We present an investigation of Fe-14Cr-3W-0.4Y-0.4Zr-0.18Ti (wt.%) as a reduced-activation oxide-dispersion strengthened (ODS) ferritic steel, an alternative to the "14YWT" structural alloys designed for nuclear energy applications. Gas atomization reaction synthesis (GARS) was used to produce these Zr-modified powders with a non-equilibrium (metastable) phase that enable a heat treatment (delayed) route for producing nanoscale oxidedispersion strengthening. In situ synchrotron X-ray diffraction and transmission electron microscopy were used to analyze phase evolution as a function of temperature and time, revealing formation of highly dispersed oxide nanoprecipitate phases at temperatures above those needed for powder consolidation and shaping of components. This would allow fabrication of net-shape parts using conventional powder-processing methods prior to thermal activation of a reaction producing nanocrystalline Y-(Ti, Zr)-O particles, with a size of 20 +/- 7 nm. These results can inform processing of tubes, cladding, sheets, and plates for use in advanced fission and fusion reactors.
Nickel-based alloys have a wide variety of structural applications due to their high corrosion resistance and mechanical strength which depend on solid solution strengthening, or the formation of oxides and/or intermetallic precipitation for their properties. In this study, the microstructure of six Ni-Cr-Y-Ti-Al powder batches designed for the production of oxide dispersion strengthened nickel were compared. These batches varied in chemistry and atomization technique used which included Gas Atomization Reactive Synthesis (GARS). The batches of powder were then consolidated via Additive Manufacturing (AM) Powder Bed Fusion using Laser Beam (PBF-LB) and characterized via transmission electron microscopy to elucidate the influence of powder feedstock (i.e. synthesis methodology and chemistry) on the PBF-LB microstructure. The study investigates (i) how the amount of yttrium and titanium additions in the powder feedstock and the addition of oxygen during the processing (through GARS) affect the microstructure of the powder itself and the AM printed microstructure, and (ii) how the control of oxygen addition in the printing atmosphere during the PBF-LB printing process itself is another important parameter for achieving the formation of the wanted oxide dispersion versus the stabilization of the cellular structure (often observed in AM processed alloys). Microstructural characterization of both powder particles and additively manufactured nickel alloys in this study provide important insights into the movement of yttrium within the material upon solidification, particularly along cell boundaries, and how yttrium behaves depending on alloy chemistry. When a threshold of yttrium content is reached within the system, yttrium consistently reacts to form an intermetallic along cell boundaries instead of forming oxide nanoparticles.
The properties of metal produced through powder metallurgy depends on the feedstock used. Powders produced via gas atomization reaction synthesis (GARS) are used to produce oxide dispersion strengthened alloys. The desired powder size range can vary for each consolidation technique. However, powder microstructure also can vary with powder particle size, which in turn can impact the microstructure and properties of the consolidated parts. In this study, GARS powders are characterized via inductively coupled plasma mass spectroscopy, inert gas fusion, and high-resolution x-ray diffraction to determine variations in elemental and phase compositions. Transmission electron microscopy was used to understand microstructure variations as a function of chemistry and size. Across the three batches tested intermetallic content was 0.73-1.35 wt% in the 0-20 mu m powder batch and increased to 2.46-3.80 wt% in the coarse 45-106 mu m batch. Across all batches, volume percent of surface oxidation decreased with powder diameter, with volume percents within the range of 0.75-1.2 % across 10 mu m powder particles, and below 0.4 % across coarse powder particles approximately 100 mu m in diameter. These observations were supported by inert gas fusion measurements. However, the oxide layer was thicker in coarse powder particles due to a slower cooling rate. Increasing oxygen content in atomization gas to 2000 ppm and adding yttrium increased both the surface oxidation content and yttrium intermetallic content. Lastly, inter- metallic phases within the powder coarsened with powder size. Intermetallic morphology changed from fine spherical intermetallic and columnar dendritic growth to a cellular structure with finer spherical intermetallic, to coarse irregular intermetallic and intermetallic along grain boundaries as a result of slower cooling rate and solidification rate in coarse powder particles. The addition of zirconium does not appear to significantly change intermetallic morphology, but the composition changed from a Y-Fe rich intermetallic to a Y-Zr-Fe intermetallic.
Oxide Dispersion Strengthened (ODS) steels are promising candidate alloys for structural and cladding applications in extreme environments. They contain a high density of nanoscale oxides for high temperature mechanical strength and radiation resistance. In this work, gas atomization reaction synthesis (GARS) was used to produce powders that were used for additive manufacturing (AM) Laser Powder Bed Fusion consolidation of ODS steels, in order to skip the traditional mechanical alloying of blended yttria and alloy powders. Powder containing iron, chromium, and tungsten with varying amounts of yttrium, titanium, oxygen and zirconium were used to produce ODS steel samples. AM consolidated specimens and powder samples were characterized with transmission electron microscopy. TEM imaging, diffraction patterns, and energy dispersive X-ray spectroscopy (EDS) was used to identify phases present before and after consolidation across chemistries. The effect of the controlled oxygen input (from GARS) and the oxide-forming additions (Y, Ti, Zr) on precipitate size distribution and composition is substantiated and discussed.
Fe−6.5%Si has higher electrical resistivity, lower magnetocrystalline anisotropy, and lower magnetostriction than traditional Fe−3.2%Si silicon steel. The reduced iron losses of Fe−6.5%Si render it a highly favorable candidate for high-speed motors and transformers. However, large-scale production of wide Fe−6.5%Si tape by rapid solidification can be challenging mainly because of its high melting point. In this work, boron is alloyed to Fe−6.5%Si to reduce its melting temperature and interfacial energy to improve the alloy’s processability. Boron additions from 0.01 wt.% to 2.24 wt.% into Fe−6.5%Si and its effect on ribbon thickness, grain size, magnetic, and mechanical properties were studied. Minor boron alloying significantly changed the melt pool stability and wetting on the quench wheel and in turn increased the quench rate with minimum impact on the magnetic saturation and ductility. Boron addition of < 0.06 wt.% was also found beneficial to the magnetic property of the alloy by lowering both its hysteresis and eddy current losses.
Lithium-ion batteries offer the highest energy density of any currently available portable energy storage technology. By using different anode materials, these batteries could have an even greater energy density. One material, tin, has a theoretical lithium capacity (994 mAh/g) over three-times higher than commercial carbon anode materials. Unfortunately, to achieve this high capacity, bulk tin undergoes a large volume expansion, and the material pulverizes during cycling, giving a rapid capacity fade. To mitigate this issue, tin must be scaled down to the nano-level to take advantage of unique micromechanics at the nanoscale. Synthesis techniques for Sn nanoparticle anodes are costly and overly complicated for commercial production. A novel one-step process for producing carbon-coated Sn nanoparticles via spark plasma erosion (SPE) shows great promise as a simple, inexpensive production method. The SPE method, characterization of the resulting particles, and their high-capacity reversible electrochemical performance as anodes are described. With only a 10% addition of these novel SPE carbon-coated Sn particles, one anode composition demonstrated a reversible capacity of ~460 mAh/g, achieving the theoretical capacity of that particular electrode formulation. These SPE carbon-coated Sn nanoparticles are drop-in ready for present commercial lithium-ion anode processing and would provide a ~10% increase in the total capacity of current commercial lithium-ion cells.
Oxide dispersion strengthened (ODS) steels, traditionally fabricated by ball milling and conventional powder metallurgy techniques to achieve bulk form, followed by intricate rolling and thermal treatment steps to achieve plate or sheet form. Here, we present a novel processing route that combines cold spray (CS) with friction stir processing (FSP) to manufacture ODS steel plate directly from gas atomization reaction synthesis (GARS)-prepared powder, thus no rolling steps involved. Microstructural and mechanical characterizations were performed to assess the quality and properties of the resulting ODS steel plate. Our findings demonstrate that the slightly porous CS deposited layer was fully consolidated after FSP, yielding a fully dense ODS steel plate that exhibited a favorable tradeoff between strength and ductility upon extraction from the substrate. Furthermore, through microstructural analysis, we revealed the presence of an appreciable density (similar to 10(22)/m(3)) of nano-sized oxide particles, with the majority being smaller than 5 nm via the combined CS + FSP fabrication route. This work serves as a first proof-of-concept demonstration of the manufacturing approach described herein, offering a possible alternative route for producing ODS steel plates.
Dy-free sintered magnets were fabricated by blending Neo powder with different grain boundary diffusion alloy powders. Cu, CeAl and CeAlCu have a negative effect on H cj of magnets, while PrAlCu and AlCuGa have a positive effect. The PrAlCu-added magnet achieves the best magnetic properties among all magnets with the additions of different diffusion alloys. With increasing PrAlCu from 0-10 wt.%, H cj of the magnets gradually increases from the original 14.5 kOe to 19.2 kOe. The magnet with 7.5 wt.% PrAlCu obtains a H cj of 18 kOe and (BH) max of 39.1 MGOe. It is found that Pr and Cu in PrAlCu alloy is mainly distributed at grain boundary and triple junctions, leading to a reduced coupling among grains, thus an enhanced H cj . The grain boundary engineering by adding an appropriate alloy is an effective method to improve H cj of Dy-free NdFeB magnets.
Previous research suggested that friction-based processing is a promising method for fabricating oxide dispersion-strengthened (ODS) steel. In this study, we combined friction consolidation and friction extrusion to successfully manufacture ODS steel rods using precursor powder made with gas atomization reaction synthesis. We examined the microstructure evolution from the initial powder to the final extruded rod, which revealed the dispersion process of Y. Additionally, by comparing the microstructures of three rods extruded at different temperatures, we showed that low-temperature friction extrusion effectively enhanced microstructure uniformity and prevented grain coarsening, leading to improved mechanical properties. Our findings provide practical guidelines for adjusting processing parameters in the production of ODS steel using friction-based processing.
High density portable energy storage is desirable owing to the energy requirements of portable electronics and electric vehicles. The Li-ion battery’s high energy density could be even further improved through the utilization of alternative materials (instead of carbon) for the anode, such as Sn or Si. Nonetheless, the large volume expansion upon lithiation, up to ~300% for Li22Si5, causes pulverization and rapid capacity degradation during cycling. Sn also forms a Li22Sn5 compound with the equivalent stoichiometric Li capacity but with enhanced ductility. Nano-sized Si and Sn have demonstrated distinctive nanoscale properties, facilitating the retention of higher capacities, particularly when coated with carbon, which improves mechanical stability. To date, the methods of synthesizing coated Si, Sn, or Si-Sn alloyed nanoparticles are complicated, costly, and not readily scalable to meet the demands of cost-effective manufacturing. Spark plasma erosion in a hydrocarbon dielectric has been explored as a one-step process to produce Sn-Si alloy nanoparticles coated with a thin carbon film, offering a scalable and cost-effective processing route. The resulting Sn-Si particles exhibited a bi-modal size distribution at ~5 nm and ~500 nm and were carbon-coated, as intended, from the hydrocarbon dielectric breakdown. The spark-eroded nanoparticles were thoroughly characterized using TEM/EDS, XPS, AES, SSNMR, and TGA, and their improved electrochemical performance was assessed through half-cell experiments.
Density-functional theory (DFT) is used to identify phase-equilibria in multi-principal-element and high-entropy alloys (MPEAs/HEAs), including duplex-phase and eutectic microstructures. A combination of composition-dependent formation energy and electronic-structure-based ordering parameters were used to identify a transition from FCC to BCC favoring mixtures, and these predictions experimentally validated in the Al-Co-Cr-Cu-Fe-Ni system. A sharp crossover in lattice structure and dual-phase stability as a function of composition were predicted via DFT and validated experimentally. The impact of solidification kinetics and thermodynamic stability was explored experimentally using a range of techniques, from slow (castings) to rapid (laser remelting), which showed a decoupling of phase fraction from thermal history, i.e., phase fraction was found to be solidification rate-independent, enabling tuning of a multi-modal cell and grain size ranging from nanoscale through macroscale. Strength and ductility tradeoffs for select processing parameters were investigated via uniaxial tension and small-punch testing on specimens manufactured via powder-based additive manufacturing (directed-energy deposition). This work establishes a pathway for design and optimization of next-generation multiphase superalloys via tailoring of structural and chemical ordering in concentrated solid solutions.
The overall Science-based Acceleration of the Full Value Stream for Metal Additive Manufacturing (AM): Expedited Powder Development and Additive Manufacturing Deployment (“X-P4AM”) project objective is to drastically reduce the time-to-market barriers for new additive alloys of interest in automotive and aerospace applications, through computational alloy design with rapid screening and down- selection via synthesis of candidate alloys with rapid solidification. The project will also refine the technology in high pressure gas atomization to improve the production of commercial quantities of selected powders with high powder yields and enhanced powder quality. A new aluminum (Al) alloy based on an Al-Ce-X composition, enhanced powder production, and optimized AM build parameterization provided a critical step in widespread adoption of AM technology for automotive applications, in this case. The individual background and capabilities of the Party are ideally suited to the successful execution of this work. The included work enhanced the Contractors’ AM capabilities, a core competency of the Contractors, and developed a close working relationship with the Participant in the area of aluminum powder alloys and their end use.
Dy-free sintered magnets were fabricated by blending Neo powder with different amount of PrCu powder. With increasing PrCu from 0-10 wt.%, Hcj of the magnets gradually increases from the original 14.5 kOe to 18.6 kOe. The highest (BH)max achieved was 35.0 MGOe with 7.5 wt.% PrCu. It was found that PrCu was mainly distributed at grain boundary and triple junctions, leading to a reduced coupling among grains, thus an enhanced Hcj. The grain boundary engineering by the diffusion of PrCu alloy is an effective method to improve Hcj of Dy-free magnets.