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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 163 records · Page 9
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Direct observations and characterization of crack closure during microstructurally small fatigue crack growth via in-situ high-energy X-ray characterization

This study provides direct observation of the crack closure mechanism of a naturally occurring, tortuous, 3D microstructurally small fatigue crack (SFC) in additively manufactured Inconel 718. In-situ non-destructive characterization is performed using high-energy X-ray diffraction techniques to capture the evolution of the 3D microstructure and micromechanical response in the vicinity of the crack front. Based on the stress state of twelve grains analyzed at the crack tip, the crack closure events of the SFC front was found to be spatially heterogeneous with respect to loading progression governed by the local stress state of the grains (specifically the stress reversal from compression to tension). From this analysis, three grains that displayed different degrees of crack closure were further investigated, based on the orientation of the crack relative to the grains and the associated modality of crack growth. The stress normal to the crack plane and the associated degree of Mode I crack behavior were correlated with events of the crack opening earlier during the loading cycle. This was further corroborated by diffraction spot spreading analysis that quantified the crystallographic lattice distortion caused by the opening crack. Additionally, the detailed characterization of the opening behavior of the grains located at the crack tip and their associated states of stress elucidates the mechanism governing crack closure and will inform future modeling efforts of this phenomenon.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Microstructure and water absorption of ancient concrete from Pompeii: An integrated synchrotron microtomography and neutron radiography characterization

There is renewed interest in using advanced techniques to characterize ancient Roman concrete due to its exceptional durability and low-carbon footprint. In the present work, samples were drilled from the “Hospitium” in Pompeii and were analyzed by synchrotron microtomography (μCT) and neutron radiography to study how the microstructure, including the presence of induced cracks, affects their water adsorption. The water distribution and absorptivity were quantified by neutron radiography. The 3D crack propagation, pore size distribution and orientation, tortuosity, and connectivity were analyzed from μCT results using advanced imaging methods. Porosity was also measured by mercury intrusion porosimetry (MIP) as a reference. Ductile fracture patterns were observed once cracks were introduced. Compared to Portland cement mortar/concrete, the Pompeii samples had relatively high porosity, low connectivity, and a similar coefficient of capillary penetration. In addition, permeability was predicted from models based on percolation theory and pore structure data to evaluate the fluid transport properties. Understanding the microstructure of ancient Pompeii concrete is important because it could inspire the development of modern concrete with high durability.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Synthesis and characterization of redox-active ferric nontronite

Heterogeneous redox reactions on clay mineral surfaces control mobility and bioavailability of redox-sensitive nutrients and contaminants. Iron (Fe) residing in clay mineral structures can either catalyze or directly participate in redox reactions; however, chemical controls over its reactivity are not fully understood. In our previous work we demonstrated that converting a minor portion of Fe(III) to Fe(II) (partial reduction) in the octahedral sheet of natural Fe-rich clay mineral nontronite (NAu-1) activates its surface, making it redox-active. In this study we produced and characterized synthetic ferric nontronite (SIP), highlighting structural and chemical similarities and differences between this synthetic nontronite and its natural counterpart NAu-1, and probed whether mineral surface is redox-active by reacting it with arsenic As(III) under oxic and anoxic conditions. We demonstrate that synthetic nontronite SIP undergoes the same activation as natural nontronite NAu-1 following the partial reduction treatment. Similar to NAu-1, SIP oxidized As(III) to As(V) under both oxic (catalytic pathway) and anoxic (direct oxidation) conditions. The similar reactivity trends observed for synthetic nontronite and its natural counterpart make SIP an appropriate analog for laboratory studies. The development of chemically pure analogs for ubiquitous soil minerals will allow for systematic research of the fundamental properties of these minerals.

Environmental Molecular Sciences Laboratory↗
DOE OSTI2017

Characterization of upgraded fast pyrolysis oak oil distillate fractions from sulfided and non-sulfided catalytic hydrotreating

Catalytic hydroprocessing of pyrolysis oils from biomass produces hydrocarbons that can be considered for liquid fuel production. This process requires removal of oxygen and cracking of the heavier molecular weight bio-oil constituents into smaller fragments at high temperatures and pressures under hydrogen. A comprehensive understanding of product oils is useful to optimize cost versus degree of deoxygenation. Additionally, a better understanding of the chemical composition of the distillate fractions can open up other uses of upgraded oils for potentially higher-value chemical streams. We present in this paper the characterization data for five well-defined distillate fractions of two hydroprocessed oils with different oxygen levels: a low oxygen content (LOC, 1.8% O, wet basis) oil and a medium oxygen content (MOC, 6.4% O, wet basis) oil. Elemental analysis and 13C NMR results suggest that the distillate fractions become more aromatic/unsaturated as they become heavier. Our results also show that the use of sulfided catalysts directly affects the S content of the lightest distillate fraction. Carbonyl and carboxylic groups were found in the MOC light fractions, while phenols were present in the heavier fractions for both MOC and LOC. PIONA analysis of the light LOC fraction shows a predominance of paraffins with a minor amount of olefins. These results can be used to direct future research on refinery integration and production of value-added product from specific upgraded oil streams.

biofuel↗
DOE OSTI2015

Nanoscale building blocks in a novel lithium arsenotungsten bronze: Synthesis and characterization

We report on a novel compound Li{sub 3}AsW{sub 7}O{sub 25} obtained by solid-state reaction and characterized by diffraction and spectroscopic methods. The bronze-type compound crystallizes in the orthorhombic space group Pbca with a=724.38(3) pm, b=1008.15(4) pm, c=4906.16(17) pm and Z=8. The structure is built up by chains of WO{sub 6} octahedra interconnected by AsO{sub 4} tetrahedra and WO{sub 6} octahedra forming a polyhedral arrangement as seen in intergrowth tungsten bronzes. The X-ray single crystal structure refinement allows solving the complex arsenotungstate framework. The powder neutron diffraction data analysis locates the lithium atoms. Thermal analysis showed that Li{sub 3}AsW{sub 7}O{sub 25} is stable up to its melting at 1135(3) K followed by a decomposition at 1182(5) K. The Kubelka–Munk treatment of the UV–vis spectrum revealed a wide band gap in the range of 2.84–3.40 eV depending on the presumed electron transition type. - Graphical abstract: Crystal structure of Li{sub 3}AsW{sub 7}O{sub 25} showing different schematic components. - Highlights: • A report on a novel compound Li{sub 3}AsW{sub 7}O{sub 25} obtained by solid-state reaction. • Chains and nano-blocks of WO{sub 6} octahedra and AsO{sub 4} tetrahedra formed a structure like intergrowth tungsten bronzes. • X-ray diffraction allowed solving the complex arsenotungstate framework. • Powder neutron diffraction data analysis locates the lithium atoms. • UV–vis spectrum revealed the band-gap.

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

Synthesis and characterization of new fluoride-containing manganese vanadates A{sub 2}Mn{sub 2}V{sub 2}O{sub 7}F{sub 2} (A=Rb, Cs) and Mn{sub 2}VO{sub 4}F

Large single crystals of A{sub 2}Mn{sub 2}V{sub 2}O{sub 7}F{sub 2} (A=Rb, Cs) and Mn{sub 2}VO{sub 4}F were grown using a high-temperature (~600 °C) hydrothermal technique. Single crystal X-ray diffraction and powder X-ray diffraction were utilized to characterize the structures, which both possess MnO{sub 4}F{sub 2} building blocks. The A{sub 2}Mn{sub 2}V{sub 2}O{sub 7}F{sub 2} series crystallizes as a new structure type in space group Pbcn (No. 60), Z=4 (Rb{sub 2}Mn{sub 2}V{sub 2}O{sub 7}F{sub 2}: a=7.4389(17) Å, b=11.574(3) Å, c=10.914(2) Å; Cs{sub 2}Mn{sub 2}V{sub 2}O{sub 7}F{sub 2}: a=7.5615(15) Å, b=11.745(2) Å, c=11.127(2) Å). The structure is composed of zigzag chains of edge-sharing MnO{sub 4}F{sub 2} units running along the a-axis, and interconnected through V{sub 2}O{sub 7} pyrovanadate groups. Temperature dependent magnetic susceptibility measurements on this interesting one-dimensional structural feature based on Mn{sup 2+} indicated that Cs{sub 2}Mn{sub 2}V{sub 2}O{sub 7}F{sub 2} is antiferromagnetic with a Neél temperature, T{sub N}=~3 K and a Weiss constant, θ, of −11.7(1) K. Raman and infrared spectra were also analyzed to identify the fundamental V–O vibrational modes in Cs{sub 2}Mn{sub 2}V{sub 2}O{sub 7}F{sub 2}. Mn{sub 2}(VO{sub 4})F crystalizes in the monoclinic space group of C2/c (no. 15), Z=8 with unit cell parameters of a=13.559(2) Å, b=6.8036(7) Å, c=10.1408(13) Å and β=116.16(3)°. The structure is associated with those of triplite and wagnerite. Dynamic fluorine disorder gives rise to complex alternating chains of five-and six-coordinate Mn{sup 2+}. These interpenetrating chains are additionally connected through isolated VO{sub 4} tetrahedra to form the condensed structure. - Graphical abstract: New vanadate fluorides A{sub 2}Mn{sub 2}V{sub 2}O{sub 7}F{sub 2} (A=Rb, Cs) and Mn{sub 2}(VO{sub 4})F have been synthesized hydrothermally. Upon cooling, the one-dimensional Mn(II) substructure results in antiferromagnetic ordering. Display Omitted - Highlights: • Single crystals of A{sub 2}Mn{sub 2}V{sub 2}O{sub 7}F{sub 2}, (A=Rb, Cs) and Mn{sub 2}VO{sub 4}F were grown hydrothermally. • The use of fluoride mineralizers in the synthesis led to the formation of new compounds without OH{sup −} groups. • The structure of A{sub 2}Mn{sub 2}V{sub 2}O{sub 7}F{sub 2} features zigzag chains of MnO{sub 4}F{sub 2} units. • Cs{sub 2}Mn{sub 2}V{sub 2}O{sub 7}F{sub 2} exhibits antiferromagnetic ordering with a Neel temperature of ~3 K. • Mn{sub 2}VO{sub 4}F possesses a condensed framework structure with disordered fluorine atoms.

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

Characterizing the nano-structure and defect structure of nano-scaled non-ferrous structural alloys

The presence and interaction of nanotwins, geometrically necessary dislocations, and grain boundaries play a key role in the mechanical properties of nanostructured crystalline materials. Therefore, it is vital to determine the orientation, width and distance of nanotwins, the angle and axis of grain boundary misorientations as well as the type and the distributions of dislocations in an automatic and statistically meaningful fashion in a relatively large area. In this paper, such details are provided using a transmission electron microscope-based orientation microscopy technique called ASTAR™/precession electron diffraction. The remarkable spatial resolution of this technique (~ 2 nm) enables highly detailed characterization of nanotwins, grain boundaries and the configuration of dislocations. This orientation microscopy technique provides the raw data required for the determination of these parameters. The procedures to post-process the ASTAR™/PED datasets in order to obtain the important (and currently largely hidden) details of nanotwins as well as quantifications of dislocation density distributions are described in this study. - Highlights: • EBSD cannot characterize defects such as dislocations, grain boundaries and nanotwins in severely deformed metals. • TEM based orientation microscopy technique called ASTAR™/PED was used to resolve the problem. • Locations and orientations of nanotwins, dislocation density distribution and grain boundary characters can be resolved. • This work provides the bases for further studies on the interactions between dislocations, grain boundaries and nanotwins. • The computation part is explained sufficiently which helps the readers to post process their own data.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Three dimensional microstructural characterization of nanoscale precipitates in AA7075-T651 by focused ion beam (FIB) tomography

The size and distribution of precipitates in Al 7075 alloys affects both the mechanical and corrosion behavior (including stress corrosion cracking and fatigue corrosion) of the alloy. Three dimensional (3D) quantitative microstructural analysis of Al 7075 in the peak aged condition (T651) allows for a better understanding of these behaviors. In this study, Focused ion beam (FIB) tomography was used to characterize the microstructure in three dimensions. Analysis of grains and precipitates was performed in terms of volume, size, and morphology. It was found that the precipitates at the grain boundaries are larger in size, higher in aspect ratios and maximum Feret diameter compared to the precipitates inside the grains, due to earlier nucleation of the precipitates at the grain boundaries. Our data on the precipitates at the interface between grains and Mg{sub 2}Si inclusion show that the surfaces of inclusion (impurity) particles can serve as a location for heterogeneous nucleation of precipitates. - Highlights: •Focused ion beam (FIB) tomography was used to characterize the microstructure of Al 7075 in three dimensions. •Analysis of grains and precipitates was performed in terms of volume, size, and morphology. •Precipitates at the grain boundaries have larger size and aspect ratio compared to the precipitates inside the grains.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Characterization of as-welded microstructure of heat-affected zone in modified 9Cr–1Mo–V–Nb steel weldment

Non-equilibrium microstructure of the heat-affected zone (HAZ) in the as-welded modified 9Cr–1Mo–V–Nb pipe steel (P91) weldment deposited by gas tungsten arc welding (GTAW) and flux core arc welding (FCAW) has been characterized by field-emission scanning electron microscope (FESEM) and electron backscatter diffraction (EBSD). The heterogeneous structures in the sub-layers of the as-welded HAZ are attributable to phase transformations caused by the welding thermal cycles and the local structure variations in the as-received base metal. Coarse-grained heat-affected zone (CGHAZ) has a prior austenite grain (PAG) size of 20 μm. Fine uniformly-distributed precipitates and a higher fraction of MX carbonitrides are observed in the CGHAZ. Fine-grained heat-affected zone (FGHAZ) consists of the finest grains (1.22 μm measured by EBSD, 5 μm PAG size), coarse undissolved M{sub 23}C{sub 6} carbides within the PAG boundaries and fine nucleated M{sub 23}C{sub 6} particles within the martensite laths. Inter-critical heat-affected zone (ICHAZ) consists of partially austenitized grains and over-tempered martensite laths. EBSD kernel average misorientation (KAM) map in the FGHAZ close to the ICHAZ illustrates the greatest local strain variations with a moderate normalized KAM value of 0.92°. The majority (88.1%) of the matrix grains in the CGHAZ are classified as deformed grains by EBSD grain average misorientation (GAM) evaluation. The FGHAZ close to the ICHAZ has the most recrystallized grains with an area fraction of 14.4%. The highest density variation of precipitates within grains in the FGHAZ originates from the inhomogeneous chemistry in the base metal. - Highlights: •A comprehensive characterization of the as-welded HAZ of P91 weldment is conducted. •Structural features in the each layer of the HAZ are quantified by EBSD. •Structural heterogenities in HAZ are due to welding cycle and base metal structure. •FGHAZ contains the finest grain structure and largest precipitate density variation.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Dynamic shear localization of a titanium alloy under high-rate tension characterized by x-ray digital image correlation

Highlights: • First systematic error analyses for XDIC • First XDIC study of Ti-6Al-4V under dynamic tension • Deformation mode transition induces dynamic ductility decrease. • Dynamic shear localization due to rate-dependent microvoid coalescence process. - Abstract: Dynamic and quasi-static tension experiments are conducted on Ti-6Al-4V alloys, with in situ, synchrotron-based, high-speed, x-ray phase contrast imaging implemented to characterize the dynamic deformation and fracture process of Ti alloys at the Advanced Photon Source. X-ray digital imaging correlation (XDIC) is applied for strain field mapping. The size distribution of x-ray speckles are quantified via a morphological analysis, with a mean of ∼20 μm. Systematic error analyses of displacement and strain field measurements are firstly conducted for XDIC, and demonstrate that the displacement and strain errors can be controlled below 0.01 pixel and 0.1%, respectively. Mesoscale strain characteristics measured via XDIC are consistent with and reveal mechanisms for the bulk-scale stress–strain responses. Under dynamic tension, a sharp transition to strain softening occurs when the bulk strain exceeds about 0.04, which leads to a lower dynamic fracture strain (0.08) than the quasi-static one (0.1). The corresponding strain filed mapping demonstrates that shear deformation localizations grow and coalesce rapidly into a narrow shear deformation band under dynamic loading, while tensile deformation and necking progresses gradually under quasi-static loading. Scanning electron microscopy shows that void nucleation occurs mainly at the interface of α and β phases for both quasi-static and dynamic tension. However, microvoids coalesce preferentially along colony boundaries or the boundary α phase under quasi-static tension, but along the maximum shear stress direction (across colonies) under dynamic tension. Fractography of recovered samples also shows consistent features.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Detector Characterization for Quantitative Spectral Radiography of Uranium Powder Samples

Pacific Northwest National Laboratory (PNNL) is developing a prototype spectral x-ray radiography (SpecX) non-destructive assay system for noninvasive material mass quantification of uranium-bearing powders. The SpecX system uses a custom material estimation algorithm, which requires a high-fidelity pixel-by-pixel detector response model for accurate quantification. We performed a detailed characterization and built a model of a High-Energy X-ray Imaging Technology (HEXITEC) CdTe pixelated spectral detector. Here we present the detector characterization which led to that model, including a determination of the pixel-wise energy calibration, the detection efficiency, the detector uniformity, the detector stability, and a comparison of methods to remove charge-shared events.

spectral X-ray radiography, pixelated detector, ca↗
DOE OSTI2017

Characterizing the lipid and metabolite changes associated with placental function and pregnancy complications using ion mobility spectrometry-mass spectrometry and mass spectrometry imaging

Successful pregnancy is dependent upon discrete biological events, which include embryo implantation, decidualization, and placentation. Problems associated with each of these events can cause infertility or conditions such as preeclampsia. A greater understanding of the molecular changes associated with these complex processes is necessary to aid in identifying treatments for each condition. Previous nuclear magnetic resonance spectroscopy and mass spectrometry studies have been used to identify metabolites and lipids associated with pregnancy-related complications. However, due to limitations associated with conventional implementations of both techniques, novel technology developments are needed to more fully understand the initiation and development of pregnancy related problems at the molecular level. In this perspective, we describe current analytical techniques for metabolomic and lipidomic characterization of pregnancy complications and discuss the potential for new technologies such as ion mobility spectrometry-mass spectrometry and mass spectrometry imaging to contribute to a better understanding of the molecular changes that affect the placenta and pregnancy outcomes.

Environmental Molecular Sciences Laboratory↗
DOE OSTI2016

BEAM: A Computational Workflow System for Managing and Modeling Material Characterization Data in HPC Environments

Improvements in scientific instrumentation allow imaging at mesoscopic to atomic length scales, many spectroscopic modes, and now—with the rise of multimodal acquisition systems and the associated processing capability—the era of multidimensional, informationally dense data sets has arrived. Technical issues in these combinatorial scientific fields are exacerbated by computational challenges best summarized as a necessity for drastic improvement in the capability to transfer, store, and analyze large volumes of data. The Bellerophon Environment for Analysis of Materials (BEAM) platform provides material scientists the capability to directly leverage the integrated computational and analytical power of High Performance Computing (HPC) to perform scalable data analysis and simulation via an intuitive, cross-platform client user interface. This framework delivers authenticated, “push-button” execution of complex user workflows that deploy data analysis algorithms and computational simulations utilizing the converged compute-and-data infrastructure at Oak Ridge National Laboratory's (ORNL) Compute and Data Environment for Science (CADES) and HPC environments like Titan at the Oak Ridge Leadership Computing Facility (OLCF). In this work we address the underlying HPC needs for characterization in the material science community, elaborate how BEAM's design and infrastructure tackle those needs, and present a small sub-set of user cases where scientists utilized BEAM across a broad range of analytical techniques and analysis modes.

96 KNOWLEDGE MANAGEMENT AND PRESERVATION↗
DOE OSTI2024

Geospatial characterization of low-temperature heating and cooling demand in residential, commercial, manufacturing, agricultural, and data center sectors for potential geothermal applications in the United States

Thermal demand for heating and cooling has been predominantly supplied by fossil fuel combustion in the United States, although low-carbon alternatives are extensively available including geothermal, solar thermal, and waste heat. Here, this study analyzed end-use energy consumption, fuel expenditure, and data center commissioned power data to geospatially characterize the U.S. low-temperature heating and cooling demand at the county level in residential, commercial, manufacturing, agricultural, and data center sectors and understand potential opportunities for geothermal applications. In the analysis, the regional-scale energy consumption data was incorporated with system efficiencies to address actual demand and was then disaggregated with weighting factors to the county level. The results indicated that total low-temperature heating and cooling demand is 16.7 EJ, combining heating demand of 10.8 EJ and cooling demand of 5.9 EJ. Overall, 59.9 % (10 EJ) of the low-temperature heating and cooling demand occurred in the residential sector. The heating and cooling demand visualized in maps represented that the geospatial distribution of heating and cooling demand in the residential and commercial sectors is governed by the number of housing units and climate zone designations, while heating and cooling demand in the manufacturing, agricultural, and data center sectors is dependent on the number and location of facilities. The results also demonstrated that geothermal heat pumps are broadly used in the residential and commercial sectors for heating and cooling in the U.S. Midwest, South, and Northeast regions but are limited in the West, implying great decarbonization potential in the future.

15 GEOTHERMAL ENERGY↗