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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Effect of Carbon Doping on CO 2 –Reduction Activity of Single Cobalt Sites in Graphitic Carbon Nitride

Single atom catalysts have demonstrated interesting activity in a variety of applications. In this study, we prepared single C o2+ sites on graphitic carbon nitride (C 3 N 4 ), which was doped with carbon for enhanced activity in visible-light CO 2 reduction. The synthesized materials were characterized with a variety of techniques, including microscopy, X-ray powder diffraction, UV-vis spectroscopy, infrared spectroscopy, photoluminescence spectroscopy, and X-ray absorption spectroscopy. Here, doping C 3 N 4 with carbon was found to have profound effect on the photocatalytic activity of the single Co 2+ sites. At relatively low levels, carbon doping enhanced the photoresponse of C 3 N 4 in the visible region and improved charge separation upon photoactivation, thereby enhancing the photocatalytic activity. Furthermore, high levels of carbon doping were found to be detrimental to the photocatalytic activity of the single Co 2+ sites by altering the structure of C 3 N 4 and generating defect sites responsible for charge recombination.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2019

The effects of material anisotropy on secondary processing of additively manufactured CoCrMo

Components produced by near net shape additive manufacturing processes often require subsequent subtractive finishing operations to satisfy requisite surface finish and geometric tolerances. It is well established that the microstructure and properties of the as-built component are sensitive to the additive processing history. Therefore, downstream secondary processes may be affected by the as-built components’ mechanical behavior. In this work we study the sensitivity of secondary machining operations on CoCrMo samples produced via laser powder bed fusion. Utilizing novel high-throughput mechanical testing, microstructure characterization, and a rigorous statistical analysis we investigate the degree of material anisotropy present in the as-built material. We then study the effects of this anisotropy on secondary processing via slot milling experiments. Our results indicate that mechanical anisotropy is driven by both the morphology of the microstructure as well as crystallographic texture. Furthermore, the machining force response is correspondingly sensitive to these sources of anisotropy, which has the potential to impact how manufacturers finish additively built parts.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Liquid crystalline behavior and photoluminescence of lanthanide decanoate nanoparticles synthesized by microwave radiation

Luminescent lanthanide decanoate nanoparticles (LnC 10 NPs; Ln = Pr, Nd, Sm, Eu, Gd, Er) with spherical morphology (<100 nm) have been synthesized via a facile microwave (MWV) method using Ln(NO 3 ) 3 ·xH 2 O, ethanol/water, and decanoic acid. These hybrid nanomaterials adopt a lamellar structure consisting of inorganic Ln 3+ layers separated by a decanoate anion bilayer and exhibit liquid crystalline (LC) phases during melting. The particle size, crystalline structure, and LC behavior were characterized using transmission electron microscopy (TEM), differential scanning calorimetry (DSC), and powder X-ray diffraction (ambient and heated). Thermal analysis indicated the formation of Smectic A LC phases by LnC 10 nanoparticles, with the smaller lanthanides (Ln = Sm, Gd, Er) displaying additional solid intermediate and Smectic C phases. The formation of LC phases by the smaller Ln 3+ suggests that these nanoscale materials have vastly different thermal properties than their bulk counterparts, which do not exhibit LC behavior. In this work, photoluminescence spectroscopy revealed the LnC 10 NPs to be highly optically active, producing strong visible emissions that corresponded to expected electronic transitions by the various Ln 3+ ions. Under long-wave UV irradiation (λ = 365 nm), bright visible luminescence was observed for colloidal suspensions of Nd, Sm, Eu, Gd, and ErC 10 NPs. To the best of the authors’ knowledge, this is the first reported synthesis of nanoscale metal alkanoates, the first report of liquid crystalline behavior by any decanoate of lanthanides smaller than Nd, and the first observation of strong visible luminescence by non-vitrified lanthanide alkanoates.

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

Distinctive exchange bias and unusual memory effects in magnetically compensated Pr 0.75 Gd 0.25 ScGe

Tuning the chemistry of materials often leads to discoveries of interesting phenomena that expand basic science and support practical applications. Here we show how different spin–orbit coupling in light and heavy lanthanides can be exploited to create complex magnetic ground states and thereby unusual spontaneous exchange bias (SEB), conventional exchange bias (CEB), and magnetic memory effects in almost ideally magnetically compensated Pr 0.75 Gd 0.25 ScGe, which is a representative of the PrScGe–GdScGe solid solution. We report the synthesis and detailed characterization of Pr 0.75 Gd 0.25 ScGe by X-ray powder diffraction, scanning electron microscopy, and magnetization measurements in magnetic fields up to 140 kOe. Partial substitution of a light lanthanide, Pr, with a heavy lanthanide, Gd, results in a complex magnetic ground state, which includes large spontaneous and conventional exchange biases reaching magnitudes of ~1.7 kOe and ~3.5 kOe, respectively, at T = 2 K, as well as shape dependent magnetic compensation and bias phenomena occurring in small external fields.

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

Crystal-field states and defect levels in candidate quantum spin ice Ce 2 Hf 2 O 7

Here, we report the synthesis of powder and single-crystal samples of cerium pyrohafnate and their characterization using neutron diffraction, thermogravimetry and x-ray absorption spectroscopy. We evaluate the amount of nonmagnetic Ce 4+ defects and use this result to interpret the spectrum of crystal-electric field transitions observed using inelastic neutron scattering. The analysis of these single-ion transitions indicates the dipole-octupole nature of the ground-state doublet and a significant degree of spin-lattice coupling. The single-ion properties calculated from the crystal-electric field parameters obtained spectroscopically are in good agreement with bulk magnetic susceptibility data down to about 1 K. Below this temperature, the behavior of the magnetic susceptibility indicates a correlated regime without showing any sign of magnetic long-range order or freezing down to 0.08 K. We conclude that Ce 2 Hf 2 O 7 is another candidate to investigate exotic correlated states of quantum matter, such as the octupolar quantum spin ice recently argued to exist in the isostructural compounds Ce 2 Sn 2 O 7 and Ce 2 Zr 2 O 7 .

36 MATERIALS SCIENCE↗
DOE OSTI2020

Tailoring Surface Roughness Using Additive Manufacturing to Improve Internal Cooling

Abstract Surface roughness present on internal cooling channels produced with additive manufacturing has been previously shown to augment heat transfer and pressure loss to levels similar to traditionally cast turbulators. Given the ability of the surface roughness to improve the cooling performance of small cooling channels, the question arises on whether there is an optimal combination of random roughness features to maximize internal cooling performance. To investigate this question, test coupons with different surface roughness morphologies and magnitudes were manufactured by manipulating the parameters in the laser powder bed fusion additive manufacturing process. The coupons were tested to characterize the friction factor and Nusselt number of the cooling channels over a range of Reynolds numbers. Results showed that certain roughness combinations outperformed others, increasing the internal cooling performance of the channels. Additionally, manipulation of the performance using the process parameters allowed for reductions in build time, which could be useful for controlling component cost.

Engineering↗
DOE OSTI2021

Raman Microscopy Analysis of Wyoming CarbonSAFE Pilot Well Thin Sections for Mineralogy and Organic Matter Characterization

Scanning confocal Raman microspectroscopy (RMS) was used to analyze thin sections for inorganic mineral content and for evaluation of organic material (OM). Thin sections were selected from a stratigraphic test well core in the Powder River Basin, Wyoming under the Wyoming CarbonSAFE project. The well was analyzed with a variety of rock and fluid characterization techniques to determine the feasibility of a commercial-scale CO2 storage site. RMS complements other analyses, including traditional petrography, SEM, porosity and permeability, and XRD For this aspect of the study, RMS is especially important in the evaluation of OM in sealing lithologies. At prospective geologic CO2 storage sites, it is imperative to assess the unconventional oil and gas potential of seals to ensure that any future development would not compromise the integrity of the seals. Whole-slide mineralogical surveys were performed on thin sections from various shale and sandstone formations. Surveys were analyzed with Direct Classical Least Squares to identify and quantify minerals. The location and concentration of minerals was color-coded and overlaid on optical images for visualization of the distribution of minerals. Dense hyperspectral Raman mapping of OM was performed on five thin sections. Eleven spectral parameters diagnostic of organic type and thermal maturity were used to train a Partial Least Squares (PLS) calibration against a set of artificially matured samples spanning the pre- to mid-oil window. The PLS was applied to the study set and a post-mature set. Additionally, the PLS was applied to each point in hyperspectral maps for visualization of trends in maturity across sample sets and discrimination of organic matter types within a given map. In inorganic surveys on thin sections, a total of 14 unique inorganic minerals were identified in Raman spectra including quartz, dolomite, calcite, hematite and anhydrite. Shale thin sections tended to be dominated by organic material. OM was often observed mixed with inorganic minerals. Sand- and mudstones were dominated by inorganic minerals. The PLS extrapolated the post-mature set to reflectances >1.2%. The study set ranged from very immature to postmature in the median of map fit-peak parameters. However, point maturity maps indicate that matrix OM in all study samples is immature and that discreet organic particles selected for mapping, which may be inertinites, bias medians towards more-mature. The work demonstrates the capabilities of RMS to perform both whole-slide mineralogy and OM analysis with applications to formation evaluation in oil & gas, carbon sequestration and mining. Here, analysis of sealing formations in the well indicates high levels of immature organic matter that would not be a viable target for future oil production that could compromise the CO2 storage site. The work brings together diverse disciplines from geology and petrography to analytical chemistry, big data and microscopy.

Myers, Grant↗
DOE OSTI2020

Combustion of Silane-Hydrogen-Nitrous oxide Mixtures: Analysis of Laminar Flame Propagation and Condensed Products

The laminar burning rate, the explosion pressure, and the pressure rise coefficient have been measured for silane-nitrous oxide-argon mixtures using the spherically expanding flame technique in a constant volume combustion chamber. For these three parameters, the values obtained were higher than for hydrogen-nitrous oxide-argon and typical hydrocarbon-based mixtures. As an example, a maximum burning rate of 1800 g/m 2 s was measured at 101 kPa, whereas under similar conditions, a maximum burning rate around 950 g/m 2 s has been reported for hydrogen-nitrous oxide-argon mixtures. Here, the condensed combustion products formed in the silane-nitrous oxide-argon flames were sampled and characterized using electron micrograph, electronic diffraction, energy-dispersive spectroscopy, and X-ray powder diffraction. For all equivalence ratios, silica spherical particles with a mean diameter in the range 200-300 nm were observed. In addition, for mixtures with Φ ≥2.2, silicon nanowires were formed. X-ray diffraction experiments showed that the silicon nanowires are composed of a material referred to as “metal silicon” characterized by a cubic structure (lattice parameter: a = 5.425 Å) with the Fm-3m space group.

42 ENGINEERING↗
DOE OSTI2022

On a Unified Core Characterization Methodology to Support the Systematic Assessment of Rare Earth Elements and Critical Minerals Bearing Unconventional Carbon Ores and Sedimentary Strata

A significant gap exists in our understanding and ability to predict the spatial occurrence and extent of rare earth elements (REE) and certain critical minerals (CM) in sedimentary strata. This is largely due to a lack of existing, systematic, and well-distributed REE and CM samples and analyses in United States sedimentary basins. In addition, the type of sampling and characterization performed to date has generally lacked the resolution and approach required to constrain geologic and geographic heterogeneities typical of subsurface, mineral resources. Here, we describe a robust and systematic method for collecting core scale characterization data that can be applied to studies on the contextual and spatial attributes, the geologic history, and lithostratigraphy of sedimentary basins. The methods were developed using drilled cores from coal bearing sedimentary strata in the Powder River Basin, Wyoming (PRB). The goal of this effort is to create a unified core characterization methodology to guide systematic collection of key data to achieve a foundation of spatially and geologically constrained REEs and CMs. This guidance covers a range of measurement types and methods that are each useful either individually or in combination to support characterization and delineation of REE and CM occurrences. The methods herein, whether used in part or in full, establish a framework to guide consistent acquisition of geological, geochemical, and geospatial datasets that are key to assessing and validating REE and CM occurrences from geologic sources to support future exploration, assessment, and techno-economic related models and analyses.

54 ENVIRONMENTAL SCIENCES↗
NASA NTRS1984

Rapid solidification and dynamic compaction of Ni-base superalloy powders

A Ni-base superalloy containing 13Al-9Mo-2Ta (in at. percent) has been characterized in both the rapidly solidified condition and after dynamic compaction. Dynamically compacted specimens were examined in the as-compacted condition and observations related to current theories of interparticle bonding. In addition, the recrystallization behavior of the compacted material at relatively low temperature (about 0.5-0.75 Tm) was investigated.

Field, R. D.↗
NASA NTRS2002

Characterization of the Temperature Capabilities of Advanced Disk Alloy ME3

The successful development of an advanced powder metallurgy disk alloy, ME3, was initiated in the NASA High Speed Research/Enabling Propulsion Materials (HSR/EPM) Compressor/Turbine Disk program in cooperation with General Electric Engine Company and Pratt & Whitney Aircraft Engines. This alloy was designed using statistical screening and optimization of composition and processing variables to have extended durability at 1200 F in large disks. Disks of this alloy were produced at the conclusion of the program using a realistic scaled-up disk shape and processing to enable demonstration of these properties. The objective of the Ultra-Efficient Engine Technologies disk program was to assess the mechanical properties of these ME3 disks as functions of temperature in order to estimate the maximum temperature capabilities of this advanced alloy. These disks were sectioned, machined into specimens, and extensively tested. Additional sub-scale disks and blanks were processed and selectively tested to explore the effects of several processing variations on mechanical properties. Results indicate the baseline ME3 alloy and process can produce 1300 to 1350 F temperature capabilities, dependent on detailed disk and engine design property requirements.

Gabb, Timothy P.↗
DOE OSTI2024

Trickier than It Looks: Isomerization between Five- and Six-Coordinated Zinc in Heterometallic Li 2 Zn 2 Molecule

This report describes the synthesis and characterization of two hetero bi metallic Li–Zn coordination isomers [Li 2 Zn 2 (tbaoac) 6 ] (tbaoac = tert -butyl acetoacetato) that have been isolated separately by the same stoichiometric reaction run in different organic solvents. The 6-coordinated zinc isomer ( 6-Zn ) was synthesized in acetone with high yield, while the 5-coordinated one ( 5-Zn ) was readily obtained from ethanol. The 5-Zn isomer has a low solubility in organic solvents such as alkanes and haloalkanes, while its 6-Zn counterpart exhibits a good solubility in almost all common solvents. Two isomeric molecules feature similar centrosymmetric tetranuclear cyclic assemblies, which are different in their arrangement of tbaoac ligands. While all ligands act as μ 2 -type in the structure of 5-Zn , the two tbaoac groups chelating Li appear as μ 3 -type in 6-Zn , thus providing an additional coordination for Zn ions. However, the real structural transformation between these isomers was shown to be more complex than simply making or breaking a couple of Zn–O bonds. X-ray single-crystal structure analysis, powder X-ray diffraction, multinuclear NMR, DART mass spectrometry, ICP-OES analysis, and TGA have been employed for the characterization of the isomers. The combination of powder X-ray diffraction and 1 H NMR investigation revealed that 6-Zn isomer can be quantitatively transformed to 5-Zn in ethanol, while the reverse conversion instantly takes place in acetone.

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

The homometallic warwickite V{sub 2}OBO{sub 3}

Highlights: • New mixed valent vanadium borate. • Multiple phase transitions on cooling. • High resolution synchrotron powder X-ray diffraction data. - Abstract: The synthesis, structure and elementary magnetic characterization of the homometallic warwickite V{sub 2}OBO{sub 3} are reported. The material adopts the orthorhombic warwickite structure type at room temperature, space group Pnma (No. 62) with lattice parameters a = 9.2317(1) Å, b = 3.1172(1) Å, and c = 9.5313(1) Å. Temperature-dependent magnetic susceptibility, electrical resistivity, and specific heat measurements show anomalies near 35 K, between 135 K and 150 K, and near 260 K, with the transition at ~ 35 K likely to a ferrimagnetic state. High resolution synchrotron powder X-ray diffraction data at temperatures between 295 K and 90 K display significant peak splitting upon cooling, indicating that at least one crystallographic symmetry change occurs at low temperatures.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1987

Thermo-oxidatively stable condensation polyimides containing 1,1,1-triaryl-2,2,2-trifluoroethane dianhydride and diamine monomers

Nine new condensation polyimides containing the trifluorophenylethylidene linkage were synthesized by the amic-acid route. Several other polyimides, including some with the hexafluoroisopropylidene linkage, were also prepared as controls. Amic-acid solutions were characterized by determining their inherent viscosities prior to thermal conversion into polyimide films. Glass transition temperatures (T sug g), thermogravimetric analysis (TGA), and isothermal weight loss data were obtained for the films. The films were pulverized into molding powders which, in turn, were thermally processed under pressure into neat resin discs. The discs were also characterized by T sub gs and 316 C and 371 C isothermal weight losses. The film study identified two new polyimides with T sub gs greater that 371 C and two new polyimides with low rates of weight loss. The resin discs exhibited the same overall trends in T sub g and weight loss as the respective films, however the weight loss per unit surface area was always greater, presumably due to voids or to mechanical degradation induced during preparation of the molding powders.

Alston, William B.↗
DOE OSTI2023

Background optimization of powder electron diffraction for implementation of the e-PDF technique and study of the local structure of iron oxide nanocrystals

The local structural characterization of iron oxide nanoparticles is explored using a total scattering analysis method known as pair distribution function (PDF) (also known as reduced density function) analysis. The PDF profiles are derived from background-corrected powder electron diffraction patterns (the e-PDF technique). Due to the strong Coulombic interaction between the electron beam and the sample, electron diffraction generally leads to multiple scattering, causing redistribution of intensities towards higher scattering angles and an increased background in the diffraction profile. In addition to this, the electron–specimen interaction gives rise to an undesirable inelastic scattering signal that contributes primarily to the background. The present work demonstrates the efficacy of a pre-treatment of the underlying complex background function, which is a combination of both incoherent multiple and inelastic scatterings that cannot be identical for different electron beam energies. Therefore, two different background subtraction approaches are proposed for the electron diffraction patterns acquired at 80 kV and 300 kV beam energies. From the least-square refinement (small-box modelling), both approaches are found to be very promising, leading to a successful implementation of the e-PDF technique to study the local structure of the considered nanomaterial.

36 MATERIALS SCIENCE↗
NASA NTRS2017

Development and Hot-fire Testing of Additively Manufactured Copper Combustion Chambers for Liquid Rocket Engine Applications

NASA and industry partners are working towards fabrication process development to reduce costs and schedules associated with manufacturing liquid rocket engine components with the goal of reducing overall mission costs. One such technique being evaluated is powder-bed fusion or selective laser melting (SLM), commonly referred to as additive manufacturing (AM). The NASA Low Cost Upper Stage Propulsion (LCUSP) program was designed to develop processes and material characterization for GRCop-84 (a NASA Glenn Research Center-developed copper, chrome, niobium alloy) commensurate with powder-bed AM, evaluate bimetallic deposition, and complete testing of a full scale combustion chamber. As part of this development, the process has been transferred to industry partners to enable a long-term supply chain of monolithic copper combustion chambers. To advance the processes further and allow for optimization with multiple materials, NASA is also investigating the feasibility of bimetallic AM chambers. In addition to the LCUSP program, NASA has completed a series of development programs and hot-fire tests to demonstrate SLM GRCop-84 and other AM techniques. NASA's efforts include a 4K lbf thrust liquid oxygen/methane (LOX/CH4) combustion chamber and subscale thrust chambers for 1.2K lbf LOX/hydrogen (H2) applications that have been designed and fabricated with SLM GRCop-84. The same technologies for these lower thrust applications are being applied to 25-35K lbf main combustion chamber (MCC) designs. This paper describes the design, development, manufacturing and testing of these numerous combustion chambers, and the associated lessons learned throughout their design and development processes.

Gradl, Paul R.↗
NASA NTRSDate not supplied

Thin-wall Internal Channel Geometry and Surface Enhancements for Heat Exchangers using Laser Powder Directed Energy Deposition

Additive Manufacturing (AM) has offered many new design and manufacturing opportunities for components across various industries. As AM evolves there is a need to better understand outputs of the process including geometric limitations, surface texture, and post-processing surface enhancements for specific application requirements. One possible application area of AM are components using thin-wall (~1 mm) microchannel heat exchangers for subsystems across aerospace and industrial applications. Laser Powder Bed Fusion (L-PBF) is a common process for complex internal channels but the build diameter is limited to approximately 600 mm. Laser Powder Directed Energy Deposition (LP-DED) is being evaluated to produce thin-wall microchannel heat exchangers at scales beyond the L-PBF process. Successful deployment of the LP-DED technology requires characterization of geometric features from the process and potential improvements to the surface using post-processing. Surface texture, inclusive of roughness and waviness, is one of the critical attributes of AM that effects the friction factor and pressure drop within a heat exchanger and lacks data for the LP-DED process. This presentation will provide an overview of the characterization work completed of the LP-DED process for thin-walls and small channel geometry representative of various high performance alloys including NASA HR-1 and GRCop-42. An overview of the experiments conducted with varying LP-DED parameters, evaluation of various internal channel geometry, geometric build features, and resulting surface texture will be provided along with a summary of conclusions from these experiments. This study presents characterization of 2.5 mm microchannels using LP-DED, mechanisms that cause the surface texture which include powder adherence and material droop, and angled walls have a significant impact on the thickness and surface texture. Results will also be presented on various surface enhancement processes that allow for tuning of the wetting surface for friction factor, heat transfer, or fatigue life performance requirements.

Additive Manufacturing↗
NASA NTRS1988

Investigation of a SiC/Ti-24Al-11Nb composite

A summary of ongoing research on the characterization of a continuous fiber reinforced SiC/Ti-24Al-11Nb (at percent) composite is presented. The powder metallurgy fabrication technique is described as are the nondestructive evaluation results of the as-fabricated composite plates. Tensile properties of the SiC fiber, the matrix material, and the 0-deg SiC/Ti-24Al-11Nb composite (fibers oriented unidirectionally, parallel to the loading axis) from room temperature to 1100 C are presented and discussed with regard to the resultant fractography. The as-fabricated fiber-matrix interface has been examined by scanning transmission electron microscopy and the compounds present in the reaction zone have been identified. Fiber-matrix interaction and stability of the matrix near the fiber is characterized at 815, 985, and 1200 C from 1 to 500 hr. Measurements of the fiber-matrix reaction, the loss of C-rich coating from the surface of the SiC fiber, and the growth of the Beta depleted zone in the matrix adjacent to the fiber are presented. These data and the difference in coefficient of thermal expansion between the fiber and the matrix are discussed in terms of their likely effects on mechanical properties.

Brindley, P. K.↗