaded along two different crystallographic directions with a split Hopkinson pressure bar integrated with an in situ x-ray imaging and diffraction system. Bulk stress histories are measured, simultaneously with x-ray phase contrast imaging (XPCI) and Laue diffraction. Damage evolution is quantified with grayscale maps from XPCI. Single-crystal Si exhibits pronounced anisotropy in fracture modes, and thus fracture strengths and damage evolution. For loading along [11¯ 0] and viewing along [001], (1¯1¯0)[11¯ 0] cleavage is activated and induces horizontal primary cracks followed by perpendicular wing cracks. However, for loading along [011¯] and viewing along [111], random nucleation and growth of shear and tensile-splitting crack networks lead to catastrophic failure of materials with no cleavage. The primary-wing crack mode leads to a lower characteristic fracture strength due to predamage, but a more concentrated strength distribution, i.e., a higher Weibull modulus, compared to the second loading case. Furthermore, the sequential primary cracking, wing cracking and wing-crack coalescence processes result in a gradual increase of damage with time, deviating from theoretical predictions. Particle size and aspect ratios of fragments are discussed with postmortem fragment analysis, which verifies fracture modes observed in XPCI.

36 MATERIALS SCIENCE↗
DOE OSTI2024

The Pixel Anomaly Detection Tool : a user-friendly GUI for classifying detector frames using machine-learning approaches

Data collection at X-ray free electron lasers has particular experimental challenges, such as continuous sample delivery or the use of novel ultrafast high-dynamic-range gain-switching X-ray detectors. This can result in a multitude of data artefacts, which can be detrimental to accurately determining structure-factor amplitudes for serial crystallography or single-particle imaging experiments. Here, a new data-classification tool is reported that offers a variety of machine-learning algorithms to sort data trained either on manual data sorting by the user or by profile fitting the intensity distribution on the detector based on the experiment. This is integrated into an easy-to-use graphical user interface, specifically designed to support the detectors, file formats and software available at most X-ray free electron laser facilities. The highly modular design makes the tool easily expandable to comply with other X-ray sources and detectors, and the supervised learning approach enables even the novice user to sort data containing unwanted artefacts or perform routine data-analysis tasks such as hit finding during an experiment, without needing to write code.

47 OTHER INSTRUMENTATION↗
DOE OSTI2023

Hints of Growth Mechanism Left in Supercrystals

Supercrystals of DNA-functionalized nanoparticles arevisualizedin three dimensions using X-ray ptychographic tomography, and theirreciprocal spaces are mapped with small-angle X-ray scattering inorder to better understand their internal defect structures. X-rayptychographic tomography reveals various types of defects in an assemblythat otherwise exhibits a single crystalline diffraction pattern.On average, supercrystals composed of smaller nanoparticles are smallerin size than supercrystals composed of larger particles. Additionally,supercrystals composed of small nanoparticles are typically aggregatedinto larger "necklace-like" structures. Within theselarger structures, some but not all pairs of connected domains arecoherent in their relative orientations. In contrast, supercrystalscomposed of larger nanoparticles with longer DNA ligands typicallyform faceted crystals. The combination of these two complementaryX-ray techniques reveals that the crystalline assemblies grow by aggregationof smaller assemblies followed by rearrangement of nanoparticles.

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

In situ high-temperature X-ray diffraction study of Sc-doped titanium oxide nanocrystallites

Titanium dioxide is an inexpensive wide-gap highly ionic semiconductor with striking photocatalytic capabilities in several heterogeneous photoredox reactions. A small crystal size is desirable to maximize the surface area, since photocatalytic reactions occur at the surface of a photocatalyst. Presented in this work are the synthesis and microstructural characterization of 4 at.% Sc-doped TiO 2 (4SDT) prepared by water-based co-precipitation. The crystal structure of 4SDT was examined via in situ high-temperature powder X-ray diffraction experiments from 25 to 1200°C. Rietveld analysis revealed single-phase anatase up to 875°C, while at 900°C the anatase-to-rutile phase transformation occurred and at higher temperatures additional reflections of Sc-rich phases (Sc 2 TiO 5 from 975°C and Ti 3 Sc 4 O 12 or Sc 2 O 3 at 1200°C) were observed. Debye function analysis (DFA) was applied to model the total scattering pattern directly in reciprocal space, allowing the reconstruction of Ti vacancies. Both Rietveld and DFA methods were applied to estimate the nanocrystallite size and shape with consistent growth in crystallite size with temperature: an ellipsoid shape with equatorial ~4.7 nm / axial (001) ~6.9 nm at 25°C to equatorial ~27.9 nm / axial (001) ~39.6 nm at 900°C refined by Rietveld analysis, versus a cylinder shape with D a , b = 4.3 nm and size dispersion σ ab = 1.5 nm, L c = 4.9 nm and σ c = 2.3 nm at 25°C to D a , b = 21.4 nm, σ ab = 8.3 nm, L c = 23.9 and σ c = 10.9 nm at 900°C estimated by DFA. The microstructural changes obtained by Rietveld and DFA methods were supported by high-resolution transmission electron microscopy image analysis, as well as by the less direct nitrogen sorption techniques that provide information on the size of non-agglomerated and dense particles. The Ti site-occupancy factor showed a linear increase from 0.6–0.8 at 25°C to unity at 900°C for anatase, and from ~0.7 at 900°C to unity at 1200°C for rutile, via Rietveld analysis and DFA.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Structural and magnetic characteristics of PVA/CoFe{sub 2}O{sub 4} nano-composites prepared via mechanical alloying method

Highlights: • Single phase CoFe{sub 2}O{sub 4} nano-particles synthesized in one step by mechanical alloying. • PVA/CoFe{sub 2}O{sub 4} magnetic nano-composites were fabricated via mechanical milling. • FTIR confirmed the interaction between PVA and magnetic CoFe{sub 2}O{sub 4} particles. • Increasing in milling time and PVA amount led to well dispersion of CoFe{sub 2}O{sub 4}. - Abstract: In this research, polyvinyl alcohol/cobalt ferrite nano-composites were successfully synthesized employing a two-step procedure: the spherical single-phase cobalt ferrite of 20 ± 4 nm mean particle size was synthesized via mechanical alloying method and then embedded into polymer matrix by intensive milling. The results revealed that increase in polyvinyl alcohol content and milling time causes cobalt ferrite particles disperse more homogeneously in polymer matrix, while the mean particle size and shape of cobalt ferrite have not been significantly affected. Transmission electron microscope images indicated that polyvinyl alcohol chains have surrounded the cobalt ferrite nano-particles; also, the interaction between polymer and cobalt ferrite particles in nano-composite samples was confirmed. Magnetic properties evaluation showed that saturation magnetization, coercivity and anisotropy constant values decreased in nano-composite samples compared to pure cobalt ferrite. However, the coercivity values of related nano-composite samples enhanced by increasing PVA amount due to domain wall mechanism.

36 MATERIALS SCIENCE↗
NASA NTRS2005

Lunar and Planetary Science XXXVI, Part 6

Contents include the following: A Model for Multiple Populations of Presolar Diamonds. Characterization of Martian North Polar Geologic Units Using Mars Odyssey THEMIS Data. Effect of Flow on the Internal Structure of the Martian North Polar Layered Deposits. Elemental Abundance Distributions in Basalt Clays and Meteorites: Is It a Biosignature? Early Results on the Saturn System from the Composite Infrared Spectrometer. NanoSIMS D/H Imaging of Isotopically Primitive Interplanetary Dust Particles. Presolar (Circumstellar and Interstellar) Phases in Renazzo: The Effects of Parent Body Processing. Catastrophic Disruption of Hydrated Targets: Implications for the Hydrated Asteroids and for the Production of Interplanetary Dust Particles. Chemical and Mineralogical Analyses of Particles from the Stratospheric Collections Coinciding with the 2002 Leonid Storm and the 2003 Comet Grigg-Skjellerup Trail Passage. An Analysis of the Solvus in the CaS-MnS System. ESA s SMART-1 Mission at the Moon: First Results, Status and Next Steps. Europa Analog Ice-splitting Measurements and Experiments with Ice-Hunveyor on the Frozen Balaton-Lake, Hungary. Chromium on Eros: Further Evidence of Ordinary Chondrite Composition. Dust Devil Tracks on Mars: Observation and Analysis from Orbit and the Surface. Spatial Variation of Methane and Other Trace Gases Detected on Mars: Interpretation with a General Circulation Model. Mars Water Ice and Carbon Dioxide Seasonal Polar Caps: GCM Modeling and Comparison with Mars Express Omega Observations. Component Separation of OMEGA Spectra with ICA. Clathrate Formation in the Near-Surface Environment of Titan. Space Weathering: A Proposed Laboratory Approach to Explaining the Sulfur Depletion on Eros. Sample Collection from Small Airless Bodies: Examination of Temperature Constraints for the TGIP. Sample Collector for the Hera Near-Earth Asteroid Sample Return Mission. A Rugged Miniature Mass-Spectrometer for Measuring Aqueous Geochemistry on Mars. Martian and Lunar Pyroxene Microstructures Studied by Single-Crystal X-Ray Diffraction.

Source record↗
DOE OSTI2021

Quantitative agreement between dynamical rocking curves in ultrafast electron diffraction for x-ray lasers

Electron diffraction through a thin patterned silicon membrane can be used to create complex spatial modulations in electron distributions. By precisely varying parameters such as crystallographic orientation and wafer thickness, the intensity of reflections in the diffraction plane can be controlled and by placing an aperture to block all but one spot, we can form an image with different parts of the patterned membrane, as is done for bright-field imaging in microscopy. The patterned electron beams can then be used to control phase and amplitude of subsequent x-ray emission, enabling novel coherent x-ray methods. Furthermore, the electrons themselves can also be used for femtosecond time resolved diffraction and microscopy. As a first step toward patterned beams, we demonstrate experimentally and through simulation the ability to accurately predict and control diffraction spot intensities. We simulate MeV transmission electron diffraction patterns using the multislice method for various crystallographic orientations of a single crystal Si(001) membrane near beam normal. The resulting intensity maps of the Bragg reflections are compared to experimental results obtained at the Accelerator Structure Test Area Ultrafast Electron Diffraction (ASTA UED) facility at SLAC. Furthermore, the fraction of inelastic and elastic scattering of the initial charge is estimated along with the absorption of the membrane to determine the contrast that would be seen in a patterned version of the Si(001) membrane.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2018

Single-shot 3D coherent diffractive imaging of core-shell nanoparticles with elemental specificity

We report 3D coherent diffractive imaging (CDI) of Au/Pd core-shell nanoparticles with 6.1nm spatial resolution with elemental specificity. We measured single-shot diffraction patterns of the nanoparticles using intense x-ray free electron laser pulses. By exploiting the curvature of the Ewald sphere and the symmetry of the nanoparticle, we reconstructed the 3D electron density of 34 core-shell structures from these diffraction patterns. To extract 3D structural information beyond the diffraction signal, we implemented a super-resolution technique by taking advantage of CDI’s quantitative reconstruction capabilities. We used high-resolution model fitting to determine the Au core size and the Pd shell thickness to be 65.0±1.0nm and 4.0±0.5nm, respectively. We also identified the 3D elemental distribution inside the nanoparticles with an accuracy of 3%. To further examine the model fitting procedure, we simulated noisy diffraction patterns from a Au/Pd core-shell model and a solid Au model and confirmed the validity of the method. We anticipate this super-resolution CDI method can be generally used for quantitative 3D imaging of symmetrical nanostructures with elemental specificity.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗
DOE OSTI2019

Preparation and Thermophysical Investigations of CoFe{sub 2}O{sub 4}-based Nanofluid: a Potential Heat Transfer Agent

Cobalt ferrite nanoparticles were synthesized by employing chemical co-precipitation technique. The structure, morphology, elemental composition, and magnetization studies of cobalt ferrite nanoparticles were carried by XRD, FE-SEM, EDS, and VSM techniques, respectively. Rietveld refined XRD pattern exhibited the single-phase cubic spinel structure with Fd-3m space group. FE-SEM images indicated some agglomeration of spherical grains which can be attributed to high surface energy and magnetic interactions. Presence of peaks of respective elements (Co, Fe, and O) in EDS spectrum showed formation of CoFe{sub 2}O{sub 4}. The M–H loop recorded at 300 K revealed superparamagnetic behavior and explained by fine particles size. The blocking temperature of the CoFe{sub 2}O{sub 4}nanoparticles from FC-ZFC curve was found to be 144 K. Cobalt ferrite–ethylene glycol nanofluids of various concentrations 0.0–1.0% in steps of 0.2% were prepared by ultrasonically assisted two-step technique. Thermophysical parameters such as thermal conductivity, specific heat, viscosity, and density were investigated as a function of both volume fraction and temperature. The experimental and theoretical value of each sample was correlated. The thermal conductivity was significantly enhanced with an increase in volume fraction and temperature.

36 MATERIALS SCIENCE↗