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At least 829 records · Page 46
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Additive manufacturing of complexly shaped SiC with high density via extrusion-based technique – Effects of slurry thixotropic behavior and 3D printing parameters

Here, additive manufacturing of dense SiC parts was achieved via an extrusion-based process followed by electrical-field assisted pressure-less sintering. The aim of this research was to study the effect of the rheological behavior of SiC slurry on the printing process and quality, as well as the influence of 3D printing parameters on the dimensions of the extruded filament, which are directly related to the printing precision and quality. Different solid contents and dispersant- Darvan 821A concentrations were studied to optimize the viscosity, thixotropy and sedimentation rate of the slurry. The optimal slurry was composed of 77.5 wt% SiC, Y 2 O 3 and Al 2 O 3 powders, 0.25 wt% dispersant and 0.01 wt% defoamer. The printing parameters studied included extrusion pressure, nozzle size, layer height and printing speed; the one that had the most prominent effect on filament width and height was indicated as layer height. The nozzle inner diameter of 1.04 mm, speed of 350 mm/min, layer height of 0.7 mm and extrusion air pressure of 0.31 MPa were the optimal printing parameters. Furthermore, the relationship between the printing parameters and the filament dimensions was successfully predicted by using machine learning and grey system theory. Finally, the relative density of the printed SiC parts sintered at 1900 oC reached 94.7±1.5%.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Recent advances in single-atom catalysts and single-atom alloys: opportunities for exploring the uncharted phase space in-between

Single-atom catalysts (SACs) have gained significant world-wide attention for exhibiting distinct reactivity and selectivity for important reactions, while utilizing precious metals at the ultimate limit of efficiency. SACs involving reducible oxide supports are good catalysts for oxidation reactions, and metal-acid site pairs enable Csingle bondC bond formation, but SACs can deactivate by sintering under reducing conditions. On the other hand, single-atom alloys (SAAs) are robust towards sintering and exhibit exceptional catalytic performance for a wide range of reactions under reducing conditions but can deactivate under oxidizing environments. Therefore, there is tremendous opportunity to explore and exploit catalytic reactivity between the SAC and SAA extremes. Furthermore, this paper focuses on recent advances in both fields and highlights prospects for future research.

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

Effects of various parameters of different porous transport layers in proton exchange membrane water electrolysis

Porous transport layers (PTLs) play an important role in proton exchange membrane water electrolysis (PEMWE) cells. The PTL facilitates water and gas transport, as well as thermal and electrical conduction, and is required to sustain good contact with adjacent components. It is expected that using PTLs with variations in material properties such as structure, composition, thickness and wettability results in performance changes of the PEMWE. Here, a general mathematical PEMWE model is developed that separates and analyzes the contributions of ohmic, activation, diffusion and Nernst potentials. For model validation, three inherently different anode PTL structures (carbon paper, sintered titanium particles, and titanium felt) are operated over a range of conditions. Additionally, the effects of PTL wettability were used to verify the model using Polytetrafluoroethylene (PTFE) treated Toray papers with PTFE loading ranging from 0% to 20%. The modeling results of both PTFE treated and untreated materials show good agreement with the experimental data. Mass transport or diffusion loss is the primary reason for performance differences between PTFE treated and untreated PTLs. Sintered titanium PTLs with thicknesses above 1 mm suffer from up to 33% increased ohmic losses without indicating any obvious changes in activation and diffusion losses when compared to untreated PTLs. The losses of the cell increase when using PTFE treated Toray paper. Individual contributions are quantified and assigned to increased ohmic, activation, and diffusion losses. In conclusion, the proposed model offers insights into the overpotential contributions of a PEMWE. It is a useful tool for predicting performance of various PTL materials and can be applied for PTL development and optimization efforts.

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

Conductive spinels derived from Co–Mn based alloy precursor for SOFC cathode-side contact application

The utilization of gas-atomized Co–Mn based alloy precursor is a promising approach to lowering the sintering temperature of the spinel contact layer and enhancing its performance. In this work, simulated interconnect/contact/cathode cells are employed to investigate the effects of different metallic precursors (i.e., three Co–Mn based alloy powders and a mixture of Co + MnO 2 powders) on the microstructure and performance of the reactively-sintered MnCo 2 O 4 -based contact layer. While excellent overall electrical performance is observed for all the cells with the four contact precursors during 1000-h testing at 800 °C in air, the cell with the Ce-doped alloy contact precursor shows the lowest cell area specific resistance (ASR) and ASR degradation rate. Cross-sectional observation of the tested cells is conducted to assess the compatibility of the contact layer with adjacent components as well as its effectiveness in reducing the Cr 2 O 3 scale growth and blocking Cr migration from the interconnect to the cathode.

08 HYDROGEN↗
DOE OSTI2022

Reticulated porous lanthanum strontium manganite structures for solar thermochemical hydrogen production

Porous ceramic foams are utilized in various fields and applications due to their advantageous properties such as high porosity, high specific surface area, and controlled permeability. Non-stoichiometric oxide foams are of particular interest for the solar thermochemical production of hydrogen in directly irradiated solar receivers due to their enhanced heat transfer capabilities and structural integrity. Here we report the fabrication of lanthanum strontium manganite replica foams and their solar thermochemical water splitting performance. Highly porous (>80%) foams were produced with controlled structure and tested in a high temperature water splitting furnace to demonstrate stability and overall performance. The temperature profile of the burnout and sintering of the foam structure were altered based on simultaneous differential scanning calorimetry and thermal gravimetry analysis. Two-step sintering was used both to retain micron-sized pores (D50 = 0.4 μm) on the foam's struts and to limit grain growth to a grain size of ~1 μm. The structural characteristics were confirmed by porosimetry and scanning electron microscopy. The foams were repeatedly cycled, producing approximately 200 μmol/g of H 2 per cycle. Water splitting performance was tested for 50 cycles and approximately 35 h at 1400 °C. No statistical difference in the effective hydrogen production per cycle was observed, which is promising for long-term redox cycle stability.

08 HYDROGEN↗
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 OSTI2026

Aluminum bonded SmCo5 magnets with enhanced mechanical strength

Despite their versatility and easy manufacturability, polymer-bonded magnets find limited application due to their limited mechanical properties and temperature resistance. In this study, we developed mechanically robust, aluminum-bonded SmCo5 magnets by utilizing a low-temperature, shear-assisted friction consolidation technique. Bonded magnets with varying magnetic phase content were fabricated at processing temperature of 500°C, and their microstructures, magnetic, mechanical, and electrical properties were systematically investigated. The resulting bonded-magnets showed effective consolidation with nanocrystalline microstructures. Magnetic properties were found to be tunable through variations in binder phase content, with coercivity reaching values up to 15.3 kOe (1217.5 kA/m) and maximum magnetic energy product up to 3.6 MGOe (28.7 kJ/m3), which are comparable to other bonded magnets. Electrical resistivities were lower than the polymer-bonded magnets, but comparable to the sintered ones. We observed an average flexural strength of 223 MPa for 60 vol.% SmCo5/Al sample, which is nearly two times higher than the reported values for sintered and bonded Sm-Co magnets. Our research demonstrated an effective approach to fabricate metal-bonded permanent magnets with superior magnetic and mechanical properties potentially applicable for high temperature applications.

Poudel Chhetri, Tej Bahadur↗
DOE OSTI2024

Stabilization and manipulation of highly concentrated copper single atoms by high entropy oxides

Facile and controllable methodologies capable of providing single atom catalysts (SACs) with high-density active metal sites and sintering-resistance under harsh conditions are highly desired and grand challenges in heterogeneous catalysis. Herein, the entropy effect was leveraged to stabilize and manipulate the electronic properties of copper SACs. The as-developed ultrasonication-driven approach could integrate highly concentrated Cu SAs within the lattice of fluorite-structured high entropy oxide (HEFO) under ambient conditions (CuO-HEFO). The dual benefits from the high entropy effect of the support and the in-situ lattice engineering led to the generation of abundant Cu 1+ species and oxygen defects, together with ultra-high stability and sintering-resistance under extremely harsh conditions. This was confirmed by deploying non-high entropy support (CuO-CeO 2 ) or Cu sites located on the surface of HEFO (CuO@HEFO). In conclusion, the catalytic activity of CuO-HEFO surpassed that of CuO-CeO 2 and CuO@HEFO in CO oxidation together with well-maintained long-term stability and resistance to gas impurities.

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

Densification of the entropy stabilized oxide (Mg 0.2 Co 0.2 Ni 0.2 Cu 0.2 Zn 0.2 )O

The first entropy-stabilized oxide, (Mg 0.2 Co 0.2 Ni 0.2 Cu 0.2 Zn 0.2 )O, was reported in 2015. Initial studies synthesized this material using solid state processing and were limited to densities < 80%. Here, we report a straightforward solid state route to sinter samples to densities up to 98% of the theoretical by identifying the role of oxygen and promoting the resulting mechanisms in densification. Previous works have studied effects of cation stoichiometry on the entropy-driven reaction to form a single phase, but few have explored the associated effects of anion stoichiometry and/or redox chemistry on both phase stability and densification. We demonstrate here that tuning heating rate and pO 2 during heating of initially-homogeneous calcined powders can enhance densifying diffusion processes and enable reliable sintering of dense (Mg 0.2 Co 0.2 Ni 0.2 Cu 0.2 Zn 0.2 )O samples.

MATERIALS SCIENCE↗
DOE OSTI2025

Direct ink writing of aqueous-based Gadolinium (III) oxide slurries

Gadolinium (III) oxide (gadolinia, Gd 2 O 3 ) has recently been identified as an intriguing material for applications in the medical, solid oxide fuel cell, and nuclear industries. This interest drives the need for developing and understanding manufacturing techniques that can produce dense Gd 2 O 3 structures. Direct ink writing (DIW), an extrusion-based additive manufacturing method, has also garnered interest because of its capability to produce dense ceramic parts with increased complexity in an economical manner. In this study, DIW was explored as a manufacturing technique for Gd 2 O 3 . Experiments were performed to develop Gd 2 O 3 bearing inks capable of being processed via DIW. Ink solids loading and sintering temperatures were varied to assess their impact on the final density and microstructure. Optimum sintering conditions are proposed and were experimentally verified at a dwell temperature of 1500°C. Gd 2 O 3 samples were successfully manufactured using DIW, achieving densities greater than 96 % of the theoretical density.

36 MATERIALS SCIENCE↗
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 OSTI2025

High temperature tensile properties of H13 tool steel fabricated via binder jet additive manufacturing

H13 is one of the most used steels for hot work tooling applications like die casting. Binder jet additive manufacturing (BJAM) offers a cost-effective solution to fabricate tools with performance enhancing features like internal cooling channels. While full densification of BJAM H13 has been demonstrated in the literature, the room and high temperature tensile properties of the material, and the effect of post-process treatments like hot isostatic pressing (HIP), and heat treatment (HT) are unknown. Here we use HIP+HT to obtain a combination of ultimate tensile strength (UTS) and elongation to failure that is superior to H13 fabricated via laser powder bed fusion and wire arc additive manufacturing. HIP+HT BJAM H13 has a superior UTS (1836 MPa) compared with conventionally processed (1671 MPa) H13 but has lower plastic elongation. We report that as-sintered samples have an extensive network of continuous grain boundary (GB) carbides that contribute to brittle fracture. HIP+HT results in partial dissolution of GB carbides and formation of a fine martensitic microstructure resulting in superior tensile strength and elongation compared with as-sintered H13. We use thermo-kinetic calculations to rationalize the effects of HIP+HT on microstructure and properties.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Additive manufacturing of silicon carbide for nuclear applications

Additive manufacturing (AM) is a rapidly evolving technology being considered for nuclear applications. A special focus on AM to fabricate nuclear-grade silicon carbide (SiC) is explored in this paper. First, we present currently available AM processing options for SiC. AM methods commonly used for other ceramics, in which the feedstocks are forms of polymers, powders, and/or reactive chemical vapors, are also applicable to SiC. SiC phases are formed by pyrolysis of pre-ceramic polymer, direct reaction of powder precursors, sintering of SiC powders, or chemical vapor deposition/infiltration. Second, we discuss how the different microstructures of SiC materials fabricated by various processing methods affect their behavior in nuclear environments. Third, we discuss state-of-the-art AM technologies for the fabrication of relatively pure SiC, which show great potential to retain its strength under neutron irradiation: (1) binder jet printing followed by chemical vapor infiltration, (2) laser chemical vapor deposition, and (3) selective laser sintering of SiC powders.

36 MATERIALS SCIENCE↗
DOE OSTI2025

UO2 microstructural evolutions induced by Ni, Mo, and W dopants for intentional forensics

The concept of tagging nuclear fuel with a chemical barcode to enable forensics analysis across the nuclear fuel cycle is an area of active investigation, particularly to ensure fabrication viability without disrupting current fuel performance. This study explored the feasibility of using Ni, Mo, and W isotopic double-spikes as dopants in UO2 fuel from the perspective of fuel fabrication. Doped UO2 pellets were produced using conventional fuel fabrication processes, including powder mixing, sieving, pressing, and sintering in a reductive atmosphere. Two composition levels, 100 and 1000 ppm, were evaluated for each dopant element with isotopic double-spike configurations. For the Ni system, additional dopant concentrations of 250 and 500 ppm were produced with nonperturbed isotopic ratios. The results demonstrated that successful incorporation of Ni, Mo, and W double-spikes into UO2 pellets occurred with minimal shift in final density or dopant loss during pellet fabrication. Isotopic analysis confirmed the presence of the double-spike signature even when diluted with natural isotopic material in ratio of 1:5 in the fabrication process. Microstructural examinations revealed different impacts on grain size compared with undoped UO2. This study showed that Ni incorporation up to ∼500 ppm promoted moderate grain growth, whereas the Mo and W systems caused grain size reduction at all concentrations. Changes in the UO2 lattice parameter as a function of composition were detected exclusively for Ni up to 500 ppm, indicating that the Ni solid solution was the main factor for the observed grain growth. Insoluble (Mo and W) or supersaturated (Ni > 500 ppm) conditions produced grain size reduction. The Ni-doped pellets in the solution range resulted in a final microstructure within fuel specifications, demonstrating its potential benefits of employing complex dopant systems for potential nuclear forensic applications.

36 MATERIALS SCIENCE↗
DOE OSTI2026

The influence of iron incorporation on the microstructure and crystal chemistry of UO 2 fuel

The incorporation of dopants into UO 2 is of interest for both doped advanced fuel and nuclear forensics research. Suitable forensics dopants, or taggants, for nuclear fuels are ones that do not adversely affect the performance of the parent material while still being traceable during key stages of the fuel’s life cycle. In this paper, we present our efforts to understand the effects of doping UO 2 with Fe 2 O 3 under multiple parameters, such as Fe concentration (0–3000 wppm), sintering temperature (1673 K, 1773 K, and 1973 K), sintering time (2–12 h), and atmosphere (reducing and inert). Here, we investigated densification behavior, microstructure evolution, and lattice defects based on the geometric densities, scanning electron microscopy (SEM), X-ray diffractograms, and Raman spectra. The effect of Fe on the microstructure and crystal chemistry of UO 2 is very complex, especially at the intermediate temperature (1773 K), where we found that densification kinetics are enhanced and that lattice contraction occurs for doping concentrations greater than 1000 wppm Fe.

Crystallography↗
DOE OSTI2025

Etching-assisted upcycling of Ni-lean to Ni-rich cathode materials

Upcycling is recognized as a sustainable recycling approach for spent lithium-ion batteries. However, existing upcycling methods typically involve intricate pretreatment or post-treatment steps, complicating their practical application. Here, in this study, we propose a straightforward, etching-assisted upcycling method that effectively transforms polycrystalline Ni-lean cathodes into high-performance single crystal Ni-rich cathodes. During the etching step, nickel acetate was dissolved into acetic acid and then polycrystalline NMC111 are etched in the solution. Finally, polycrystalline NMC111 are converted into single crystal particles coated with amorphous nickel acetate. This significantly enhances elemental diffusion during subsequent sintering by minimizing both particle size and the contact distance between NMC111 and nickel acetate. As elemental diffusion is improved and acetate ions decompose completely during sintering, the process requires neither additional pretreatment nor post-treatment. The resulting cathode materials (Etched-UP622) exhibit superior structural and electrochemical properties compared to the Control622, achieving an energy density of 719.7 Wh/kg, approximately 56.7 mAh/g higher than Control622 and 125.5 Wh/kg higher than NMC111. Etched-UP622 also delivers higher discharge capacity, improved rate performance and cycling stability, surpassing Control622 and NMC111. Meanwhile, NMC811 also can be synthesized by the proposed strategy, and the discharge capacity can reach 166.9 mAh/g at 1C, similar to 14 mAh/g higher than Control811. Overall, this etching-assisted strategy simplifies the upcycling process and offers a scalable, sustainable route for producing high-quality cathode materials.

Acid etching↗
DOE OSTI2026

The structure, composition, and performance impact of a YSZ-GDC interdiffusion layer in solid oxide electrolysis cells

This study provides a combined experimental and computational investigation into the structure and impact of the cation interdiffusion layer that appears at the gadolinium doped ceria (GDC)/yttria stabilized zirconia (YSZ) interface in solid oxide electrolysis cells (SOECs). Scanning transmission electron microscopy (STEM) illustrates that a ∼0.4 μm interdiffusion layer (IDL) with an intermixed cation distribution and fine grain size forms upon sintering. STEM identifies that the interdiffusion layer exists in the cubic fluorite structure despite changes in cation composition. The interdiffusion layer microstructure formed during sintering does not change during SOEC testing at either 1.3V or heightened voltage pulse testing. Modeling predicts that ionic conductivity may decrease in the interdiffusion layer due to Coulombic trapping between mobile oxygen vacancies and excess Gd 3+ acceptor dopants. Yet, the density and continuous nature of the layer should benefit cell stability by substantially reducing the formation of SrZrO 3 , which is corroborated by STEM and Synchrotron X-ray diffraction (XRD). We conclude that the interdiffusion layer acts as a beneficial barrier to Sr diffusion, when operating in a regime where electrolyte void formation is not observed.

organic↗