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At least 955 records · Page 53

Polymer Composites Reinforced by Carbon-Allotrope Fillers for Selective Laser Sintering (SLS) - A Review

The limited commercial availability of applicable polymer powders has hindered the widespread implementation of SLS as a legitimate manufacturing method. This is partly due to the mechanism of SLS, which requires powders to meet rigid specifications if processing is to be successful. Furthermore, powders that do meet requirements are often incapable of producing quality, high-performance parts. Academic and industrial research has focused on composite development to overcome this problem. The incorporation of fillers including calcium carbonate, molybdenum disulfide, and aluminum have all been found to influence the processing behavior of PA12 powder and ultimately, the properties of the final part.3-5 Here, the thermal and mechanical properties of sintered composite parts produced using polymer powders reinforced by various carbon-based fillers is discussed.

36 MATERIALS SCIENCE↗

Modeling Nondestructive Defect Detection in Additively Manufactured Metallic Structures for Nuclear Applications

The future of quickly, economically produced metallic nuclear reactor parts with minimal supply-chain dependence lies in Laser Powder Bed Fusion (LPBF) Additive Manufacturing (AM): a 3D printing method involving laser melting and net shaping stainless steel and Inconel metallic powder into a solid structure. However, intrinsic features in LPBF frequently leads to the formation of materials defects, such as pores, within 3D printed structures. As safe long-term use in energy applications requires knowledge of all relevant defects before deployment in a reactor, we must develop methods for nondestructive detection of these defects. We are investigating Pulsed Thermal Tomography (PTT), which is a non-contact nondestructive imaging method scalable to arbitrary structure size. Thermal tomography (TT) is a computational method for 3D spatial reconstruction of material thermal effusivity from flash or pulsed thermography temperature data cube. Thermography data cube consists of 2D surface temperature measurements at different times. The objective of the present work is to investigate limits on defect detection in AM metallic structures with PTT. To this effect, we modeled PTT with COMSOL heat transfer computer simulations. We developed a layered media COMSOL simulation consisting of a Stainless Steel 316 (SS316) plate with an internal layer of un-sintered SS316 powder. Thermophysical properties of the powder layer were modeled with equivalent volume mixing model. To account for partial sintering at the boundary of the defect, the transition between solid and powder layers was modeled as a Gaussian. Using data from COMSOL simulations, we reconstructed depth-dependent thermal effusivity, which allowed defect visibility estimation. A series of parametric studies determined that at 1mm depth, 50µm is the smallest detectable defect. In addition, classification of the defects which can lead to early fatigue of the metallic structure in a reactor is briefly discussed.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Investigation of Luminescent Ceria as a Plutonium Oxide Simulant. Final Report

Plutonium oxide powders from various production lines at Los Alamos National Laboratory are stored and transported in specially designed “SAVY-4000”, “Hagan”, or other containment systems. Cerium oxide powder has been used as a less-hazardous simulant powder for testing accidental release from these containers under various operational scenarios. This work investigates the development and use of fluorescent cerium oxide powders as a more easily detectable, and potentially quantifiable, simulant powder for plutonium oxide container systems

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Binder Jet Printing of H13 Tool Steel

ORNL and Carpenter worked on evaluating H13 powders with different powder size distributions for deposition via binder jet additive manufacturing (AM). Binder jet AM has the potential to be a costeffective technique for fabrication of near net shaped tools with complex geometries and internal features such as cooling channels that can improve the production efficiency of injection/compression molding tools. However, a critical challenge in binder jet AM is the densification of the said tool for it to be usable. Powder size distribution can affect the process settings required to deposit the material and the subsequent sintering behavior. In this collaborative effort ORNL and Carpenter demonstrated that the process variables depend on the powder size distribution while the carbon pickup during sintering depends on the binder burnout atmosphere and temperature. On the other hand, there was no noticeable difference in the microstructural evolution of H13 deposited using the different powder size distributions.

42 ENGINEERING↗

Develop Direct 3D Building as a Transformational 3D Printing

Phase 1 of this project recognizes the key advantages of direct 3D building (3DB) by literature research, initial experiments, and analyses. The fundamental enhancement in powder density, layer thickness, and their uniformities are attributed to the independence from high blade speed and powder flowability. The increase in layer quality, before selective fusion, is found qualitatively significant for a step change in process robustness when the unrepeatability of 3D printing (3DP) remains a challenge in serial volume production. The reduced challenge of powder flowability should not only entail improvement in build quality but also reduce powder cost from the strict morphology and size specs. The concurrent selective fusion and powder surface preparation eliminate the need for frequent recoating pauses to increase build speed. On-going experiments include density cup measurements by X-ray scanning and recoating performance evaluation by a rotating disk system to verify some of the results.

42 ENGINEERING↗

An Integrated Flame Spray Process for Low Cost Production of Battery Materials for Lithium Ion Batteries and Beyond

The overall objective of this project was to develop an advanced manufacturing technology for Li-ion battery materials production at low cost and in a green chemical process using glycerol as solvent to replace water. It was aimed at developing a prototype pilot production line to reduce production cost by at least 25% to the baseline. During the course of this project, research was conducted to understand spray drying and combustion of eutectic solvent precursors of glycerol and metal salts (acetates) in the formation of mixed metal oxide powders. Reactor design and optimization were done to facilitate spray drying and combustion in powder formation and processing. Various cathode materials powders were produced, including lithium nickel-cobalt-manganese oxide (NCM) and lithium nickel-cobalt-aluminum oxide (NCA). These cathode materials powders were tested in half coin cells for their performances, with materials performances of 160 mAh/g for NCM111 and 200 mAh/g for NCA. NCA powders were also produced using a slurry spray-drying process and tested in full pouch cells. A pilot scale flame assisted spray drying reactor was constructed and demonstrated for its production rate exceeding the target of production rate of four metric tons per year. The work performed in this project has been documented in 9 peer reviewed journal publications, 8 conference presentations, and two IP disclosures/patent applications.

25 ENERGY STORAGE↗

Evaluation of AddUp Precision L-PBF Technology for Tooling and Other Industrial Applications

ORNL (Contractor) and AddUp Inc. (Participant) collaborated to enable the adoption of laser powder bed fusion for tooling applications, critical for reshoring the manufacturing sector in the U.S. Most of the work on laser powder bed fusion has focused on high value materials such as Ti-6Al-4V and Inconel 718 for niche applications in aerospace, biomedical and energy sectors. In this collaboration, ORNL and AddUp worked laser powder bed fusion of maraging steels for tooling applications while leveraging the unique ability of the AddUp laser powder bed fusion system to deposit fine powders. We demonstrated that the AddUp technology is capable of depositing complex artifacts and features such as overhangs within desired tolerances. We also showed that direct aging of the deposited parts result in simultaneously higher strength and elongation compared to the conventional two step heat treatments, which could result in significant energy savings. Finally, we developed thermos-kinetic models to enable design of heat treatments for optimal material properties compared to the energy intensive empirical methods currently used. The report summarizes the detailed findings of this collaboration.

36 MATERIALS SCIENCE↗

Additively Manufacturing Nitinol Shape Memory Alloys for Advanced Actuator Designs

The objective of this research was to understand the role of feedstock production in the phase transformation behavior of additively manufactured Ni-Ti alloys for advanced actuator design. Industrial adoption of additively manufactured Ni-Ti alloys depends on the ability to produce repeatable phase transformation behavior, quantified here by the austenite to martensite transformation on heating. Small variations in the alloy composition may have a significant effect on the temperature at which this transformation occurs. This project showed that the powder characteristics play an important role in determining this behavior. Increases in the surface area per unit volume of the powder, either as a function of size distribution or morphology, have the effect of reducing the Ti content in the alloy through the formation of Ti-rich oxides on the powder surface, which has the effect of depressing the transformation temperature. Preferential Ni vaporization during additive manufacturing can partially offset this effect. To achieve repeatable results, it is important to understand the effect of powder oxidation, and to control the powder characteristics.

36 MATERIALS SCIENCE↗

Process Intensification for Nanostructure Aluminum Extrusions

A new technology called Shear Assisted Processing and Extrusion (ShAPE™), pioneered at the Pacific Northwest National Laboratory (PNNL), has the potential to revolutionize the US extrusion industry. Maturation of the ShAPE™ process would create a new cross cutting US manufacturing technology that advances three key the objectives within AMO; namely, nanomaterials processing, process intensification, and materials for extreme and harsh environments. PNNL and SCM Metals Products, Inc. (SCM), a division of Kymera International, will collaborate to mature the ShAPE™ extrusion process beyond TRL 3 to increase the likelihood of its adoption by industry. PNNL’s custom (one-of-a-kind in the world) ShAPE™ machine will be used to extrude round rods of high strength aluminum alloy feedstock powder provided by SCM. As proof-of-concept, PNNL has previously extruded 5 mm diameter rods with SCM aluminum alloy powder AL-12.4TM. This project aims to scale up the process to a diameter of 25 mm while retaining the excellent mechanical properties achieved for the 5 mm diameter rods. The degree of process intensification with ShAPE™ will also be estimated. The primary objectives of this project are as follows. 1) Fabricate 25 mm diameter nanostructured extrusions in bulk, directly from AL-12.4TM aluminum alloy powder without the need for canning, degassing, compaction, and other intermediate steps typical of powder metallurgy extrusion. 2) Achieve a microstructure with an ultrafine grained (UFG <1 µm) aluminum matrix having refined and homogenously distributed nanoscale second phases. 3) Show that the ram force can be significantly reduced compared to conventional powder metallurgy extrusion of the same material and estimate the extent of process intensification that may be possible with ShAPE™. 4) Demonstrate improved high-temperature mechanical properties compared to conventional extrusion of the same material. The following tasks will be undertaken to achieve these objectives. PNNL will develop the die set and process parameters necessary to fabricate Al-12.4TM extrusions with a 25 mm diameter. Microstructural analysis will be performed by PNNL while mechanical testing will be conducted by SCM. With information learned from the process development and characterization, PNNL will perform an estimate of the degree of process intensification that may be possible with ShAPE™.

42 ENGINEERING↗

Preliminary Characterization and Evaluation on FFF Manufactured 316H and ODS Steels

The Advanced Materials and Manufacturing Technology (AMMT) program develops cross-cutting technologies in support of a broad range of nuclear reactor technologies and maintains U.S. leadership in materials and manufacturing technologies for nuclear energy applications. The overarching vision of AMMT is to accelerate the development, qualification, demonstration, and deployment of advanced materials and manufacturing technologies to enable reliable and economical nuclear energy. Solid-state advanced manufacturing techniques can overcome some of the challenges in liquid-based additive manufacturing (AM) processes and should therefore be considered in material design and manufacturing as well. The work presented in this report forms part of a study on solid-state AM techniques of 316 stainless steels (SS) and oxide dispersion strengthened (ODS) steel components and supports the vision and goals of the AMMT program relevant to accelerate the development and deployment of advanced manufacturing processes. Achieving this can provide a safety improvement through larger safety margins, economic benefit for higher efficiency during operation, and a cost reduction through more effective manufacturing processes and less waste. This study provides preliminary information on development of the fused-filament fabrication (FFF) process using different powder types to demonstrate the sensitivity, and therefore the characterization of these sample components. The full solid-state manufacturing feasibility study will be completed and reported in a final feasibility evaluation during 2025. The study investigation used two 14YWT ODS powder batches, which provided information and the effect of different powder morphologies on manufacturability. The two 316SS powders demonstrated the effect of powder size on the manufacturability using FFF. Two product forms, namely a honeycomb structure and flat samples, were manufactured to demonstrate the flexibility of product form.

36 MATERIALS SCIENCE↗

AGR-5/6/7 Fuel Fabrication Report

The U.S. Department of Energy Office of Nuclear Energy (DOE NE) and the Idaho National Laboratory (INL) Advanced Reactor Technologies (ART) Advanced Gas Reactor (AGR) Fuel Development and Qualification program (referred to as AGR Fuel program hereafter) are pursuing qualification of tristructural isotropic (TRISO) coated particle fuel for use in high temperature gas cooled reactors (HTGRs). The AGR Fuel program was established to provide a fuel qualification data set in support of the licensing and operation of an HTGR. BWX Technologies Nuclear Operations Group (BWXT-NOG) was subcontracted to fabricate the fuel for the AGR program. Several investments and innovations were realized in preparation to fabricate fuel for the AGR-5/6/7 irradiation experiments that brought fuel fabrication fully out of the laboratory and into engineering-scale operations. These included: • Increased the kernel fabrication line capacity and uniformity • Upgraded ancillary support equipment and processes for the tristructural isotropic (TRISO) coating furnace • Demonstrated efficient production of the matrix precursor powder by dry jet milling of co mingled components • Demonstrated an engineering-scale method for quick and efficient overcoating TRISO particles with the matrix precursor • Demonstrated an automated, multi cavity compacting system with a volumetric feed system • Demonstrated a combined-cycle thermal treatment furnace These changes increased production rates of some of these processes by an order of magnitude or more while eliminating the use of flammable solvents, multiple grinding and sorting operations, and the weighing out of individual die charges. Three fuel kernel lots were fabricated for production of the fuel for AGR-5/6/7. The initial lot (J52R-16-39316) was certified to fuel specifications but was not used because the kernels had a high fraction of internal fissures that caused an unacceptable fraction of the kernels to fragment when charged to the coating furnace where the TRISO coating would be deposited. Fragmented kernels increased the dispersed uranium in the particles and produced a worrisome fraction of dimpled particles with an elevated probability of in-pile failure. After some efforts to identify the cause of the fissure formation, two additional lots were produced with much lower fissure fractions, J52R-16-69317 and 69318. The latter kernel lot was a backup to the first and was not needed. Multiple kernel batches were composited to form each of the lots so as to simulate a commercial-scale operation where kernel batches would also be composited. Multiple TRISO coating runs were performed and the product characterized so that several could be composited into a TRISO lot. TRISO lot J52R-16-98005 conformed to all fuel specifications except the mean outer pyrocarbon (OPyC) layer thickness was thinner than specified. Furthermore, it was determined that the TRISO lot had a dispersed uranium fraction (DUF) that might result in the compacts not meeting the DUF specification. A review of the role of the OPyC layer and consequences of the DUF by the Technical Coordination Team and INL concluded that the fuel was acceptable for use in the AGR-5/6/7 irradiation experiment. The TRISO particles were overcoated with the matrix precursor that had been produced in a jet-milling operation. The overcoating was performed in equipment originally designed to coat pharmaceuticals. The overcoating process performed well; producing highly spherical and uniform overcoats requiring little upgrading and no recycle or rework. TRISO particles were overcoated with the matrix precursor to achieve nominal volumetric packing fractions (PFs) of TRISO particles of 25% and 40% for the irradiation experiments. The 40% PF compacts occupy the first and fifth test capsule in the test train while the inner three capsules are loaded with 25% PF compacts. The resinated graphite matrix precursor powder was a derivative of the German A3-27 matrix formulation, which differs from previous AGR irradiation campaigns that used an A3-3 formulation. Jet milling of the matrix powder precursor produced a finer mean graphite particle size than the milling operations used for the A3-3 matrix powder precursor. Changes made in the matrix formula and equipment yielded compacts with significantly higher matrix density than was attained in previous AGR irradiation campaigns. The changes in the matrix formulation and the means of milling the powders also complicated resolution of the three fuel compact defect fractions, DUF, exposed kernel fraction (EKF), and the silicon carbide defect fraction (SDF). Characterization data from BWXT-NOG had some anomalous results, so samples of the fuel compacts and overcoated TRISO particles were also analyzed by Oak Ridge National Laboratory (ORNL) to ensure that the defect fractions were accurately characterized.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Article

An article includes a substrate and a structure including direct metal laser melted material of predetermined thickness attached to the substrate, the structure formed by providing and depositing a metal alloy powder to form an initial layer having a preselected thickness and shape including at least one aperture, melting the metal alloy powder with a focused energy source, transforming the powder layer to a sheet of metal alloy, sequentially depositing an additional layer of the metal alloy powder over the sheet of metal alloy, the additional preselected shape including an aperture corresponding to the aperture in the initial layer, and melting each additional layer of the metal alloy powder with the focused energy source, increasing the thickness of the sheet and forming at least one aperture having a predetermined profile, the article further including a passageway through the structure including the aperture and a corresponding metering hole.

Lacy, Benjamin Paul↗

Methods of forming fuel rods comprising porous fuel materials

A method of forming a fuel rod for a nuclear reactor comprises disposing a powder comprising particles of a fuel material on a substrate, exposing the powder to energy from an energy source to form a first layer of a nuclear fuel, the first layer comprising inter-granular bonds between the particles of the fuel material, disposing additional powder comprising particles of the fuel material over the first layer of the nuclear fuel, and exposing the additional powder to energy from the energy source to form a second layer of the nuclear fuel and to form the nuclear fuel to have a void fraction greater than about 0.20, the second layer comprising inter-granular bonds between the additional powder and the first layer of the nuclear fuel. Related nuclear fuels comprising a porous structure, fuel rods, nuclear reactors, and methods are disclosed.

O'Brien, Robert C.↗

A Bayesian Approach to the Eagar–Tsai Model for Melt Pool Geometry Prediction with Implications in Additive Manufacturing of Metals

Here, this paper focuses on improving the melt pool geometry predictions and quantifying uncertainties using an adapted version of the Eagar–Tsai (E–T) model that incorporates temperature-dependent properties of the material as well as powder conditions. Additionally, Bayesian inference is employed to predict distributions for the E–T model input parameters of laser absorptivity and powder bed porosity by incorporating experimental results into the analysis. Monte Carlo uncertainty propagation is then used with these parameter distributions to estimate the melt pool depth and associated uncertainty. Our results for the 316L stainless steel suggest that both the absorptivity and powder bed porosity are strongly influenced by the laser power. In contrast, the scanning speed has only a marginal effect on both the absorptivity and powder bed porosity. We constructed a printability map using the Bayesian E–T model based on power-dependent input parameter values to demonstrate the merit of the approach. The Bayesian approach improved the accuracy in predicting the keyhole regions in the laser power-scan speed parameter space for the 316L stainless steel. Although applied to a specific adaptation of the E–T model, the method put forth can be extended to quantify uncertainties in other numerical models as well as in the estimation of unknown parameters.

316L Stainless Steel (SS).↗

Crystal structure of aminopentamide hydrogen sulfate, (C 19 H 25 N 2 O)(HSO 4 )

The crystal structure of aminopentamide hydrogen sulfate has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Aminopentamide hydrogen sulfate crystallizes in space group P2 1 /c (#14) with a = 17.62255(14), b = 6.35534(4), c = 17.82499(10) Å, β = 96.4005(6)°, V = 1983.906(14) Å 3 , and Z = 4. The structure consists of layers parallel to the bc-plane with hydrogen sulfate anions at the core and aminopentamide cations on the outside. There is a strong charge-assisted O49–H53∙∙∙O52 hydrogen bond between the hydrogen sulfate anions. This hydrogen bond links the anions in a chain parallel to the b-axis. The cation forms a discrete N–H∙∙∙O hydrogen bond to the anion. The amide group also forms two weaker discrete hydrogen bonds to the anion. The three N–H∙∙∙O hydrogen bonds link the cations and anions into columns parallel to the b-axis. This commercial material from USP contained an unidentified impurity, the powder pattern of which could be indexed on a monoclinic unit cell. The powder pattern has been submitted to ICDD for inclusion in the Powder Diffraction File™ (PDF®).

36 MATERIALS SCIENCE↗

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↗

Filament Extension Atomization for High Solids Loading in Energy Efficient Spray Drying Systems

We demonstrate that we could scale FEA to reach outputs needed by industrial production, while increasing solids loading of the sprayed product by at least 30% and maintaining equal or better spray powder. After testing a wide range of products, in collaboration with industry partners we decided on our primary spray products of dry whey and WPC-80, two common materials processed and sold by US manufacturers with different parameters. We sprayed these with FEA at solids loadings of 70% for dry whey and 45% for WPC-80 with a spray output with particle sizes similar to industrial particles sizes and reduced variation in particle size. We simultaneously scaled up FEA first with a multi-nip with 6 nips surrounding a central roller with parallel axis of rotation and eventually with a tapered design that solved problems we encountered with our initial design. We were able to achieve output from a single array from our first design of up to 4.7 liters per minute (L/min) and from an array of our second multi-nip of 8 L/min exceeding expectations. This demonstrates that FEA technology can indeed be scaled up to meet the needs of industrial production. More arrays can be added as necessary to meet a wide range of spray dryer designs. We also tested FEA to create dried powders from a small scale (10 L/hour of water removal) spray dryer. Though we were not able to produce large quantities of powder from FEA due to challenges in integration, the powder we produced was higher quality and produced from higher solids loading materials. From our technoeconomic analysis we for a typically sized spray dryer, we estimate a 27% cost reduction and 41% energy and carbon reduction for WPC-80 and a 39-57% cost reduction and 52-76% energy reduction for sweet dry whey (depending on the exact product).

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

Compatibility of LaFe13−x−yMnxSiyH1.6 and Eutectic Liquid GaInSn Alloy

The heat transfer rate of magnetocaloric regenerators is a topic of extensive research and the cyclability of these regenerators is critical to the operation of systems with a high coefficient of performance (e.g., potentially >22, significantly higher than typical vapor compression cooling technologies). To enable a high operating frequency that will result in a high specific cooling power, the heat transfer fluid should have high thermal conductivity and lower specific heat, i.e., higher thermal diffusivity. Eutectic metal alloys possess these qualities, such as gallium–indium–tin (Galinstan), whose thermal diffusivity has been found to be approximately an order of magnitude higher than water. For this study, the effects of eutectic liquid Galinstan exposure on the phase stability of LaFe13−x−yMnxSiyH1.6 magnetocaloric powders in an active magnetic regenerator device were investigated. The powders were characterized before and after exposure to Galinstan using X-ray diffraction, in which the phases were determined using the Rietveld refinement technique and X-ray fluorescence. It was found that after Galinstan exposure, hydrogen containing phases were present in the powder, suggesting that the hydrogen was lost from the magnetocaloric phase. The magnetocaloric phase degradation indicates that the powder was incompatible with the Galinstan metal in an environment with moisture.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗