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At least 721 records · Page 40

Pressureless sintering of dual-phase, high-entropy boride–carbide ceramics

Here, dual-phase, high-entropy boride–carbide ceramics were densified by pressureless sintering. Relative densities up to approximately 96% were obtained for ceramics containing about 30 vol% high-entropy boride and 70 vol% high-entropy carbide. Isostatic pressing at 200 MPa resulted in higher relative densities of both the green bodies and final ceramics compared to uniaxial pressing. The highest relative density of 96.3% was achieved for a ceramic that was isostatically pressed at 200 MPa and sintered at 2300°C for 2 h. Grain sizes of the resulting ceramics were approximately 2 µm. This is the first report of pressureless sintering of dual-phase, high-entropy boride–carbide ceramics.

36 MATERIALS SCIENCE↗

MO-G-18C-07: Improving T2 Determination and Quantification of Lipid Methylene Protons in Proton Magnetic Resonance Spectroscopy at 3 T

Purpose: To improve proton magnetic resonance spectroscopy (MRS) transverse relaxation (T{sub 2}) determination and quantification of lipid methylene chain (1.3 ppm) protons by rewinding their J-coupling evolution. Methods: MRS experiments were performed on four lipid phantoms, namely, almond, corn, sunflower and oleic acid, using a 3 T Philips MRI scanner with a transmit/receive birdcage head coil. Two PRESS (Point RESolved Spectroscopy) pulse sequences were used. The first PRESS sequence employed standard bandwidth (BW) (∼550 Hz) RF (radiofrequency) refocussing pulses, while the second used refocussing pulses of narrow BW (∼50 Hz) designed to rewind J-coupling evolution of the methylene protons in the voxel of interest. Signal was acquired with each sequence from a 5×5×5 mm{sup 3} voxel, with a repetition time (TR) of 3000 ms, and with echo times (TE) of 100 to 200 ms in steps of 20 ms. 2048 sample points were measured with a 2000 Hz sampling bandwidth. Additionally, 30 mm outer volume suppression slabs were used to suppress signal outside the voxel of interest. The frequency of the RF pulses was set to that of the methylene resonance. Methylene peak areas were calculated and fitted in MATLAB to a monexponentially decaying function of the form M{sub 0}exp(-TE/T{sub 2}), where M{sub 0} is the extrapolated area when TE = 0 ms and yields a measure of concentration. Results: The determined values of M{sub 0} and T{sub 2} increased for all fatty acids when using the PRESS sequence with narrow BW refocussing pulses. M{sub 0} and T{sub 2} values increased by an average amount (over all the phantoms) of 31% and 14%, respectively. Conclusion: This investigation has demonstrated that J-coupling interactions of lipid methylene protons causes non-negligible signal losses which, if not accounted for, Result in underestimations of their levels and T{sub 2} values when performing MRS measurements. Funded by the Natural Sciences and Engineering Research Council of Canada and the Canadian Breast Cancer Foundation - Prairies.NWT.

60 APPLIED LIFE SCIENCES↗

TU-D-201-07: Severity Indication in High Dose Rate Brachytherapy Emergency Response Procedure

Purpose: Understanding the corresponding dose to different staff during the High Dose Rate (HDR) Brachytherapy emergency response procedure could help to develop a strategy in efficiency and effective action. In this study, the variation and risk analysis methodology was developed to simulation the HDR emergency response procedure based on severity indicator. Methods: A GammaMedplus iX HDR unit from Varian Medical System was used for this simulation. The emergency response procedure was decomposed based on risk management methods. Severity indexes were used to identify the impact of a risk occurrence on the step including dose to patient and dose to operation staff by varying the time, HDR source activity, distance from the source to patient and staff and the actions. These actions in 7 steps were to press the interrupt button, press emergency shutoff switch, press emergency button on the afterloader keypad, turn emergency hand-crank, remove applicator from the patient, disconnect transfer tube and move afterloader from the patient, and execute emergency surgical recovery. Results: Given the accumulated time in second at the assumed 7 steps were 15, 5, 30, 15, 180, 120, 1800, and the dose rate of HDR source is 10 Ci, the accumulated dose in cGy to patient at 1cm distance were 188, 250, 625, 813, 3063, 4563 and 27063, and the accumulated exposure in rem to operator at outside the vault, 1m and 10cm distance were 0.0, 0.0, 0.1, 0.1, 22.6, 37.6 and 262.6. The variation was determined by the operators in action at different time and distance from the HDR source. Conclusion: The time and dose were estimated for a HDR unit emergency response procedure. It provided information in making optimal decision during the emergency procedure. Further investigation would be to optimize and standardize the responses for other emergency procedure by time-spatial-dose severity function.

60 APPLIED LIFE SCIENCES↗

Quantifying Volume Change in Porous Electrodes via the Multi-Species, Multi-Reaction Model

Automotive manufacturers are working to improve individual cell and overall pack design by increasing their performance, durability, and range, while reducing cost; and active material volume change is one of the more complex aspects that needs to be considered during this process. As the time from initial design to manufacture of electric vehicles is decreased, design work that used to rely solely on testing needs to be supplemented or replaced by virtual methods. As electrochemical engineers drive battery and system design using model-based methods, the need for coupled electrochemical/mechanical models that take into account the active material change utilizing physics based or semi-empirical approaches is necessary. In this study, we illustrated the applicability of a mechano-electrochemical coupled modeling method considering the multi-species, multi-reaction model as popularized by Verbrugge and Baker. To do this, validation tests were conducted using a computer-controlled press apparatus that can control the press displacement and press force with precision. The coupled MSMR volume change model was developed and its applicability to graphite and NMC cells was illustrated. The increased accuracy of the model considering the coupled MSMR volume change approach shows in the importance of accounting for individual gallery volume change behavior on cell level predictions.

25 ENERGY STORAGE↗

Combining Spectroscopic Techniques to Determine the Optical Constants of Powdered Lactose

A method for deriving the optical constants (n/k) of organic powdered materials using pressed pellets in the mid-infrared spectral range is introduced that combines variable angle spectroscopic ellipsometry and transmission spectroscopy. The approach is applied to lactose, in which three different forms of pellets were pressed and measured: A pure lactose pellet and a mixed lactose/KBr pellet with a large analyte percentage were used for ellipsometric measurements, and a KBr transmission pellet with only a small analyte percentage were used for transmission measurements. The transmission data provide an initial set of oscillators and improve the spectral fitting of weak absorption features (k<0.01). Ellipsometric data for the pure and mixed pellets are then fit simultaneously to derive the final n/k values for lactose from 6000-400 cm-1. An alternative method just using the ellipsometric data from the mixed pellet and the transmission data is also presented and shows good agreement with the multi-sample analysis, providing a simpler method for powders that do not press easily into pure pellets. Finally, the derived optical constants are used to model the reflectance data, demonstrating a good match with the measured reflectance spectra if non-idealities are included.

Yokosuk, Michael O.↗

Reproductive and leaf litterfall fluxes in forest ecosystem sites globally (1950-2022)

Forest allocation of net primary productivity (NPP) to reproduction is poorly quantified globally, despite its critical role in forest regeneration and a well-supported trade-off with allocation to growth. Although field measurements of total NPP are rare, our work finds that a proxy for reproductive carbon allocation constructed from leaf (L) and reproductive (R) litterfall fluxes, R/(R+L), is strongly correlated with R/NPP, facilitating analysis across a wide range of sites where biometric estimates of NPP are not available (R² = 0.85; Hanbury-Brown et al., 2022, Ward et al., in prep). To investigate relationships between ecosystem-scale reproductive allocation (RA) and climate, soil fertility, and stand age gradients, we conducted a literature search and synthesized 824 observations of annual average leaf and reproductive litterfall fluxes across forest sites globally. The zip file includes 1) a folder Data/ containing the litterfall data ("GlobalForestRA_data.csv") and metadata ("GlobalForestRA_metadata.doc") files. The data file includes geographic coordinates, long-term mean annual temperature and precipitation (1970-2000, extracted from WorldClim2.1), leaf and reproductive litterfall fluxes, sampling interval and protocols, forest characteristics (dominant leaf morphology, information pertaining to forest age and successional stage, and disturbance history) and soil properties (% sand, %silt, %clay, total phosphorus (P), nitrogen (N), cation exchange capacity (CEC) and pH) extracted from SoilGrids250 and from on-site measurements, where available. The metadata file contains information about each variable reported in the data file, including data sources, processing methods, and all references. The Data folder contains two additional files used to create Figure 1; these are described in greater detail in the README.2) R scripts GloalForestRA_analysis.r and GlobalForestRA_SI.r and a folder /Functions used to produce results, figures, and tables in the manuscript Ward et al. (in press)3) a README file describing how the data and R scripts can be used to reproduce statistical results, figures, and tables found in the manuscript. Ward et al. (in press)This repository can also be found at: https://github.com/r-ward/Global_Analysis_ForestRA.Ward, R.E., Zhang-Zheng, H. Aernethy, K., Adu-Bredu, S., Arroyo, L., Bailey, A. et al. (in press). Forest age rivals climate to explain reproductive allocation patterns in forest ecosystems globally. Ecology Letters. Hanbury-Brown, A.R., Ward, R.E. & Kueppers, L.M. (2022). Forest regeneration within Earth system models: current process representations and ways forward. New Phytol., 235, 20–40.Ward et al. (2025), Forest age rivals climate to explain reproductive allocation patterns in forest ecosystems globally, in prep.

54 ENVIRONMENTAL SCIENCES↗

Continuous wave laser irradiation of explosives

Quantitative measurements of the levels of continuous wave (CW) laser light that can be safely applied to bare explosives during contact operations were obtained at 532 nm, 785 nm, and 1550 nm wavelengths. A thermal camera was used to record the temperature of explosive pressed pellets and single crystals while they were irradiated using a measured laser power and laser spot size. A visible light image of the sample surface was obtained before and after the laser irradiation. Laser irradiation thresholds were obtained for the onset of any visible change to the explosive sample and for the onset of any visible chemical reaction. Deflagration to detonation transitions were not observed using any of these CW laser wavelengths on single crystals or pressed pellets in the unconfined geometry tested. Except for the photochemistry of DAAF, TATB and PBX 9502, all reactions appeared to be thermal using a 532 nm wavelength laser. For a 1550 nm wavelength laser, no photochemistry was evident, but the laser power thresholds for thermal damage in some of the materials were significantly lower than for the 532 nm laser wavelength. No reactions were observed in any of the studied explosives using the available 300 mW laser at 785 nm wavelength. Tables of laser irradiance damage and reaction thresholds are presented for pressed pellets of PBX9501, PBX9502, Composition B, HMX, TATB, RDX, DAAF, PETN, and TNT and single crystals of RDX, HMX, and PETN for each of the laser wavelengths.

45 MILITARY TECHNOLOGY, WEAPONRY, AND NATIONAL DEF↗

Uranium Silicide/Nitride Pellet Fabrication Demonstration: Report on Powder Characteristics (Final CRADA Report)

This report details experimental procedures and results of work at the Idaho National Lab to fabricate U 3 Si 2 and UN ceramic powders from their basic elements. The reaction procedure centers on arc melting using a cold, copper hearth. The reacted "buttons" are then ground into powder, and the powder is characterized. The preliminary experiments utilized feeding pieces of metallic U and Si (in the proper ratio) into the arc-melting furnace for melting into "buttons." This melting was repeated several times with the intent of homogenizing the reaction to produce phase pure U 3 Si 2 powder. However, sintering of the pressed-powder at over 1400C showed partial melting and slumping of the pellets. Characterization of the powder using x-ray diffraction (XRD) indicated the crystalline portion of the powder was U 3 Si 2 . However, further investigations indicated a significant portion (12.4%) of the powder was amorphous Si that was transformed into crystalline Si after a period of annealing. Therefore, a greatly improved method of powder fabrication was developed using mixing fine powders of U and Si together, pressing into a pellet, followed by arc melting and grinding into U 3 Si 2 powder. This method was highly successful in producing high phase purity (>98.5% U 3 Si 2 ) powder. One feature of this method is that the fine U powder is made by a hydride/de-hydride cycle. The equipment available at INL only allows for fabrication of relatively small batches, and the method (using INL equipment) is somewhat labor intensive. The powder was used to successfully press and sinter U 3 Si 2 pellets ("Final Report on Pellet Fabrication," INL/LTD-13-29465). A limited attempt was made to fabricate high purity UN powder using the fine U powder made at INL (hydride/de-hydride method) and heating it under flowing nitrogen gas. X-ray diffraction was used to characterize the resulting powder, and a Rietveld refinement was performed on the data. The refinement showed a result of 70.0% UN and 30.0% U 2 N 3 . It is thought that the UN content can be easily increased

Source record↗

Improved Processing of High Alloy Steels for Wear Components in Energy Generation Systems, Transportation and Manufacturing Systems

Oak Ridge National Laboratory (ORNL), in Partnership with Avure Technologies Inc. and Carpenter Technology Corporation, explored methods to improve durability of steels considered essential to bearings in wind turbine applications by using hot isostatic pressing of steel alloy powders as a manufacturing method. The objective of the project was to evaluate the wear mechanism of selected high alloy tool steels, 440C, 440XH, and M62, fabricated by powder metallurgy (PM) techniques via the hot isostatic press (HIP) process, and compare these results to two conventionally produced wrought alloys, 52100 and M50. Samples from the five candidate metals were characterized microstructurally via optical and scanning microscopy methods. A micro-pit wear testing machine was purchased and used to simulate bearing loads in a wind turbine gear box The candidate samples were subsequently heat treated in accordance with industrial protocols and machined into wear test specimens suitable for the micro-pit wear testing machine. Wear testing produced surfaces that were subsequently analyzed for wear and damage using both optical microscopy and scanning electron microscopy methods. Optimized rolling-sliding experiments with a relatively small slip ratio (5%) and higher load (650N) exhibited signs of abrasive wear on all specimens, but not all specimens had the same degree of micro-pitting damage. The conventional wrought 52100 steel had the most severe micro-pitting, consisting of distorted craters, many of which were connected by micro-cracks. Cross-sectional examination showed multiple micro-cracks extending into the alloy microstructure from the same pit. The depth of the cracks was several times the depth of the micro-pit. Type 440XH had the least amount of micro-pitting damage under similar test conditions. Micro-pits on 440HX were more localized and the micro-cracks associated with them tended to avoid carbides during propagation. Abrasive processes were observed on all the test specimens and were produced by debris from mico-pitting. The combination of micro-pitting in conjunction with abrasive processes could work together to worsen the surface damage, diminishing bearing service life. The results suggest that there is a potential advantage of PM consolidated high alloy tool steels, such as 440XH produced via hot isostatic pressing to better resist micro-pitting when compared to other alloy types and wrought processing methods.

Peter, William H.↗

Bridging the Divide: Linking Genomics to Ecosystem Responses to Climate Change: Final Report

Over the project period, we have addressed the following objectives: 1) assess the effects of altered precipitation patterns (i.e., increased variability in growing season precipitation) on genetic diversity of the dominant C4 grass species, Andropogon gerardii, and 2) experimentally assess the impacts of extreme climatic events (heat wave, drought) on responses of the dominant C4 grasses, A. gerardii and Sorghastrum nutans, and the consequences of these response for community and ecosystem structure and function. Below is a summary of how we have addressed these objectives. Objective 1 After ten years of altered precipitation, we found the number of genotypes of A. gerardii was significantly reduced compared to the ambient precipitation treatments (Avolio et al., 2013a). Although genotype number was reduced, the remaining genotypes were less related to one another indicating that the altered precipitation treatment was selecting for increasingly dissimilar genomes (based on mean pairwise Dice distance among individuals). For the four key genotypes that displayed differential abundances depending on the precipitation treatment (G1, G4, and G11 in the altered plots and G2 in the ambient plots), we identified phenotypic differences in the field that could account for ecological sorting (Avolio & Smith, 2013a). The three altered rainfall genotypes also have very different phenotypic traits in the greenhouse in response to different soil moisture availabilities (Avolio and Smith, 2013c). Two of the genotypes that increased in abundance in the altered precipitation plots had greater allocation to root biomass (G4 and G11), while G1 allocated more biomass aboveground. These phenotypic differences among genotypes suggests that changes in genotypic structure between the altered and the ambient treatments has likely occurred via niche differentiation, driven by changes in soil moisture dynamics (reduced mean, increased variability and changes in the depth distribution of soil moisture) under a more variable precipitation regime, rather than reduced population numbers (A. gerardii tiller densities did not differ between altered and ambient treatments; p = 0.505) or a priori differences in genotype richness (Avolio et al.2013a). This ecological sorting of genotypes, which accounts for 40% of all sampled individuals in the altered plots, is an important legacy of the press chronic climate changes in the RaMPs experiment. Objective 2 In May 2010, we established the Climate Extremes Experiment at the Konza Prairie Biological Station. For the experiment, a gradient of temperatures, ranging from ambient to extreme, were imposed in 2010 and 2011 as a mid-season heat wave under well-watered or severe drought conditions. This study allowed us for the first time to examine species-specific thresholds of responses to climate extremes and assess how these phenotypic responses may impact selection of particular genotypes, with the ultimate goal of linking alterations in individual performance and genetic diversity to ecosystem structure and functioning. We found that tallgrass prairie was resistant to heat waves, but it was not resistant to extreme drought, which reduced aboveground net primary productivity (ANPP) below the lowest level measured in this grassland in almost thirty years (Hoover et al. in press(a)). This extreme reduction in ecosystem function was a consequence of reduced productivity of both C4 grasses and C3 forbs. This reduction in biomass of the C4 grasses (Andropogon gerardii and Sorghastrum nutans) was, in part, due to significant reductions in photosynthesis, leaf water potential and productivity with drought in the dominant grasses species, with S. nutans was more sensitive than A. gerardii to drought (Hoover et al. in press(b)). However, the dominant forb was negatively impacted by the drought more than the dominant grasses, and this led to a reordering of species abundances within the plant community. Although this change in community composition persisted post-drought, ANPP recovered completely the year after drought due to rapid demographic responses by the dominant grass, compensating for loss of the dominant forb. Overall, our results show that an extreme reduction in ecosystem function attributable to a climate extreme (e.g., low resistance) does not preclude rapid ecosystem recovery. Given that dominance by a few species is characteristic of most ecosystems, knowledge of the traits of these species and their responses to climate extremes will be key for predicting future ecosystem dynamics and function. In addition, our research suggests that water stress will dominate photosynthetic and productivity responses caused by discrete drought and heat wave events, rather than direct or additive effects of heat stress, with differential sensitivity in these grasses altering future ecosystem function.

54 ENVIRONMENTAL SCIENCES↗

Processing and Characterization of Sol-Gel Cerium Oxide Microspheres

Of interest to space exploration and power generation, Radioisotope Thermoelectric Generators (RTGs) can provide long-term power to remote electronic systems without the need for refueling or replacement. Plutonium-238 (Pu-238) remains one of the more promising materials for thermoelectric power generation due to its high power density, long half-life, and low gamma emissions. Traditional methods for processing Pu-238 include ball milling irregular precipitated powders before pressing and sintering into a dense pellet. The resulting submicron particulates of Pu-238 quickly accumulate and contaminate glove boxes. An alternative and dust-free method for Pu-238 processing is internal gelation via sol-gel techniques. Sol-gel methodology creates monodisperse and uniform microspheres that can be packed and pressed into a pellet. For this study cerium oxide microspheres were produced as a surrogate to Pu-238. The similar electronic orbitals between cerium and plutonium make cerium an ideal choice for non-radioactive work. Before the microspheres can be sintered and pressed they must be washed to remove the processing oil and any unreacted substituents. An investigation was performed on the washing step to find an appropriate wash solution that reduced waste and flammable risk. Cerium oxide microspheres were processed, washed, and characterized to determine the effectiveness of the new wash solution.

36 MATERIALS SCIENCE↗

Oak Ridge National Laboratory Preparation of Sintered 237 NpO 2 Pellets for Irradiation to Produce 238 Pu Oxide

The reference flowsheet for production of 238 Pu is by irradiation of targets containing pellets cold-pressed from a mix of NpO 2 and Al, which are referred to as cermet pellets or compacts. Oxide pellets, cold-pressed from NpO 2 , are being considered because elimination of the aluminum constituent has significant advantages in a production operation. Details of a fabrication process to make NpO 2 pellets, from preparation of neptunium oxide powder through sintering of the pressed pellets, are given. Pellets were prepared of required density and tight dimensional tolerance for fabrication of test targets that are currently being irradiated at the Oak Ridge National Laboratory High Flux Isotope Reactor. This work is part of the effort to reestablish domestic production of 238 Pu for the National Aeronautics and Space Administration and the Department of Energy.

36 MATERIALS SCIENCE↗

Final Scientific Findings Report- Hydro Research Foundation- Research Awards Program

The Research Awards Program was established in 2014 by the Hydro Research Foundation (Foundation) to support research efforts for the hydropower industry. Using the previously funded Fellowship Program that ran from 2010-2015, the Research Awards Program (RAP or program) captured the lessons learned from the Fellowship program and fine-tuned a nation-wide graduate level research program to support innovation, research and workforce development. The RAP was funded through a $2 million-dollar grant through the Department of Energy’s Water Power Program within the Energy Efficiency and Renewable Energy office (DOE). This award made possible, 33 research projects by 32 students from 21 universities in 11 states. The grant widely engaged the industry by providing the opportunity to work with 25 organizations as well as 63 students and advisors. The funded research focused on a topic list selected by industry and worked to cover a breadth of research needs across many disciplines, basins and types of hydropower issues. The funded work, answered pressing research needs in the fields of the following disciplines; civil engineering, mechanical engineering, environmental engineering, electrical engineering, geography, fisheries, wildlife, water resources, geology, energy science and materials innovation. The Foundation estimates that 116 individuals benefited from this research through either direct mentorship (42), research (32), overseeing the research (31), partnerships (7) and the day-to-day management of the program (4). This investment by DOE showcases how private-public partnerships can leverage limited funds to create a wide range of research products. The project objective was to build on the successful Fellowship Program to develop and execute the RAP on a national level. The program sought to provide competitively awarded hydropower-related graduate-level research awards. The intent of the RAP was to support beneficial, innovative research related to conventional or pumped-storage hydropower. It also sought to stimulate interest among students and universities in this research arena and provide students with a foundation for productive careers within the hydropower industry. The outcome was 33 research findings with 100% of proposed research completed. In addition, 87% of students chose to either join the hydropower industry or continue their hydropower related research at their universities. These research findings advanced the understanding of pressing research topics within the hydropower industry and met the objective of the funding. An ancillary benefit the program identified through this funding was, not only did 63 students and advisors work on hydropower within the academia space, but now there are more professors and students teaching hydropower at the university level. The program saw an addition of 12 new professors, teaching assistants, and graduate researchers continuing to simulate interest in hydropower. Another interesting outcome is that during this grant funding, the program saw alumni of the predecessor program, who are now professors, applying for the RAP with their students. A unique element of this funding is there was significant cost-share provided by host universities, who did not charge facilities and administration overhead to the student’s research awards. In addition, each university provided laboratories, computing capacity and research facilities to support the research which is extraordinarily unique to grant funding at the university level. The total cost share exceeded 30% of the total grant cost. The funding clearly reached many sectors of the industry to provide helpful work and continue building hydropower’s next generation of innovation and workforce. The Foundation has established a broad network of universities interested and engaged in hydropower. The work was supported by the hydropower industry through donations of meeting space, conference registrations, in-kind contributions, mentorship and support of students. The Foundation would recommend finding a vehicle to further advance programs like the graduate level research through competitions, competitively funded awards and student research. It will take many universities to advance hydropower’s most pressing challenges. To let a program like the RAP dwindle away would incapacitate research at universities.

13 HYDRO ENERGY↗

Progress on Synthesis of Low Content Inert Matrix Fuel Pellets

Progress was made on optimizing hot-press parameters for preparing fuel for two different coating methods: chemical vapor deposition (CVD) and chemical vapor infiltration (CVI). Surrogate materials, CeO 2 and ZrO 2 , were used in place of UO 2 and PuO 2 for fuel development. Although the more porous CeO 2 pellets were not successfully made to the extent that CVI would work with them as intended, hot-press parameters were optimized such that the pellets could be coated using CVD. The ZrO 2 was denser and therefore could more successfully be pressed to CVI standards; however, further improvement is needed before the process is implemented. Future work will continue to explore the optimization of a porous structure for CVI.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Dissolution of Additively Manufactured Mo Disks and Structures for Accelerator Based Production of Mo-99

The press-and-sinter approach for production of Mo targets has been successfully tested and demonstrated. The main advantage of this process is that it uses readily available technology and tools that have been tuned for production of various metal and metal oxide targets. However, certain target design specifications, such as dimensional accuracy of the diameter and thickness of the disks, are required for proper fit into a target holder and therefore place strict tolerances on sintered Mo disks intended for accelerator production. Furthermore, having a target composed of multiple disks poses certain challenges for post-irradiation processing, where there is a potential for spillage of individual disks during the manipulation for dissolution inside a processing hot cell. Additive manufacturing (AM), also referred to as 3D printing, provides capabilities to design and build a single-piece Mo target that provides the opportunity for better geometry for optimized production of Mo-99, improved cooling capability, and safer post-irradiation handling. A drawback of AM Mo structures is roughness of finished surfaces, which could reduce the effectiveness of gas cooling systems. Process development for AM Mo structures using selective laser melting is described in work by Gibson and Lowden. For post-irradiation processing, it is important to look at the dissolution behavior of AM Mo structures in comparison to readily dissolved press-and-sinter Mo targets. The dissolution behavior of press-and-sinter targets has been well documented in our previous reports. In this report, we discuss results of dissolution experiments conducted with AM Mo disks and structures (provided by Oak Ridge National Laboratory [ORNL]) in 50% hydrogen peroxide (H 2 O 2 ).

36 MATERIALS SCIENCE↗

Status of Additive Manufacturing Capabilities for Processing Refractory Alloys Under the Mo-99 Program

The enriched 100 Mo target, denoted as aMo, that Northstar Medical Radioisotopes is developing to produce 99 Mo from an accelerator-based method is a disk-type geometry with a 0.5–0.715 mm thickness and a 29 mm outer diameter. A press and sinter method was adopted to fabricate these samples from aMo powder feedstock. Inherent porosity from the press and sinter method makes the disks more easily dissolvable during 99 Mo postprocessing. However, the disk-type geometry will be subject to thermal stresses due to temperature variations once the geometry is in line with the accelerated electron beam, causing warping and possible failure. Additive manufacturing (AM) processes such as laser powder bed fusion (LPBF) enable the manufacturing of custom, complex geometries that may otherwise be difficult to produce with more conventional methods (e.g., press and sinter approach). Therefore, the National Nuclear Security Administration’s Molybdenum-99 Program invested in developing an AM facility dedicated to processing and printing refractory powders. This report details the LPBF process, how irregular refractory powder can be prepared for LPBF, and the equipment that is available to support the program.

36 MATERIALS SCIENCE↗

Small Punch Testing of Molybdenum-99 Targets

Northstar Medical Radioisotopes is developing an accelerator-based method to produce 99 Mo, which is a parent isotope of the commonly used 99m Tc medical isotope. The Mo targets being designed for the accelerator will be produced from enriched 100 Mo, also known as aMo . Pressed and sintered powder feedstock is used to fabricate aMo targets, producing 29 mm disk-shaped targets. The targets are subjected to 1–6 days in line of an electron beam with subsequent dissolution of the disk to retain the 99 Mo, which decays to 99m Tc at radio-pharmacies. The press and sinter method is advantageous because the inherent porosity produced by this method enables increased surface area and therefore increased flow of dissolution media, decreasing the dissolution time and reducing the need for a highly acidic media. Although porosity aids in dissolution, it reduces the mechanical strength and ductility. Targets require good mechanical integrity when subjected to the conditions in the accelerator. Therefore, Northstar is seeking methods to rapidly test disk samples after fabrication to assure mechanical performance metrics are achieved. This report details the design and testing of a small punch test (SPT) that accommodates the 29 mm disk. Initial data were used to relate the SPT data to tensile properties, such as the yield strength (YS), ultimate tensile strength (UTS), and total elongation to failure. Although the SPT has been established as a somewhat reliable method for testing metallic materials, few studies have applied the SPT to refractory materials such as Mo. Based on tensile testing performed at Oak Ridge National Laboratory on different Mo samples, correlation between the Mo tensile and SPT properties could be performed, establishing a standard calibration that could be applied to other Mo samples. To test the efficacy of the SPT with Mo, multiple different disk batches were fabricated under different conditions (e.g., pressure, lubricant) with commercially available pure Mo powder. Generally, only a UTS could be well defined because the press and sinter disks failed under brittle fracture, making it difficult to determine the YS and elongation. Compared with disks fabricated with aMo powder, the aMo samples underperformed their pure nat Mo counterparts. This report summarizes the current status of the SPT, but further evaluation is needed before it can be applied as a reliable quality assurance tool.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

Near-net shaping of high-density, complex, spatially-tailored ceramics for extreme environments

The purpose of this subcontract is for LLNL to collaborate with the Subcontractor (UCSB) in the areas of binder jet additive manufacturing (BJAM), hot pressing (HP), finite element modeling (FEM), and multi-material sintering studies. LLNL wants to further develop its hot pressing, AM, and modeling capabilities through LLNL’s Early Career Faculty Program. This work will focus on developing a method to hot press complex-shaped ceramic parts through the co-deposition of a structural/functional ceramic and sacrificial mold material in one assembly via multi-material binder jet printing. The method aims to produce dense, near-net shaped parts with applications relevant to a wide variety of fields including aerospace, defense, and energy.

36 MATERIALS SCIENCE↗