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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 991 records · Page 55
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Recent Advances in Piezoelectric Wafer Active Sensors for Structural Health Monitoring Applications

In this paper, some recent piezoelectric wafer active sensors (PWAS) progress achieved in our laboratory for active materials and smart structures (LAMSS) at the University of South Carolina: http: //www.me.sc.edu/research/lamss/ group is presented. First, the characterization of the PWAS materials shows that no significant change in the microstructure after exposure to high temperature and nuclear radiation, and the PWAS transducer can be used in harsh environments for structural health monitoring (SHM) applications. Next, PWAS active sensing of various damage types in aluminum and composite structures are explored. PWAS transducers can successfully detect the simulated crack and corrosion damage in aluminum plates through the wavefield analysis, and the simulated delamination damage in composite plates through the damage imaging method. Finally, the novel use of PWAS transducers as acoustic emission (AE) sensors for in situ AE detection during fatigue crack growth is presented. The time of arrival of AE signals at multiple PWAS transducers confirms that the AE signals are originating from the crack, and that the amplitude decay due to geometric spreading is observed.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Analysis of the CO 2 Chemisorption in Li 5 FeO 4 , a New High Temperature CO 2 Captor Material. Effect of the CO 2 and O 2 Partial Pressures

Pentalithium ferrite (Li 5 FeO 4 ) was tested in this paper as possible CO 2 captor, both by theoretical calculations and experimental measurements. The pristine Li 5 FeO 4 compound with orthorhombic structure was synthesized via solid-state reaction and it was structural and microstructurally characterized. Later, sample was heat-treated at temperatures from room temperature to 900 °C under different CO 2 or CO 2 –O 2 atmospheres. Li 5 FeO 4 exhibits excellent CO 2 chemisorption abilities with a capture capacity about 12.9 mmol/g, which is outstanding in comparison to other previously reported ceramic captors. This material is able to react with CO 2 from 200 °C to approximately 715 °C showing a high kinetic of reaction even at CO 2 partial pressure values as low as 0.2. Finally and additionally, results suggest that oxygen addition does enhance the CO 2 chemisorption on Li 5 FeO 4 at temperatures below 700 °C, although oxygen addition seems to favor the desorption process at higher temperatures.

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

Advances and Achievements in In Situ Analysis of Corrosion and Structure–Property Relationship in Mg Alloys

Every year, TMS Magnesium Committee carefully selects a special topic in magnesium (Mg) related research and development not only having the hottest subject from both academic and industrial perspectives but also demonstrating major achievements within this subject. Following last year’s topic on Mg microallying [1], this year’s focus is on in-situ methods and associated techniques in their broad definition spanning from laboratory- to large- scale facilities to process monitoring. The applications of in-situ techniques have a wide spectrum from the analysis of melts and liquid-solid transitions to solid-state phenomena during thermo-mechanical processing and heat treatments to surface interactions with various environments. Therefore, such works are of significant interest to scientists working in the area of Mg alloy development as well as to a much broader audience from both academia and industry. This interest is primarily caused by challenges in the analysis of structure-property relationship in Mg alloys, and even cursory glance of literature reveals sharp increase of publications relevant to this topic recently. For instance, very high reactivity of Mg as well as its well-known propensity to substantially alter structure upon unloading in mechanical testing makes it difficult to understand and thus to simulate correlation between microstructures observed in post-mortem analysis and physical processes during testing or fabrication. However, recent advances in in-situ analysis based on large-scale research facilities such as neutron scattering and synchrotron radiation sources as well as microscopy-based, acoustic emission, and other more traditional techniques allowed significant achievements. Apart from apparent development of relevant experimental techniques, a significant part of this success should also be attributed to increasing accessibility of the facilities and simplification of their use from a user perspective. The selection of articles in this special topic is quite far from comprehensive review covering all aspects of in-situ methods available for metallic materials development. However, this was not the purpose in any case. Instead, this selection is intended to present several studies on Mg alloys and Mg-based composites with the use of in-situ techniques. In addition, it overviews two techniques, ‘Acoustic Emission’ (AE) and ‘Ambient-Pressure X-ray Photoelectron Spectroscopy’ (AP-XPS), that are rather novel to the Mg community. These studies are supposed to give readers representative examples of such techniques potential and to help in navigating the spectrum of modern state-of-the-art analytical methods facilitating the development of Mg alloys. These articles are organized in the order corresponding to typical Mg alloy lifecycle from material preparation and solidification to thermo-mechanical processing and product fabrication to degradation.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Correlation between surface chemistry, density and band gap in nanocrystalline WO3 thin films

Nanocrystalline WO3 thin films were produced by sputter-deposition by varying the ratio of argon to oxygen in the reactive gas mixture during deposition. The surface chemistry, physical characteristics, and optical properties of nanocrystalline WO3 films were evaluated using X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), atomic force microscopy (AFM), X-ray reflectivity (XRR), and spectrophotometric measurements. The effect of ultra-microstructure was significant on the optical properties of WO3 films. The XPS analyses indicate the formation of stoichiometric WO3 with tungsten existing in fully oxidized valence state (W6+). However, WO3 films grown at high oxygen concentration (>60%) in the sputtering gas mixture were over stoichiometric with excess oxygen. XRR simulations, which are based on isotropic WO3 film - SiO2 interface - Si substrate model, indicate that the density of WO3 films is sensitive to the oxygen content in the sputtering gas. The spectral transmission of the films increased with the increasing oxygen. The band gap of these films increases from 2.78 eV to 3.25 eV with increasing oxygen. A direct correlation between the film-density and band gap in nanocrystalline WO3 films is established based on the observed results.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Magnetic Sorbent for the Removal of Selenium(IV) from Simulated Industrial Wastewaters: Determination of Column Kinetic Parameters

A novel meso- and microporous tire-derived-carbon support with magnetic iron oxide nanoparticle adsorbents that selectively adsorbs Se(IV) ions from simulated contaminated water has been developed. In this work, the physicochemical characteristics of the composite adsorbent are characterized with respect to porosity and surface area, chemical composition, and microstructure morphology. The kinetics of this composite adsorbent in a fixed-bed setting has been determined. Several column runs were conducted and analyzed by inductively coupled plasma-optical emission spectroscopy (ICP-OES) to determine the concentration gradient vs time. These results were then fit to a pseudo-second order rate law to obtain equilibrium values. Combining calculated equilibrium values with effluent concentration data, enabled the application of the Adams–Bohart model to determine reaction constants and column coefficients. Column parameters obtained from different flow rates and fittings of the Adams–Bohart model were remarkably consistent. These findings enable the application of this sorbent to fixed-bed column systems and opens up further research into mixed pollutants tests with real wastewater and scaling of selenium pollutant removal.

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

Solid-state synthesis of YAG powders through microwave coupling of oxide/carbon particulate mixtures

The rapid synthesis of yttrium aluminum garnet (Y 3 Al 15 O 12 , YAG) powder was investigated through the use of microwave irradiation of the oxide precursor system. For this investigation, an external hybrid heating source was not used. Instead, the rapid heating of the precursor materials (yttria and alumina powders, which are typically transparent to 2.45 GHz microwaves) was initiated by mixing an intrinsic absorbing material (carbon) into the original oxide precursors. The effect of the carbon characteristics, such as carbon source, concentration, particle size, and agglomerate microstructure were evaluated on the efficiency of coupling and resultant oxide reaction. The microwave power was varied to optimize the YAG conversion and eliminate intermediate phase formation. Interactions between the conductive carbon particles and the dielectric oxides within the microwave exposure produced local arching and micro-plasma formation within the powder bed, resulting in the rapid formation of the refractory YAG composition. This optimal conduction led to temperatures of 1000°C that could be achieved in less than 5 min resulting in the formation of > 90 vol% YAG. The understanding of a conductor/dielectric particulate system here, provided insight into possible application of similar systems where microwave irradiation could be used for enhanced solid-state formation, local melting events, and gas phase reactions with a composite powder media.

36 MATERIALS SCIENCE↗
DOE OSTI2018

A green degumming process of ramie

Ramie provides the longest and strongest natural fiber in textile industry, but its traditional degumming process is costly and requires a large amount of alkali, which causes serious environmental concerns. In this study, a steam explosion (STEX) treatment followed by sodium percarbonate (SP) soak degumming process was investigated. Microstructure, chemical composition and mechanical properties of the refined ramie fibers were comprehensively characterized. The residual gum content was below 5%, the fineness was higher than 1600 Nm (6.25 dtex), the breaking tenacity was 5.4 cN/dex, and the whiteness was above 50%. All of the properties met the requirements of Chinese national standard, and the breaking tenacity and whiteness were notably better than those of the fibers degummed traditionally. Additionally, environmental impacts of the new degumming process were evaluated. Only 50% chemicals were needed for the new process, and chemical oxygen demand (COD) of the waste reduced to 35% of the traditional method. Therefore, the new method was more environment-friendly and economically feasible. It has great potential for industry applications.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Evaluating the Rheo-electric Performance of Aqueous Suspensions of Oxidized Carbon Black

Here, the macroscopic properties of carbon black suspensions are primarily determined by the agglomerate microstructure built of primary aggregates. Conferring colloidal stability in aqueous carbon black suspensions should thus have a drastic impact on their viscosity and conductivity. Carbon black was treated with strong acids following a wet oxidation procedure. An analysis of the resulting particle surface chemistry and electrophoretic mobility was performed in evaluating colloidal stability. Changes in suspension microstructure due to oxidation were observed using small-angle X-ray scattering. Utilizing rheo-electric measurements, the evolution of the viscosity and conductivity of the carbon black suspensions as a function of shear rate and carbon content was thoroughly studied. The carboxyl groups installed on the carbon black surface through oxidation increased the surface charge density and enhanced repulsive interactions. Electrostatic stability inhibited the formation of the large-scale agglomerates in favor of the stable primary aggregates in suspension. While shear thinning, suspension conductivities were found to be weakly dependent on the shear intensity regardless of the carbon content. Most importantly, aqueous carbon black suspensions formulated from electrostatically repulsive primary aggregates displayed a smaller rise in conductivity with carbon content compared to those formulated from attractive agglomerates.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Trace Impurities Identified as Forensic Signatures in CMX-5 Fuel Pellets Using X-ray Spectroscopic Techniques

We report that small-particle analysis is a highly promising emerging forensic tool for analysis of interdicted special nuclear materials. Integration of microstructural, morphological, compositional, and molecular impurity signatures could provide significant advancements in forensic capabilities. We have applied rapid, high-sensitivity, hard X-ray synchrotron chemical imaging to analyze impurity signatures in two differently fabricated fuel pellets from the 5th Collaborative Materials Exercise (CMX5) of the IAEA Nuclear Forensics International Working Group. The spatial distributions, chemical compositions, and morphological and molecular characteristics of impurities were evaluated using X-ray absorption near-edge structure (XANES) and X-ray fluorescence chemical imaging to discover principal impurities, their granularity, particle sizes, modes of occurrence (distinct grains vs incorporation in the UO 2 lattice), and sources and mechanisms of incorporation. Differences in UO 2+x stoichiometry were detected at the microscale in nominally identical UO 2 ceramics (CMX5-A and CMX5-B), implying the presence of multiple UO 2 host phases with characteristic microstructures and feedstock compositions. Al, Fe, Ni, W, and Zr impurities and integrated impurity signature analysis identified distinctly different pellet synthesis and processing methods. For example, two different Al, W, and Zr populations in the CMX5-B sample indicated a more complex processing history than the CMX5-A sample. K-edge XANES measurements reveal both metallic and oxide forms of Fe and Ni but with different proportions between each sample. Altogether, these observations suggest multiple sources of impurities, including fabrication (e.g., force-sieving) and feedstock (mineral oxides). This study demonstrates the potential of synchrotron techniques to integrate different signatures across length scales (angstrom to micrometer) to detect and differentiate between contrasting UO 2 fuel fabrication techniques.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Biodegradable High-Molecular-Weight Poly(pentylene adipate- co -terephthalate): Synthesis, Thermo-Mechanical Properties, Microstructures, and Biodegradation

Poly(pentylene adipate-co-terephthalate) (PPAT) is a promising biobased and biodegradable polymer that can replace polyethylene in flexible packaging films where biodegradability is desired. High-molecular-weight (100K–145 KDa) aliphatic–aromatic polyester PPAT was successfully synthesized, and the effects of reaction conditions on molecular weight were reported. PPAT polyesters were characterized for polymer compositions, number-average unit length, thermal transitions, and rheological properties. PPAT compression-molded films were characterized for crystallinity and tensile properties to correlate micro- and macroproperties. PPAT compression-molded films exhibited up to a 76% higher tensile modulus than compression-molded films from poly(butylene adipate-co-terephthalate) (PBAT), making PPAT films potentially comparable with compression-molded films from linear low-density polyethylene (LLDPE). Finally, PPAT is biodegradable in soil and freshwater environments with estimated 90% biodegradation times of 504–580 and 604–845 days, respectively, while PBAT takes 971 days in soil and 395 days in freshwater.

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

Defect and structural evolution under high-energy ion irradiation informs battery materials design for extreme environments

Understanding defect evolution and structural transformations constitutes a prominent research frontier for ultimately controlling the electrochemical properties of advanced battery materials. Herein, for the first time, we utilize in situ high-energy Kr ion irradiation with transmission electron microscopy to monitor how defects and microstructures evolve in Na- and Li-layered cathodes with 3d transition metals. Our experimental and theoretical analyses reveal that Li-layered cathodes are more resistant to radiation-induced structural transformations, such as amorphization than Na-layered cathodes. The underlying mechanism is the facile formation of Li-transition metal antisite defects in Li-layered cathodes. The quantitative mathematical analysis of the dynamic bright-field imaging shows that defect clusters preferentially align along the Na/Li ion diffusion channels ( a-b planes), which is likely governed by the formation of dislocation loops. Our study provides critical insights into designing battery materials for extreme irradiation environments and understanding fundamental defect dynamics in layered oxides.

25 ENERGY STORAGE↗
DOE OSTI2017

Bright x-rays reveal shifting deformation states and effects of the microstructure on the plastic deformation of crystalline materials

The plastic deformation of crystalline materials is usually modeled as smoothly progressing in space and time, yet modern studies show intermittency in the deformation dynamics of single-crystals arising from avalanche behavior of dislocation ensembles under uniform applied loads. However, once the prism of the microstructure in polycrystalline materials disperses and redistributes the load on a grain-by-grain basis, additional length and time scales are involved. Thus, the question is open as to how deformation intermittency manifests for the nonuniform grain-scale internal driving forces interacting with the finer-scale dislocation ensemble behavior. In this work we track the evolution of elastic strain within individual grains of a creep-loaded titanium alloy, revealing widely varying internal strains that fluctuate over time. Here, the findings provide direct evidence of how flow intermittency proceeds for an aggregate of ~700 grains while showing the influences of multiscale ensemble interactions and opening new avenues for advancing plasticity modeling.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Design of non-fluorinated proton exchange membranes from Poly(Terphenyl fluorenyl isatin) with fluorene-linked sulfonate groups and microblock structures

Proton exchange membranes (PEMs) are essential components in energy storage and conversion devices, such as fuel cells and electrolyzers. Here, in this study, we developed a series of non-fluorinated PEMs from poly(terphenyl fluorenyl isatin) with fluorene-pendent disulfonate groups. These polymers feature a microblock structure composed of hydrophobic blocks, hydrophilic blocks, and alternating blocks, arising from the differences in reactivity, concentration, and solubility between the hydrophobic p-terphenyl and hydrophilic disulfonated fluorene monomers. As a result, the sulfonic acid groups are unevenly distributed along the polymer chains, forming densely charged regions (IEC = 3.52 meq/g) with large ion clusters and lightly charged regions (IEC = 2.16 meq/g) with small ion clusters. This microstructure, combined with the degree of sulfonation, significantly influences the overall properties of the membranes, including robust mechanical strength (47.1–63.2 MPa), high thermal stability (up to 270 °C), low swelling ratio (18–25% at 80 °C), and high proton conductivity (136–169 mS/cm in deionized water at 80 °C). The PFLSH60 membrane demonstrated comparable fuel cell performance to Nafion 212. Its hydrogen crossover current density was more than two times lower (0.86 mA/cm 2 for PFLSH60 compared to 1.83 mA/cm 2 for Nafion 212) under testing conditions of 80 °C and 100% RH. This significantly reduced crossover improves fuel utilization in fuel cell stacks. This work offers valuable insights into the design of robust, high-performance PEMs by systematically analyzing the relationships between membrane structure, properties, and performance.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Molecular-Resolution Electron Imaging of Defects and Dynamics at the Ice-Water Interface

Water crystallization into hexagonal ice (type I h ) is one of the most critical processes relevant to the Earth’s environment and human activities. However, despite recent breakthroughs in imaging non-equilibrium condensed ice structures, the ice-water interface has never been imaged at a molecular resolution. This is primarily due to the low stability of the hydrogen bonds in ice under high-resolution microscopy conditions and a lack of methods to prepare compatible samples. Here, this presentation describes the first molecular-resolution imaging of ice crystallized from liquid water and the ice-water interface using high-resolution transmission electron microscopy (HRTEM). By encapsulating deionized (DI) water between two amorphous carbon (a-C) TEM grids and subsequently freezing it with liquid N 2 on a cryo sample stage, we generated two types of ice: non-equilibrium, condensed ice from the atmosphere and encapsulated ice from the DI water (Fig. 1A). Condensed ice usually shows irregular, spherulitic shapes (Fig. 1B). Selected area electron diffraction (SAED) shows that they are a mixture of cubic and hexagonal crystals (Fig. 1C). On the contrary, encapsulated ice forms thin films that contain large-area single-crystalline regions of hexagonal ice oriented along the [0001] zone axis (Fig. 1D). Differential electron energy-loss spectroscopy (EELS) confirmed the high purity of the encapsulated ice free from organic contaminations that are common in other encapsulation methods for HRTEM such as graphene liquid cells. These single-crystalline areas are robust under the electron beam up to ~100 e/Å 2 s. Aberration-corrected HRTEM imaging in these areas achieved a line resolution of ~1.3 Å (Fig. 1E and F). This platform allows us to study near-equilibrium ice structures and dynamics at an unprecedented spatial resolution (Fig. 2). For example, we discovered subdomain-rich regions near the defective crystal edges despite the structure appearing single-crystalline according to diffraction criteria. These subdomains connect via low-angle grain boundaries with flat energy landscapes as a function of tilt angles (according to simulations), showing the high tolerance of ice to defect structures. When we tuned the sample temperature and electron flux rate, we observed radiolysis-controlled bubble generation and dissolution in ice single crystals near a steady state of bubble dynamics. Furthermore, rich beam-induced melting and recrystallization dynamics were observed at the ice-water interface with lattice resolution. These data represent the first observation of the ice-water phase transformation at the sub-nanometer level. In summary, the methods developed in this work enabled molecular-resolution observations of ice and the ice-water interface and shed light on the microstructures and phase transformation pathways. Finer control on the temperature, electron irradiation profile, and imaging detector could eventually lead to real-time observation of ice nucleation in water and address long-standing questions in the nucleation pathways.

74 ATOMIC AND MOLECULAR PHYSICS↗
DOE OSTI2022

A classical equation that accounts for observations of non-Arrhenius and cryogenic grain boundary migration

Observations of microstructural coarsening at cryogenic temperatures, as well as numerous simulations of grain boundary motion that show faster migration at low temperature than at high temperature, have been troubling because they do not follow the expected Arrhenius behavior. This work demonstrates that classical equations, that are not simplified, account for all these oddities and demonstrate that non-Arrhenius behavior can emerge from thermally activated processes. According to this classical model, this occurs when the intrinsic barrier energies of the processes become small, allowing activation at cryogenic temperatures. Additional thermal energy then allows the low energy process to proceed in reverse, so increasing temperature only serves to frustrate the forward motion. This classical form is shown to reconcile and describe a variety of diverse grain boundary migration observations.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Gas Sensing Properties of Epitaxial LaBaCo 2 O 5.5+δ Thin Films

Chemical reactivity and stability of highly epitaxial mixed-conductive LaBaCo 2 O 5.5+δ (LBCO) thin films on (001) LaAlO 3 (LAO) single-crystalline substrates, fabricated by using pulsed laser deposition system, were systematically investigated. Microstructure studies from x-ray diffraction indicate that the films are c-axis oriented with the interface relationship of [100] LBCO //[100] LAO and (001) LBCO //(001) LAO . LBCO thin films can detect the ethanol vapor concentration as low as 10ppm and the response of LBCO thin film to various ethanol vapor concentrations is very reliable and reproducible with the switch between air and ethanol vapor. Moreover, the fast response of the LBCO thin film, as the p-type gas sensor, is better than some n-type oxide semiconductor thin films and comparable with some nanorods and nanowires. These findings indicate that the LBCO thin films have great potential for the development of gas sensors in reducing/oxidizing environments.

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

Thermomechanical Modeling of Laser-Induced Structural Relaxation and Deformation of Glass: Volume Changes in Fused Silica at High Temperatures [Thermo-mechanical modeling of laser-induced structural relaxation and deformation of SiO 2 glass]

In a fully coupled thermomechanical model of the nanoscale deformation in amorphous SiO 2 due to laser heating is presented. Direct measurement of the transient, nonuniform temperature profiles was used to first validate a nonlinear thermal transport model. Densification due to structural relaxation above the glass transition point was modeled using the Tool-Narayanaswamy (TN) formulation for the evolution of structural relaxation times and fictive temperature. TN relaxation parameters were derived from spatially resolved confocal Raman scattering measurements of Si–O–Si stretching mode frequencies. These thermal and microstructural data were used to simulate fictive temperatures which are shown to scale nearly linearly with density, consistent with previous measurements from Shelby et al. Volumetric relaxation coupled with thermal expansion occurring in the liquid-like and solid-like glassy states lead to residual stresses and permanent deformation which could be quantified. But, experimental surface deformation profiles between 1700 and 2000 K could only be reconciled with our simulation by assuming a roughly 2 × larger liquid thermal expansion for a-SiO 2 with a temperature of maximum density ~150 K higher than previously estimated by Bruckner et al. Calculated stress fields agreed well with recent laser-induced critical fracture measurements, demonstrating accurate material response prediction under processing conditions of practical interest.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Single-crystal sapphire microstructure for high-resolution synchrotron X-ray monochromators

We report on the growth and characterization of several sapphire single crystals for the purpose of x-ray optics applications. Structural defects were studied by means of laboratory double-crystal X-ray diffractometry and white beam synchrotron-radiation topography. The investigations confirmed that the main defect types are dislocations. The best quality crystal was grown using the Kyropoulos technique with a dislocation density of 10 2 -10 3 cm -2 and a small area with approximately 2*2 mm 2 did not show dislocation contrast in many reflections and has suitable quality for application as a backscattering monochromator. As a result, a clear correlation between growth rate and dislocation density is observed, though growth rate is not the only parameter impacting the quality.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗