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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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All sourcesNASA NTRSDOE OSTI
NASA NTRS2018

Investigation of Alpha Silicon Carbide / Carbon Fiber Proposed (2H & 6H-SiC) / C

A commercially available alpha silicon carbide coated carbon 12k fiber tow was subjected to rigorous inspection and testing. The pyrolized polyacrylonitrile (PAN) fiber had gone through a conversion process that resulted in a thin layer of SiC forming on the exterior of the fiber. The fibers? surface was characterized by x-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES) and scanning electron microscopy (SEM). Powdered x-ray diffraction (XRD) examined the bulk material properties. Transmission electron microscopy (TEM) coupled with energy-dispersive X-ray spectroscopy (EDS) examined the crystallinity of the SiC. A number of pristine samples were used to determine elongation rate and tensile strength.

Trunek, Andrew↗
NASA NTRSDate not supplied

The Zircon-Reidite Shock Transformation: A Tem Study of Reidite Produced at A Newly Established 21.2 GPa Shock Pressure Threshold

The high-pressure polymorph of zircon (Zr2SiO4) is reidite, a phase with the scheelite structure that was first discovered to form at ca. 12 GPa in static high-pressure experiments [1]. Reidite was subsequently found to occur in naturally shocked zircons from several terrestrial impact localities [2,3], as well as in shock recovery-reverberation experiments performed above 20 GPa [4]. The nature and distribution of reidite occurrences in terrestrial impact localities has pointed to its potential use as a shock pressure indicator, as well as to the importance of understanding its age-reset effects in zircon geochronology [3]. In this study we have used coordinated SEM/Electron Backscatter Diffraction (EBSD) and Field-Emission Scanning Transmission Electron Microscopy (FE-STEM) to study the micro- and nanostructure of reidite and its shocked zircon host produced at 21.2 GPa under experimental shock recovery/reverberation conditions [5]. Our results document the TEM microstructure of reidite formed at a 21.2 GPa experimental shock pressure that is significantly lower than that observed in previous studies [4]. At these conditions the sample developed a diverse set of microstructures that have not been previously documented on the TEM scale.

shock metamorphism↗
DOE OSTI2018

Corrosion Evaluation of CoCrFeMnNi High-Entropy Alloys (HEAs) for Corrosion Protection of Natural Gas Transmission Pipelines

High-entropy alloys (HEAs), are multicomponent alloys composed of at least five elements with compositions of 5-35 atomic % for each element. These alloys are being investigated for corrosion protection of natural gas transmission pipelines by studying their behavior under aqueous acidic conditions. Electrochemical and immersion experiments were carried out in 3.5 weight % NaCl solution at pH 4 and 40°C. Oxygen was purged out from the solution by using CO2 as stripping gas. The electrochemical experiments included potentiodynamic and electrochemical impedance spectroscopy tests, used to calculate corrosion rates. Potentiodynamic polarization curves, including cyclic voltammograms, were used to explain active, active-passive, and passive regions of these alloys and susceptibility to localized corrosion. Surface characterization of the corroded samples were performed using scanning electron microscopy (SEM) and x-ray diffraction (XRD). The results of the immersion and electrochemical testing indicate that some of the HEAs have better corrosion performance than commercial alloys UNS N10276, UNS K03014, and UNS 31600.

03 NATURAL GAS↗
DOE OSTI2019

EBSD characterization of metallic nuclear fuel

Grain structure and texture are important in all materials as they influence most mechanical properties. In particular for nuclear materials texture can influence material properties important for reactor performance, such as swelling, yield stress, fracture toughness etc. Moreover such data are of primary importance to develop and validate physics-based models for nuclear fuels based on microstructure evolution during irradiation (e.g. MARMOT). Scanning Electron Microscopy (SEM) coupled with Electron Back Scatter Diffraction (EBSD) has been proven as an effective technique for evaluating grain size, shape, and orientation. However it has been seldom used for nuclear fuels. This has been mostly related to difficulties in handling and preparing such materials for EBSD analyses. Particularly challenging remains sample preparation for metallic irradiated fuels, as they are prone to rapid oxidation. Indeed EBSD analyses require the elimination of any surface defect or oxide layer as the signal arise from 50-100 nm depth in the material. At Idaho National Laboratory (INL) great effort has focused in developing techniques to obtain suitable surfaces for EBSD analyses. In this paper the first results from EBSD analyses obtained from a wide range of nuclear materials will be presented. Sample analyzed included fresh U, U-Zr, Pu-Zr , and U-Mo, including some irradiated fuel.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

Experimental Investigation of Polymer Induced Fouling of Heater Tubes in the First-Ever Polymer Flood Pilot on Alaska North Slope

Mineral fouling in heat exchangers has been extensively investigated by researchers in recent times. The oil and gas industry has a long history of fouling issues in production systems as a result of produced fluids treatment. Due to decline in production rates in oilfields new technologies are being developed and field tested in pilots. Polymer flooding is one such technology that involves addition of polymers to injection fluids to enhance oil production. A polymer flood pilot has been set up in the Schrader Bluff viscous oil reservoir at Milne Point field on the Alaska North Slope (ANS). The results from the pilot are encouraging, however a major concern of the operator is the influence of polymer on the production system after breakthrough, especially the fouling in heat exchangers. This study investigates the propensity of polymer fouling on the heater tubes as a function of different variables, with the ultimate goal of determining safe and efficient operating conditions. This work applies a multi-experimental approach to study the severity of polymer-induced fouling in both dynamic and static states of produced fluids as well as studying the stability of polymer solutions at different temperatures. A unique experimental setup was designed and developed in-house to simulate the fouling process on the heating tube. The influence of heating tube skin temperature, tube material, and polymer concentration on fouling tendency was investigated. Each test was run five times with the same tube, and in each run, the freshly prepared synthetic brine and polymer solution was heated from 77°F to 122°F to mimic field-operating conditions. The heating time and fouling amount were recorded for each run. Dynamic Scale Loop (DSL) tests were conducted to study fouling due to polymer at different temperatures (165°F to 350°F) in a dynamic state of fluid flow where the fluids mimic the residence time of fluids in the heat exchanger on the field pilot. Cloud point measurement has also been conducted to find the critical temperature at which the polymer in solution becomes unstable and precipitates out. The morphology and composition of the deposit samples were analyzed by environmental scanning electron microscopy (ESEM) and X-ray diffraction (XRD), respectively. It was found that the presence of polymer in produced fluids would aggravate the fouling issues on both carbon steel and stainless-steel surfaces at all tested skin temperatures. Only higher skin temperatures of 250°F and 350°F could cause polymer-induced fouling issues on the copper tube surface, and the fouling tendency increased with polymer concentration. At the lower skin temperatures of 165°F, no polymer-induced fouling was identified on the copper tube. A critical temperature that is related to the cloud point of the polymer solution was believed to exist, below which polymer-induced fouling would not occur, and only mineral scale was deposited but above which the polymer would aggravate the fouling issue. The cloud point of the tested polymer solution was determined to be between 220°F and 230°F. In the DSL tests it was found that at higher skin temperatures of 250°F and 350°F tube blocking was observed in the DSL tests whereas the tests at 165°F and 200°F did not show any tube blocking in the same time period. These experiments also manifested the influence of cloud point of the solution as deposit rate increased significantly in both carbon steel and stainless-steel tubes when the skin temperature was higher than the solution cloud point. The results of this study have provided guidance to the operator for the field-operations.

Dhaliwal, Anshul↗
DOE OSTI2018

Elevated temperature transmission Kikuchi diffraction in the SEM

Highlights: • The potential of high temperature in-situ TKD characterization is demonstrated. • High quality Kikuchi patterns can be obtained at high temperature. • The very local heat of the MEMS-based heating system minimises infrared radiation. • TKD is a suitable technique for in-situ studies of solid state dewetting. - Abstract: Transmission Kikuchi diffraction (TKD) facilitates automated orientation mapping of thin films in scanning electron microscopes (SEM). In this study TKD is applied for the first time to perform in-situ annealing experiments on gold thin films deposited on a MEMS-based heating system. The very local heating associated with this system enables reliable TKD measurements at elevated temperatures without notable disturbance from infrared radiation. The dewetting of an Au thin film into Au nanoparticles upon heating is followed with orientation mapping in a temperature range between 20 °C and 900 °C. The local thickness variation associated with the dewetting is observed qualitatively by observing the intensity of the transmitted beam, which decreases as the film thickness increases locally. The results of this study reveal that TKD is a well suited technique to study thin-film stability and solid state dewetting. Moreover, the outcome of this methodological study provides a baseline for further in-situ crystallographic studies of electron transparent samples in the SEM.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2017

Aberration corrected STEM by means of diffraction gratings

In the past 15 years, the advent of aberration correction technology in electron microscopy has enabled materials analysis on the atomic scale. This is made possible by precise arrangements of multipole electrodes and magnetic solenoids to compensate the aberrations inherent to any focusing element of an electron microscope. In this paper, we describe an alternative method to correct for the spherical aberration of the objective lens in scanning transmission electron microscopy (STEM) using a passive, nanofabricated diffractive optical element. This holographic device is installed in the probe forming aperture of a conventional electron microscope and can be designed to remove arbitrarily complex aberrations from the electron's wave front. In this work, we show a proof-of-principle experiment that demonstrates successful correction of the spherical aberration in STEM by means of such a grating corrector (GCOR). Our GCOR enables us to record aberration-corrected high-resolution high-angle annular dark field (HAADF-) STEM images, although yet without advancement in probe current and resolution. Finally, improvements in this technology could provide an economical solution for aberration-corrected high-resolution STEM in certain use scenarios.

47 OTHER INSTRUMENTATION↗
DOE OSTI2015

Electrical properties of radio-frequency sputtered HfO{sub 2} thin films for advanced CMOS technology

The Hafnium oxide (HfO{sub 2}) high-k thin films have been deposited by radio frequency (rf) sputtering technique on p-type Si (100) substrate. The thickness, composition and phases of films in relation to annealing temperatures have been investigated by using cross sectional FE-SEM (Field Emission Scanning Electron Microscope) and grazing incidence x-ray diffraction (GI-XRD), respectively. GI-XRD analysis revealed that at annealing temperatures of 350°C, films phases change to crystalline from amorphous. The capacitance-voltage (C-V) and current-voltage (I-V) characteristics of the annealed HfO{sub 2} film have been studied employing Al/HfO{sub 2}/p-Si metal–oxide–semiconductor (MOS) structures. The electrical properties such as dielectric constant, interface trap density and leakage current density have been also extracted from C-V and I-V Measurements. The value of dielectric constant, interface trap density and leakage current density of annealed HfO{sub 2} film is obtained as 23,7.57×1011eV{sup −1} cm{sup −2} and 2.7×10{sup −5} Acm{sup −2}, respectively. In this work we also reported the influence of post deposition annealing onto the trapping properties of hafnium oxide and optimized conditions under which no charge trapping is observed into the dielectric stack.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Synthesis of polyaniline/SnO{sub 2} nanocomposite and its improved electrochemical performance

Highlights: • Supercapacitors based on PANI/SnO{sub 2} nanocomposite were reported. • Supercapacitors using this material gave a specific capacitance of 501 F g{sup −1}. • Capacitance retention was 85.8% over 2000 charge–discharge cycles. - Abstract: SnO{sub 2} was prepared by the hydrothermal route. Aniline monomer was polymerized in the suspension of SnO{sub 2} to form inorganic–organic nanocomposite materials, in which SnO{sub 2} particles were embedded within polyaniline (PANI). Morphological and structural characterizations of the prepared samples were carried out using scanning electron microscope; transmission electron microscope; power X-ray diffraction and Fourier transform infrared spectroscopy. Their electrochemical properties were also investigated using cyclic voltammetry, galvanostatic charge–discharge and electrochemical impedance spectroscopy. The as-prepared nanocomposites had excellent properties in the capacitance, and its specific capacitance was up to 501 F g{sup −1} with a specific energy density of 66.8 W h kg{sup −1} at a power density of 960.6 W kg{sup −1}. The device fulfilled the requirement of long durability necessary for an energy storage system, since after 2000 galvanostatic charge–discharge cycles, retention of 85.8% in capacitance was observed. These results indicated that the PANI/SnO{sub 2} had a synergistic effect of the complementary properties of both components.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Enhanced Magneto-optical and Antibacterial Studies of Bi{sub 1−x}Mg{sub x}FeO{sub 3} (0.0 ≤ x ≤ 0.15)) Nanoparticles

Mg-doped BiFeO{sub 3} (Bi{sub 1−x}Mg{sub x}FeO{sub 3} (0.00 ≤ x ≤ 0.15)) nanoparticles (NPs) have been successfully prepared by simple solution combustion method using urea as fuel. The obtained product was sintered at 550 °C for 2 h to get pure-phase formation. The as-prepared samples were characterized by powder X-ray diffraction (XRD), Fourier transform infrared (FT-IR), field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), transmission electron microscope (TEM), ultraviolet–visible (UV-Vis) absorption, photoluminescence (PL) spectra, and vibrating sample magnetometer (VSM) analysis. Powder XRD study revealed that all products exhibit rhombohedral structure with pure-phase formation. The average crystallite size of the samples decreased from 56.25 to 46.15 nm with increasing the concentration of Mg (x = 0.00, 0.05, 0.10, and 0.15). Surface morphology of the samples were analyzed by FE-SEM and TEM micrograph techniques, and the grain distribution was not quite homogeneous and observed agglomeration of the particles, which is mainly due to the magnetic interaction among them. EDX analysis confirmed the presence of Bi, Fe, O, and Mg elements without any form of impurity peak in all products. PL spectra shows a high intense peak at 464 nm, which is attributed to blue emission. The saturation magnetization is enhanced with increasing Mg doping level at RT. Antibacterial activity of Bi{sub 1−x}Mg{sub x}FeO{sub 3} NPs was found to be enhanced with increase in Mg doping concentration as it causes a reduction in the grain size of the samples.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2015

Fabrication, characterization and photocatalytic properties of Ag/AgI/BiOI heteronanostructures supported on rectorite via a cation-exchange method

Highlights: • Ag/AgI/BiOI-rectorite was prepared by twice cation-exchange process. • Ag/AgI/BiOI-rectorite photocatalyst possessed SPR and adsorption capacity. • Ag/AgI/BiOI-rectorite exhibited highly photocatalytic activity. • Trapped holes and ·O{sub 2}{sup −} were formed active species in the photocatalytic system. - Abstract: In this work, a new plasmonic photocatalyst Ag/AgI/BiOI-rectorite was prepared via a cation exchange process. The photocatalyst had been characterized by X-ray powder diffraction (XRD), Raman spectra, nitrogen sorption (BET), field-emission scanning electron microscope (FE-SEM), X-ray photoelectron spectroscopy (XPS) and UV–vis diffuse reflectance spectroscopy (DRS). The photocatalytic activity, which was evaluated by degradation of rhodamine B (RhB) and bisphenol A (BPA) under visible light irradiation, was enhanced significantly by loading Ag/AgI/BiOI nanoparticles onto rectorite. The photogenerated holes and superoxide radical (·O{sub 2}{sup −}) were both formed as active species for the photocatalytic reactions under visible light irradiation. The existence of metallic Ag particles, which possess the surface plasmon resonance effect, acted as an indispensable role in the photocatalytic reaction.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2015

Surface-interface exploration of Mg deposited on Si(100) and oxidation effect on interfacial layer

Using scanning tunneling microscopy and spectroscopy, Auger electron spectroscopy, and low energy electron diffraction, we have studied the growth of Mg deposited on Si(100)-(2 × 1). Coverage from 0.05 monolayer (ML) to 3 ML was investigated at room temperature. The growth mode of the magnesium is a two steps process. At very low coverage, there is formation of an amorphous ultrathin silicide layer with a band gap of 0.74 eV, followed by a layer-by-layer growth of Mg on top of this silicide layer. Topographic images reveal that each metallic Mg layer is formed by 2D islands coalescence process on top of the silicide interfacial layer. During oxidation of the Mg monolayer, the interfacial silicide layer acts as diffusion barrier for the oxygen atoms with a decomposition of the silicide film to a magnesium oxide as function of O{sub 2} exposure.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Nanocomposites based on thermoplastic elastomers with functional basis of nano titanium dioxide

Nanocomposites based on a thermoplastic elastomer (TPE) (low-density polyethylene (LDPE) and 1,2-polybutadiene in a ratio of 60/40) with functional titanium dioxide nanoparticles of different nature, TiO{sub 2}/TPE, have been prepared and investigated by a complex of methods (X-ray diffraction analysis using X-ray and synchrotron radiation beams, scanning electron microscopy, transmission electron microscopy, and X-ray energy-dispersive spectroscopy). The morphology of the composites is found to be somewhat different, depending on the TiO{sub 2} characteristics. It is revealed that nanocomposites with cellular or porous structures containing nano-TiO{sub 2} aggregates with a large specific surface and large sizes of crystallites and nanoparticles exhibit the best deformation‒strength and fatigue properties and stability to the effect of active media under conditions of ozone and vapor‒air aging.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Influence of Iron Content on Microstructure and Magnetic Properties of Sr{sub 0.3}La{sub 0.4}Ca{sub 0.3}n(Fe{sub 2}O{sub 3})Co{sub 0.4}

In this work, the hexagonal ferrite Sr{sub 0.3}La{sub 0.4}Ca{sub 0.3}n (Fe{sub 2}O{sub 3})Co{sub 0.4}, where n ranging from 5.5 to 6.0 with a step of 0.1, and magnetic powders and magnets were synthesized by solid-states reaction. The microstructure of the magnetic powders was investigated by X-ray diffraction (XRD). And then we can found that a single magnetoplumbite phase is obtained for magnetic powders as a result when 5.6 ≤ n ≤ 5.8. When the iron content in the magnetic powders increased continuously, the diffraction peaks of α-Fe{sub 2}O{sub 3} were observed. Scanning electron microcopy (SEM) was used to explore the micrographs of the magnets and the hexagonal-shaped crystals were found obviously. The magnetic properties of the M-type hexagonal ferrites Sr{sub 0.3}La{sub 0.4}Ca{sub 0.3}n(Fe{sub 2}O{sub 3})Co{sub 0.4} were studied by using vibrating sample magnetometry. The saturation magnetization (M{sub s}) first increased and then began to decrease with the n increasing. While the coercivity first decreased with the n from 5.5 to 5.9 and then increased when n ≥5.9. The coercivity (H{sub c}) of the hexagonal ferrite Sr{sub 0.3}La{sub 0.4}Ca{sub 0.3}n(Fe{sub 2}O{sub 3})Co{sub 0.4} reaches the maximum value (H{sub c} = 1130 Oe) when the iron content (n = 5.5).

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Damage morphology study of high cycle fatigued as-cast Mg–3.0Nd–0.2Zn–Zr (wt.%) alloy

Laser scanning confocal microscopy (LSCM) and Electron back-scattered diffraction (EBSD) were applied to the study of surface morphology variation of as-cast Mg–3.0Nd–0.2Zn–Zr (NZ30K) (wt.%) alloy under tension-compression fatigue test at room temperature. Two kinds of typical damage morphologies were observed in fatigued NZ30K alloy: One was parallel lines on basal planes led by the cumulation of basal slips, called persistent slip markings (PSMs), and the other was lens shaped, thicker and in less density, led by the formation of twinning. The surface fatigue damage morphology evolution was analyzed in a statistical way. The influences of stress amplitude and grain orientation on fatigue deformation mechanisms were discussed and the non-uniform deformation among grains and the PSMs, within twinning were described quantitatively. - Highlights: • Fatigue morphology evolution was studied by Laser Scanning Confocal Microscopy. • 3D morphology of persistent slip markings and twins was characterized. • Non-uniform deformation among grains, the PSMs and twins were quantified. • Initiations of fatigue crack were clearly investigated.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Temperature-dependent transformation from whisker- to nanoparticle-strengthened composite interface in the Al{sub 2}O{sub 3}/Ag-based alloy system and mechanical properties of the joints

Al{sub 4}B{sub 2}O{sub 9}-whisker-coated Al{sub 2}O{sub 3} ceramics were bonded by AgCu–4.5 wt.%Ti alloy in vacuum. The microstructure of the whisker-coated Al{sub 2}O{sub 3} joints was investigated by scanning electron microscopy, transmission electron microscopy and X-ray diffraction. A continuous (Cu,Al){sub 3}Ti{sub 3}O layer formed against the alloy at lower bonding temperatures, and a complex transition zone bordering the whiskers was observed, which consisted of Ag nanoparticles, titanium oxides, TiB{sub 2}, (Cu,Al){sub 3}Ti{sub 3}O nanoparticles and possible Ag{sub 3}Al. As the bonding temperature increased, the Al{sub 2}O{sub 3}/AgCuTi interface was found to transform from whisker- to nanoparticle-strengthened composite region. Bend test results revealed that both the whiskers grown on Al{sub 2}O{sub 3} and the dispersive nanoscale products in the alloy played positive roles in improving the joint properties. The maximum bend strength of the whisker-coated Al{sub 2}O{sub 3} joints was 313 MPa at the bonding temperature of 820 °C. - Highlights: • Al{sub 4}B{sub 2}O{sub 9}-whisker-coated Al{sub 2}O{sub 3} ceramics were bonded by AgCu–4.5 wt.%Ti alloy in vacuum. • Microstructures of whisker-coated Al{sub 2}O{sub 3} joints were investigated in detail. • Both whiskers and the dispersive nanoscale products can improve the joint properties. • The maximum bend strength of the whisker-coated Al{sub 2}O{sub 3} joints was 313 MPa.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Synthesis, Structure, and Spectroscopy of Epitaxial EuFeO 3 Thin Films

Rare earth iron perovskites RFeO3, where R is a rare earth cation, exhibit an array of magnetic, catalytic, optical, and electrochemical properties. Here we study EuFeO3 films synthesized by molecular beam epitaxy to improve our understanding of the optical properties of ferrites. A combination of X-ray diffraction, X-ray reflectivity, Rutherford backscattering spectroscopy, and scanning transmission electron microscopy was used to characterize the film structure and cation composition. X-ray absorption spectroscopy confirms the nominal 3+ valence states of Eu and Fe. The optical properties of EuFeO3 were investigated using variable-angle spectroscopic ellipsometry between the photon energies of 1.25 and 5 eV. We find that EuFeO3 is a semiconductor with an onset of optical absorption near 2.5 eV. The absorption spectrum of EuFeO3 is blue-shifted with respect to LaFeO3 films, a result that is attributed to the structural differences between the two materials.

Choquette, Amber K.↗
DOE OSTI2016

Impedance spectroscopy studies in cobalt ferrite-reduced graphene oxide nanocomposite

(1-x)Cobalt ferrite-(x)reduced graphene oxidenanocomposites with x=0, 0.1, 0.2 and 0.3 were prepared by the ultrasonic method. The crystal symmetry modification due to reduced graphene oxide and cobalt ferrite interaction has been studied by employing the X-ray diffraction technique. Morphology of the samples was studied by the Field emission scanning electron microscopy (FE-SEM). Study on electrical properties of the cobalt ferrite-reduced graphene oxide nanocomposites explores the possible application of these composites as anode material. Impedance decreases with an increase in frequency as well as temperature, which supports an increase in ac electrical conductivity. The modified Debye relaxation model can explain the behavior of impedance in cobalt ferrite-reduced graphene oxide nanocomposites.

77 NANOSCIENCE AND NANOTECHNOLOGY↗