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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 721 records · Page 40
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Probing lithiation and delithiation of thick sintered lithium-ion battery electrodes with neutron imaging

As lithium-on (Li-ion) batteries increase in their prevalence and the range of applications expands, there is a need to understand and exploit the limits of electrochemical performance. Probing the internal processes in Li-ion batteries provides insights into the electrochemical characteristics of the cells as well as information necessary for rational cell design. In this manuscript an in situ method, neutron imaging, is applied to Li-ion full cells to track the lithiation/delithiation processes in the electrodes during discharge. The electrodes comprise thick sintered films of only active material, which improves the number of discrete points that are mapped for net changes in neutron intensity through the electrode. The lithiation/delithiation processes are qualitatively consistent with calculations of the Li + concentration and discharge profiles of the cells. These results illustrate that neutron imaging can experimentally probe and confirm limitations in the electrochemical performance of Li-ion full cells, particularly those with thick electrodes.

25 ENERGY STORAGE↗
DOE OSTI2021

Impact of electrode porosity architecture on electrochemical performances of 1 mm-thick LiFePO4 binder-free Li-ion electrodes fabricated by Spark Plasma Sintering

Thick electrodes with high active material loadings have been intensively studied over the last couple of decades in pursuit of achieving high energy density systems. To optimize and enhance the electrochemical performance of such electrodes, one has to control the pore morphology by, for example, varying the pore size and shape, and the level of porosity. In the present work, the fabrication of thick binder-free LiFePO4 (LFP) electrodes with two different pore sizes (12 and 20 mu m) and porosities (21 vol% and 44 vol%) using Spark Plasma Sintering (SPS) and templating approach is reported. The well-controlled porous architecture inside the thick electrodes is realized by fine-tuning experimental parameters. The impact of porosity architecture on electrochemical performance is quantified and correlated with the 3D tortuosity values determined from both micro-computed tomography and electrochemical impedance-based experimental methods. Based on the micro-computed tomography data analysis, estimated tortuosity values along X, Y, and Z axes reveal an anisotropic effect perpendicularly to the SPS compression axis (Z-direction). This is particularly profoundly observed in the samples with larger pores (20 mu m). The correlation between morphological properties and the rate capability performance is established indicating that the capacity loss happens mainly due to the Li-ion diffusion limitations.

Cathode material↗
DOE OSTI2015

Investigation of deformation micro-mechanisms in nickel consolidated from a bimodal powder by spark plasma sintering

Bulk polycrystalline nickel compact was processed by spark plasma sintering from heterogeneous powder consisting of a mixture of nanometer and micrometer sized particles. The consolidated samples inherited the bimodal structure of the starting powder and was composed of ~ 55 vol.% coarse-grained (with the grain size larger than 1 μm) and ~ 45 vol.% ultrafine-grained (with an average grain size of ~ 550 nm) components. The deformation mechanisms were established by EBSD, X-ray line profile analysis and in-situ TEM observations. In the ultrafine-grained volume, the deformation occurred mainly through the activation of dislocation sources emitting full or partial dislocation either from grain interior or grain boundaries. Besides dislocation activity, rolling and sliding of nanograins were also observed during deformation by in-situ transmission electron microscopy, which have a considerable contribution to the observed high strain rate sensitivity of the bimodal microstructure. The cracks formed during deformation easily propagated in the nanograin regions due to the weaker particle bonding caused by the relatively high fraction of native oxide layer on the surface of the initial nanoparticles. - Highlights: • Bulk bimodal polycrystalline Ni was processed by SPS from a heterogeneous powder. • High SRS of the flow stress was observed which enhanced ductility and strength. • In-situ TEM revealed dislocation sources inside and at the boundaries of UFGs. • Twinning, partial dislocation and NG rolling were observed at crack tip vicinity. • The high SRS pertained to both dislocation activity in CG and NG rolling.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

The distribution and mechanism of pore formation in copper foams fabricated by Lost Carbonate Sintering method

In this research, utilizing X-ray computed tomography (XCT), geometrical characterization, and pore formation mechanisms of highly porous copper foams manufactured by powder metallurgical (PM) process are investigated. Open-cell copper foams with porosity percentages of 60% and 80% and with a pore size within the range of 300–600 μm were manufactured by using potassium carbonate as a space holder agent via the Lost Carbonate Sintering (LCS) technique. XCT and SEM were also employed to investigate the three-dimensional structure of foams and to find the effect of the parameters of the space holders on the structural properties of copper foams. The result showed an excellent correlation between the structural properties of the foams including the size and shape of the pores, porosity percentage, volume percentage, particle size, and the shape of the sacrificial agent used. Also, the advanced image analysis of XCT images indicated fluctuations up to ± 10% in porosity distribution across different cross-sections of the foams. Simultaneous thermal analysis (STA: DTA–TG) was also used to study the thermal history of the powders used during the manufacturing process of the foams. The results indicated that the melting and thermal decomposition of the potassium carbonate occurred simultaneously at 920 °C and created the porous structure of the foams. By combining the STA result with the result of the tension analysis of cell walls, the mechanisms of open-pore formation were suggested. In fact, most open pores in the samples were formed due to the direct contact of potassium carbonate particles with each other in green compact. Also, it was found that the thermal decomposition of potassium carbonate particles into gaseous CO{sub 2} led to the production of gas pressure inside the closed pores, which eventually caused the creation of cracks on the cell walls and the opening of the pores in foam's structure. - Highlights: • Structural characterization of copper foam produced by LCS method is investigated by tomography images. • The ability of LCS technique to control structural features of produced foams was proved. • The mechanisms of open pores formation were presented.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Dislocation density in fine grain-size spark-plasma sintered aluminum measured using high brightness synchrotron radiation

In this study, three-dimensional orientation mapping of samples of aluminum prepared by spark plasma sintering (SPS) with average grain sizes of 5 μm and 1 μm has been carried out using high-brightness synchrotron radiation, from which the geometrically necessary dislocation (GND) density has been determined. The low average measured GND density values confirm that the SPS process can be used to produce samples containing grains with dislocation density similar to that of fully recrystallized coarse-grained samples. Values of GND density are also compared to those obtained from electron back-scatter diffraction studies on the same material, highlighting the significantly higher angular resolution of the synchrotron data. For the 5 μm grain-size sample the measured GND density can account for a large fraction of the previously observed positive Hall-Petch deviation of this material. For the 1 μm grain-size sample, however, the GND-based strengthening contribution is much smaller than the reported positive Hall-Petch deviation, such that the additional strength may be reliably associated with dislocation source-limited strengthening.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Solid-state reaction mediated microstructural evolution in a spark plasma sintered in situ Ti–B 4 C composite

For this study, a novel porosity-free in situ Ti–B 4 C composite was fabricated via spark plasma sintering (SPS). Detailed analysis of the phase evolution, coupling results from XRM, XRD and SEM-EBSD-EDS, indicate that primarily TiB 2 precipitates formed due to the in-situ reactions between the boron-carbide and titanium powders. The precipitation of TiB 2 resulted in the formation of a graphitic C-rich thin layer circumscribing the partially reacted B 4 C particles. Further progression of the in-situ reaction leads to the out-diffusion of the excess carbon from the B 4 C particles, across the graphite and TiB 2 phases, forming TiC upon reacting with the titanium matrix. Therefore, the final microstructure primarily consisted of TiB 2 , TiC, and partially reacted B 4 C phases, with small amounts of TiB, α-Ti, and graphite. Furthermore, the microstructure in these SPS processed in situ composites appeared to be the product of a solid-state Ti–B 4 C diffusion couple, substantially different from their fusion-based additively manufactured counterparts. Nano-indentation tests revealed a remarkably high average hardness of ~25 GPa for this SPS-processed Ti–B 4 C composite and comparable (with literature) phase-specific hardness and modulus values for the constituent TiB 2 , TiC, and B 4 C phases.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Electric-field-assisted-sintering of rare-earth oxide dispersion strengthened Fe-Cr-Mo alloys

Oxide dispersion-strengthened (ODS) alloys are widely recognized for their exceptional high-temperature strength, creep resistance, and radiation tolerance, making them indispensable for advanced nuclear reactors, aerospace, and energy systems. Achieving a fine and stable dispersion of oxide nanoparticles is critical, as these particles act as strong barriers to dislocation motion and effective sinks for irradiation-induced defects, ensuring structural integrity under extreme conditions. Here, in this study, Fe–Cr–Mo-based ODS alloys were fabricated via mechanical alloying and consolidated using electric-field-assisted sintering (EFAS) with additions of Y 2 O 3 , La 2 O 3 , and CeO 2 . EFAS processing produced ultrafine-grained microstructures (average grain size <1 μm) with uniformly distributed oxide clusters (2–4 nm). Atom probe tomography revealed that La 2 O 3 -containing alloys exhibited the highest nanoparticle number density, resulting in superior tensile strength compared to yttria- and ceria-bearing counterparts. The combined effect of grain refinement and rare-earth oxide dispersion significantly enhanced mechanical performance, demonstrating the potential of EFAS for developing high-strength ferritic alloys for demanding environments such as nuclear systems.

36 - MATERIALS SCIENCE↗
DOE OSTI2025

Amorphous complexion-aided sintering enables scalable processing of bulk nanocrystalline Cu-Zr with high strength and compressive plasticity

Nanocrystalline alloys can have exceptional strengths, yet due to limited microstructural stability it is difficult to fabricate bulk pieces through traditional processing routes that retain nanosized grains. In this study, centimeter-sized Cu-Zr alloy pellets were fabricated via a simple and improved powder metallurgy processing route. Different consolidation temperatures and times were employed to investigate the effect of amorphous grain boundary complexions on densification and the resulting mechanical properties. Bulk compression tests were carried out, with the samples that were hot pressed at 900 °C for 10 h exhibiting an excellent combination of average yield strength of 722 ± 45 MPa and average failure strain of 25.3 ± 2.4 %. Furthermore, we find that a powder processing route which enables amorphous complexion-assisted sintering leads to samples that (1) reach full density without requiring quenching treatments or other complex processing, (2) demonstrate appreciable plasticity, and (3) have strength that competes with commercially available high-strength Cu alloys.

Bulk nanocrystalline alloy↗
DOE OSTI2019

Radiative Properties of Coal Ash Deposits with Sintering Effects

The heat-transfer characteristics in the fireside of a pulverized-coal furnace are affected, among other factors, by the physical and chemical characteristics of the ash deposits. Indeed, the physical state of the ash deposits and their chemical composition determine the radiative and conductive properties of the furnace walls. Particularly, several complex mechanisms are involved in the radiative heat-transfer process at the walls that restricts the absorption of the incident radiation of the flame, particles, and hot gases. These mechanisms involve dependencies on the radiation spectrum due to the ash chemical composition and ash-sintering effects that enhance or hinder the overall heat transfer. In this work, the complex mechanisms that describe the heat exchange in the presence of ash deposits and their impact on the prediction of the wall emissivity and ultimately the wall heat transfer in a real system are discussed.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2024

Pelletization with Spark Plasma Sintering and Characterization of Metal Iodides: An Assessment of Long-Term Radioiodine Immobilization Options

Four promising iodine “getter” materials (Ag, Cu, Bi, and Sn) for radioiodine capture were assessed in their pure metal-iodide (MI x ) pelletized forms to compare relative chemical durabilities. To study chemical durability, commercial MI x compounds of AgI, BiI 3 , BiOI, CuI, and SnI 4 were converted to dense monolithic pellets using spark plasma sintering. Semidynamic leach testing in the form of modified ASTM C1308 tests was then performed on the pellets in two different forms including unmounted (as-pressed) specimens (i.e., “U”) and epoxy-mounted specimens (i.e., “M”) with polished surfaces. The chemical durability results and sample characterizations showed that three of the five MI x compounds tested (i.e., AgI, CuI, and BiOI) displayed moderate to high leach resistances. Further, the remaining two MI x compounds (i.e., BiI 3 and SnI 4 ), which are both desirable iodine waste forms due to their high iodine loading capacities, readily decomposed during leach testing, indicated by crystallographic changes in the specimens as well as large amounts of iodine detected in the leachate solutions. The instabilities of BiI 3 and SnI 4 raise uncertainties for using the base metals/cations (i.e., Bi 0 /Bi 3+ and Sn 0 /Sn 4+ , respectively) as viable getters for radioiodine capture due to likely poor waste form chemical durabilities after capture and consolidation into waste forms.

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

Toward the Design of a Hierarchical Perovskite Support: Ultra-Sintering-Resistant Gold Nanocatalysts for CO Oxidation

We report that an ultrastable Au nanocatalyst based on a heterostructured perovskite support with high surface area and uniform LaFeO 3 nanocoatings was successfully synthesized and tested for CO oxidation. Strikingly, small Au nanoparticles (4–6 nm) are obtained after calcination in air at 700 °C and under reaction conditions. The designed Au catalyst not only possessed extreme sintering resistance but also showed high catalytic activity and stability because of the strong interfacial interaction between Au and the heterostructured perovskite support.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Study on corrosion behaviors of sintered Nd-Fe-B magnets in different environmental conditions

Nd-Fe-B magnets have outstanding magnetic properties, but their corrosion resistance is poor because the rare-earth-rich phases in them are easily oxidized. In this article, we report an investigation of the corrosion behaviors of sintered Nd-Fe-B magnets with varied compositions in different corrosion conditions. The weight losses of the magnets after corrosion testing were measured after brushing off the corrosion products. The magnetic flux losses of the magnets were measured using a fluxmeter. A scanning electron microscope equipped with an energy dispersive x-ray analysis system was employed to observe the corrosion morphology. It was found that the humid-heat resistance of the magnets was obviously improved by partially substituting Dy for Nd and adding minor Co. The corrosion products and morphologies of Nd-Fe-B magnets for the autoclave test were different from those for the constant humid-heat test. The corrosion rates of the magnets for the former were much slower than for the latter; this is probably because the high-pressure steam led to an oxygen-deficient atmosphere, and the liquid film on the surface of the magnet specimens hindered the diffusion of oxygen into the bulk for the autoclave test.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Magnetization reversal mechanism of a sintered Nd-Fe-B magnet with Dy segregation

The magnetization reversal mechanism of a sintered Nd-Fe-B magnet with Dy segregation near grain boundaries (GB) was studied using spin polarized scanning electron spectroscopy and magnetization measurements. More fine magnetic domains near GB were found in the magnet with Dy segregation than in the magnet without treatment. Magnetic modifications near the GB had no effect on the magnetization development. The domain wall motion of a quasihard magnetic component in the magnet with Dy segregation was suppressed in comparison with those in the magnet without treatment; this could also be confirmed in the different behaviors of asymmetry components toward a magnetic field direction between both magnets. From analyzing the probability of rotating magnetization near the GB, the magnetization reversal of the magnet with Dy segregation was more difficult to produce than those of the magnet without treatment.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Temperature dependence of magnetic behaviour in very fine grained, spark plasma sintered NiCuZn ferrites

Recently, using spark plasma sintering technique, a family of very fine grained, fully dense NiCuZn ferrites have been produced, which show constant permeability up to several 10 MHz. These ferrites can be used for filtering purposes in high frequency applications where a wide frequency band is required. In this paper, we study the magnetization processes taking place in these nano grained materials, in the frequency interval of 100 kHz to 5 MHz. Using a fluxmetric hysteresis graph, permeability, loss, and BH loops are measured at different temperatures, from -5 deg. C to 110 deg. C. Results are compared to the behavior of micrometric grain size ferrites, which are commonly used for power electronic and high frequency applications.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Fabrication and Spark plasma sintering of nanostructured bismuth telluride (Bi{sub 2}Te{sub 3})

Thermoelectric (TE) devices can harvest residual low-grade waste heat energy. Bismuth telluride (Bi{sub 2}Te{sub 3}) and its alloys are mostly used TE materials in the bulk form for making TE modules. We report a simple, fast and very high yield synthetic process for the bulk Bi{sub 2}Te{sub 3} nanopowders with hexagonal plate like morphology. Spark plasma sintering (SPS) process has been optimized in order to preserve nanostructure while achieving a high compaction density of the pellets. Electron microscopy analysis was used to determine the effect of SPS parameters during compaction on the grain growth. Optimal conditions for the fabricated nanopowder was determined as 673 K, 70 MPa pressure with no holding time, which resulted in average lateral grain size in the range of 165-190 nm for a compact density of 98%. About 50% reduction of thermal conductivity was observed as compared to its bulk counterparts, revealing the feasibility of suggested route in the preservation of nanostructure and enhanced phonon scattering.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Temperature modeling for analysis and design of the sintering furnance in HTR fuel type of ball

One of the factors that determine the safety of the operation of the sintering furnace fuel HTR ball is the temperature distribution in the ceramic tube furnace. The temperature distribution must be determined at design stage. The tube has a temperature of 1600 °C at one end and about 40 °C at the other end. The outside of the tube was cooled by air through natural convection. The tube is a furnace ceramic tube which its geometry are 0.08, 0.09 and 0.5 m correspondingly for the inner tube diameter, outer tube diameter and tube length. The temperature distribution of the tube is determined by the natural convection coefficient (NCF), which is difficult to be calculated manually. The determination of NCF includes the Grasshoff, Prandtl, and Nusselt numbers which is a function of the temperature difference between the surrounding air with the ceramic tube. If the temperature vary along the tube, the complexity of the calculations increases. Thus the proposed modeling was performed to determine the temperature distribution along the tube and heat transfer coefficient using a self-developed software which permit the design process easier.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
DOE OSTI2013

Plastic deformation and sintering of alumina under high pressure

Plastic deformation of alumina (Al{sub 2}O{sub 3}) under high pressure was investigated by observing the shape changes of spherical particles, and the near fully dense transparent bulks were prepared at around 5.5 GPa and 900 °C. Through analyzing the deformation features, densities, and residual micro-strain of the Al{sub 2}O{sub 3} compacts prepared under high pressures and temperatures (2.0–5.5 GPa and 600–1200 °C), the effects of plastic deformation on the sintering behavior of alumina have been demonstrated. Under compression, the microscopic deviatoric stress caused by grain-to-grain contact could initiate the plastic deformation of individual particles, eliminate pores of the polycrystalline samples, and enhance the local atomic diffusion at the grain boundaries, thus produced transparent alumina bulks.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2013

Study of microstructure and semiconductor to metallic conductivity transition in solid state sintered Li{sub 0.5}Mn{sub 0.5}Fe{sub 2}O{sub 4−δ} spinel ferrite

Li{sub 0.5}Mn{sub 0.5}Fe{sub 2}O{sub 4} ferrite has been prepared by solid state sintering route. XRD pattern showed single phased cubic spinel structure. The samples exhibited typical character of plastoferrite with ring shaped surface microstructure. New feature observed in the present ferrite is the frequency activated conductivity transition from semiconductor to metallic state above 800 K. The increase of conductivity with frequency in the semiconducting regime follows Jonscher power law, while decrease of conductivity in metallic regime obeys Drude equation. The conductivity in semiconductor regime has been understood by hopping mechanism of localized charge carriers among the cations in B sites of cubic spinel structure. At higher temperatures, overlapping of electronic orbitals from neighbouring ions and free particle like motion of lighter Li{sup +} ions among interstitial lattices contributed metallic conductivity. The samples provided evidence of localized nature of the charge carriers at lower temperatures and increasing delocalized character with the increase of measurement temperature. From application point of view, such ferrites behave as semiconductor at low temperature and allow electromagnetic wave to pass through, but transform into a metallic reflector with negative dielectric constant at high temperature.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗