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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 19 records

Systematic analysis of melt pool dynamics in laser processing of mixed powder feedstocks

Functionally graded materials (FGMs) fabricated via additive manufacturing of blended powders offer the potential to spatially tailor properties for new technologies, such as fusion first-wall systems, turbine blades, and spacecraft. However, processing these materials is difficult due to the multiplicity of processing parameters to optimize, all of which must be changed as substrate material, powder feedstock compositions, and melt pool dynamics evolve. Here, this work systematically evaluates the qualitative and quantitative effects of these variables on the melt pool size, shape, composition, and particle distribution in an exemplar Ti-Ta system, and connects the experimental results to Marangoni flow behavior and phenomena observed in other systems. Increasing laser power linearly increases melt pool size and layer thickness, driving engineering considerations such as part/geometrical tolerances. Decreasing laser velocity changes the melt pool shape from lenticular to convex and reduces chemical homogeneity due to extreme thermal and compositional gradients between the melt pool center and boundaries. Thermophysical property differences between the powder feedstock and substrate material, as well as the directionality of the gradient, affect dilution and melt pool dynamics, which in turn affect the melt pool boundary characteristics, shape, and uniformity. Mixed powder feedstocks of intermediate compositions do not behave according to linear interpolations between single-material endpoints, instead building taller and wider melt pools. As such, it is recommended to quantify process maps for at least one intermediate composition in the FGM or multi-material system of interest to ensure optimized processing parameters, predictable melt pool sizes and shapes, and compositional and spatial precision.

Dissimilar↗

Fatigue of laser powder bed fusion processed 17-4 stainless steel using prior process exposed powder feedstock

The rapid pace of development seen in the metal additive manufacturing (AM) process of laser powder-bed fusion (LPBF) requires in-step advances in processes qualification to enable full-scale adoption. This particularly applies to quantifying how powder feedstock conditions impact end-component quality. Here this study examines how in-machine 17-4 stainless steel powder feedstocks are affected by prior LPBF processes, and how these effects impact subsequent builds. Examinations of powder morphology, chemistry, flowability, and rheology were conducted to characterize the powder conditions. The resultant effects of powder feedstock condition on produced component quasi-static tensile and high-cycle fatigue properties were analyzed. Fatigue life was analyzed using a reliability modeling approach that enabled a robust statistical comparison of life. Powder characteristics were found to evolve with powder exposure to prior LPBF processes, particularly in the extremes of powder size distribution and measures of bulk flow. No significant effects of these changes on tensile properties were observed. Reliability modeling methods, including the lognormal and Weibull distributions as well as the empirical survival function, are shown to be effective tools for modeling fatigue variability in LPBF manufactured components. Through these tools, fatigue life was found to be invariant with changes in powder condition.

42 ENGINEERING↗

Binder jetting additive manufacturing of silicon carbide ceramics: Development of bimodal powder feedstocks by modeling and experimental methods

A limitation of binder jetting additive manufacturing is the low density of fabricated parts. Mixing powders with different sizes is a promising approach to increase powder bed packing density and, hence, printed part density. However, in previous studies mixed powder feedstock was prepared by trial and error method. In this research, both modeling and experimental methods were used to prepare the bimodal powder feedstocks. Analytical packing model was introduced for irregular powders. A bimodal powder was prepared by mixing two different-sized silicon carbide powders (i.e. coarse and fine) using ball mill, and their tap densities were measured. Silicon carbide plates were printed using the coarse and bimodal powders by a commercial binder jetting system. Results showed that the modeling method could predict the tap density of bimodal powders with high accuracy. The printed parts from bimodal powder achieved higher green densities than those from the unimodal powder.

36 MATERIALS SCIENCE↗

Developing New Polymeric Powder Feedstocks for Selective Laser Sintering: Emphasizing Particle Size and Shape

Although selective laser sintering is considered a major player in the additive manufacturing community, significant limitations exist when it comes to processing the polymeric powder feedstocks in the laser sintering machine. While these limitations – such as inadequate and uneven heating and complex thermal phenomena leading to curling and shrinkage – cannot be ignored and are being addressed in the community, it is also vitally important to turn our attention to the expansion of commercially available powder feedstocks. A major drawback of SLS is the lack of available feedstocks. At Los Alamos National Laboratory, a primary desire for advancement in the manufacturing or development of new feedstocks lies in the nuclear weapons applications program. New feedstocks with greater thermal stability and performance would provide the opportunity for insertion of production parts, rather than just prototype parts. Additionally, the ability to print with so-called commodity polymers like polyethylene and polypropylene poses great economic advantages for prototyping and production of large batches of parts. However, a gap exists between the Lab’s needs and what is commercially available – a gap which could be filled by collaboration with the broader industrial sector. Furthermore, connecting with and building relationships with industry partners allows for greater control and input in the developmental process of new powders. This would provide reliable feedstocks, improved quality assurance, and overall higher performance of processes across the additive manufacturing community.

36 MATERIALS SCIENCE↗

The effect of varying powder feedstock chemistry and printing atmosphere on the microstructure of additively manufactured nickel-based ODS alloys: Role on stabilization of cellular structures vs. oxide dispersion formation

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.

36 MATERIALS SCIENCE↗

Standardization Gaps in Powder Feedstock Characterization and Establishing Acceptability for Reuse in Additive Manufacturing

Characterization techniques for powder feedstocks used in additive manufacturing (AM) have long been relied upon to describe the inputs to an AM workflow. However, functional gaps remain between tests to measure intrinsic and extrinsic properties with the direct performance within AM equipment. Furthermore, the common practice of reusing powder through multiple build cycles introduces effects and changes to feedstock performance that are otherwise difficult to measure quantitatively. Here, standardization and the development of new test methods have not kept pace with the rapid evolution of the AM industry and its reliance on highly coupled process-structure–property-performance relationships.

Characterization and Analytical Technique↗

The effect of powder feedstock and heat treatment on the thermal and mechanical properties of binder jet printed ZrC

In this study, zirconium carbide (ZrC) disks were fabricated using binder jet printing to study the effect of powder feedstock, print parameters, and heat treatment on flowability and final materials properties. A median volumetric particle size smaller than 10 μm was shown to cause the powder to stop flowing during printing. Disks were printed using ZrC with suitable flowability and then heat-treated at temperatures between 1800°C and 2200°C for 1 or 5h. The density, part shrinkage, thermal diffusivity, and fracture strength all increased with increasing temperature and time. The heat-treated disks were then heated to 2200°C for 5h and the properties converged for disks of the same particle size, indicating the hottest temperature and longest time of exposure dictates the final properties. Lastly, it was shown that larger particles produce lower density materials with worse thermal diffusivity, most likely because of poor connectivity between particles after heat treatment.

36 MATERIALS SCIENCE↗

Packing density optimization and recyclability of multi-modal SiC powder feedstocks in binder jet additive manufacturing

Achieving high powder packing density is critical in binder jet additive manufacturing (BJAM), as it directly influences the final part density, mechanical properties, and sintering behavior. Multi-modal powder blends, which combine particles of different sizes, have been explored as a strategy to optimize packing efficiency and minimize defects. In this study, bimodal and trimodal powder blends were obtained by mixing silicon carbide powder in three different sizes. These results show that increased powder density is achievable with bimodal powder blends but is reduced in trimodal blends, and it was found that a 13 % increase in the powder tap density was achieved using a bimodal blend of powder. The powder size distribution of the bimodal blend was measured at various stages during binder jet additive manufacturing and, no measurable powder separation occurred even after eight prints. Altogether, this study shows limited advantage to trimodal powder blends but good promise for bimodal blends for increasing printed density while maintaining reusability in the binder jet process.

Aguirre, Trevor G. [Oak Ridge National Laboratory ↗

Synthesis of nanograined zirconium diboride microsphere powder feedstock via emulsification of suspensions

Ceramic nanograined materials have desirable characteristics compared to their macroparticle counterparts but are rarely used in industrial applications due to issues with poor handleability and health hazards. Due to interparticle forces that become more dominant as the particle size decreases, it is difficult to use nanomaterials to fill dies, spread on surfaces, or flow through hoppers found in various manufacturing processes. In this work, we report a scalable gelcasting solution and unique emulsification process to create microspheres composed of nanoscale powders to enhance the flowability and handleability of nanomaterials. The gelcasting solution and emulsification process can be used with any nanoparticle composition that can be suspended in a liquid phase. This paper reports the effects of various parameters on zirconium diboride microsphere formation, such as surfactant content and mixing conditions. The microspheres maintain the nano-scale characteristics of the powder but improve its flowability by using cross-linked polyvinyl alcohol to combine irregularly shaped zirconium diboride nanoparticles with a particle diameter of 60 nm into larger spherical particles with a d 50 ~25 μm. This hierarchical feedstock engineering design combine the positive characteristics of materials across both length scales and improve the flowability of the feedstock from a Hausner Ratio of 1.56 to 1.19. The materials produced using this technique can be used in thermal plasma spray, die filling for hot pressing or spark plasma sintering, and binder jet printing applications.

36 MATERIALS SCIENCE↗

Influence of Powder Characteristics and Processing Methods on Creep Performance of Powder Metallurgy Hot Isostatic Pressed SS316

The U.S. nuclear energy expansion goals are driving the demand for manufacturing routes that can rapidly produce large, complex, near net shape components. Powder metallurgy hot isostatic pressing (PM HIP) is an advanced manufacturing technique that can be economically scaled-up, while alleviating the supply chain challenges that forging and casting face in terms of cost and lead time constraints. This makes PM-HIP a viable technology to aid and accelerate large-scale part manufacturing for nuclear applications. However, large-scale qualification and deployment of this technology require a thorough understanding of the influence of powder feedstock quality, powder handling history, hot isostatic pressing (HIP) parameters, and subsequent heat treatment on microstructural evolution and elevated temperature mechanical performance. The present work focusses on 316 austenitic stainless steel (SS316) which is most commonly used in high temperature environments for nuclear applications Results from this study show that PM HIPed SS316 meets ASME tensile requirements at room temperature and at elevated temperature. However, creep performance of PM-HIPed SS316 remains inferior to its wrought counterpart, demonstrating that tensile performance alone is not a reliable metric for long duration high temperature integrity. Further, this report delineates powder derived microstructural features that govern creep damage, with key evidences pointing to “microstructural inheritance” from gas atomized powder feedstocks. Commercial SS316 powders of varying chemical compositions and recycling histories were studies, and the results showed large differences in elemental segregation, oxide surface layers and secondary phase distributions. Multi-scale characterization revealed segregation of chromium, molybdenum, manganese and silicon at the boundaries and the precipitation of manganese-, silicon-, and molybdenum-oxides. During HIP consolidation, these surface oxides transform into decorated prior particle boundaries (PPBs) and grain boundary inclusions that persist through conventional post-HIP solution annealing treatment. The retained oxides in post-HIP microstructures were found to influence grain growth, precipitation behavior, and ultimately creep cavitation and fracture. Such post-HIP heat treatments are therefore limited by a complex trade-off between grain growth, and oxide coarsening which aggravate creep damage by acting as nucleation sites for cavities. The objective of this work is to establish an integrated processing–structure–property framework for PM-HIP 316 stainless steel by investigating the influence of powder feedstock characteristics in pre- and post-HIP processing as well as to understand the significance of post-HIP heat treatment on microstructural evolution and creep properties. The results from this report emphasize the significance of powder feedstock integrity in improving creep performance of PM-HIPed SS316, by highlight the effect of rapid solidification, elemental segregation, oxide formation and powder recycling on microstructural defect inheritance following HIP consolidation. Rather than considering HIP processing, solution annealing, and mechanical performance independently, this report treats powder production, HIP consolidation, post-HIP thermal processing, and creep deformation as interconnected stages within a continuous metallurgical process. The resulting framework will provide a scientific basis for developing feedstock engineering strategies capable of improving long-term reliability of PM-HIP stainless steels and accelerating their qualification for advanced nuclear applications.

Ajjarapu, Pavan [Oak Ridge National Laboratory (OR↗

Effect of 316 stainless steel powder processing conditions on microstructure

One parameter that has both economic and performance effects in the manufacturing of steel parts is the powder feedstock used. 316 L steel powder can be produced through water atomization or gas atomization, where both the powder size and the atomization process determine the cost of powder feedstock. Gas atomized powder is spherical and has a lower oxygen content than water atomized powder, making it the preferred choice for performance, but comes at a higher financial cost. Here, in this study, various 316 L powder batches are characterized to understand physical properties and microstructural variations. Density and flowability were determined using gas pycnometry and Hall flow tests. Powder morphology and porosity were qualitatively analyzed via optical microscopy and scanning electron microscopy, Finally, transmission electron microscopy was used to determine changes in phases present. Spherical gas atomized powder of 30–100 μm contained Mn$-$Si rich oxides both on the surface and within the matrix. Meanwhile, irregular water atomized powder 30 μm in diameter contained silicon oxides without manganese. All powder particles contained a nickel rich cellular structure which was shown to support the formation of additional phases. While literature has observed general microstructural features across 316 L powder particles, transmission electron microscopy (TEM) in this study has identified variations in precipitation and cell structures. Information regarding morphology, flowability, density, and phase distributions can be applied to understand variations in part consolidation, which will in turn show which powder aspects are significant for production.

Chemical segregation↗

UN Synthesis, Fabrication, and Characterization and UC Oxidation Study in support of Advanced LEU Fuel Concepts

Uranium nitride and carbide-based fuels are proposed for use in advanced LEU fuel systems. This report details recent development work to study synthesis, sintering and fabrication methods for single phase UN in monolithic geometries. These samples were intended to support a variety of irradiation testing conditions by tailoring enrichment, geometry, and compositional requirements. Two methods were under evaluation for synthesizing uranium nitride powder – carbothermic reduction-nitridation (CTR-N) of UO 2 powder feedstock and hydride-dehydride/nitridation (HDN) of uranium metal feedstock. Pellets were fabricated from powder feedstocks via conventional pressing and sintering methods. As-fabricated feedstocks and pellets were evaluated via X-ray diffraction (XRD) for phase purity and sintered materials were characterized for density. Both the CTR N and the HDN methods were successfully demonstrated as an effective process for fabricating phase pure UN. Additionally, results from machining efforts for UN are detailed. This report also contains information on a study trying to elucidate the oxidation mechanisms of sintered uranium carbide samples fabricated from feedstock synthesized via an arc-melting method.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Quantifying dislocation density in Al-Cu coatings produced by cold spray deposition

This work quantifies the plastic deformation in terms of dislocation density for a series of cold sprayed Al-Cu coatings with copper contents from 2 mass% to 5 mass%. The success of the deposition and consolidation of the feedstock powders during the cold spray process rely on the occurrence of significant plastic deformation. Inert gas atomized Al-Cu alloy powders were sprayed onto substrates made of an Al-Cu-Mg-Mn alloy (AA2024) to produce dense coatings using a low pressure cold spray system with helium as the carrier gas. X-ray diffraction patterns were obtained from the Al-Cu feedstock powder material and the cold sprayed coatings using a monochromatic X-ray source, and the dislocation density was determined via an X-ray whole profile analysis. Increasing the Cu alloy content (from 2 mass% to 5 mass%) systematically increased the dislocation density in the Al-Cu coatings from (4.3 ± 0.5) × 10 14 m -2 to (7.5 ± 0.8) × 10 14 m -2 . The dislocation densities in the feedstock powders ranging from (0.4 ± 0.1) × 10 14 m -2 to (1.8 ± 0.2) × 10 14 m -2 were all lower than the dislocation densities in the corresponding coatings. The increasing deformation level in the Al-Cu coatings with Cu additions were confirmed by the classic and modified Williamson-Hall analyses of X-ray diffraction data, and peak breadth measurements from neutron diffraction data. Finally, a high density of dislocations was also observed in these coatings via electron backscatter diffraction and transmission electron microscopy.

36 MATERIALS SCIENCE↗

Preliminary Report on Compositional Specification for Printed 316SS

The Advanced Materials and Manufacturing Technologies Program is focused on accelerating the development and deployment of advanced materials and components fabricated via additive manufacturing (AM). A key challenge for the widespread adoption of AM is the variability in material properties, which can originate from powder feedstock, process parameters, geometry, and the machine. AM powder feedstock compositions are based on those developed for conventional manufacturing. However, the smaller melt pools combined with multiple melt cycles over the course of a build can have substantial effects on the local phase selection resulting from minor batch-to-batch feedstock variability. Therefore, this report focuses on coupling CALPHAD calculations with data mining and visualization to aid the development of compositional specifications for stainless steel 316, an important alloy for nuclear applications and suitable for AM. This work reports that δ-ferrite formation has a stronger dependence on the amount of nickel in the alloy despite nickel being an austenite stabilizer. These findings show the need for exercising a tighter control on the amount of nickel in the alloy compared with the amount of chromium, which is a ferrite stabilizer.

36 MATERIALS SCIENCE↗

Cold spray manufacturing of oxide-dispersion strengthened (ODS) steels using gas-atomized and ball-milled 14YWT powders

The cold spray deposition process has been investigated for the manufacture of 14YWT oxide-dispersion strengthened (ODS) steel, a nanostructured ferritic alloy (NFA), using gas-atomized and ball-milled feedstock powders. Cold spraying of the gas-atomized powder resulted in a thick dense deposit, but annealing them above 900 °C induced grain growth and heterogeneous precipitation of nanoparticles, thus resulting in lower hardness (~ 170 HV) compared to 14YWT ODS steel manufactured by the conventional method. The ball-milled powder (Fe-14Cr-3W-0.4Ti-0.2Y-0.125O) was cryomilled in liquid N 2 to achieve small particle sizes followed by annealing in a H 2 /Ar environment at 1000 °C and 1100 °C to reduce the hardness from ~ 8 GPa to ~ 5 GPa. Both smaller particle sizes and lower hardness of annealed powders made them amenable to the cold spray deposition process, resulting in thick and dense deposits, while retaining the favorable fully solutionized microstructure of the ball-milled powders. The microstructure of the as-deposited ODS exhibited very fine grain sizes (50–250 nm) with a uniform dispersion of Y-Ti-O nanoprecipitates in the ferritic steel matrix. The hardness values of the cold spray deposits using the powders annealed at 1000 °C and 1100 °C was 770 HV and 496 HV, respectively. Post-heat treatment of the as-deposited material up to 1100 °C showed a high-density microstructure with uniformly dispersed nanoscale oxide particles. The hardness of the annealed deposits up to 1000 °C had a notably higher hardness than bulk 14YWT ODS steel manufactured by conventional methods. The study demonstrates that cold spray deposition of the microstructurally-tailored feedstock powders can be used to successfully manufacture ODS steel with microstructure and properties comparable to those produced by the conventional methods, while providing for an attractive option for the more rapid and cost-effective manufacturing of ODS steel cladding tubes.

14YWT↗

Development of Binder Jet Compatible Silicon Carbide Mixtures for Increased Sintered Density

Binder jet additive manufacturing can process a variety of ceramic powder feedstocks to manufacture near net shape green parts that are subsequently sintered to achieve densification. In particular, silicon carbide (SiC) is a promising ceramic material for heat exchangers in energy storage applications and binder jet is a well-suited process for manufacturing these heat exchangers due to the often geometrically complex designs. However, the need for good powder flowability in binder jet printing often limits the feedstock powder to be larger particles rather than that of ultra fine submicron powders used in conventional ceramic processing, which are more readily densified during sintering. The present work explores the use of various powder mixtures and sintering settings to identify strategies for achieving high density sintered parts in binder jet compatible systems without the use of infiltration. Liquid-phase sintering additives and bimodal powder mixtures are explored alongside different sintering temperatures, rates, atmospheres, and hold times. Two mixtures were found to be good candidates for further exploration: 1) 90 wt% 0.6 µm SiC + 6.25 wt% Al 2 O 3 + 3.75 wt% Y 2 O 3 mixture achieved the highest sintered relative density of 91.2%; and 2) a bimodal mixture comprised of 45 wt% 10 µm SiC + 45 wt% 0.6 µm SiC + 6.25 wt% Al 2 O 3 + 3.75 wt% Y 2 O 3 had the best powder flowability of the powders measured and a 75.1% sintered relative density.

25 ENERGY STORAGE↗

Process Intensification for Nanocomposite Aluminum Extrusions: CRADA 411 (Final Report)

The project evaluated the feasibility of using Shear Assisted Processing and Extrusion (ShAPE) for the fabrication of extrusions with a diameter of 0.5” and higher from an Al-alloy powder feedstock that contains nanoscale second phases for achieving enhanced elevated temperature strength. PNNL has previously extruded 0.2” diameter rods with high strength aluminum alloy powder Al-12.4TM. This project aimed to scale the process up to a diameter of 1.0” at a length of >24” while retaining the excellent mechanical properties achieved for the 0.2” diameter rods. As part of the project, extrusion dies were fabricated with various design features. As an example, scroll features on the tool die face was introduced to enhance powder mixing, and reduce extrusion load. Varying extrusion ratios were used to obtain better microstructural homogeneity. Use of tool design features together with the optimization of process parameters helped in the fabrication of extrusions that were up to 48” long with a diameter of 0.5” using Al-12.4 TM powder feedstock in a two-step process involving cold compaction followed by extrusion. Extrusions with a diameter of 1.0” could also be fabricated, but limitations on the extent of consolidation were experienced as a result of the torque and ram force capacity of the current ShAPE machine.

36 MATERIALS SCIENCE↗