Powder Injection Overmolding of High Burnup Light Water Reactor Fuels
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Overview of the PM-HIP work performed on stainless steel 316H as part of the microreactor program. High temperature mechanical testing was performed, with concerns identified with the creep-fatigue performance. Variations in feedstock and processing parameters did not conclusively identify the primary factor in the reduced creep-fatigue performance.
First experimental results from the Lithium Evaporations to Advance PFCs in ST40 (LEAPS) program.
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. Overall, this study shows limited advantage to trimodal powder blends but good promise for trimodal blends for increasing printed density while maintaining reusability in the binder jet process.
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. Overall, this study shows limited advantage to trimodal powder blends but good promise for trimodal blends for increasing printed density while maintaining reusability in the binder jet process.
The aluminum cladding of research-reactor fuel undergoes general corrosion with resulting formation of adherent aluminum (oxy)hydroxide films during in-reactor and post-discharge exposure to water under various conditions and temperatures. These (oxy)hydroxides contain chemically-bound water that poses challenges for extended dry storage due to the risk of thermal or radiolytic decomposition releasing free water and/or hydrogen and oxygen gases. This study comprised laboratory experiments of thermal drying behavior of aluminum (oxy)hydroxides to identify approaches for reducing bound water on fuel cladding prior to sealed dry storage. Effective drying strategies for adherent (oxy)hydroxides on fuel cladding will improve the safety of dry storage by mitigating potential avenues for additional corrosion and/or generation of flammable gases inside the storage canister. This work is part of a broader investigation to address knowledge gaps and technical data needs for dry storage of aluminum-clad spent nuclear fuel (ASNF), which included investigation of (oxy)hydroxide formation on aluminum alloy substrates immersed in water, characterization of service-grown films from ASNF, and radiolytic yield of hydrogen from (oxy)hydroxide powders and films. The current work comprises experimental thermal dehydration of aluminum trihydroxides (bayerite and gibbsite) characteristic of low-temperature (<80 deg. C) corrosion in water and aluminum oxyhydroxide (boehmite) characteristic of high temperature (>80 deg. C) corrosion in water. First, commercially produced (oxy)hydroxide powders (boehmite and gibbsite) were tested via thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The effort aimed to identify or confirm key temperature ranges/thresholds for the thermal decomposition reactions, as well as impacts of ramp rate and hold times, for drying of isolated, high-surface-area (oxy)hydroxides. The information gleaned from powder tests was used to guide subsequent drying tests on adherent (oxy)hydroxide films grown on aluminum alloy substrates. TGA was used to analyze small samples of the aluminum coupons with adherent (oxy)hydroxide films. Specimens were characterized both pre- and post-drying using X-ray diffraction (XRD) to determine the film composition and scanning electron microscopy (SEM) to determine its morphology. Drying of adherent (oxy)hydroxide films was anticipated to pose additional complications relative to drying of (oxy)hydroxide powders. Anticipated challenges include achieving sufficient drying of the (oxy)hydroxide at low-enough temperature to avoid melting or other undesirable phase changes in the aluminum substrate and overcoming transport limitations of water through the thickness of a dense film or through a tortuous pore structure to reach the outer surface of the film. Inn addition, dehydration of (oxy)hydroxides significantly changes the film density, which may lead to substantial alterations in the morphology, including potential cracking and spalling of the film. TGA/DSC tests of gibbsite powders resulted in successful conversion to boehmite or alumina, depending on the maximum temperature reached. At low ramp rates (≤5 deg. C/min), the conversion to boehmite occurred around 300 deg. C (210-340 deg. C). XRD confirmed that boehmite was the only phase detected after tests reaching 450 deg. C. The transition to alumina occurred around 510 deg. C (470-550 deg. C), with XRD detecting only alumina after tests reaching at least 600 deg. C. Boehmite powders dehydrated to alumina at about 400 deg. C (330-460 deg. C) for coarse (77-μm particle diameter) powder and about 490 deg. C (420-520 deg. C) for fine (0.7-μm particle diameter) powder. For all powders tested, the maximum percent mass loss after drying to high temperature slightly exceeded the theoretical mass loss for complete dehydration of the stoichiometric (oxy)hydroxide to alumina, which is likely attributable to physisorbed water in the powder. Drying of a thick (∼8.6 μm), predominantly bayerite adherent film displayed a dramatic change in film morphology, with the initially continuous trihydroxide film cracking into sections on the order of 50 μm square and partially delaminating. The outermost layer of the film completely faked of in some regions. The layer exposed under the spalled oxide also displayed prominent cracking, with spacing on the order of 10 μm, but this surface layer appeared to remain completely adhered to the aluminum substrate. TGA showed mass losses per unit surface area up to ∼1.0 mg/cm{sup 2}. XRD characterization of the remaining oxide was inconclusive, with no crystalline phases detected. (authors)
The risk of inhalation exposure to elevated concentrations of hydrogen sulfide (H2S) and ammonia (NH3) during the agitation of stored swine manure is high. Once or twice a year, farmers agitate manure before pump-out and application to fields. Agitation of the swine manure causes the short-term releases of highly toxic levels of H2S and NH3. In our previous pilot-scale studies, the biochar powder showed significant mitigation of H2S and NH3 emissions when it was surficially applied to manure immediately before agitation. However, fine biochar powder application poses hazards by itself and may not be practical to apply on a farm scale, especially when livestock and workers are present. We hypothesized that applying pelletized biochar to manure surfaces is just as effective as applying powder to protect farmers and animals from excessive exposure to H2S and NH3. This work reports on the lab-scale proof-of-the-concept trials with biochar pellets on the lab scale. The objective was to compare the biochar pellets and biochar powder on their effectiveness of mitigation on H2S and NH3 gases during 3-h-long swine manure agitation. Three scenarios were compared in (n = 3) trials: (i) control, (ii) 12.5 mm thick surficial application to manure surface of biochar powder, and (iii) an equivalent (by mass) dose of pelletized biochar applied to the manure surface. The biochar powder was bound with 35% (wt) water into ~5 × 10 mm (dia × length) pellets. The biochar powder was significantly (p < 0.05) more effective than the biochar pellets. Still, pellets reduced total H2S and NH3 emissions by ~72% and ~68%, respectively (p = 0.001), compared with ~99% by powder (p = 0.001). The maximum H2S and NH3 concentrations were reduced from 48.1 ± 4.8 ppm and 1810 ± 850 ppm to 20.8 ± 2.95 ppm and 775 ± 182 ppm by pellets, and to 22.1 ± 16.9 ppm and 40.3 ± 57 ppm by powder, respectively. These reductions are equivalent to reducing the maximum concentrations of H2S and NH3 during the 3-h manure agitation by 57% and 57% (pellets) and 54% and 98% (powder), respectively. Treated manure properties hinted at improved nitrogen retention, yet they were not significant due to high variability. We recommend scaling up and trials on the farm-scale level using biochar pellets to assess the feasibility of application to large manure surfaces and techno-economic evaluation.
Iron nitride magnets offer the potential for large magnetic remanence magnets absent any rare earth materials [1]. This project was submitted in response to the funding opportunity announcement (FOA) from the Advanced Manufacturing Office (AMO) of the Office of Energy Efficiency & Renewable Energy (EERE) of the Department of Energy (DOE): DE-FOA-0001465: Advanced Manufacturing Projects for Emerging Research Exploration; Topic Area 1: Advanced Materials; Subtopic 1.1: Innovative Advanced Materials Manufacturing for Clean Energy to explore nitriding iron powder using a fluidized bed technique which if successful would accomplish nitriding the iron powder with reduce industrial energy intensity. Of particular concern when using metal powders at high temperatures in a fluidized bed reactor is the defluidization temperature of the bed, also known as the ‘bed collapse’ temperature. Above the defluidization temperature the metal powders can no longer fluidize and instead become an undesirable packed powder bed. Using the published results from the Institute of Process Engineering at the Chinese Academy of Sciences in Beijing, China, FeNix Magnetics was able to develop a spreadsheet calculation that allowed predictive guidelines for the defluidization temperature of iron powder based on the type of carrier gas, flow rate of the carrier gas, and the iron powder diameter. FeNix Magnetics was not able to conclude whether the temperatures to avoid bed defluidization that were achievable in a fluidized bed reactor actually resulted in nitriding the iron powder to the required level. In order to measure the amount of nitrogen in the iron powder, FeNix Magnetics contracted with the DOE sponsored Advanced Photon Source (APS) at Argonne National Laboratory to conduct X-Ray diffraction measurements. Unfortunately, due to COVID-19 restrictions, the DOE sponsored APS was closed and unable to provide X-Ray Diffraction measurements during this program.
Urbix Resources is a company specializing in graphite powder processing and purification. Urbix is looking to become the first domestic supplier of nuclear-grade graphite in the United States. This has led to a Cooperative Research and Development Agreement (CRADA) being established between the Oak Ridge National Laboratory (ORNL) and Urbix Resources, with the goal of characterizing a purified graphite feedstock supplied by Urbix Resources. The resulting data will then be used to determine the viability of a large-scale nuclear graphite production and qualification campaign. These characterization methods have been performed on the as-received graphite feedstock, a heat-treated batch of the feedstock, a milled batch of the feedstock, and a nuclear-grade graphite powder historically used in fuel production. The data from the heat-treated and milled feedstock will determine how different processing methods affect the powder’s physical properties, whereas the data from the nuclear grade graphite will provide information about the characteristics of a graphite previously accepted for nuclear applications. All of these powders have been characterized individually and as part of a resin-graphite blend (herein referred to as matrix) that has been used in past fuel experiments. The results of these experiments show that the Urbix powder and nuclear-grade graphite powder display notably different properties from one another in many cases, but this discrepancy may have been the result of the typical particle size of each powder. This hypothesis is supported by tests conducted on the milled powder, which showed a closer resemblance in properties to the nuclear-grade graphite than the as-received powder. The method for pressing the graphite matrix also had a noticeable effect on the measured properties.
This Laboratory Directed Research and Development project developed and applied closely coupled experimental and computational tools to investigate powder compaction across multiple length scales. The primary motivation for this work is to provide connections between powder feedstock characteristics, processing conditions, and powder pellet properties in the context of powder-based energetic components manufacturing. We have focused our efforts on multicrystalline cellulose, a molecular crystalline surrogate material that is mechanically similar to several energetic materials of interest, but provides several advantages for fundamental investigations. We report extensive experimental characterization ranging in length scale from nanometers to macroscopic, bulk behavior. Experiments included nanoindentation of well-controlled, micron-scale pillar geometries milled into the surface of individual particles, single-particle crushing experiments, in-situ optical and computed tomography imaging of the compaction of multiple particles in different geometries, and bulk powder compaction. In order to capture the large plastic deformation and fracture of particles in computational models, we have advanced two distinct meshfree Lagrangian simulation techniques: 1.) bonded particle methods, which extend existing discrete element method capabilities in the Sandia-developed , open-source LAMMPS code to capture particle deformation and fracture and 2.) extensions of peridynamics for application to mesoscale powder compaction, including a novel material model that includes plasticity and creep. We have demonstrated both methods for simulations of single-particle crushing as well as mesoscale multi-particle compaction, with favorable comparisons to experimental data. We have used small-scale, mechanical characterization data to inform material models, and in-situ imaging of mesoscale particle structures to provide initial conditions for simulations. Both mesostructure porosity characteristics and overall stress-strain behavior were found to be in good agreement between simulations and experiments. We have thus demonstrated a novel multi-scale, closely coupled experimental and computational approach to the study of powder compaction. This enables a wide range of possible investigations into feedstock-process-structure relationships in powder-based materials, with immediate applications in energetic component manufacturing, as well as other particle-based components and processes.
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.
Methods and apparatuses for in situ synthesis of SiC, CMCs, and MMCs are disclosed, comprising: providing an apparatus having: an electromagnetic energy source; an autofocusing scanner; a powder system for SiC and one or more powders; a powder delivery system; a shielding gas comprising argon and/or nitrogen; and a computer coupled to and configured to control the energy source, scanner, powder system, and powder delivery system to deposit layers of the sample; programming the computer with specifications of the sample; using the computer to control electromagnetic radiation, mixing ratio, and powder deposition parameters based on the specifications of the sample; and using the autofocusing scanner to focus and scan the electromagnetic radiation onto the sample while the powders are concurrently deposited by the powder delivery system onto the sample to create a melting pool to deposit one or more layers onto the sample. Other embodiments are described and claimed.
A micro-alloyed copper powder, Cu-0.3Zr-0.15Ag wt.%, was produced using gas atomization reaction synthesis. Zirconium was added to copper to sequester the oxygen present as copper oxide surface films on the powder particles. The as-received powders, as well as the intentionally oxidized powders were used to fabricate solid test articles by electron beam powder bed fusion additive manufacturing. Dense samples fabricated from as-received powder demonstrated nominal UTS, yield, and elongation values at 260 MPa, 150 MPa, and 34%, respectively. The average electrical conductivity of these samples was measured at 95% of the international annealed copper standard (IACS). Samples fabricated from the oxidized powder exhibited nominal UTS, yield, and elongation of 241 MPa, 146 MPa, and 43%, respectively, with an electrical conductivity of 95 % IACS. During characterization, it was observed that, rather than forming nano-scale dispersoids, the Zirconia (ZrO 2 ) appeared as discontinuous stringers in the metallographic cross-sections that crossed grain and melt pool boundaries. This was rationalized by tracing the presence of the micro-alloying addition of elemental zirconium, which was found to react with surface oxides dissociated in the melt pool to form ZrO 2 , which then solidified on the surface of the melt pool through an allotropic transformation to monoclinic ZrO 2 in discontinuous films and spheroids ranging in size from nanometers to microns. This was confirmed by microscopic analysis of the tops of the melt pools. On subsequent melt passes, these ZrO 2 structures were displaced and redistributed within the melt pool.
Pentaerythritol tetranitrate (PETN) is one of the most commonly used explosives for both military and mining applications. PETN is used in EBW (exploding bridge wire) and EFI (exploding foil initiator) detonator devices. Due the widespread usage of PETN, studies focusing on how the explosive changes with age, primarily its function in detonators has received particular interest. Aging studies have identified several factors that affect PETN detonator function over time, most notably the specific surface area of the explosive powder. Though small-scale studies have been performed on specific detonator systems with isolated batches of material, what is missing is a large statistically-significant study focusing on PETN aging characteristics - such as powder coarsening - and their influence on detonator performance. Herein we report the first large statistically viable PETN aging study focusing on four batches of PETN powder from the same stock of PETN using two stabilizers, polysaccharide and TriPEON. PETN was aged both as a free-flowing powder as well as in modified EBW RP-2 detonators, for one month at 75 °C. The PETN powder has been analyzed chemically using Fisher specific surface area analysis, SEM imaging and light scattering particle size analysis. Additionally the detonators were tested for performance through voltage-sweep threshold testing and function time measurements. Findings from the study indicate that aging at 75 °C for one month significantly changes the specific surface area and particle size of unstabilized PETN, leading to increases in detonator function time, but not detonator threshold values. Powders stabilized with TriPEON displayed less significant increases in function time, while powder stabilized with polysaccharide exhibited no aging effects, despite the high temperature aging.