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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 91 records · Page 5
All sourcesNASA NTRSDOE OSTI
DOE OSTI2011

Methotrexate intercalated ZnAl-layered double hydroxide

The anticancerous drug methotrexate (MTX) has been intercalated into an ZnAl-layered double hydroxide (LDH) using an anion exchange technique to produce LDH-MTX hybrids having particle sizes in the range of 100-300 nm. X-ray diffraction studies revealed increases in the basal spacings of ZnAl-LDH-MTX hybrid on MTX intercalation. This was corroborated by the transmission electron micrographs, which showed an increase in average interlayer spacing from 8.9 A in pristine LDH to 21.3 A in LDH-MTX hybrid. Thermogravimetric analyses showed an increase in the decomposition temperature for the MTX molecule in the LDH-MTX hybrid indicating enhanced thermal stability of the drug molecule in the LDH nanovehicle. The cumulative release profile of MTX from ZnAl-LDH-MTX hybrids in phosphate buffer saline (PBS) at pH 7.4 was successfully sustained for 48 h following Rigter-Peppas model release kinetics via diffusion. - Graphical abstract: ZnAl-layered double hydroxide intercalated with methotrexate ({approx}34% loading) promises the possibility of use of ZnAl-LDH material as drug carrier and in controlled delivery. Highlights: > ZnAl-layered double hydroxide methotrexate nanohybrid has been synthesized. > XRD and TEM studies on nanohybrid revealed successful intercalation of methotrexate. > TG and CHN analyses showed {approx}34 wt% of methotrexate loading into the nanohybrid. > Possibility of use of ZnAl-LDH material as drug carrier and in delivery.

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

Phonon properties of nanosized MnWO{sub 4} with different size and morphology

Highly hierarchical barlike and flowerlike MnWO{sub 4} microcrystals have been synthesized for the first time by a hydrothermal method, where ethanolamine (EA) and cetyltrimethylamonnium bromide (CTAB) play important roles in directing growth and self-assembly of these structures. The possible formation process has been proposed. In addition, platelike nanosized MnWO{sub 4} was also synthesized by annealing of a precursor obtained by coprecipitation method. The obtained samples were characterized by XRD, SEM, TEM, Raman and IR methods. Raman spectra showed relatively weak dependence on particle size and morphology of the particles. In contrast to this behavior, IR-active bands showed pronounced shifts and changes in relative intensities on particle size and the morphology. Origin of this behavior is discussed. - Graphical Abstract: SEM images of MnWO{sub 4} particles prepared by hydrothermal process at 150 deg. C (left panel) and 200 deg. C (right panel). Highlights: > Hydrothermal synthesis with ethanolamine enables growth of hierarchical nanosized MnWO{sub 4} particles. > Annealing of a precursor obtained by coprecipitation method enables growth of platelike MnWO{sub 4} nanoparticles. > Raman and IR spectra of MnWO{sub 4} nanoparticles depend on both size and morphology of the nanoparticles. > We discuss origin of this behavior.

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

Selective synthesis of boron nitride nanotubes by self-propagation high-temperature synthesis and annealing process

Four types of BN nanotubes are selectively synthesized by annealing porous precursor in flowing NH{sub 3} and NH{sub 3}/H{sub 2} atmosphere at temperature ranging from 1000 to 1200 deg. C in a vertical furnace. The as-synthesized BN nanotubes, including cylinder, wave-like, bamboo-like and bubble-chain, are characterized by XRD, FTIR, Raman, SEM, TEM and HRTEM. Three phenomenological growth models are proposed to interpret growth scenario and structure features of the four types of BN nanotubes. Selectivity of nanotubes formation is estimated as approximately 80-95%. The precursor containing B, Mg, Fe and O prepared by self-propagation high-temperature synthesis (SHS) method plays a key role in selective synthesis of the as-synthesized BN nanotubes. Chemical reactions are also discussed. - Graphical Abstract: Four types of BN nanotubes are selectively synthesized by annealing porous precursor prepared by self-propagation high-temperature synthesis. Three phenomenological growth models are proposed to reveal growth scenario and characteristics of the as-synthesized BN nanotubes. Highlights: > Four types of BN nanotubes are selectively synthesized by annealing porous precursor. > Selectivity of BN nanotubes formation is estimated as approximately 80-95 wt%. > Three growth models are proposed to interpret growth of the as-synthesized BN nanotubes. > The precursor prepared by SHS method plays a key role in selective synthesis process.

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

Preparation, characterization, and infrared emissivity property of optically active polyurethane/TiO{sub 2}/SiO{sub 2} multilayered microspheres

Optically active polyurethane/titania/silica (LPU/TiO{sub 2}/SiO{sub 2}) multilayered core-shell composite microspheres were prepared by the combination of titania deposition on the surface of silica spheres and subsequent polymer grafting. LPU/TiO{sub 2}/SiO{sub 2} was characterized by FT-IR, UV-vis spectroscopy, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), SEM and TEM, and the infrared emissivity value (8-14 {mu}m) was investigated in addition. The results indicated that titania and polyurethane had been successfully coated onto the surfaces of silica microspheres. LPU/TiO{sub 2}/SiO{sub 2} exhibited clearly multilayered core-shell construction. The infrared emissivity values reduced along with the increase of covering layers thus proved that the interfacial interactions had direct influence on the infrared emissivity. Besides, LPU/TiO{sub 2}/SiO{sub 2} multilayered microspheres based on the optically active polyurethane took advantages of the orderly secondary structure and strengthened interfacial synergistic actions. Consequently, it possessed the lowest infrared emissivity value. - Graphical Abstract: Optically active polyurethane/titania/silica (LPU/TiO{sub 2}/SiO{sub 2}) multilayered core-shell composite microspheres were prepared by the combination of titania deposition on the surface of silica spheres and subsequent polymer grafting. Highlights: > Optically active polyurethane based on tyrosine was used for the modification of nanoparticles. > LPU/TiO{sub 2}/SiO{sub 2} multilayered core-shell microspheres were prepared and characterized. > Interfacial interactions and secondary structure affected the infrared emissivity of composite.

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

Preparation and characterization of ordered porous carbons for increasing hydrogen storage behaviors

We prepared ordered porous carbons (PCs) by using a replication method that had well-organized mesoporous silica as a template with various carbonization temperatures in order to investigate the possibility of energy storage materials. The microstructure and morphologies of the samples are characterized by XRD, TEM, and FT-Raman spectroscopy. N{sub 2} adsorption isotherms are analyzed by the t-plot method, as well as the BET and the H-K method in order to characterize the specific surface area, pore volume, and pore size distribution of the samples, respectively. The capacity of the hydrogen adsorption of the samples is evaluated by BEL-HP at 77 K and 1 bar. From the results, we are able to confirm that the synthesis of the samples can be accurately governed by the carbonization temperature, which is one of the effective parameters for developing the textural properties of the carbon materials, which affects the behaviors of the hydrogen storage. - Graphical abstract: It is described that the considerable long-range ordering and the presence of mono-dimensional aligned channels between the two aligned nanorods of the porous framework from the SBA-15 was retained in the T-950 sample during the carbonization process. Highlights: > Ordered porous carbons (PCs) are synthesized with various carbonization temperatures by using a replication method. > Carbonization temperature plays an important role in shrinking the micropores during the carbonization process of PCs. > The textural and structural properties of the PCs are good parameters for enhancing the hydrogen storage capacity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

Thermochemical and kinetic aspects of the sulfurization of Cu-Sb and Cu-Bi thin films

CuSbS{sub 2} and Cu{sub 3}BiS{sub 3} are being investigated as part of a search for new absorber materials for photovoltaic devices. Thin films of these chalcogenides were produced by conversion of stacked and co-electroplated metal precursor layers in the presence of elemental sulfur vapour. Ex-situ XRD and SEM/EDS analyses of the processed samples were employed to study the reaction sequence with the aim of achieving compact layer morphologies. A new 'Time-Temperature-Reaction' (TTR) diagram and modified Pilling-Bedworth coefficients have been introduced for the description and interpretation of the reaction kinetics. For equal processing times, the minimum temperature required for CuSbS{sub 2} to appear is substantially lower than for Cu{sub 3}BiS{sub 3}, suggesting that interdiffusion across the interfaces between the binary sulfides is a key step in the formation of the ternary compounds. The effects of the heating rate and sulfur partial pressure on the phase evolution as well as the potential losses of Sb and Bi during the processes have been investigated experimentally and the results related to the equilibrium pressure diagrams obtained via thermochemical computation. - Graphical Abstract: Example of 3D plot showing the equilibrium pressure surfaces of species potentially escaping from chalcogenide films as a function of temperature and sulfur partial pressure. Bi{sub (g)}, Bi{sub 2(g)}, and BiS{sub (g)} are the gaseous species in equilibrium with solid Bi{sub 2}S{sub 3(s)} considered in this specific example. The pressure threshold plane corresponds to the pressure limit above which the elemental losses from 1 {mu}m thick films exceeds 10% of the original content per cm{sup 2} area of film and dm{sup 3} capacity of sulfurization furnace under static atmosphere conditions. The sulfurization temperature/sulfur partial pressure boundaries required to minimise the elemental losses below a given value can be easily read from the 2D projection of the intersection curves into the T-p{sub S2} plane. Highlights: Black-Right-Pointing-Triangle Sulfurization of Sb-Cu and Bi-Cu metal precursors for thin film PV applications. Black-Right-Pointing-Triangle Kinetics shows the rate determining step to be the interdiffusion of binary sulfides. Black-Right-Pointing-Triangle Phase evolution is consistent with Pilling-Bedworth coefficients of Cu, Sb and Bi. Black-Right-Pointing-Triangle Elemental losses can be minimised via the use of equilibrium pressure diagrams.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2010

Structure and Properties of Magnetic (Co, Fe, Fe{sub 3}C and Ni) Carbon Beads

Nanoparticles exhibit unique physical properties due to the surface or quantum-size effects. Particular attention has been focused on magnetic nanoparticles and substantial progress has been done in this field. In this work magnetic composites, consisting of elementary metals or carbides nanocrystallites, stabilized in carbon matrix, were prepared by the procedure comprising formation of appropriate metal acrylamide complexes, followed by frontal polymerization and pyrolysis of the polymer at various temperatures. Application of frontal polymerization and further pyrolysis enables formation of composite beads consisting of Co, Fe, Fe{sub 3}C or Ni nanocrystallites stabilized in carbon matrix. It was found that the lowest pyrolysis temperature, which enables the production of metallic nanocrystallites, was 673 K for Co and Ni, and 773 K for Fe. The magnetic properties of the beads, percentage of the metallic component, their composition and shape depended on the pyrolysis temperature. Extracts on the basis of composites containing Fe{sub 3}C showed no cytotoxicity, whereas those containing Co and Ni exhibited negligible cytotoxicity up to concentrations of 6.25 mg/ml.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Fabrication and characterization of extended arrays of Ag{sub 2}S/Ag nanodot resistive switches

Well-ordered Ag{sub 2}S/Ag nanodot arrays with a density of >60 Gbit/in.{sup 2} have been fabricated by sputtering Ag on a silicon substrate using ultrathin porous anodic aluminum oxide membranes as shadow masks, followed by sulfurization treatment at room temperature. The morphology, microstructure, and electrical properties of the as-prepared nanodots were characterized by scanning electron microscopy, x-ray diffractometry, transmission electron microscopy, and conductive atomic force microscopy, respectively. Well-defined resistive switching behavior was observed in these nanodots, and the ON/OFF ratio was found to be higher than 10{sup 2}. The Ag{sub 2}S/Ag nanodot arrays hold substantial promise for use as ultrahigh density nonvolatile memory devices.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Structure and resistivity of bismuth nanobelts in situ synthesized on silicon wafer through an ethanol-thermal method

Bismuth nanobelts in situ grown on a silicon wafer were synthesized through an ethanol-thermal method without any capping agent. The structure of the bismuth belt-silicon composite nanostructure was characterized by scanning electron microscope, energy-dispersive X-ray spectroscopy, and high resolution transmission electron microscope. The nanobelt is a multilayered structure 100-800 nm in width and over 50 {mu}m in length. One layer has a thickness of about 50 nm. A unique sword-like nanostructure is observed as the initial structure of the nanobelts. From these observations, a possible growth mechanism of the nanobelt is proposed. Current-voltage property measurements indicate that the resistivity of the nanobelts is slightly larger than that of the bulk bismuth material. - Graphical Abstract: TEM images, EDS, and electron diffraction pattern of bismuth nanobelts. Highlights: Black-Right-Pointing-Pointer Bismuth nanobelts in situ grown on silicon wafer were achieved. Black-Right-Pointing-Pointer Special bismuth-silicon nanostructure. Black-Right-Pointing-Pointer Potential application in sensitive magnetic sensor and other electronic devices.

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

Fully reversible hydrogen absorption and desorption reactions with Sc(Al{sub 1-x}Mg{sub x}), x=0.0, 0.15, 0.20

The hydrogen storage properties of Sc(Al{sub 1-x}Mg{sub x}), x=0.0, 0.15, 0.20, have been studied by X-ray powder diffraction, thermal desorption spectroscopy, pressure-composition-isotherms and scanning electron microscopy techniques. Hydrogen is absorbed from the gas phase at 70 kPa and 400 {sup o}C under the formation of ScH{sub 2} and aluminium with magnesium in solid solution. The reaction is fully reversible in vacuum at 500 {sup o}C and shows the hydrogenation-disproportionation-desorption-recombination (HDDR) behaviour. The activation energy of desorption was determined by the Kissinger method to 185 kJ/mol. The material is stable up to at least six absorption-desorption cycles and there is no change in particle size during cycling. -- Graphical abstract: XRD pattern of Sc(Al{sub 1-x}Mg{sub x}). From the top: x=0, 0.15, 0.20. The hydrogen absorption properties were studied by thermal desorption spectroscopy, pressure-composition-isotherms and scanning electron microscopy techniques. Display Omitted

36 MATERIALS SCIENCE↗
DOE OSTI2010

Physical Property of Magnesium Doped Barium Hexaferrite Particles By Citrate Precursor Route In Presence Of Surfactants

M-type Barium Magnesium hexaferrite with the composition BaMg{sub 2}Fe{sub 10}O{sub 19} was successfully prepared with and without surfactant by using a citrate precursor route. The obtained precursors were calcined at various temperatures. The crystalline structure, phase analysis and particle size were investigated by using X-ray diffraction (XRD), Fourier Transform infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM) techniques. It is observed that the surfactant addition controls the microstructure of the formed Barium Magnesium hexaferrite particles and the type of surfactant plays a crucial role in deciding the morphology of particles.

36 MATERIALS SCIENCE↗
DOE OSTI2016

High-resolution three-dimensional structural microscopy by single-angle Bragg ptychography

Coherent X-ray microscopy by phase retrieval of Bragg diffraction intensities enables lattice distortions within a crystal to be imaged at nanometre-scale spatial resolutions in three dimensions. While this capability can be used to resolve structure–property relationships at the nanoscale under working conditions, strict data measurement requirements can limit the application of current approaches. Here, in this work, we introduce an efficient method of imaging three-dimensional (3D) nanoscale lattice behaviour and strain fields in crystalline materials with a methodology that we call 3D Bragg projection ptychography (3DBPP). This method enables 3D image reconstruction of a crystal volume from a series of two-dimensional X-ray Bragg coherent intensity diffraction patterns measured at a single incident beam angle. Structural information about the sample is encoded along two reciprocal-space directions normal to the Bragg diffracted exit beam, and along the third dimension in real space by the scanning beam. Finally, we present our approach with an analytical derivation, a numerical demonstration, and an experimental reconstruction of lattice distortions in a component of a nanoelectronic prototype device.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Combined elemental and microstructural analysis of genuine and fake copper-alloy coins

Innovative noninvasive material analysis techniques are applied to determine archaeometallurgical characteristics of copper-alloy coins from Florence's National Museum of Archaeology. Three supposedly authentic Roman coins and three hypothetically fraudolent imitations are thoroughly investigated using laser-induced plasma spectroscopy and time of flight neutron diffraction along with 3D videomicroscopy and electron microscopy. Material analyses are aimed at collecting data allowing for objective discrimination between genuine Roman productions and late fakes. The results show the mentioned techniques provide quantitative compositional and textural data, which are strictly related to the manufacturing processes and aging of copper alloys. (laser applications)

36 MATERIALS SCIENCE↗
DOE OSTI2020

Multigrid Optimization for Large-Scale Ptychographic Phase Retrieval

Ptychography is a popular imaging technique that combines diffractive imaging with scanning microscopy. The technique consists of a coherent beam that is scanned across an object in a series of overlapping positions, leading to reliable and improved reconstructions. Ptychographic microscopes allow for large fields to be imaged at high resolution at the cost of additional computational expense. Herein, we propose a multigrid-based optimization framework to reduce the computational burdens of large-scale ptychographic phase retrieval. Our proposed method exploits the inherent hierarchical structures in ptychography through tailored restriction and prolongation operators for the object and data domains. Our numerical results show that our proposed scheme accelerates the convergence of its underlying solver and outperforms the ptychographical iterative engine, a workhorse in the optics community.

97 MATHEMATICS AND COMPUTING↗
DOE OSTI2011

Investigation on Growth and Surface Analysis of DAST Single Crystals

We have explored the growth of bulk size N, N-dimethylamino-N'-methylstilbazolium p-toluenesulphonate (DAST) using slope nucleation method. The grown crystal was characterized by single crystal X-ray diffraction (XRD), and CHN analyses. The surface morphology of the crystal was analyzed using Scanning electron microscopy (SEM).

36 MATERIALS SCIENCE↗
DOE OSTI2014

In situ X-ray ptychography imaging of high-temperature CO{sub 2} acceptor particle agglomerates

Imaging nanoparticles under relevant reaction conditions of high temperature and gas pressure is difficult because conventional imaging techniques, like transmission electron microscopy, cannot be used. Here we demonstrate that the coherent diffractive imaging technique of X-ray ptychography can be used for in situ phase contrast imaging in structure studies at atmospheric pressure and elevated temperatures. Lithium zirconate, a candidate CO{sub 2} capture material, was studied at a pressure of one atmosphere in air and in CO{sub 2}, at temperatures exceeding 600 °C. Images with a spatial resolution better than 200 nm were retrieved, and possibilities for improving the experiment are described.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2011

Influence of slag chemistry on the hydration of alkali-activated blast-furnace slag - Part I: Effect of MgO

The hydration and the microstructure of three alkali activated slags (AAS) with MgO contents between 8 and 13 wt.% are investigated. The slags were hydrated in the presence of two different alkaline activators, NaOH and Na{sub 2}SiO{sub 3}.5H{sub 2}O (WG). Higher MgO content of the slag resulted in a faster reaction and higher compressive strengths during the first days. The formation of C(- A)-S-H and of a hydrotalcite-like phase was observed in all samples by X-ray diffraction (XRD), thermal analysis (TGA) and scanning electron microscopy (SEM) techniques. Increasing the MgO content of the slag from 8 to 13% increased the amount of hydrotalcite and lowered the Al uptake by C-S-H resulting in 9% higher volume of the hydrates and a 50 to 80% increase of the compressive strength after 28 days and longer for WG activated slag pastes. For NaOH activated slags only a slight increase of the compressive strength was measured.

36 MATERIALS SCIENCE↗
DOE OSTI2010

Semianalytic model of electron pulse propagation: Magnetic lenses and rf pulse compression cavities

The analytical Gaussian electron pulse propagation model of Michalik and Sipe [J. Appl. Phys. 99, 054908 (2006)] is extended to include the action of external forces on the pulse. The resultant ability to simulate efficiently the effect of electron optical elements (e.g., magnetic lenses and radio-frequency cavities) allows for the rapid assessment of electron pulse delivery systems in time-resolved ultrafast electron diffraction and microscopy experiments.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗