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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 1,585 records · Page 88
All sourcesNASA NTRSDOE OSTI
DOE OSTI2015

Femtosecond laser structuring of silver-containing glass: Silver redistribution, selective etching, and surface topology engineering

Femtosecond direct laser writing in silver-containing phosphate glasses allows for the three-dimensional (3D) implementation of complex photonic structures. Sample translation along or perpendicular to the direction of the beam propagation has been performed, which led to the permanent formation of fluorescent structures, either corresponding to a tubular shape or to two parallel planes at the vicinity of the interaction voxel, respectively. These optical features are related to significant modifications of the local material chemistry. Indeed, silver depletion areas with a diameter below 200 nm were evidenced at the center of the photo-produced structures while photo-produced luminescence properties are attributed to the formation of silver clusters around the multiphoton interaction voxel. The laser-triggered oxidation-reduction processes and the associated photo-induced silver redistribution are proposed to be at the origin of the observed original 3D luminescent structures. Thanks to such material structuring, surface engineering has been also demonstrated. Selective surface chemical etching of the glass has been obtained subsequently to laser writing at the location of the photo-produced structures, revealing features with nanometric depth profiles and radial dimensions strongly related to the spatial distributions of the silver clusters.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Chemical and Morphological Structure of Transgenic Switchgrass Organosolv Lignin Extracted by Ethanol, Tetrahydrofuran, and $\mathcal{γ}$-Valerolactone Pretreatments

We report the recalcitrance of lignocellulosic biomass is a challenge in biological-based biorefinery systems due to the complex physicochemical structure of plant cell walls. Pretreatment and genetic modification are two approaches in biomass conversion that have succeeded in modifying the structure of lignocellulose to enable better enzymatic deconstruction. However, the structural differences among pretreatment-solubilized lignin isolated from switchgrass genotypes have not been extensively investigated. Here, three organosolv pretreatment systems-ethanol (EtOH), tetrahydrofuran (THF), and γ-valerolactone (GVL)-were used on wild-type (WT) and two transgenic switchgrasses. All organosolv pretreatments caused a significant reduction in the molecular mass of lignins; particularly, up to ~90% decrease was observed in EtOH-pretreated lignin compared to untreated lignin. The WT EtOH lignin also presented the smallest particle size among all WT lignins. THF pretreated transgenic lignins showed a higher molecular mass, β-O-4 linkages, and aliphatic hydroxyl content compared to EtOH and GVL pretreated lignin. The number of hydrogen bonds between lignin and the organic solvents calculated from the molecular dynamics simulations followed the same trend as the experimentally determined reduction in lignin molecular mass. The results revealed the structural changes of solubilized lignin isolated from wild-type and transgenic switchgrass after different organosolv pretreatments.

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

Impact of surface hydrophilicity on the ordering and transport properties of bicontinuous microemulsions

Microemulsions (MEs) have many industrial applications, where recent developments have shown that MEs can be utilized for electrochemical applications, including potentially in redox flow batteries. However, understanding the structure and dynamics of these systems, including at a surface, is needed to direct and rationally control their electrochemical behavior. While bulk solution measurements have provided insight into their structure, their assembly at an interface also impacts the electron (to the electrode) and ion (across the surfactant) charge transfer processes in the system. To address this shortcoming, neutron reflectivity experiments and molecular simulations have been completed that document the near surface structure of a series of deuterated water (D 2 O)/polysorbate-20/toluene MEs on hydrophilic and amphiphilic surfaces. These results show that the microemulsions form complex layered structures near a hard electrode surface, where most layers are not purely one component. Decreasing the D 2 O concentration in the ME increases the number of and purity of the layers established on the solid surface. These lamellar-type layers transition from the surface to the bulk microemulsion as a series of mixed layers (i.e., containing oil, water, and surfactant) that are consistent with perforated lamellae. Additionally, these mixed lamellae appear to become more perforated with oil and water pathways on an amphiphilic surface. Furthermore, the purity and thickness of these layers will influence the accessibility of an electrode by redox active species, as well as ion transport required to satisfy the electroneutrality condition.

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

Synthesis and characterization of MoB{sub 2−x} thin films grown by nonreactive DC magnetron sputtering

DC magnetron sputtering was used to deposit molybdenum boride thin films for potential low-friction applications. The films exhibit a nanocomposite structure with ∼10 nm large MoB{sub 2−x} (x > 0.4) grains surrounded by a boron-rich tissue phase. The preferred formation of the metastable and substoichiometric hP3-MoB{sub 2} structure (AlB{sub 2}-type) is explained with kinetic constraints to form the thermodynamically stable hR18-MoB{sub 2} phase with a very complex crystal structure. Nanoindentation revealed a relatively high hardness of (29 ± 2) GPa, which is higher than bulk samples. The high hardness can be explained by a hardening effect associated with the nanocomposite microstructure where the surrounding tissue phase restricts dislocation movement. A tribological study confirmed a significant formation of a tribofilm consisting of molybdenum oxide and boron oxide, however, without any lubricating effects at room temperature.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Improving Bending Moment Measurements on Wind Turbine Blades

Full-scale fatigue testing of wind turbine blades is conducted using resonance test techniques where the blade plus additional masses is excited at its first resonance frequency to achieve the target loading amplitude. Because there is not a direct relationship between the force applied by an actuator and the bending moment, the blade is instrumented with strain gauges that are calibrated under static loading conditions to determine the sensitivity or relationship between strain and applied moment. Then, during dynamic loading the applied moment is calculated using the strain response of the structure. A similar procedure is also used in the field to measure in-service loads on turbine blades. Because wind turbine blades are complex twisted structures and the deflections are large, there is often significant cross-talk coupling in the sensitivity of strain gauges placed on the structure. Recent work has shown that a sensitivity matrix with nonzero cross terms must be employed to find constant results when a blade is subjected to both flap and lead-lag loading. However, even under controlled laboratory conditions, potential for errors of 3 percent or more in the measured moment exist when using the typical cross-talk matrix approach due to neglecting the influence of large deformations and torsion. This is particularly critical when considering a biaxial load as would be applied on the turbine or during a biaxial fatigue test. This presentation describes these results demonstrating errors made when performing current loads measurement practices on wind turbine blades in the lab and evaluating potential improvements using enhanced cross-talk matrix approaches and calibration procedures.

17 WIND ENERGY↗
DOE OSTI2020

Direct functionalization of C-H bonds by electrophilic anions

Bond formation between two of the most inert molecules, alkanes and [B12X12]2- (X = Cl, Br), is performed in a two step process. Fragmentation of [B12X12]2- in the gas phase generates highly reactive [B12X11]- ions which spontaneously react with alkanes. The reaction mechanism was investigated using tandem mass spectrometry and gas-phase vibrational spectroscopy combined with electronic structure calculations. This effort revealed the unprecedented and counterintuitive electrophilic substitution of a proton in an alkane by a negatively charged ion resulting in a B-C bond formation. The product is a dianionic [B12X11CnH2n+1]2- species, in which H+ is electrostatically bound to the dianion. High flux ion soft-landing was performed to co-deposit [B12X11]- and complex organic molecules (phthalates) in thin layers on surfaces. Molecular structure analysis of the product films revealed that C-H functionalization by [B12X11]- occured in the presence of other more reactive functional groups. This observation demonstrates the utility of highly reactive fragment ions for defined bond formation processes and may pave the way to the use of gas phase ion chemistry for chemical synthesis in the condensed phase.

Warneke, Jonas↗
DOE OSTI2018

Structural basis for the second step of group II intron splicing

The group II intron and the spliceosome share a common active site architecture and are thought to be evolutionarily related. Here we report the 3.7 Å crystal structure of a eukaryotic group II intron in the lariat-3' exon form, immediately preceding the second step of splicing, analogous to the spliceosomal P complex. This structure reveals the location of the intact 3' splice site within the catalytic core of the group II intron. The 3'-OH of the 5' exon is positioned in close proximity to the 3' splice site for nucleophilic attack and exon ligation. The active site undergoes conformational rearrangements with the catalytic triplex having different configurations before and after the second step of splicing. We describe a complete model for the second step of group II intron splicing that incorporates a dynamic catalytic triplex being responsible for creating the binding pocket for 3' splice site capture.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2015

An insight into the origin of low-symmetry bridging phase and enhanced functionality in systems containing competing phases

High piezoelectric activity of ferroelectrics with morphotropic phase boundary (MPB) compositions has been the focus of numerous recent investigations. The concept of a bridging low-symmetry phase between competing phase structures of the MPB composition remains controversial due to the compositional inhomogeneity near the MPB and the lack of appropriate experimental techniques to delineate the complex crystal structures. We have studied a simple ferroelectric BaTiO 3 by employing a high resolution synchrotron-based technique, in which the formation of different symmetry regions due to chemical inhomogeneity can be ruled out. As a result, we observed two types of thermotropic phase boundaries, revealing the importance of interphase-strain in the formation of a bridging phase between competing phases and the enhancement of functionality.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

Embedded Sensor Development in Metallic Structures for the Transformational Challenge Reactor

The ability to make minimally intrusive measurements of process conditions has tremendous potential for improving system performance and control in applications such as nuclear power generation. Towards this end, emerging and evolving advanced manufacturing methods, such as additive manufacturing, present new opportunities for more seamlessly integrating sensing with structure. This technical report summarizes the progress of work performed to assess the feasibility of embedding commercial off-the-shelf (COTS) sensors in a metallic reactor core using advanced manufacturing methods. The progress of four research and development tasks are documented: 1) A survey of COTS sensors for nuclear applications that are candidates for embedded fabrication, 2) Development of a conceptual framework for investigating the feasibility of sensor embedment, 3) Definition of structural geometries and other characteristics that will represent compelling proof-of-concept, and 4) Preliminary prototyping of embedded sensors. For the purposes of this initial study, nuclear grade K-type thermocouples were selected for investigation of embedment methodologies. This sensor was selected as an initial candidate because it represents one of the simplest sensor configurations that can provide useful process information. A selective laser melting (SLM) additive manufacturing process was used to fabricate structures with complexity representative of the core design of the transformational challenge reactor (TCR) and methods were developed to embed a thermocouple with a complex two-dimensional routing path. There are many challenges associated with embedding sensors during the additive manufacturing process including securing the sensor in the structure, relocating the part in the additive machine if using a “pick and place” sensor placement method, mitigating the potential for powder contamination, optimizing energy deposition parameters to build as closely as possible around the sensor path and improve structural integrity of the part, and tuning energy deposition to mitigate thermally induced warpage of the sensor and part as well as potential for damaging the sensing device. Preliminary results indicate that it is feasible to integrate the sensor while minimally compromising the structural integrity of the part and preserving sensor performance. This first phase of this work focused on developing a workflow for embedding sensors and controlling energy deposition during the additive manufacturing process to better understand the build characteristics around the sensor. Future work will perform more in-depth characterization of prototype parts using X-ray computed tomography and scanning electron microscopy to better understand fabricated structures, performance testing of embedded sensors in high temperature environments, adding new embedded measurement modalities, embedding devices with dissimilar materials in contact with additive powders, and the development of methods for embedding sensors with three-dimensional routing paths.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2019

Electric Form Factor of the Neutron from Asymmetry Measurements

The overwhelming majority of visible mass in the universe is composed of protons and neutrons, collectively known as nucleons, which are arguably the most important strongly interacting systems to study. A nucleon may naively be thought of as a composite object built out of three non-interacting sub-objects, known as quarks, in the large energy limit; however, the structure of the nucleon is much more complicated, and consequently far richer, than a simple valence-quark picture. There are sea quarks in addition to valence quarks that interact strongly via the exchange of gluons resulting in a complex vacuum structure, and the collective system must give rise to the observed properties of the nucleon, e.g. the radius and mass. The nucleon is the most well-studied hadron and yet there are still unresolved complexities in the calculation of properties from first principles of QCD; this represents a central problem in nuclear physics. The theoretical difficulty with the nucleon requires experimentation, which is steadily increasing the knowledge of nucleon structure and the strong interaction. The subject of this thesis pertains to nucleon electromagnetic form factors which are fundamental quantities containing information on the spatial and momentum distributions of charge and current within the nucleon. Nucleon form factors may be accessed through well-understood leading order electromagnetic processes with a leptonic probe, and provide strong constraints on testing non-perturbative QCD and nuclear structure models. The form factor ratio of the neutron has been extracted via a beam-target helicity asymmetry measurement. The Jefferson Lab Hall A experiment E02-013 ran in 2006 utilizing the 6 GeV CEBAF for its high-duty, longitudinally polarized electron beam. The double-arm coincidence experiment detected the quasielastically scattered electrons in a large angular and momentum acceptance spectrometer. The recoiling nucleons were detected and momentum analyzed in a large scintillator-iron based neutron detector. The analysis of a previously unpublished extraction of the electric form factor of the neutron is presented.

Obrecht, Richard↗
DOE OSTI2018

Influence of Chemistry and Misfit Dislocation Structure on Dopant Segregation at Complex Oxide Heterointerfaces

Complex oxide heterostructures and thin films have emerged as promising candidates for diverse applications. Lattice mismatch between the two oxides lead to the formation of misfit dislocations, which influence vital material features. Trivalent dopant segregation to misfit dislocations at semi-coherent oxide heterointerfaces, while not well understood, is anticipated to impact interface-governed properties. Atomistic simulations elucidating the influence of misfit dislocations on dopant segregation at SrTiO 3 /MgO heterointerfaces are reported. SrO- and TiO 2 -terminated interfaces that have differing misfit dislocation structure were considered for trivalent dopants segregation. At SrO-terminated interface, dopants tend to segregate toward but not precisely to the heterointerface, whereas at TiO 2 -terminated interface, dopants exhibit a thermodynamic preference to accumulate at the heterointerface. Most favorable segregation sites at SrO-terminated interface are located within the coherent terrace, whereas those at TiO 2 -terminated interface are at misfit dislocation intersections. Atomic layer chemistry and the resulting misfit dislocation structure at the heterointerface, along with concomitant strain at the heterointerface due to mismatched dopants, play a critical role in influencing the observed trends for dopant segregation. Overall, the present results offer a fundamental atomic scale perspective of dopant behavior at semi-coherent complex oxide heterointerfaces and the interplay between dopant chemistry, interface chemistry, and misfit dislocation structure.

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

Tuning the microstructures of decavanadate-based supramolecular hybrids via regularly changing the spacers of bis(triazole) ligands

With tuning the ligands from bte, btp, btb to bth, four new decavanadate-based metal–organic hybrid compounds, [Zn(bte)(H{sub 2}O){sub 4}][Zn{sub 2}(bte)(H{sub 2}O){sub 10}](V{sub 10}O{sub 28})·8H{sub 2}O, [Zn{sub 2}(btp){sub 4}(H{sub 2}O){sub 6}](H{sub 2}V{sub 10}O{sub 28})·4H{sub 2}O, [Zn(H{sub 2}O){sub 6}][Zn{sub 2}(btb){sub 2}V{sub 10}O{sub 28}(H{sub 2}O){sub 6}]·4H{sub 2}O, and [Zn{sub 2}(bth)(H{sub 2}O){sub 10}](H{sub 2}V{sub 10}O{sub 28})·6H{sub 2}O (bte=1,2-bis(1,2,4-triazol-1-yl)ethane, btp=1,3-bis(1,2,4-triazol-1-y1)propane, btb=1,4-bis(1,2,4-triazol-1-y1)butane, bth=1,6-bis(1,2,4-triazol-1-y1)hexane), have been synthesized under conventional conditions. The four compounds represent the first examples of decavanadate-based metal–organic hybrids constructed by Zn–bis(triazole) complexes. Their structural analyses show that the four compounds possess different Zn–bis(triazole) structural motifs and various finally structures, which verifies that regular changing the spacers of ligands is an effective strategy to tuning the structures of polyoxometalate-based hybrids. Also, the electrochemical studies show that the compounds have good electrocatalytic activities towards oxidation of nitrite molecules ascribed to V-centers. - Graphical abstract: Four compounds representing the first examples of V{sub 10}O{sub 28}-based hybrids constructed by Zn–bis(triazole) complexes have been synthesized by changing the spacers of the ligands and their electrocatalytic properties have been investigated. - Highlights: • The first examples of V{sub 10}O{sub 28}-based hybrids constructed by Zn-bis(triazole) complexes. • Verifying that changing the spacers of ligands is a strategy to tuning structures. • Showing good electrocatalytic activities toward oxidation of nitrite molecules.

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

Affinity propagation clustering of full-field, high-spatial-dimensional measurements for robust output-only modal identification: A proof-of-concept study

Determination of the model order is a challenging problem in system identification, especially in output-only or operational modal identification where some modes are weakly excited. While existing methods such as the stabilization diagram method (spectral information) are effective, they do not scale to high-dimensional data, which is usually needed for high-fidelity characterization of structural dynamics and has been made available in the emerging full-field measurement techniques using optical methods such as photogrammetry and laser vibrometers. In this proof-of-concept study we present a new non-parametric, data-driven approach for robust output-only identification of high-spatial-dimensional modal parameters of basic structures by efficiently processing and interactively exploiting the full-field measurement (i.e., very dense spatial measurement points). Specifically, we first over-estimate the system model once, producing a pool of candidate modes associated with their modal frequencies and full-field, high-spatial-dimensional mode shapes. This is accomplished by a data-driven method termed affinity propagation clustering (APC), where the active clusters, which are the active modes in our formulations, emerge from the "message-passing" procedure and does not require a pre-determination of the cluster number (mode or model order). Next, rather than using the spectral information to distinguish the physical and spurious modes in the stabilization diagram method, we exploit and visualize the spatial, full-field mode shape associated with each candidate mode to do so. We conduct extensive experiments on basic structural models with comparisons to a few existing methods. The results indicate that the new method is computationally efficient for identifying high-spatial-dimensional modal parameters, and robust to identify weak modes by exploiting the full-field measurement. We also discuss its applicability and limitations for structures with complex geometry (shapes).

42 ENGINEERING↗
DOE OSTI2015

Crystal structure of a mononuclear Ru II complex with a back-to-back terpyridine ligand: [RuCl(bpy)(tpy–tpy)] +

We report the structural characterization of [6',6''-bis(pyridin-2-yl)-2,2':4',4'':2'',2''-quaterpyridine](2,2'-bipyridine)chloridoruthenium(II) hexafluoridophosphate, [RuCl(C 10 H 8 N 2 )(C 30 H 20 N 6 )]PF 6 , which contains the bidentate ligand 2,2'-bipyridine (bpy) and the tridendate ligand 6',6''-bis(pyridin-2-yl)-2,2':4',4'':2'',2'''-quaterpyridine (tpy–tpy). The [RuCl(bpy)(tpy–tpy)] + monocation has a distorted octahedral geometry at the central Ru II ion due to the restricted bite angle [159.32 (16)°] of the tridendate ligand. The Ru-bound tpy and bpy moieties are nearly planar and essentially perpendicular to each other with a dihedral angle of 89.78 (11)° between the least-squares planes. The lengths of the two Ru—N bonds for bpy are 2.028 (4) and 2.075 (4) Å, with the shorter bond being opposite to Ru—Cl. For tpy–tpy, the mean Ru—N distance involving the outer N atoms trans to each other is 2.053 (8) Å, whereas the length of the much shorter bond involving the central N atom is 1.936 (4) Å. The Ru—Cl distance is 2.3982 (16) Å. The free uncoordinated moiety of tpy–tpy adopts a trans,trans conformation about the interannular C—C bonds, with adjacent pyridyl rings being only approximately coplanar. The crystal packing shows significant π–π stacking interactions based on tpy–tpy. The crystal structure reported here is the first for a tpy–tpy complex of ruthenium.

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

Novel Fast Cure Silicone Inks for Single-Step, Support-Free 3D Printing of Tall, Overhanging, and High Aspect Ratio Structures

Silicone elastomers have a broad variety of applications, such as soft robotics, biomedical devices, and structural metamaterials. The extrusion-based method known as direct ink write (DIW) has enabled the production of additively manufactured silicone structures. However, this method is limited to manufacturing mostly planar or pseudo-3D structures. Due to the low self-supporting capabilities of extruded strands for traditional silicone-based “inks,” obtaining tall or overhanging structures, or structures comprised by thin walls is not feasible. Here, in this study, a novel Fast Cure silicone-based ink is demonstrated that enables manufacturing of complex 3D structures. The Fast Cure ink is a two-part mixture and silicone structures are produced by inline mixing and coextrusion of a part containing a catalyst (part A) and a part containing a crosslinker (part B). By the virtue of crosslinking, the extruded strands rapidly rigidize, increasing their self-supportive capacity. Hence, structures can be obtained with superior shape retention and previously unobtainable parts are realized that are tall, with aspect ratios higher than 3, and have overhanging features, achieving inclination angles smaller than 35° with respect to the printing plane. These minimal sag parts are achieved without requiring extra curing or mechanisms, support structures, or suspension baths.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Coexistence of tunable Weyl points and topological nodal lines in ternary transition-metal telluride TaIrT e 4

Here we report a combined theoretical and experimental study on TaIrTe 4 , a potential candidate for a minimal model of type-II Weyl semimetals. Unexpectedly, an intriguing node structure with 12 Weyl points and a pair of nodal lines protected by mirror symmetry was found by first-principles calculations. Some signatures of the complex electronic structure, such as topologically nontrivial band crossings and topologically trivial Fermi arcs, are cross-validated by angle-resolved photoemission spectroscopy. Through external strain, the number of Weyl points can be reduced to a theoretical minimum of four, and the appearance of the nodal lines can be switched between different mirror planes in momentum space. The coexistence of switchable Weyl points and nodal lines establishes transition-metal chalcogenides as a unique test ground for topological state characterization and engineering.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Inorganic anion-dependent assembly of zero-, one-, two- and three-dimensional Cu(II)/Ag(I) complexes under the guidance of the HSAB theory: Synthesis, structure, and magnetic property

To systematically explore the influence of inorganic anions on building coordination complexes, five novel complexes based on 1-(benzotriazole-1-methyl)−2-propylimidazole (bpmi), [Cu(bpmi){sub 2}(Ac){sub 2}]·H{sub 2}O (1), [Cu(bpmi){sub 2}(H{sub 2}O){sub 2}]·2NO{sub 3}·2H{sub 2}O (2), [Cu(bpmi)(N{sub 3}){sub 2}] (3), [Ag(bpmi)(NO{sub 3})] (4) and [Cu{sub 3}(bpmi){sub 2}(SCN){sub 4}(DMF)] (5) (Ac{sup −}=CH{sub 3}COO{sup −}, DMF=N,N-Dimethylformamide) are synthesized through rationally introducing Cu(II) salts and Ag(I) salt with different inorganic anions. X-ray single-crystal analyses reveal that these complexes show interesting structural features from mononuclear (1), one-dimensional (2 and 3), two-dimensional (4) to three-dimensional (5) under the influence of inorganic anions with different basicities. The structural variation can be explained by the hard-soft-acid-base (HSAB) theory. Magnetic susceptibility measurement indicates that complex 3 exhibits an antiferromagnetic coupling between adjacent Cu(II) ions. - Graphical abstract: Five new Cu(II)/Ag(I) complexes show interesting structural features from mononuclear, one-dimension, two-dimension to three-dimension under the influence of inorganic anions. The structural variation can be explained by the HSAB theory. - Highlights: • Five inorganic anion-dependent complexes are synthesized. • Structural variation can be explained by the hard-soft-acid-base (HSAB) theory. • The magnetic property of complex has been studied.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗