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At least 1,135 records · Page 63

Mechanical Performance of Additively Manufactured ODS 316L and 316H Stainless Steels

This work package within the Advanced Materials and Manufacturing Technologies (AMMT) program focused on the mechanical and microstructural characterization of oxide dispersion strengthened (ODS) stainless steels produced using advanced manufacturing techniques. The research aimed to identify an accelerated development path for ODS alloys by integrating additive manufacturing (AM) technologies with recent advancements in ODS materials and traditional manufacturing methods. For FY 24, the research specifically targeted exploring an accelerated development path for ODS alloys by combining AM technologies with these advancements. Novel AM and post-build processing routes were developed for ODS austenitic alloys, including Fe-Cr-Ni alloys such as 316L and 316H. Electron microscopy and mechanical characterizations were conducted to evaluate the impact of process variables on microstructure and properties, with the goal of optimizing these properties economically. Traditionally, producing ODS alloys involves multi-day, high-energy mechanical milling of alloy powder with yttria powder, followed by milled-powder consolidation through extrusion or other methods, and additional thermomechanical processing (TMP) for property control. To overcome the challenges associated with this complex and costly approach, we propose exploring alternative, cost-effective processing routes that emphasize AM and traditional TMP methods. The new processing routes for ODS alloys have achieved significantly higher strengths—several times greater than those of wrought stainless steels—while maintaining substantial ductility and fracture toughness. This report outlines the novel and economical AM-based processing routes for ODS austenitic alloys, combined with post-build TMPs, and discusses the mechanical and microstructural characteristics of the developed materials.

36 MATERIALS SCIENCE↗

Improved PARE (Pressurized Airborne Release Equipment) for Damage Ratio, Airborne Release Fraction and Respirable Fraction Testing (Version 4)

This paper describes an improved version of the PARE (Pressurized Airborne Release Equipment) system (Sutter 1983a and Sutter 1983b and Ballinger et al 1987) for powder venting testing. This effort seeks to improve the accuracy of risk estimation for the venting of pressurized powders and the venting of gases through pressurized powders. This includes experimental measurement for estimating DR (damage ratio), ARF (airborne release fraction) and RF (respirable fraction) quantities. The present study was performed to address previously indicated problematic factors (i.e. noted gaps) (US DOE 1994).

42 ENGINEERING↗

Evaluation of DED and LPBF Fe-based Alloys Process Application Envelopes based on Performance, Process Economics, Supply Chain Risks, and Reactor-specific Targeted Components

The U.S. Department of Energy (DOE), Office of Nuclear Energy (NE), Advanced Materials and Manufacturing Technologies (AMMT) program aims to develop extreme-environment materials solutions for use in the deployment of advanced nuclear reactors and the sustainment of the current fleet. To achieve this objective, a combination of experiment, a computational tool, and machine learning (ML) for the design of materials is adopted for the maturation of materials for nuclear technology. Through advanced manufacturing techniques such as laser powder bed fusion (LPBF) and laser powder direct energy deposition (LP-DED), components with complex geometries can be fabricated with reduced time and effort. Such advanced manufacturing methods can also provide the opportunity to improve materials performance through optimized microstructures and mechanical properties. However, existing engineering alloys are not always well suited for fabrication with additive manufacturing (AM), as their compositions have been tuned to optimize fabrication via conventional methods. Thus, similar alloys with modified compositions that are better suited for AM can be studied for improved performance. Over the past three years, the AMMT teams from Argonne National Laboratory (ANL) and Pacific Northwest National Laboratory (PNNL) studied various known Fe-based alloys by evaluating their initial printability using LPBF, and an AMMT-developed down-selection and decision matrix reduced the number of alloys to be studied from six to three in fiscal year (FY) 2024. Additionally, in FY 2024, for parallel evaluation, these three alloys were studied using LPDED. While LPBF is better for small- to medium-sized components with high detail and internal features, LP-DED combines a material feed system to place the powder onto the exact spot where the laser will melt the material. This AM method can be easily scaled to extremely large components and provides high build rate speeds compared to those of conventional LPBF systems. Additionally, DED is a better choice for complex geometries and compositional gradients.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Exxon Mobil-NETL Testing of DAC Materials

This joint initiative is aimed at extending our understanding of real DAC testing conditions at the NETL DAC testbed facility. Of particular focus will be: • Small Scale testing of powdered and formulated materials (supplied by ExxonMobil) to evaluate various performance metrics under DAC process cycles • Pilot scale testing of formulated materials at larger scales ExxonMobil will work with NETL to shake down equipment, validate testing methods, and define best practices for data analysis. Three tasks are proposed: 1. Validation of multi-cycle test data on powdered and formulated materials to benchmark various performance metrics of these materials. 2. Steam regeneration of powdered samples at small scale to define baseline performance under commercially relevant conditions. 3. Pilot scale testing of larger formulated materials to test commercially relevant samples under actual process cycles.

36 MATERIALS SCIENCE↗

Understanding Biases in Sample Preparation Techniques for Coupled Scanning Electron Microscopy and MAMA PuO 2 Morphological Analysis

In this project, the scanning electron microscopy (SEM) sampling method used during the statistical design study (SDS) was investigated to determine if any sampling biases were present in the analyzed data. Using standard particle size distribution powders from the National Institute of Standards and Technology (NIST 1984 standard reference material) with the origin wet dispersion method, it was determined that a bias to smaller particles was present. This was supported by theoretical calculations using Stokes’ law to determine the settling rate of spherical particles of roughly the same size and mass as those found in the SDS. Based on the theoretical calculations, it was determined that the settling rate for each of the 76 powder sets in the SDS could be unique based on specific particle shape and mass distributions, making a universal correction factor/formula not applicable. Therefore, priority shifted to developing an improved wet dispersion method that significantly reduced the particle settling rate for all particle size and shapes. This was achieved by replacing the original solvent (isopropyl alcohol) with a heavy liquid (lithium heteropolytungstates), which dramatically slowed the settling rate and allowed for the capture of a suitable homogeneous aliquot. SEM imaging and Morphological Analysis for Material Attribution (MAMA) software analysis were conducted on the NIST standard, and the SEM/MAMA data were compared to data captured by a dynamic image analysis particle size analyzer. The resulting data confirmed that the new wet dispersion method does indeed deliver an improved representative aliquot to the SEM stub. For instance, in the NIST certificate, the average particle size is ~17.1 µm ± 2.2 µm with a normal distribution. The initial wet dispersion method resulted in a drastically reduced average particle size of 6.1 µm in addition to a non-representative heavy bi-modal distribution whereas the improved LST wet dispersion method resulting in an average particle size that was much closer to the NIST certificate (12.7 µm) with a similar normal distribution. Although the improved method was still short of the NIST certificate average, atomic force microscopy analysis determined that the resulting ~20-25% reduction in size was due to particles sinking into the carbon sticky tape used for SEM imaging. It is believed that that this bias can be calibrated in a much more predicable manner than the original settling rate bias. In addition, the matching normal distribution curves between the NIST certificate and the heavy liquid method indicate a much-improved representative aliquot has been sampled and imaged. A surrogate CeO 2 powder was used to reflect PuO 2 more accurately and to aid in implementing radiological controls and shielding. The resulting data sets from the SEM/MAMA method and the particle size analyzer give almost identical average particle sizes and particle distribution statistics. Future work will re-analyze several select runs from the SDS to determine if morphological signatures can be found with the improved sampling method.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A&L Annual Report: GRM-MAPS

Exploding Bridge Wire (EBW) is an important design for initiating detonators relevant to several LLNL systems. In such designs, a metal bridge wire is in direct contact with a porous secondary high explosive (HE), typically pressed to around 50% of its crystalline density. Initiation is believed to occur through shock waves generated when the bridge wire is made to explode via the rapid passing of a strong current pulse. Permeametry is an important characterization tool for the porous powdered HE (PETN, HMX, etc.) component in such devices. Such powders are well known to coarsen with age, with an accompanying deterioration in performance, which includes increased function time and sensitivity. Among various material characteristics, one that has been shown to correlate the most with such performance parameters is the flow-permeable surface area (FSSA), measured using air-permeametry. Commercially available permeametry apparatuses, such as that from Fisher Scientific or a more modern version from Micromeritics suffer from a few drawbacks, most notably as related to monitoring age-related changes in FSSA. This is because it requires re-compaction of the aged powder into the permeametry tube, which in most cases leads to an unwanted increase in FSSA. To address this and a few other shortcomings, we have been developing a modern version of the permeameter, Gee-Reinstein-Maiti Modern Air-Permeametry System (GRM-MAPS). In this report, we summarize progress made in FY25 toward perfecting and calibrating the instrument, which we aim at deploying within surveillance in FY26.

36 MATERIALS SCIENCE↗

Additive manufacturing of amorphous metal soft magnetic composites

Soft magnet alloys are used as magnetic cores for electric motors, transformers, wind turbines and other power generation systems. Soft magnetic cores are expensive and time consuming to manufacture in the complex shapes required for next-generation devices using conventional press and sinter powder metallurgy. The objective of this effort is to additively manufacture high performance soft magnets, with reduced cost and reduced material waste and 10x lower energy (core) loss at the high operating frequencies of many electric machines. Laser powder bed fusion additive manufacturing is used as the fabrication method. Electrical steel and amorphous alloys atomized powders are used as a feedstock materials. Magnetic cores are printed in topology optimized structures such as the Hilbert curve because this has been shown to reduce energy losses by minimizing the eddy currents that circulate within the magnet at high frequencies. In our project, we succeed in printing FeSi 3.5wt% and FeSi 6.5wt% electrical steels, and iron-based soft magnetic amorphous alloys in the shape of Hilbert and Peano curve topology optimized structures. We found that the Peano curve has a higher cut-off frequency than the Hilbert curve, and that amorphous alloys have high cut-off frequencies and higher mechanical hardness than electrical steels. Processing conditions such as laser power, scan speed, and hatching pattern were optimized to achieve high density prints, and optimize magnetic performance. We find that the printing of amorphous alloy soft magnetic cores may be technoeconomically feasible for large scale applications such as transformers, for which supply chain issues and the labor costs of manual fabrication of magnetic cores is prohibitive in some cases.

36 MATERIALS SCIENCE↗

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↗

Near-Net-Shape HIP Manufacturing for sCO2 Turbomachinery Cost Reduction

sCO2 turbomachinery that operates above 650°C requires the use of γ' strengthened Ni-based superalloys, leading to high cost and barrier of market adoption. Near-net-shape (NNS) HIP manufacturing with 282® alloy powder is being developed for sCO2 turbine components, with a significant estimated cost reduction. Tensile, creep, low cycle fatigue properties of argon gas atomized and plasma atomized powders were evaluated and compared to sand cast HAYNES® 282®. While tensile strength and fatigue life outperformed sand cast material, a 10~25% debit in the creep stress capability was observed due to the fine grain size and presence of prior particle boundaries (PPBs). Finite element model calibrated by powder rheological properties accurately predicted the nonuniform shrinkage during HIP, providing HIP tooling design to achieve the target dimension. A 20 lbs. turbine nozzle ring was successfully demonstrated within 0.01 inch dimensional tolerance at the vanes. A 1700lbs. turbine casing with complex internal struts and manifolds was also demonstrated being close to the target dimension.

14 SOLAR ENERGY↗

Additive Manufacturing of Tool Steels

This article provides a brief overview of additive manufacturing (AM) of tool steels via various AM technologies such as laser powder bed fusion, electron powder bed fusion, blown powder directed energy deposition, and binder jet AM. The discussion includes process overview and covers the mechanism, advantages, and applications of each of these techniques.

Nandwana, Peeyush↗

Effect of Remnant Carbon and Etching of Particles on Pyrolysis Bonded Silicon Carbide (PBSC)

Silicon carbide (SiC) formed through pyrolysis of preceramic polymers loaded with SiC particles has gained significant attention for applications such as coatings, composite matrix modifications, and most importantly additive manufacturing. This work presents combined synchrotron XRD, Raman spectroscopy, scanning electron microscopy, nano-indentation, and Vickers indentation of pyrolysis bonded SiC to shed light on the changes of composition and mechanical properties of these materials. Characterization was performed on samples that were heat treated ranging from the synthesis 850 °C up to 1500 °C. Pre-treatments of the powders prior to pellet synthesis, such as heat treatment and etching using a hydrofluoric acid (HF), were investigated. It is shown that the degradation of mechanical properties when exposed to higher temperatures is due to the burnout of amorphous carbon clusters remnant of the pyrolysis process of the preceramic polymer. Furthermore, prior HF etching and removal of the native oxide layer of the powders showed improved density and hardness values in the final pellets. The average Vickers hardness of the control samples were 4.59 GPa and later 3.74 GPa when exposed to 1500 °C, while the samples synthesized using powders that were etched with HF had an average hardness value of 9.37 GPa and later 6.86 GPa when exposed to 1500 °C.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Mechanical Activation and Cation Site Disorder in MgAl 2 O 4

The synthesis and crystallographic site occupancy were investigated for MgAl 2 O 4 with and without mechanical activation of the precursor powders. Heating to 1200 °C or higher resulted in the formation of a single spinel phase regardless of whether the powders were mechanically activated or not. Neutron diffraction analysis was used to determine cation site occupancy and revealed that mechanical activation resulted in a lower degree of cation site inversion compared to the nonactivated materials, which indicated that the powders were closer to thermodynamic equilibrium. This is the first study to characterize the effects of mechanical activation on crystallographic site occupancy in magnesium aluminate spinel using neutron diffraction.

36 MATERIALS SCIENCE↗

On the Mechanical Behavior of LP-DED C103 Thin-Wall Structures

Laser Powder Directed Energy Deposition (LP-DED) can produce thin-wall features on the order of 1 mm. These features are essential for large structures operating in extreme environments such as regeneratively cooled nozzles and heat exchangers, which often make use of refractory metals. In this work, the mechanical behavior of LP-DED C103 was investigated via quasi-static tensile testing and low cycle fatigue (LCF) testing. The effects of vacuum stress relief (SR) and hot isostatic pressing (HIP) heat treatments were investigated for specimens in the vertical and horizontal build orientations during tensile testing. The AB and SR properties were lower than literature values for wrought and laser powder bed fusion (L-PBF) bulk components but higher than electron beam powder bed fusion (EB-PBF). The application of a HIP cycle improved strength by 7% and ductility by 27% past the initial as-built condition. Fracture images reveal that interlayer stress concentration sites are responsible for fracture in specimens in the vertical orientation. Meanwhile, fracture in the horizontal specimens mainly propagates at a slanted angle typical of plane stress conditions. The LCF results show cycles to failure ranging from 100 cycles to 8000 cycles for max strain levels of 2% and 0.5%, respectively. Fractography on the fatigue specimens reveals an increasing propagation zone as max strain levels are increased. The impact of these findings and future work are discussed in detail.

36 MATERIALS SCIENCE↗

Spray Drying Enzyme-Treated Cellulose Nanofibrils

Enzyme-treated cellulose nanofibrils (CNFs) were produced via a lab-scale mass colloider using bleached kraft pulp (BKP) to evaluate their processability and power requirements during refining and spray-drying operations. To evaluate the energy efficiency in the CNF refining process, the net energy consumption, degree of polymerization (DP), and viscosity were determined. Less energy was consumed to attain a given fines level by using the endoglucanase enzymes. The DP and viscosity were also decreased using the enzymes. The morphological properties of the enzyme-pretreated spray-dried CNF powders (SDCNFs) were measured. Subsequently, the enzyme-pretreated SDCNFs were added to a PP matrix with MAPP as a coupling agent. The mixture was then compounded through a co-rotating twin-screw extruder to determine whether the enzyme treatment of the CNFs affects the mechanical properties of the composites. Compared to earlier studies on enhancing PMCs with SDCNF powders, this research investigates the use of enzyme-pretreated SDCNF powders. It was confirmed that the strength properties of PP increased by adding SDCNFs, and the strength properties were maintained after adding enzyme-pretreated SDCNFs.

59 BASIC BIOLOGICAL SCIENCES↗

Synthesis and characterization of uranium trichloride in alkali-metal chloride media

Given a growing interest in uranium salts for pyrochemical processing of used fuel and uranium-fueled molten salt reactors, the synthesis of uranium trichloride in alkali-metal chloride media was investigated in a series of four experiments. Specifically, uranium metal powder and uranium hydride powder were prepared and separately blended with ammonium chloride and lithium chloride – potassium chloride eutectic in two runs, while the same powders were separately blended with ammonium chloride and sodium chloride in two additional runs. Each of the lithium chloride – potassium chloride containing blends was slowly heated to 923 K, while those containing sodium chloride were heated to 1123 K. During each heat up, the ammonium chloride sublimed into gaseous ammonia and hydrogen chloride, leading to the chlorination of uranium metal or uranium hydride and the formation of molten salt solutions of the respective chlorides. Experimental conditions were incorporated in the runs to promote formation of uranium trichloride over uranium tetrachloride in the respective media. Molten samples of each run product were taken and characterized via chemical analyses, diffractometry, and microscopy. The final products from each run were dark dense ingots of the respective salt systems with uranium concentrations ranging from 44 to 51 wt%. Chemical analyses and diffractometry identified the predominant presence of uranium trichloride in these systems; however, a possible minor presence of uranium tetrachloride could not be conclusively dismissed.

D Herrmann, Steven↗

Bentonite buffer under high temperature: laboratory experiments and coupled process modeling

Abstract. Bentonite buffer in a geological repository will be simultaneously heated from decaying radioactive waste and hydrated from the surrounding host rock, triggering complex and coupled THMC (thermal–hydrological–mechanical–chemical) processes. Understanding the THMC behavior of bentonite-based engineered barrier system (EBS) is key to the evaluation and prediction of its long-term performance. Studies on the THMC process have been focused on conditions under 100 ∘C, as most design concepts impose a thermal limit of 100 ∘C in bentonite. Recently, studies under high-temperature conditions have been conducted to evaluate the possibility of raising the thermal limit and expanding the data/knowledge base to increase the confidence level. In this abstract, we present a series of bench-scale laboratory experiments at high temperatures (up to 200 ∘C) and the corresponding modeling work. Two sets of column tests were conducted, and each set consisted of two test columns: a control column undergoing only hydration (non-heated) and an experiment column experiencing both heating and hydration (heated). During the experiment, frequent X-ray computed tomography (CT) images were collected to provide a 3D visualization of the density distribution and present the spatiotemporal evolution of (1) hydration/dehydration, (2) clay swelling/shrinkage, (3) displacement, and (4) mineral precipitation. The two sets of tests differ with respect to several experimental conditions, such as bentonite type, compacted density and water content, water chemistry, and hydration pressure, but the important difference is that the first set used bentonite powder with a dry density of 1.28 g cm−3, whereas the second set used granulated bentonite (mixture of pellets and powder) with a dry density of 1.45–1.5 g cm−3. In both sets of experiments, a comprehensive post-dismantling characterization of bentonite samples was carried out after the column tests had been running for 1.5 years. Comparing non-heated and heated columns, the temperature gradient led to lower degree of homogenization of bentonite after bentonite became fully saturated; comparing the first and second sets, granulated and powdered bentonite exhibited drastically different hydration behavior. A THM model with a 2D axisymmetric grid system was used to interpret the data from the first set of tests. The model considers the combined impact of saturation, fluid pressure, and porosity change due to swelling/compression on the spatiotemporal distribution of bulk density and movement of the thermocouple modules. Observations from the tests help us understand the early perturbation of bentonite buffer under high temperature, and data from these tests improve the calibration of key constitutive hydrological and mechanical models and, therefore, enhance the modeling capability with respect to calculating the long-term evolution of bentonite buffer.

Zheng, Liange↗

Fluid Induced Elemental and Mineralogy Alterations of Caney Shale

ABSTRACT: Studies were conducted on cores and rock cuttings recovered from two wells drilled in Caney shale in the Southern Oklahoma. Mineralogical compositions of these samples were obtained by X-Ray Diffraction (XRD) measurements using two methods of sample preparation: conventional powder (by crushing and grinding of rock fragments) and spray-drying of micronized rock powder method. Microstructure and microanalysis were acquired by Scanning Electron Microscopy/Energy Dispersive Spectroscopy (SEM/EDS). Batch experiments were then conducted using selected rock samples and fracturing fluid whilst deionized water was used as control sample for fluid/rock interaction. These were conducted at 95°C and ambient pressure for various time periods to assess the geochemical reactivity of the Caney shale. The rock samples were subsequently recovered from fluid, dried and analysis repeated using identical XRD and SEM/EDS measurements, following the same conditions. Preliminary experimental results show rock mineralogical compositions are predominantly quartz with relatively high clay content. The clay minerals are mainly illite. Carbonate content is less than 10% by weight for most samples, with other non-clay minerals pyrite, albite, dolomite, and some apatite. In general, sprayed samples showed more intense peaks and less full width at half maxima (FWHM) relative to conventional rock-powder samples. Post-experimental mineralogical changes were observed in samples with clay portions breaking down to amorphous entities. As expected, dissolution of carbonates (calcite and dolomite) was observed and newly detected dissolution of biogenic micro quartz resulted in formation of amorphous silica. 1.0 INTRODUCTION Formation of sedimentary rocks involves processes where rock sediments are emplaced with fluids starting interactions that persist over long periods. During the lithification process, sediments and fluids react and attain equilibrium state. This equilibrium is disturbed during drilling, completion, hydraulic fracturing and other operations that involve the introduction of engineered fluids into the subsurface. To return to equilibrium, dissolution and precipitation of minerals may occur. These reactions have implications on the petrophysical properties of the reservoir. Whiles dissolution and precipitation of minerals can enhance porosity and permeability, the reverse can also be true. For example, when acidic fluids are introduced into formations with high carbonate contents, carbonate minerals dissolve into solution thus increasing the porosity and permeability of the formation. In contrast, when alkaline fluids with pH above 11 are introduced into an illite-rich shale formation, the rock-fluid interaction leads to de-flocculation of illite platelets causing substantial increase in clay fines migration, consequently significant reduction in permeability (Salles et al., 2008).

Awejori, G.↗

Radioactive Cleaning Robot

Here at Fermi National Accelerator Laboratory, particle accelerators are constantly running, giving off excess radioactive dust. This dust can be extremely harmful to people and the environment, posing numerous issues. The goal of this project is to conceptualize an automated cleaning solution. With this main goal in mind, the project started with a brainstorming session. The main concept relied on the use of a powder distributing system paired with a vacuum to easily attract and trap the dust. From this main concept, multiple sketches were produced, showing a robot with pieced-together systems. With the initial idea down, each subsystem could be brought further with the inner workings being sketched out. After sketches and proof of concept were polished, the next step was to begin 3D modeling, using NX, to bring life into the sketches. With every day came new ideas, modifying the previous sketches and models as necessary. Soon after the bigger structures were fleshed out, the focus could be shifted onto the less pressing subsystems. Adding a conveyor belt and spinning brush attachment to the powder hopper allowed for more even powder distribution. Along with that, the addition of spring-loaded brushes on the vacuum nozzle ensures constant dust agitation, improving overall functionality. A few other quality of life improvements, such as a removable dust reservoir with a ramp gave a push towards real life functionality. After considering the logistics of this robot functioning in real-life, pressure plates were provided to stop the robot from crashing into its surroundings. Having all of the individual models lead to an overall assembly. Making this robot programmable allowed for this project to meet the design requirements, providing a solution to the previous dilemma.

43 PARTICLE ACCELERATORS↗