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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 235 records · Page 13
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Comparison of Electron Beam and Laser Beam Powder Bed Fusion Additive Manufacturing Process for High Temperature Turbine Component Materials, Phase II. CRADA Final Report

The evolving additive manufacturing (AM) technology is now at the point where some metallic turbine components are being fabricated for both development and production purposes. The goal of this phase II project is to continue the evaluation of AM Nickel Alloy X fabricated by electron beam (EB) or laser beam (LB) powder bed fusion (PBF) process for gas turbine applications. Microstructure, mechanical and oxidation properties characterization was conducted on test specimens produced with powders of different chemistries within the typical material specification range. Powders with high Silicon (Si) content for the LB-PBF and low Si content for the EB-PBF displayed significant cracking levels in the AM Nickel Alloy X material. Accordingly, optimum fatigue performance would require careful control of powder chemistry, optimization of the fabrication parameters for a given powder and use of hot isostatic pressing (HIP) post treatment. Oxidation testing conducted at 1472°F (800ºC) in air showed that the roughness of the EB-PBF specimens led to an increase in specimen mass change, but overall the AM specimens exhibited oxidation behavior at 1472°F (800ºC) that is appropriate for applications in gas turbine engines. Assessment of the geometric capability of the LB-PBF and EBPBF systems using artifacts representative of turbine component geometries revealed that the LB-PBF process is well-suited for the fabrication of intricate geometries needed for turbine engine fuel injector components, but further process development is required to improve the EB-PBF system feature resolution.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Nanostructured Powders Made from Flame Spray Pyrolysis for Li-Ion Cathode

Flame processes are the most economic ones to produce fine powders and have been used to produce pigment titanium oxide and fused silica in large volumes. In this work a flame spray pyrolysis (FSP) process is used to make positive electrode materials for Li-ion battery, which is made of complex metal oxide powders, such as Li(Ni1/3Mn1/3Co1/3)O2. In particular, the work was focused on making the NMC materials with stoichiometric compositions and desired morphologies. During the pyrolysis process different morphologies can be formed, involving often powders with primary nanoparticles. Such nanostructures were found to have affected the battery performance. Detailed results of the synthesis, characterization, and battery testing of the NMC powder materials will be presented.

25 ENERGY STORAGE↗
DOE OSTI2018

Microstructure and nanoindentation analysis of Mg-SiC nanocomposite powders synthesized by mechanical milling

Highlights: • Mechanical milling as an effective solution to reach a homogeneous distribution of SiC nanoparticles up to 10 vol% in Mg matrix • No deformation twinning in the nanostructured Mg matrix even after the severe plastic deformation and hard SiC nanoparticles up to 10 vol%. • Significant enhancement of nanohardness and reduced elastic modulus in the milled nanocomposite powders - Abstract: Mixtures of magnesium powder and SiC nanoparticles at various volume fractions were mechanically milled to produce nanocrystalline Mg-SiC nanocomposites. X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were utilized to characterize the microstructure of the milled powders. The microstructural evidences revealed that mechanical milling is a proper method to achieve a uniform distribution of the SiC nanoparticles, even up to 10% in the Mg matrix. Based on the results, higher volume fraction of the SiC nanoparticles raise the value of measured microstrain and reduce the crystallite size of the Mg matrix. The TEM results pointed to the fact that no deformation twinning takes place in the nanostructured Mg matrix even after severe plastic deformation through mechanical milling and the presence of hard SiC nanoparticles up to 10 vol%. The effects of nanoparticle volume fraction on mechanical properties of the milled Mg-SiC nanocomposites were evaluated using nanoindentation tests. The results clearly showed a significant enhancement of nanohardness and reduced elastic modulus in the milled powders compared to that of the reference material namely as-received pure magnesium. It was found that the SiC nanoparticles (even up to 10 vol%), well distributed in the magnesium matrix, remarkably improve the reduced elastic modulus and nanohardness of the nanocomposite powders.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2019

Lithography-based Ceramics Manufacturing Technologies

In this work, surrogate powders were prepared with lithography-based ceramic printing. Lanthanum oxide, a powder from Oak Ridge National Laboratory (ORNL), was prepared by milling, characterizing, and printing of coupon samples. The printing resulted in net-shaped green parts. Alumina, a more developed powder, was also printed and characterized at ORNL, and these parts were surrogate geometries larger than coupons that were sintered to net shape within 0.3% of the desired geometry.

36 MATERIALS SCIENCE↗
DOE OSTI2026

A solid-state extrusion pathway extensible to upcycling aluminum scrap and end-of-life permanent magnets into ductile Al-6061/SmCo 5 structural magnetic composites

Permanent magnets offer strong potential for multifunctional structural components, but their inherent brittleness limits direct integration. Here, SolidStir® Extrusion (SSE) is used to embed SmCo5 powder into AA6061 in the solid state, and the resulting microstructure, interfacial chemistry, mechanical properties, and magnetic response are systematically characterized. SSE fragments the initial SmCo 5 powder into predominantly fine particles dispersed within an ultrafine Al matrix, with a volume fraction of ∼ 4–6 % in this proof-of-concept study. Interfacial reactions form a continuous Al–Co reaction layer, with local atomic-resolution indexing consistent with Al 13 Co 4 , together with Sm–Si-rich reaction products, while the matrix contains Sm–Co–Si-rich precipitates and Mg 2 Si, producing features from nanometers to micrometers. Compared with an Al extrudate, this architecture increases yield strength by ∼ 42 % and tensile strength by ∼ 31 %, while preserving uniform elongation, and it sustains work hardening in compression from 150 to 400 °C. The composite retained hard-magnetic behavior, with axial magnetization of 12.7 A·m 2 kg −1 at 6 T and intrinsic coercivity of 9.6 kOe. These findings demonstrate that SSE can produce Al-based load-bearing magnetic composites while preserving useful SmCo5 functionality.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Polycapillary x-ray lenses for single-shot, laser-driven powder diffraction

X-ray diffraction measurements to characterize phase transitions of dynamically compressed, high-Z matter at Mbar pressures require both sufficient photon energy and fluence to create data with high fidelity in a single shot. Large-scale laser systems can be used to generate x-ray sources above 10 keV utilizing line radiation of mid-Z elements. However, the laser-to-x-ray energy conversion efficiency at these energies is low, and thermal x-rays or hot electrons result in unwanted background. We employ polycapillary x-ray lenses in powder x-ray diffraction measurements using solid target x-ray emission from either the Z-Beamlet (ZBL) long-pulse or the Z-Petawatt (ZPW) short-pulse laser systems at Sandia National Laboratories. Polycapillary lenses allow for a 100-fold fluence increase compared to a conventional pinhole aperture while simultaneously reducing the background significantly. This enables diffraction measurements up to 16 keV at the few-photon signal level as well as diffraction experiments with ZPW at full intensity.

47 OTHER INSTRUMENTATION↗
DOE OSTI2018

The evolution history of superalloy powders during hot consolidation and plastic deformation

Highlights: • Element segregations in a powder metallurgy superalloy at different states are identified. • The surface energy drives precipitation of oxides, carbides, and γ' particles on powder surface during hot consolidation. • Prior particle boundary structure is distorted and more uniformly refined grains are obtained after hot extrusion. - Abstract: Powder metallurgy superalloys are widely used to produce critical rotating parts in turbine engines. However, the issues like what is the driving force of precipitation on prior particle boundary (PPB) during consolidation and how the PPB structure evolves during plastic deformation still remain to be resolved. In this study, with the characterization of the microstructure evolution from powder, consolidation, to plastic deformation, the segregation of alloying elements on the particle boundaries at elevated temperature was analyzed by equilibrium thermodynamic calculations, and the distortion of PPB structure under large plastic deformation was quantitively simulated by finite element (FE) methods. The results indicated that surface energy serves as the main driving force of PPB precipitation and hot extrusion could distort the PPB structure and yield more uniformly refined grains.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Supply Chain Improvement & Process Modification Printing in Tantalum

Refractory metals and alloys are distinguished by their exceptional thermophysical properties, including high melting and recrystallization temperatures, remarkable strength, and superior corrosion resistance, all of which surpass those of conventional alloys. These unique characteristics position these materials as ideal candidates for applications in extreme environments. However, their potential has historically been underexploited due to limitations in processing capabilities. Recent advancements in melt-based additive manufacturing (AM) processes present opportunities to overcome these limitations. Previous Sandia studies have successfully characterized pure tantalum produced through laser powder bed fusion (LPBF) externally at Castheon, revealing that LPBF-fabricated tantalum exhibits properties exceeding those of wrought materials. This promising outcome sparked increased interest in the internal additive manufacturing of tantalum. This project aimed to establish the new SLM 280 machine at SNL-CA to successfully produce the first tantalum prints and characterize the material. Additionally, efforts were made to enhance the machine by incorporating Inert equipment to minimize oxygen content within the print volume. The results demonstrated that internally manufactured LPBF tantalum not only met but exceeded the standards of wrought materials, even prior to the integration of the additional equipment. The inert equipment is almost successfully integrated and ready for use. Future research should focus on understanding how this equipment influences the process-structure-property relationships, as well as further optimizing the printing parameters for tantalum.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Continuous-flow synthesis of thermochromic M-phase VO2 particles via rapid one-step hydrothermal reaction – effect of mixers

VO2 particles are promising materials for thermochromic smart windows that reduce building energy loss. Continuous-flow hydrothermal processes showcase advantages for synthesizing VO2 particles compared with traditional batch reaction systems. Mixers play a crucial role in particle fabrication in continuous-flow systems. In this study, a Center T-Mixer and a Collision Cross-Mixer are developed and implemented in a hot water fluidized suspension reaction (HWFSR) system. The influence of the resident time on the particle phase and size was evaluated, and properties of particles derived from systems equipped with differing mixers were compared. The resulting particles were characterized using techniques of X-ray powder diffraction (XRD) analysis, scanning electron microscopy (SEM), and differential scanning calorimetry (DSC). When compared with the Center T-Mixer, results indicate that the Collision Cross-Mixer has better control regarding the morphology and size distribution of resulting particles while improving the transition temperatures of the as-synthesized materials. HWFSR systems containing novel mixer designs are capable of producing pure M-phase VO2 particles in a single step contrary to the current reactor design that use a second postheat treatment step, and they are capable of synthesizing many other nanoparticle species, especially those requiring high temperature and pressure reaction conditions.

continuous-flow process↗
DOE OSTI2022

Proton damage in (Y,Lu,Gd) 3 (Al,Ga) 5 O 12 :Ce mixed garnet scintillators

Scintillators are vital components for nuclear instrumentation and its applications, including plasma diagnostics and imaging. As yields in controlled fusion experiments increase, the radiation tolerance of scintillator candidates for use in instrumentation is of particular importance. High radiation exposure can damage scintillating materials and alter the optical properties. The effects of radiation damage in Ce-doped mixed garnet ceramics over the compositional range (Y,Gd,Lu) 3 (Al,Ga) 5 O 12 are investigated using optical techniques. The samples were exposed to 200 keV protons to an accumulated fluence of 10 16 protons per square centimeter, then characterized using diffuse reflectance spectroscopy (DRS). DRS with visible light can assess the radiation tolerance of opaque poly-crystalline samples, which can be easily sintered from powders and thus offer distinct advantages in characterization compared to single crystals. Qualitative trends in induced absorption are presented as a function of composition, and the ideal cerium dopant concentration for Y 2 LuAl 5 O 12 is determined to be 0.60–0.75 mol.%.

47 OTHER INSTRUMENTATION↗
DOE OSTI2018

In situ observation of phase changes of a silica-supported cobalt catalyst for the Fischer–Tropsch process by the development of a synchrotron-compatible in situ/operando powder X-ray diffraction cell

In situ characterization of catalysts gives direct insight into the working state of the material. Here, the design and performance characteristics of a universal in situ synchrotron-compatible X-ray diffraction cell capable of operation at high temperature and high pressure, 1373 K, and 35 bar, respectively, are reported. Its performance is demonstrated by characterizing a cobalt-based catalyst used in a prototypical high-pressure catalytic reaction, the Fischer–Tropsch synthesis, using X-ray diffraction. Cobalt nanoparticles supported on silica were studied in situ during Fischer–Tropsch catalysis using syngas, H 2 and CO, at 723 K and 20 bar. Post reaction, the Co nanoparticles were carburized at elevated pressure, demonstrating an increased rate of carburization compared with atmospheric studies.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2018

Colloidal Synthesis of Bulk-Bandgap Lead Selenide Nanocrystals

Lead selenide quantum dots (QDs) are low-bandgap IV-VI semiconducting nanomaterials that have been studied for a variety of applications. Their preparation using colloidal methods can create small spherical to larger cubic nanocrystals, with an upper limit of ~17 nm reported to date. Here we describe methods for preparing cubic PbSe nanocrystals over a 20–40 nm size range using a twostep procedure. Specifically, ~10 nm PbSe QDs are generated using the rapid injection method, the products from which are overcoated with additional lead and selenium precursors. The use of two lead reagents were studied; lead oleate resulted in a maximum of 20 nm cubes, while more reactive lead hexyldecanoate resulted in much larger nanomaterials with bulk bandgaps. However, PbSe samples prepared with lead hexyldecanoate also contained agglomerates. Special care must be taken when characterizing larger strained nanomaterials with X-ray powder diffraction, for which the Scherrer equation is inadequate. A more rigorous approach using the Williamson–Hall method provides characterizations that are consistent with electron microscopy analysis.

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

Characteristics and Processing of Hydrogen-Treated Copper Powders for EB-PBF Additive Manufacturing

The fabrication of high purity copper using additive manufacturing has proven difficult because of oxidation of the powder feedstock. Here, we present work on the hydrogen heat treatment of copper powders for electron beam powder bed fusion (EB-PBF), in order to enable the fabrication of high purity copper components for applications such as accelerator components and vacuum electronic devices. Copper powder with varying initial oxygen contents were hydrogen heat-treated and characterized for their chemistry, morphology, and microstructure. Higher initial oxygen content powders were found to not only reduce surface oxides, but also reduce oxides along the grain boundaries and form trapped H 2 O vapor inside the particles. The trapped H 2 O vapor was verified by thermogravimetric analysis (TGA) and residual gas analysis (RGA) while melting. The mechanism of the H 2 O vapor escaping the particles was determined by in-situ SEM heated stage experiments, where the particles were observed to crack along the grain boundaries. To determine the effect of the EB-PBF processing on the H 2 O vapor, the thermal simulation and the validation of single melt track width wafers were conducted along with melting single layer discs for chemistry analysis. A high speed video of the EB-PBF melting was performed in order to determine the effect of the trapped H 2 O vapor on the melt pool. Finally, solid samples were fabricated from hydrogen-treated copper powder, where the final oxygen content measured ~50 wt. ppm, with a minimal residue hydrogen content, indicating the complete removal of trapped H 2 O vapor from the solid parts.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Characterization of Urbix Resources Natural Flake Graphite Material for Nuclear Applications (CRADA NFE-18-07340 Final Report)

Urbix Resources is a company specializing in graphite powder processing and purification. Urbix is looking to become the first domestic supplier of nuclear-grade graphite in the United States. This has led to a Cooperative Research and Development Agreement (CRADA) being established between the Oak Ridge National Laboratory (ORNL) and Urbix Resources, with the goal of characterizing a purified graphite feedstock supplied by Urbix Resources. The resulting data will then be used to determine the viability of a large-scale nuclear graphite production and qualification campaign. These characterization methods have been performed on the as-received graphite feedstock, a heat-treated batch of the feedstock, a milled batch of the feedstock, and a nuclear-grade graphite powder historically used in fuel production. The data from the heat-treated and milled feedstock will determine how different processing methods affect the powder’s physical properties, whereas the data from the nuclear grade graphite will provide information about the characteristics of a graphite previously accepted for nuclear applications. All of these powders have been characterized individually and as part of a resin-graphite blend (herein referred to as matrix) that has been used in past fuel experiments. The results of these experiments show that the Urbix powder and nuclear-grade graphite powder display notably different properties from one another in many cases, but this discrepancy may have been the result of the typical particle size of each powder. This hypothesis is supported by tests conducted on the milled powder, which showed a closer resemblance in properties to the nuclear-grade graphite than the as-received powder. The method for pressing the graphite matrix also had a noticeable effect on the measured properties.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2026

Hierarchical microstructure of Yb-filled skutterudites through ultrasonically atomized spherical powders for enhanced thermoelectric performance

Hierarchical microstructures are widely explored as a strategy to reduce lattice thermal conductivity in thermoelectric materials while preserving favorable electronic transport. Here we demonstrate that ultrasonic atomization of precursor powders provides an intrinsic pathway to generate such architectures in n-type Yb0.3Co4Sb12 skutterudites. Materials were synthesized by both conventional sealed-ampoule and ultrasonic atomization routes, each yielding essentially single-phase skutterudite after densification. However, the atomized spherical powders undergo a distinct reaction-driven microstructural evolution during thermal treatment prior to densification. Electron microscopy reveals that the skutterudite phase within the particles induces swelling, cracking, and fragmentation of the droplets before consolidation. Multimodal structural and microstructural characterizations show that densification of these fragmented powders produces a hierarchical microstructure consisting of submicron grains, micrometer-scale faceted crystallites, and powder-derived domains separated by oxide-decorated boundaries. Comprehensive thermoelectric transport measurements evidence that this multiscale architecture lowers the lattice thermal conductivity while maintaining favorable electronic transport, leading to an average ~10% enhancement in the thermoelectric figure of merit. Complementary 121Sb Mössbauer spectroscopy further indicates lattice softening in the atomized material. These results demonstrate that ultrasonic atomization provides an effective route to engineer hierarchical microstructures in skutterudite thermoelectrics and offers a promising strategy for tailoring thermal transport in energy-conversion materials.

Bouteiller, Hugo [ORNL] (ORCID:0009000421322962)↗
DOE OSTI2026

Investigation of the Surface Chemistry of Magnesium and Magnesium Alloy Powders

Magnesium (Mg) and Mg alloy powders are generally difficult to sinter at atmospheric pressure in inert atmospheres purportedly due to the presence of powder particle surface oxide layers. To better understand sintering of Mg and Mg alloy powders, x-ray photoelectron spectroscopy (XPS) was performed to characterize the surface chemistry of gas atomized pure Mg and Mg alloys AZ91D and WE43 powders. These results are used to quantitatively determine the surface chemistry of these powders. Additionally, equilibrium thermodynamic modeling of these Mg/Mg alloys materials exposed to oxygen down to part per billion concentrations are presented for relative comparison to experimental XPS results. Analysis of these results are intended to improve sintering of Mg and Mg alloy powder materials through more quantitative knowledge of powder surface chemistry.

25 ENERGY STORAGE↗
DOE OSTI2018

Synthesis and Structural Characterization of Sb-Doped TiFe{sub 2}Sn Heusler Compounds

Ternary Heusler compounds form a numerous class of intermetallics, which include two families with general compositions ABC and AB{sub 2}C, usually referred to as half- and full-Heusler compounds, respectively. Given their tunable electronic properties, made possible by adjusting the chemical composition, these materials are currently considered for the possible use in sustainable technologies such as solar energy and thermoelectric conversion. According to theoretical predictions, Sb substitution in the TiFe{sub 2}Sn full-Heusler compound is thought to yield band structure modifications that should enhance the thermoelectric power factor. In this work, we tested the phase stability and the structural and microstructural properties of such heavily doped compounds. We synthesized polycrystalline TiFe{sub 2}Sn{sub 1−x}Sb{sub x} samples, with x = 0, 0.1, 0.2 and 1.0 by arc melting, followed by an annealing treatment. The structural characterization, performed by x-ray powder diffraction and microscopy analyses, confirmed the formation of the pseudo-ternary Heusler structure (cF16, Fm-3m, prototype: MnCu{sub 2}Al) in all samples, with only few percent amounts of secondary phases and only slight deviations from nominal stoichiometry. With increasing Sb substitution, we found a steady decrease in the lattice parameter, confirming that the replacement takes place at the Sn site. Quite unusually, the as-cast samples exhibited a higher lattice contraction than the annealed ones. The fully substituted x = 1.0 compound, again adopting the MnCu{sub 2}Al structure, does not form as stoichiometric phase and turned out to be strongly Fe deficient. The physical behavior at room temperature indicated that annealing with increasing temperature is beneficial for electrical and thermoelectrical transport. Moreover, we measured a slight improvement in electrical and thermoelectrical properties in the x = 0.1 sample and a suppression in the x = 0.2 sample, as compared to the undoped x = 0 sample.

36 MATERIALS SCIENCE↗