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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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18 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Influence of Cryomilling on Crystallite Size of Aluminum Powder and Spark Plasma Sintered Component

The present investigation aims to develop nanocrystalline (NC) pure aluminum powders using cryomilling technique and manufacture bulk components using spark plasma sintering (SPS). The cryomilling was performed on pure Al powders for 2, 6, and 8 h. The cryomilled powders were then consolidated using SPS to produce bulk components. The particle morphology and crystallite size of the powders and the bulk SPS components were analyzed using scanning electron microscopy (SEM), X-ray diffraction (XRD), and transmission electron microscopy (TEM). The results showed that the crystallite size of pure Al powders decreases with increased cryomilling time. The results also showed that the SPS at elevated temperatures resulted in a slight increase in crystallite size, however, the changes were insignificant. The mechanical properties of the bulk components were determined using a Vickers microhardness tester. The hardness of the cryomilled SPS component was determined to be three times higher than that of the unmilled SPS component. The mechanism for the reduction in crystallite size with increasing cryomilling time is discussed. This fundamental study provides an insight into the development of bulk nanomaterials with superior mechanical properties for automotive, aerospace, marine, and nuclear applications.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Testing and Modeling of Functionally Graded Aluminum-Doped Zinc Oxide Using Spark Plasma Sintering and Discrete Powder Layers of Varying Composition

Functionally graded material (FGM) ZnO is made via spark plasma sintering/field-assisted sintering technique (SPS/FAST) by varying the Al dopant content along the z-axis or pressing direction. A wide range of Al content (0–5 wt%) is used by adding Al powder to nanosized ZnO powder. Thermoelectric (TE) measurements are done on the FGM and individual layers made separately. X-ray diffraction (XRD) shows two phases, ZnO and spinel phase (ZnAl 2 O 4 ). High-resolution Raman spectroscopy reveals doped ZnO and spinel phase (ZnAl 2 O 4 ) spatially and shows segregation in the layer with highest Al content. Electron backscatter diffraction (EBSD) reveals noticeable grain growth with decreasing Al content, and there is a common, random preferred orientation in all layers. The tested properties are used to simulate efficiency curves for a discretely graded, five-layer FGM as well as a homogenous material, where both graded structures provide an opportunity to widen the current density ranges and therefore the temperature range of useful energy conversion.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Manufacturing Bulk Nanocrystalline Al-3Mg Components Using Cryomilling and Spark Plasma Sintering

In the current study, pure aluminum (Al) powders were cryomilled with and without 3 wt.% pure magnesium (Mg) dopant for varying durations followed by spark plasma sintering (SPS) of powders to prepare bulk components with superior mechanical properties. The crystallite sizes were determined for powders and the bulk components by analyzing the X-ray diffraction (XRD) spectrum. The calculations indicated a reduction in crystallite size with the increase in the cryomilling duration. The results also showed a more significant decrease in the crystallite sizes for Al-3Mg samples than that of pure Al. The changes in the surface morphology of powders were characterized using scanning electron microscopy (SEM). The elemental mapping analysis at nanoscale was carried out using Energy-dispersive X-ray spectroscopy (EDX) in Scanning transmission electron microscopy (STEM). The mechanical properties of the bulk components were assessed using a Vickers Microhardness tester. The test results demonstrated an improvement in the hardness of Mg-doped components. Higher hardness values were also reported with an increase in the cryomilling duration. This article discusses the mechanisms for the reduction in crystallite size for pure Al and Al-3Mg and its subsequent impact on improving mechanical properties.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Solid-State Sintering of Core-Shell Ceramic Powders Fabricated by Particle Atomic Layer Deposition

The properties of technical ceramics are highly dependent on their microstructure, which evolves during sintering. Sintering is the process by which ceramic parts are subjected to high temperatures to activate chemical diffusion and the consumption of porosity. During the initial stage of sintering, interparticle necks between neighboring particles form and subsequently increase in size, consuming porosity as the particle centers move closer together. To experimentally determine how this process depends on particle surface composition, particle atomic layer deposition (ALD) was used to deposit a thin film of amorphous aluminum oxide (Al2O3) onto yttria-stabilized tetragonal zirconia (3YSZ) particles, producing core-shell structured powders. The uniformity of the Al2O3 film was confirmed with transmission electron microscopy and energy dispersive spectroscopy. Scanning electron microscopy was used to observe microstructural evolution during sintering, and the dihedral angles of Al2O3 and 3YSZ grains were measured to determine the ratio of interfacial energies between the 3YSZ|3YSZ, 3YSZ|Al2O3, and Al2O3|Al2O3 interfaces. Analysis of the densification kinetics revealed that the initial stage of densification is dependent on the material at the surface of the particles (ie, the Al2O3 film) and is controlled by the diffusion of Al3+ cations through Al2O3. Once the Al2O3 film has coalesced, the sintering behavior is controlled by the densification of the core material (3YSZ). Thus, core-shell powders fabricated by particle ALD sinter by a two-step process where the kinetics are dependent on the material present at interparticle contacts.

alumina↗
DOE OSTI2020

Polymer Composites Reinforced by Carbon-Allotrope Fillers for Selective Laser Sintering (SLS) - A Review

The limited commercial availability of applicable polymer powders has hindered the widespread implementation of SLS as a legitimate manufacturing method. This is partly due to the mechanism of SLS, which requires powders to meet rigid specifications if processing is to be successful. Furthermore, powders that do meet requirements are often incapable of producing quality, high-performance parts. Academic and industrial research has focused on composite development to overcome this problem. The incorporation of fillers including calcium carbonate, molybdenum disulfide, and aluminum have all been found to influence the processing behavior of PA12 powder and ultimately, the properties of the final part.3-5 Here, the thermal and mechanical properties of sintered composite parts produced using polymer powders reinforced by various carbon-based fillers is discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Onset of selective laser flash sintering of AlN

Abstract Flash sintering uses a combination of heating and electric fields to rapidly densify ceramics. Previously, it has been shown that a scanning laser can be used to initiate flash sintering in localized regions on an yttria‐stabilized zirconia (YSZ) sample in a process known as selective laser flash sintering (SLFS). In this work, we show using a combination of measurements of electric current flowing through the sample and observations of necks formed between powder particles that aluminum nitride (AlN) can also undergo SLFS. Scan conditions required to initiate SLFS are characterized over a range of laser powers and laser scan speeds in a dry nitrogen environment. It is shown that initiation of SLFS in AlN is governed by both the local input energy density per scan and heat dissipation and a numerical model is developed to predict temperatures during SLFS. Assuming the minimum temperature along the conductive path determines the onset of SLFS, the minimum temperature and time required is 450–670 K in 2–0.25 s for the pressed AlN pellets used in this study for laser scan speeds of 33–300 m/s, laser powers of 10–30 W, and an applied electric field of 3000 V/cm.

Gouws, Andre↗
DOE OSTI2022

Manufacture aluminum alloy tube from powder with a single-step extrusion via ShAPE

Mechanical performance of aluminum in terms of strength, wear and corrosion resistance, especially high-temperature strength has been shown to improve with the addition of transition metal (TM) elements of Fe, Cr, and Ti. However, these feedstock materials occur as powders. As such, the traditional fabrication process is complex and expensive because it requires multiple procedures and consumes considerable energy. This study developed Shear Assisted Processing and Extrusion (ShAPE) as a single-step process that manufactures tubes directly from Al-TM powders obtained via gas atomization. Meter-long Al-TM alloy tubes are extruded from powders with different processing conditions. The ShAPE tubes have very low porosity and the average density is 2.94 kg/cm 3 , which is equal to or higher than parts fabricated by hot extrusion and sintering. The powder-to-tube fabrication process was revealed and discussed by examining the microstructural evolution. The Vickers hardness of ShAPE tubes ranges from 110 to 140 HV through wall thickness and at different extrusion speeds. The variation in hardness was correlated with the extent of refinement of intermetallics and attributed to the shear deformation per unit extrusion length. Energy cost analysis shows that ShAPE save ~60% energy compared to the conventional sintering and extrusion processes. Results indicate ShAPE is a low-cost, high-efficiency manufacturing process for producing tubes from metallic powders.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Aluminum-doped U 3 Si 2 composite fuels with enhanced oxidation resistance

Al-doped U 3 Si 2 composite fuels with controlled microstructure were fabricated by spark plasma sintering that display greatly-improved oxidation resistance as compared with monolithic and Al-doped silicides prepared by standard powder metallurgy or arc melting. The effects of Al additives on the thermal-mechanical properties and oxidation resisance of the micron- and nano-sized U 3 Si 2 composites were investigated. Additionally, a minimal addition of 1.8 at% Al is effective to increase the onset oxidation temperature of as-fabricated U 3 Si 2 pellets to 580 °C, which can be further increased to 610 °C by thermal annealing. The Al-doped U 3 Si 2 composite fuels also display simultaneously higher hardness and fracture toughness than un-doped U3Si2. These results highlight an effective strategy by integrating minimal Al additives, microstructure control and post-thermal annealing to design advanced silicide fuels with excellent oxidation resistance, desired thermal-mechanical properties and maintained high fissile element density.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Metal (Cu,Al)/CNT Composite Wires for Energy Efficient Motors

This report summarizes the main results of research project on Metal/CNT nanocomposites conducted at University of Central Florida (UCF). It should be noted that the project was budgeted for three years, but the budget period 3 was unfortunately not funded and conducted in COVID19 pandemic years due to many reasons. The demonstration plan on the small motors was also removed according to the discussion with the DOE program manager. All research activities were focused on the (Cu,Al)/CNT material development and wire extrusion. Existing methods to fabricate Metal/CNTs were usually suffering from agglomeration of CNTs due to their density and stiffness differences. A new method is studied by the UCF research team, where CNTs are surface treated firstly, then coated with pure metals (i.e., Al, Cu, and Nickle). The metal encapsulation on CNT is expected to significantly improve the interfacial bonding between CNTs and the intimated metal matrices. The coated CNT powders were used to make sample materials through sintering, then a customized wire extrusion process was employed to fabricate wires. Measurement of material property improvements in mechanical strength, thermal conductivity, and electrical conductivity were conducted on both cylinder samples and extruded wires. In addition to the sintering process, casting on metal coated CNT powder was also investigated. The best results we achieved are summarized as follows. (1) The measured thermal conductivity of Al/CNT composite made with Ni-encapsulated CNTs and pure Al powders is about 85% better than that of pure aluminum fabricated. The measured electrical conductivity of fabricated Al/CNT is about 14-20% better than that of pure aluminum. (2) The measured electrical conductivity of Cu/CNT is about 14.5% better than that of pure copper fabricated. (3) The mechanical strengths of both Cu/CNT and Al/CNT (with about 1% wt. CNTs) are 70% better than pure metals although losing some material ductility. (4) Two-stage wire extrusion at high temperatures were designed and successfully conducted to fabricate wires of Metal/CNTs.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Compositional screening of Ce-doped (Gd,Lu,Y) 3 (Al,Ga) 5 O 12 ceramics prepared by quenching from melt and their luminescence properties

Quenching from the melt using an Optical Floating Zone furnace was investigated as a possible high-throughput preparation method in order to screen novel scintillating materials. To validate this method, polycrystalline rare-earth aluminum garnets and yttrium gallium aluminum garnets were synthesized and characterized by X-ray diffraction, photoluminescence and radioluminescence emission spectra as well as radioluminescence imaging and compared to the previously reported properties of those materials. In order to achieve rapid, but quantitative comparison of the materials, pellets fabricated from the synthesized powders were sintered; two different sintering conditions were investigated and compared. Therefore, a simplistic energy deposition and light absorption model for brightness of opaque samples under X-ray irradiation was developed to estimate the relative scintillation efficiency of the materials. Based on the results, Y 3 Al 5 O 12 , LuY 2 Al 5 O 12 and GdY 2 Al 5 O 12 seem to have the highest scintillation efficiency among the prepared samples.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Effect of Magnesium Dopant on the Grain Boundary Stability of Nanocrystalline Aluminum Powders during Cryomilling

In this investigation, pure aluminum (Al) powders were cryomilled with and without magnesium dopants to study (a) the effect of cryomilling time on the crystallite size and (b) the effect of magnesium dopant on Al to achieve grain boundary stability. The cryomilling process was carried out using liquid nitrogen for different durations. The characterization of the cryomilled powders was carried out using scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD) to understand the particle morphology, crystallite size, and elemental composition. The results demonstrated that the size of the crystallites in both Al and Mg-doped Al powders reduces as the cryomilling duration increases. The results also indicated that the preferential segregation of Mg dopant at the grain boundaries of Al provides stability to the cryomilled powders at elevated temperatures. This article discusses the mechanism for the changes in crystallite size and the effect of the Mg dopant on the grain boundary stability in Al powders.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Enhancement in Mechanical Properties of Bulk Nanocrystalline Aluminum by Grain Boundary Strengthening Mechanism

In the present work, commercially pure aluminum (Al) powders were milled at cryogenic temperatures (a) without magnesium (Mg) and (b) with 5 wt.% Mg powders for different durations. The cryomilled powders were analyzed using scanning electron microscopy (SEM), transmission electron microscopy (TEM), and x-ray diffraction (XRD) to determine the changes in particle morphology, elemental composition, and crystallite size. The results showed a reduction in crystallite size with the increase in cryomilling duration. Thereafter, the spark plasma sintering (SPS) process was carried out to manufacture bulk samples. The mechanical properties of the bulk SPS samples were assessed by conducting microhardness, tensile, and fatigue tests. The Vickers microhardness tests showed improved hardness for the Al-Mg bulk samples as compared to pure Al. The Al-Mg samples also showed an increase in tensile strength with increasing cryomilling time. Fatigue test results showed an improvement in Al-Mg components' high-cycle fatigue response. Furthermore, the mechanism for the enhancement in mechanical properties as a result of crystallite size reduction and grain boundary strengthening by the addition of Mg dopant is also discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Influence of microstructure and temperature on impact toughness of H13 steel produced by binder jet additive manufacturing

Binder Jet Additive Manufacturing (BJAM) is a promising manufacturing pathway to produce H13 steel dies and tooling with complex geometries for applications in high pressure aluminum die casting, hot stamping, and injection molding. While fully dense H13 coupons produced using BJAM have been subjected to detailed microstructure characterization, properties which are critical and relevant to the aforementioned applications, such as impact toughness, have not been reported. Here, this work evaluated the influence of microstructural characteristics and test temperature on the impact toughness of H13 produced by BJAM. Coupons were produced from three different powder size distributions (PSDs), with nominal powder size ranges of −22 μm, 10-32 μm, and 15-53 μm. Coupons were printed, sintered, hot isostatically pressed (HIPed), and heat treated by quenching and tempering. After HIPing, the measured porosities of the different PSDs were all less than 0.015 vol%. The −22 μm PSD BJAM material exhibited the best impact toughness of all three PSDs across the entire test temperature range from 25 to 400 °C, and also exhibited an ambient temperature impact toughness of 10.9 J at a hardness of 46 HRC, equivalent to minimum threshold requirements for premium grade H13. However, all three BJAM PSDs exhibited moderately lower impact toughness than premium grade wrought H13 from RT to 400 °C. We attribute this in part due to the very large prior-austenite grain (PAG) sizes near 400 μm and segregation from former liquid channels leading to greater amounts of carbide precipitation on PAG boundaries. Technical pathways for optimizing processing and chemistry of BJAM H13 to further improve impact toughness are discussed.

Binder jet additive manufacturing↗
DOE OSTI2020

Synthesis of bulk reactive Ni–Al composites using high pressure torsion

Self-propagating exothermic reactions, for instance in the nickel-aluminum (Ni-Al) system, have been widely studied to create high performance intermetallic compounds or for in-situ welding. Their easy ignition once the phase spacing is reduced below the micron scale, makes top-down methods like high-energy ball milling, ideal to fabricate such reactive nanostructures. A major drawback of ball milling is the need of a sintering step to form bulk pieces of the reactive material. However, this is not possible, as the targeted reactions would already proceed. Therefore, we investigate the ability of high pressure torsion as an alternative process, capable to produce bulk nanocomposites from powder mixtures. Severe straining of powder mixtures with a composition of 50 wt% Ni and 50 wt% Al enables fabrication of self-reactive bulk samples with microstructures similar to those obtained from ball milling or magnetron sputtering. Additionally, samples deformed at ambient temperature are highly reactive and can be ignited significantly below the Al melting point, finally predominantly consisting of Al 3 Ni 2 and Al 3 Ni, independent of the applied strain. Although the reaction proceeds first at the edge of the disk, the strain gradient present in the disks does not prevent reaction of the whole sample.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Irreversible Multielement Diffusion and the Resulting Compositional and Processing Flexibility in the Synthesis and Densification of Lithium Aluminum Lanthanum Zirconium Oxide

Despite the broad interest in Al-doped lithium lanthanum zirconium oxide (LLZO), the wide range of reported ionic conductivities suggests that the effect of processing parameters on the resulting phase purity and bulk conductivity is not well-understood. Here, in this work, we synthesized six separate series of LLZO with variations in Al concentration, Li excess, Li addition order, Li source, densification method, and mother powder to determine the effect on the composition, phase purity, density, and bulk conductivity. We found that a wider range of compositions (6.08–7.61 mol of Li and 0.06–0.23 mol of Al) than previously reported can result in cubic phase stability and that nearly all elements (Li, Al, Zr, and La) are lost to the MgO crucible during calcination and sintering. The manner in which different elements are lost is affected by the processing parameters. We observed that Al-doped LLZO shows great compositional flexibility in stabilizing the cubic phase, offering an explanation for the range of electrochemical performance metrics reported in the literature.

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

The Grain Boundary Relaxation (GBR) Approach for Manufacturing High Strength Nanocrystalline Lightweight Metals

The overarching goal of the project was to conduct research and development work as proposed in the Statement of Project Objective (SOPO) of the award document DE-FE-0009116. The project had 4 tasks and 12 milestones. All the milestone deliverables were completed. The accomplishments of the project objectives and technical discussions are described in Sections 3 and 4, respectively. The modeling and simulation work indicated that to increase the strength and stability of nanocrystalline aluminum (Al), selection of dopants, such as Mg, is necessary. It was predicted that the crystallite size should be less than 50 nm to give high strength. On the basis of modeling, cryo-milling of Al was conducted with the addition of Mg as a function of different times. The crystallite size of the cryo-milled powders was determined by XRD and TEM. Both measurements showed that the actual crystallite size of the grain was <40 nm. The thermal stability of the grain size was established as a function of temperature. It was established that the grain size was < 50 nm up to 500C. The crystallite size of the bulk sample prepared by spark plasma sintering (SPS) and cold spray (CS) additive manufacturing was less than <40 nm. The mechanical properties of the bulk samples prepared by SPS and CS, showed excellent microhardness, good tensile properties (>200 MPa) with moderate ductility and improved fatigue performance. Adding yttria stabilized zirconia (YSZ) improved the build thick of the CS sample, however the YSZ was getting embedded into the sample. A highly dense SPS samples sent for 3rd party testing to the Innovation Testing Services showed a minimum hardness of 180 HV with an average tensile strength of 512.5 MPa. The high cycle fatigue tests also showed an endurance limit of 179.5 MPa. The Energy cost evaluations showed an overall energy cost of around $\$$17.05 for the cryomilling and SPS processes and the total manufacturing cost calculations of $\$$78.14 for 1 kg of sample. The energy cost to prepare a Kg of CS sample is $\$$17.60 and the overall manufacturing cost is $\$$86.85.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Accelerating Manufacturing of Powder-Processed Strong, Lightweight and Thermally Stable Bulk Nanocrystalline Al Alloys via Engineered Interface States

The overarching goal of this program is to develop an integrated materials by design framework enabling a simple, scalable, and efficient manufacturing route for thermally stable nanocrystalline Al-based alloys with high specific strength over a range of service temperatures. The central scientific principle underpinning this program is the elucidation, and ultimately implementation in novel alloy design, of unique interfacial structures and chemistries driven by segregation in multi-component systems that give rise to unprecedented processability and properties. This program targeted nanocrystalline Al-based ternary alloys produced by mechanical alloying of powders followed by compaction and sintering with hot pressing, which are inherently scalable and inexpensive manufacturing routes, but when applied to nanocrystalline alloys are usually plagued by low density and/or poor retention of the intended nanostructures during processing. This program successfully demonstrated manufacturing of a bulk (>1 cm 3 ) nanocrystalline Al-based alloy with a combination of thermal stability, high temperature strength retention, and specific strength that exceeds the current-state-of-the-art of Al alloys. It is anticipated that the greatest technological impact will occur by demonstration of rapid and scalable manufacturing of bulk nanocrystalline Al alloys with exceptional thermal stability and mechanical performance, thus enabling increased energy efficiency in high performance power generation systems via: (i) replacement of existing components with lightweight Al-based alloys and (ii) increasing operating temperatures with property retention. The program focused on the development of a simple and efficient manufacturing route for thermally stable nanocrystalline Al-based alloys with high specific strength over a range of service temperatures. The program is expected to have direct impact on scalable and economic manufacturing of bulk nanocrystalline alloys. This program profited from the recent discovery by the project team of segregation-driven amorphous intergranular films in nanocrystalline metallic alloys that can be kinetically frozen-in at sub-solidus temperatures. These interfacial states (also known as amorphous complexions) comprise a large fraction of the total material in nanocrystalline alloys and are responsible for two beneficial characteristics that anchor the proposed work: (1) activated sintering leading to high density and (2) retained nanostructures leading to high strengths that approach a substantial fraction of the theoretical limit. More specifically, these engineered interfaces led to a three-fold benefit: (i) high-throughput materials processing with low energy budget and cost, (ii) exceptional thermal stability, and (iii) high specific strength at both room temperature and intermediate temperatures experienced during service.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗