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At least 1,513 records · Page 84
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

Contribution of Catalytic Transesterification Reactions to the Compatibilization of Poly(lactic acid)/Polycarbonate Blends: Thermal, Morphological and Viscoelastic Characterization

Samarium acetylacetonate (Sm-Acac) was added to catalyze interchange reactions between poly(lactic acid) (PLA) and polycarbonate (PC) in order to promote compatibilization and enhance the performances of the PLA/PC blend. The effects of the composition and catalyzed transesterification reactions were investigated using differential scanning calorimetry (DSC), thermogravimetry (TG), dynamic mechanical thermal analysis (DMTA) and scanning electron microscopy (SEM). DMTA and DSC analysis revealed the immiscibility of the uncatalyzed PLA/PC blends for the studied compositions because the glass transition temperatures of PC and PLA were unchanged after blending. In the PLA glassy region, PLA/PC blends exhibited lower storage moduli which increased upon heating due to the cold crystallization process. During melt mixing with Sm-Acac catalyst, PLA/PC blends were submitted to two competing processes. In one hand, Sm-Acac acted as a plasticizer and contributed in decreasing significantly the glass transition, crystallization and melting temperatures of PLA phase. In the other hand, Sm-Acac proved its efficiency in catalyzing the transesterification reactions that were evidenced by the decrease of the PLA aptitude to crystallization due to the hindering effect of the PC units inserted into the PLA chains. PLA/PC blends melt mixed with 0.25% of Sm-Acac showed a significant strengthening effect, corresponding to an increase in the storage modulus in the temperature range comprised between 70 and 90 °C. This indicated the formation of a copolymer at the interface and the promotion of adhesion as it is confirmed from the decrease in the height of the PLA Tan δ peak. At 0.5% of Sm-Acac, (90/10) PLA/PC blend revealed a new peak assigned to the glass transition of the PLA-PC copolymer, whereas the (50/50) PLA/PC blend was converted into a new random copolymer. TG analysis proved the presence of a copolymer structure presenting an intermediate thermal stability in both the catalyzed and uncatalyzed blends.

36 MATERIALS SCIENCE↗
NASA NTRS1973

A new technique for Auger analysis of surface species subject to electron-induced desorption

A method is presented to observe surface species subject to electron-induced desorption by Auger electron spectroscopy. The surface to be examined is moved under the electron beam at constant velocity, establishing a time independent condition and eliminating the time response of the electron spectrometer as a limiting factor. The dependence of the Auger signal on the surface velocity, incident electron current, beam diameter, and desorption cross section are analyzed. The method is illustrated by the Auger analysis of PTFE, in which the fluorine is removed by electron induced desorption.

Pepper, S. V.↗
DOE OSTI2016

Sponge-like silver obtained by decomposition of silver nitrate hexamethylenetetramine complex

Silver nitrate hexamethylenetetramine [Ag(NO{sub 3})·N{sub 4}(CH{sub 2}){sub 6}] coordination compound has been prepared via aqueous route and characterized by chemical analysis, XRD and electron microscopy. Decomposition of [Ag(NO{sub 3})·N{sub 4}(CH{sub 2}){sub 6}] under hydrogen and under inert has been studied by thermal analysis and mass spectrometry. Thermal decomposition of [Ag(NO{sub 3})·N{sub 4}(CH{sub 2}){sub 6}] proceeds in the range 200–250 °C as a self-propagating rapid redox process accompanied with the release of multiple gases. The decomposition leads to formation of sponge-like silver having hierarchical open pore system with pore size spanning from 10 µm to 10 nm. The as-obtained silver sponges exhibited favorable activity toward H{sub 2}O{sub 2} electrochemical reduction, making them potentially interesting as non-enzyme hydrogen peroxide sensors. - Graphical abstract: Thermal decomposition of silver nitrate hexamethylenetetramine coordination compound [Ag(NO{sub 3})·N{sub 4}(CH{sub 2}){sub 6}] leads to sponge like silver that possesses open porous structure and demonstrates interesting properties as an electrochemical hydrogen peroxide sensor. Display Omitted - Highlights: • [Ag(NO{sub 3})·N{sub 4}(CH{sub 2}){sub 6}] orthorhombic phase prepared and characterized. • Decomposition of [Ag(NO{sub 3})·N{sub 4}(CH{sub 2}){sub 6}] leads to metallic silver sponge with opened porosity. • Ag sponge showed promising properties as a material for hydrogen peroxide sensors.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Differential evolution: Global search problem in LEED-IV surface structural analysis

The search process associated with the quantitative theory–experiment comparison in Low Energy Electron Diffraction surface structural analysis can be very time consuming, especially in the case of complex materials with many atoms in the unit cell. Global search algorithms need to be employed to locate the global minimum of the reliability factor in the multi-dimensional structural parameter space. In this study we investigate the use of the Differential Evolution algorithm in Low Energy Electron Diffraction structural analysis. Despite the simplicity of its mechanism the Differential Evolution algorithm presents an impressive performance when applied to ultra-thin films of BaTiO{sub 3}(001) in a theory–theory comparison. A scaling relation of N{sup (1.47} {sup ±} {sup 0.08)} was obtained, where N is the total number of parameters to be optimized. - Highlights: • We investigated the use of the Differential Evolution algorithm (DE) for the LEED search problem. • The DE method was applied to the optimization of the surface structure of the BaTiO{sub 3}(001) ultra-thin films. • A very favorable scaling relation of N{sup 1.47} was obtained, where N is the total number of parameters to be optimized.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Crystal growth and anisotropy of high temperature thermoelectric properties of yttrium borosilicide single crystals

We studied thermoelectric properties of YB{sub 41}Si{sub 1.3} single crystals grown by the floating zone method. The composition of the grown crystal was confirmed by electron probe micro-analysis. We have determined the growth direction for the first time for these borosilicides, and discovered relatively large anisotropy in electrical properties. We measured the electrical resistivity and Seebeck coefficient along [510] (the growth direction) and [052] directions and we found that this crystal exhibits strong electrical anisotropy with a maximum of more than 8 times. An interesting layered structural feature is revealed along [510] with dense boron cluster layers and yttrium layers, with conductivity enhanced along this direction. We obtained 3.6 times higher power factor along [510] compared to that along [052]. Although the ZT of the present system is low, anisotropy in the thermoelectric properties of a boride was reported for the first time, and can be a clue in developing other boride systems also. - Graphical abstract: The growth direction ([510]) was determined for the first time in YB{sub 41}Si{sub 1.3} single crystals and revealed an interesting layered feature of boron clusters and metal atoms, along which the electrical conductivity and thermoelectric power factor was strongly enhanced. - Highlights: • We have grown YB{sub 41}Si{sub 1.3} single crystals by the floating zone method. • Growth direction of [510] determined for first time in REB{sub 41}Si{sub 1.2}. • Electrical resistivity was strongly anisotropic with possible enhancement along metal layers. • The obtained power factor along [510] is 3.6 times higher than that along [052].

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

Enhanced visible-light-driven photocatalytic activities of Bi2Fe4O9/g-C3N4 composite photocatalysts

Highlights: • The novel Bi{sub 2}Fe{sub 4}O{sub 9}/g-C{sub 3}N{sub 4} composite photocatalysts have been designed and prepared. • Combination of Bi{sub 2}Fe{sub 4}O{sub 9} and g-C{sub 3}N{sub 4} could enhance the visible-light-driven photocatalytic degradation for RhB. • The effects of Bi{sub 2}Fe{sub 4}O{sub 9}/g-C{sub 3}N{sub 4} weight ratios on photocatalytic performance in the composite have been discussed. • The Z-scheme photocatalytic mechanism was proposed and discussed in detail. - Abstract: A series of Bi{sub 2}Fe{sub 4}O{sub 9}/g-C{sub 3}N{sub 4} composite photocatalysts are prepared via a facile mixing-calcination method. The crystal structures of composites are investigated by X-ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FT-IR). The Field Emission Scanning Electron Microscope (FE-SEM) in combination with Energy Dispersive X-ray Spectroscopy (EDS) mapping analysis and Transmission Electron Microcopy (TEM) images illustrate the uniform distribution of constituent elements and clear interface between Bi{sub 2}Fe{sub 4}O{sub 9} and g-C{sub 3}N{sub 4} component. The visible-light-driven photocatalytic rates of Rhodamine B over Bi{sub 2}Fe{sub 4}O{sub 9}/g-C{sub 3}N{sub 4} composites increase and then decrease with the increase of g-C{sub 3}N{sub 4} content. The effects of Bi{sub 2}Fe{sub 4}O{sub 9}/g-C{sub 3}N{sub 4} weight ratios on photocatalytic performance are thoroughly discussed. Meanwhile, the active species trapping experiments and the electrochemical impedance spectra as well as the electronic energy-band structure estimation analysis demonstrate that the photocatalytic mechanism for Bi{sub 2}Fe{sub 4}O{sub 9}/g-C{sub 3}N{sub 4} composites is ascribed to the Z-scheme. In addition, the recyclability and stability experiments of the composite are also studied.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Effects of electromagnetic wiggler and ion channel guiding on equilibrium orbits and waves propagation in a free electron laser

In this paper, an analysis of equilibrium orbits for electrons by a simultaneous solution of the equation of motion and the dispersion relation for electromagnetic wave wiggler in a free-electron laser (FEL) with ion-channel guiding has been presented. A fluid model has been used to investigate interactions among all possible waves. The dispersion relation has been derived for electrostatic and electromagnetic waves with all relativistic effects included. This dispersion relation has been solved numerically. For group I and II orbits, when the transverse velocity is small, only the FEL instability is found. In group I and II orbits with relatively large transverse velocity, new couplings between other modes are found.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2024

Analysis of neoclassical tearing mode stabilization experiment by electron cyclotron injection in KSTAR

We report the neoclassical tearing mode (NTM) stabilization experimental results by injection of the electron cyclotron (EC) beam in KSTAR, and its analysis with integrated modelling. In the KSTAR experiment, NTM was intentionally induced and the EC beam was injected by the plasma control system (PCS) to stabilize it. Here, the EC angle was controlled based on the minimum seeking algorithm for the island growth rate. Although the EC angle was not changed significantly, the island width significantly decreased towards the end of the experiment followed by the recovery of plasma performance. To assess the NTM stabilization experiment from a stability perspective, we performed integrated modelling with TRIASSIC utilizing the reconstructed equilibrium with magnetic diagnostics and motional stark effect diagnostics. As a result, we observed that the NTM is stabilized by EC.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2023

Determining Stress in Metallic Conducting Layers of Microelectronics Devices Using High Resolution Electron Backscatter Diffraction and Finite Element Analysis

Delayed failure due to stress voiding is a concern with some aging microelectronics, as these voids can grow large enough to cause an open circuit. Local measurements of stress in the metallic layers are crucial to understanding and predicting this failure, but such measurements are complicated by the fact that exposing the aluminum conducting lines will relieve most of their stress. In this study, we instead mechanically thin the device substrate and measure distortions on the thinned surface using high resolution electron backscatter diffraction (HREBSD). These measurements are then related to the stresses in the metallic layers through elastic simulations. This study found that in legacy components that had no obvious voids, the stresses were comparable to the theoretical stresses at the time of manufacture (≈300 MPa). Distortion fields in the substrate were also determined around known voids, which may be directly compared to stress voiding models. In conclusion, the technique presented here for stress determination, HREBSD coupled with finite element analysis to infer subsurface stresses, is a valuable tool for assessing failure in layered microelectronics devices.

HREBSD↗
DOE OSTI2020

Analysis of fission product distribution and composition in the TRISO layers of AGR-2 fuel

The Advanced Gas Reactor Fuel Qualification and Development Program's second irradiation experiment focuses on the performance of fuel particles produced in an industrial-scale coating system. Ongoing post-irradiation examination efforts include exploration of tristructural-isotropic (TRISO)-coated particle fuel in the as-irradiated state and subjected to elevated temperatures to simulate accident conditions (safety testing). Scanning electron microscopy (SEM) analysis with energy dispersive x-ray spectroscopy (EDS) was used to show the distribution of fission products within the TRISO layers. The SEM analysis showed a variation of fission product distribution within the TRISO layers based on irradiation temperature, burnup, individual particle fission product inventory retention, safety testing history and kernel composition. Finally, a key observation is that particles which likely experienced higher temperature showed a greater diversity and distribution of fission products and actinides in the IPyC and SiC layers, implying that temperature is a dominant variable influencing the transport of radionuclides in TRISO particles.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2018

Dynamic recrystallization kinetics and microstructure evolution of an AZ91D magnesium alloy during hot compression

Highlights: • DRX kinetic model is developed for the aged AZ91D magnesium alloy. • The DRX behavior in different strained regions was investigated. • Four morphologies of the second phase were proposed during the hot compression tests. • The nucleation mechanisms of the DRX grains were clarified. - Abstract: The flow behavior of as-cast AZ91D magnesium alloy was evaluated by isothermal compression tests within the temperatures of 220 °C, 260 °C, 300 °C, 340 °C, and 380 °C, and the strain rates of 0.001, 0.01, 0.1, 1 and 10s{sup −1}. Based on the stress-strain curve and hyperbolic sine function, the thermal activation energy and the strain rate sensitivity of the material were determined to be 142.2726 kJ·mol{sup −1} and 0.142, respectively. The S type evolution of the dynamic recrystallization with the increasing strain that dynamic recrystallization (DRX) model obtained from stress and strain data. There was a good consistency between the proposed DRX kinetics model and microstructure observation results. Combining isothermal compression specimens with finite element and scanning electron microscopy (SEM) analysis indicated that the sample can be divided into rarely recrystallized region, partially recrystallized region and completely recrystallized region, which falls within the dense deformation zone, free deformation zone and severe deformation zone, respectively. The different forms of the β-Mg{sub 17}Al{sub 12} phase induced by compression tests were confirmed by SEM. Nucleation mechanisms of the DRX were discussed with reference to the transmission electron microscope (TEM) analysis results.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Halo-independent analysis of direct dark matter detection through electron scattering

Sub-GeV mass dark matter particles whose collisions with nuclei would not deposit sufficient energy to be detected, could instead be revealed through their interaction with electrons. Analyses of data from direct detection experiments usually require assuming a local dark matter halo velocity distribution. In the halo-independent analysis method, properties of this distribution are instead inferred from direct dark matter detection data, which allows then to compare different data without making any assumption on the uncertain local dark halo characteristics. Furthermore, this method has so far been developed for and applied to dark matter scattering off nuclei. Here we demonstrate how this analysis can be applied to scattering off electrons.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2014

Simulation study of the effects of near- and far-field heating during focused ultrasound uterine fibroid ablation using an electronically focused phased array: A theoretical analysis of patient safety

Purpose: Assess the feasibility of using large-aperture, flat ultrasonic transducer arrays with 6500 small elements operating at 500 kHz without the use of any mechanical components for the thermal coagulation of uterine fibroids. This study examines the benefits and detriments of using a frequency that is significantly lower than that used in clinical systems (1–1.5 MHz). Methods: Ultrasound simulations were performed using the anatomies of five fibroid patients derived from 3D MRI. Using electronic steering solely, the ultrasound focus from a flat, 6500-element phased array was translated around the volume of the fibroids in various patterns to assess the feasibility of completing full treatments from fixed physical locations. Successive temperature maps were generated by numerically solving the bioheat equation. Using a thermal dose model, the bioeffects of these simulations were quantified and analyzed. Results: The simulations indicate that such an array could be used to perform fibroid treatments to 18 EM{sub 43} at an average rate of 90 ± 20 cm{sup 3}/h without physically moving the transducer array. On average, the maximum near-field thermal dose for each patient was below 4 EM{sub 43}. Fibroid tissue could be treated as close as 40 mm to the spine without reaching temperatures expected to cause pain or damage. Conclusions: Fibroids were successfully targeted and treated from a single transducer position to acceptable extents and without causing damage in the near- or far-field. Compared to clinical systems, treatment rates were good. The proposed treatment paradigm is a promising alternative to existing systems and warrants further investigation.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2012

Drift and ion acoustic wave driven vortices with superthermal electrons

Linear and nonlinear analysis of coupled drift and acoustic mode is presented in an inhomogeneous electron-ion plasma with {kappa}-distributed electrons. A linear dispersion relation is found which shows that the phase speed of both the drift wave and the ion acoustic wave decreases in the presence of superthermal electrons. Several limiting cases are also discussed. In the nonlinear regime, stationary solutions in the form of dipolar and monopolar vortices are obtained. It is shown that the condition for the boundedness of the solution implies that the speed of drift wave driven vortices reduces with increase in superthermality effect. Ignoring density inhomogeniety, it is investigated that the lower and upper limits on the speed of the ion acoustic driven vortices spread with the inclusion of high energy electrons. The importance of results with reference to space plasmas is also pointed out.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2013

The use of electrical impedance spectroscopy for monitoring the hydration products of Portland cement mortars with high percentage of pozzolans

In this paper, mortars and pastes containing large replacement of pozzolan were studied by mechanical strength, thermogravimetric analysis (TGA), scanning electronic microscopy (SEM), mercury intrusion porosimetry (MIP) and electrical impedance spectroscopy (EIS). The effect of metakaolin (35%) and fly ash (60%) was evaluated and compared with an inert mineral addition (andalusite). The portlandite content was measured, finding that the pozzolanic reaction produced cementing systems with all portlandite fixed. The EIS measurements were analyzed by the equivalent electrical circuit (EEC) method. An EEC with three branches in parallel was applied. The dc resistance was related to the degree of hydration and allowed us to characterize plain and blended mortars. A constant phase element (CPE) quantified the electrical properties of the hydration products located in the solid–solution interface and was useful to distinguish the role of inert and pozzolanic admixtures present in the cement matrix.

36 MATERIALS SCIENCE↗
DOE OSTI2013

The role of alumina on performance of alkali-activated slag paste exposed to 50 °C

The strength and microstructural evolution of two alkali-activated slags, with distinct alumina content, exposed to 50 °C have been investigated. These two slags are ground-granulated blast furnace slag (containing 13% (wt.) alumina) and phosphorous slag (containing 3% (wt.) alumina). They were hydrated in the presence of a combination of sodium hydroxide and sodium silicate solution at different ratios. The microstructure of the resultant slag pastes was assessed by X-ray diffraction, differential thermogravimetric analysis, and scanning electron microscopy. The results obtained from these techniques reveal the presence of hexagonal hydrates: CAH{sub 10} and C{sub 4}AH{sub 13} in all alkali-activated ground-granulated blast-furnace slag pastes (AAGBS). These hydrates are not observed in pastes formed by alkali-activated ground phosphorous slag (AAGPS). Upon exposure to 50 °C, the aforementioned hydration products of AAGBS pastes convert to C{sub 3}AH{sub 6}, leading to a rapid deterioration in the strength of the paste. In contrast, no strength loss was detected in AAGPS pastes following exposure to 50 °C. -- Highlights: •Strength of alkali-activated slag (AAS) pastes after exposure to 50 °C is studied. •AAS pastes with high alumina content lose strength after the exposure. •C{sub 4}AH{sub 13} and CAH{sub 10} form in these AAS pastes. •Conversion of these calcium alumina hydrates is associated with the strength loss. •AAS pastes with low alumina content maintain its strength after the exposure.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Changes in microstructure characteristics of cement paste on carbonation

This study investigates the influence of carbonation on the microstructure of cement paste cast with Ordinary Portland Cement (OPC), fly ash based Portland Pozzolana Cement (PPC) and Limestone Calcined Clay Cement (LC{sup 3}) using X-ray diffraction (XRD), thermal analysis (TGA), scanning electron microscope (SEM) and mercury intrusion porosimeter (MIP). A comparison is made between samples exposed to 3% carbon dioxide concentration and those exposed to natural CO{sub 2} concentrations. It is observed that the products formed on carbonation are similar in both the exposure conditions. Distinct rims corresponding to decalcified C-S-H are observed around clinker grains in the carbonated samples. Coarsening of pore structure is observed on carbonation in all the cements and an increase in the total porosity is observed in blended cements. Thermodynamic modeling indicates irrespective of the type of cement the total solid volume is reduced on complete carbonation. The volume change occurring on carbonation obtained from experimental results and thermodynamic modeling are compared.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Optimizing dicyandiamide pretreatment conditions for enhanced structure and electronic properties of polymeric graphitic carbon nitride

Graphitic carbon nitride, a polymeric semiconductor, possesses a distinctive electronic band structure and exceptional chemical stability, making it a highly promising material for various catalytic applications such as electrocatalysis, photocatalysis, and photo-electrocatalysis. However, its practical applications remain limited due to its low active site density and poor electrical conductivity. In this study, to overcome such limitations, we have conducted a thorough investigation to explore the impact of dicyandiamide (DCDA) precursor pretreatment prior to thermal polymerization to graphitic carbon nitride. The DCDA precursor was subjected to various pretreatment methods including grinding using mortar and pestle, recrystallization through stirring or probe sonication after dissolving in deionized water, and freeze drying, prior to thermal polymerization at 550 °C for 2 hours. The structural and morphological properties of the catalysts prepared were compared and characterized by X-ray diffraction (XRD), attenuated total reflectance–Fourier transform infrared (ATR-IR) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray photoelectron spectroscopy (XPS) analysis while the electronic band gap properties were determined based on density functional theory (DFT) calculations for a set of crystalline systems having C/N ratios similar to those identified experimentally. In comparison to direct thermal polymerization, pretreated samples rendered the same product yield, diverse morphologies with flat or wrinkle structures, and reduced electrochemical resistance, making them suitable for use in various catalytic processes.

36 MATERIALS SCIENCE↗