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DOE OSTI2025

In situ Visible Light and Thermal Imaging Data from a Laser Powder Bed Fusion Additive Manufacturing Process Co-Registered to X-ray Computed Tomography and Fatigue Data

This dataset is comprised of in situ sensing data collected during a laser-based powder bed fusion additive manufacturing process, as well as rasterized scan path information, post-build X-ray computed tomography (XCT), and fatigue test results. A total of 64 cylinders, approximately 15 mm in diameter and 102 mm tall, were printed out of stainless steel 316H on a Colibrium Additive Concept Laser M2 Series 5 machine. Parameters known to produce dense material were used to construct 56 of these cylinders, while the remaining 8 cylinders were printed with relatively high energy density parameters prone to producing keyhole pores. In addition, two spatter generation blocks were constructed upstream of the 64 cylinders such that ejecta produced during the melting of the spatter generators were stochastically seeded onto the 64 cylinders. Based on previous experiments, these spatter particles were theorized to produce stochastic lack-of-fusion pores. During the construction of the build, high-resolution images of reflected light in the visible spectrum were captured both before and after recoating for each print layer. Additionally, temporally integrated thermal imaging in the near infrared spectrum produced integrated sum and max images on a layerwise basis. The multimodal in situ data has been co-registered to the build plate coordinate system, allowing for identification of process anomalies (e.g., spatter particles) apparent in the two sensors. Following construction of the build, the cylinders were subjected to XCT to identify internal flaws, and the resulting data have also been registered to the build plate coordinate system. Finally, 60 of the 64 cylinders were machined into fatigue coupons conforming to ASTM E466 and subsequently subjected to either high- or -low-cycle fatigue testing. The results of the fatigue tests have also been included in the dataset, and the XCT data corresponded to the approximate location of the gauge sections of the machine fatigue specimen geometry.

42 ENGINEERING↗

DOE OSTI2021

Multi-fidelity thermal modeling of laser powder bed additive manufacturing

Laser powder bed fusion (LPBF) Additive manufacturing (AM) has attracted interest as an agile method of building production metal parts to reduce design-build-test cycle times for systems. However, predicting part performance is difficult due to inherent process variabilities. This makes qualification challenging. Computational process models have attempted to address some of these challenges, including mesoscale, full physics models and reduced fidelity conduction models. The goal of this work is credible multi-fidelity modeling of the LPBF process by investigating methods for estimating the error between models of two different fidelities. Two methods of error estimation are investigated, adjoint-based error estimation and Bayesian calibration. Adjoint-based error estimation is found to effectively bounding the error between the two models, but with very conservative bounds, making predictions highly uncertain. Bayesian parameter calibration applied to conduction model heat source parameters is found to effectively bound the observed error between the models for melt pool morphology quantities of interest. However, the calibrations do not effectively bound the error in heat distribution.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Development of an accelerated creep testing technique via multi-specimen loading

This report summarizes a research effort undertaken by Argonne National Laboratory to accelerate the development of creep data package for code qualification. The goal is to explore new creep testing techniques to shorten the overall time needed to generate high-quality data to support an ASME code case on laser powder bed fusion 316H stainless steel. Progresses on the design and implementation of a 3-specimen load train and an innovative strain measurement method with direct potential current drop (DCPD) technique are reported.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2023

Heat Transfer Characteristics of Particle and Air Flow Through Additively Manufactured Lattice Frame Material Based on Octet-Shape Topology

Particle-to-supercritical carbon dioxide (sCO 2 ) heat exchanger is a critical component in next-generation concentrating solar power (CSP) plants. The inherently low heat transfer between falling particles and sCO 2 imposes a challenge toward economic justification of levelized cost of electricity produced through solar energy. Introduction of integrated porous media with the walls bounding particle flow has the potential to enhance the overall particle-to-sCO 2 heat exchanger performance. Here, this paper presents an experimental study on heat transfer characterization of additively manufactured lattice frame material based on Octet-shaped unit cell with particles and air as working fluids. The lattice structures were additively manufactured in stainless steel (SS) 316L and SS420 (with 40% bronze infiltration) via Binder jetting process, where the lattice porosities were varied between 0.75 and 0.9. The mean particle diameters were varied from 266 μm to 966 μm. The effective thermal conductivity and averaged heat transfer coefficient were determined through steady-state experiments. It was found that the presence of lattice enhances the effective thermal conductivity by 2–4 times when compared to packed bed of particles alone. Furthermore, for gravity-assisted particle flow through lattice panel, significantly high convective heat transfer coefficients ranging from 200 W/m2K to 400 W/m2K were obtained for the range of particle diameters tested. The superior thermal transport properties of Octet-shape-based lattice frame for particle flow makes it a very promising candidate for particle-to-sCO 2 heat exchanger for CSP application.

14 SOLAR ENERGY↗

DOE OSTI2023

Mechanical Properties of Additively Manufactured 316L Stainless Steel Before and After Neutron Irradiation–FY23

This report presents the observed mechanical behavior of the additively manufactured (AM) 316L stainless steel (SS) before and after neutron irradiation. In the Advanced Materials and Manufacturing Technologies (AMMT) program, a variety of mechanical and physical property data are generated and accumulated to assess the AM austenitic alloy for nuclear reactor applications. The testing and evaluation task in the FY 2023 focused on elucidating the effects of sampling location and build size on the mechanical properties of AM 316L SS (in stress-relieved condition) before and after neutron irradiation. The laser powder bed fusion (LPBF) process produced 316L plates of three distinct sizes from which SS-J3 miniature tensile specimens were machined from six different locations. The tensile specimens were irradiated in the High Flux Isotope Reactor (HFIR) normally to 2 and 10 dpa at the target temperatures of 300 °C and 600 °C. Post-irradiation tensile testing was performed at room temperature, 300 °C, and 600 °C. The mechanical properties of AM 316L SS were significantly influenced by the characteristic microstructures of printed materials, which include fine grains and high-density dislocations. Compared with the traditional 316L SS, AM 316L showed higher initial strength and lower ductility. Regardless of sampling location, the AM 316L steel retained relatively high strength and ductility to the highest irradiation dose. A prompt necking at yield (with little uniform ductility) was observed after irradiation at 300 °C but no embrittlement was observed up to 10 dpa. Ductilization by irradiation–the radiation-induced increase of ductility–was observed for the 600 °C irradiation only and it occurred in low dose range only. The neutron irradiation increased the data variation in many tensile property datasets, particularly after 600 °C irradiation, and no clear dependence of tensile properties on build thickness or sampling location was observed.

36 MATERIALS SCIENCE↗

DOE OSTI2025

ROTA-CAP™: An Intensified Carbon Capture System Using Rotating Packed Beds (Final Scientific/Technical Report)

GTI Energy and Carbon Clean Solutions Limited successfully designed, constructed, and operated an integrated ROTA-CAP carbon capture skid. ROTA-CAP™ is a process intensification technology, applied for post-combustion carbon capture, which utilizes the centrifugal forces generated from rotation of rotating packed beds as well as advanced solvents to achieve increased mass transfer rates 1-2 orders of magnitude higher than conventional columns while substantially decreasing footprint. The test skid, which consisted of a dual stage RPB absorber with external interstage cooling and a single stage RPB regenerator, was operated at capacities up to 0.5 tonne/day of CO 2 capture with flue gas concentrations ranging from 4% to 22% CO 2 by vol. CO 2 removal rates greater than 95% were achieved, with CO 2 product purity also exceeding 95% by vol. Over 1,600 hours of operation were accumulated throughout the project, including over 1,000 hours of operation of the with real flue gas containing at least 9.8% CO 2 by vol. The skid was operated continuously for 24 hours per day and 7 days per week over the course of 7 long-term test campaigns, with the campaigns ranging from approximately 2-4 weeks per campaign. A techno-economic analysis was performed, and a cost of capture of $\$$41.18/tonne CO 2 was calculated for the ROTA-CAP process, compared to $\$$45.75/tonne for a Cansolv-based process. These results show a cost reduction of approximately 10% compared to the Cansolv-based process. Although this still exceeds the target cost of capture of $\$$30/tonne specified for this project, GTI expects that the cost of capture can be further reduced through further optimization of the design and technology. GTI also performed an engineering design review to determine the scale-up potential of the technology, with the results of the preliminary assessment indicating that it appears to be feasible to scale up the RPB technology to 4,000 TPD. It was also determined that both horizontal and vertical rotor orientations are feasible, though there are mechanical advantages to the vertical orientation.

20 FOSSIL-FUELED POWER PLANTS↗

DOE OSTI2025

Microstructure-sensitive mechanical behavior of an additively manufactured psuedoelastic shape memory alloy

The additive manufacturing of shape memory alloys into complex geometries enables fabrication of advanced functional systems across a variety of fields and domains. This work presents results focused on the mechanical behavior of additively manufactured shape memory pseudoelastic NiTi. The deformation induced solid state phase transformation from austenite to martensite allows this system to accommodate large recoverable strains. This deformation behavior is fundamentally driven by crystal-scale transformation physics. Laser powder bed fusion processing reveals that the resulting microstructure, both grain morphology and crystallographic texture, is strongly dependent on the manufacturing processing history. Exhaustive mechanical testing demonstrates that these microstructural factors strongly impact both tensile and cyclic stress–strain behavior. Cyclic dissipative behavior, however, is similar across all tested microstructures following an initial transient period. Remarkably, analysis of spatial strain fields during tensile loading reveals two distinctly different localization “modes”. The first is initiation of localized deformation bands which continuously propagate through the tensile bar during loading. In the second mode localization is observed but lacks propagation; instead additional localization cites nucleate during subsequent loading. The latter phenomena is suspected to be driven by grain-scale deformation physics as the localized band morphologies coincide with grain morphologies. These phenomena strongly impact the resulting aggregate stress–strain behavior. Hence, manufacturers and designers of psuedoelastic functional components must at the very least consider the potential variability in properties when considering additive manufacturing processing. More ideally the process–structure–property relations can be used to further tailor and optimize final functional performance.

Additive manufacturing↗

DOE OSTI2024

Multi-functional Sorbent Development for Separation of Critical Minerals and Pollutants

Critical Metals (CMs), including Rare Earth Elements (REEs), aluminum, manganese, cobalt, and others outlined by the U.S. Department of the Interior’s Geological Survey are essential to the national and economic security of the US, and whose supply chain is susceptible to disruption. Because of the negative environmental impacts inherent with the conventional mining and processing of solid ores for CMs, adsorption-based recovery of naturally dissolved species from coal wastewaters is appealing. Acid mine drainage (AMD) remains a relatively untapped source that can be rich in REEs, and especially in Al, Mn, and other CMs. NETL’s Multi-functional Sorbent Technology (MUST) has been developed originally from the functionalized silica sorbents for carbon capture. Ongoing work aims to find AMD sites enriched with either REEs or other CM, and to perform additional field tests at these sites. Overall, our work shows the viability of recovering CMs from AMD and other coal waste streams, using a fixed-bed adsorption system that can also employ a selective elution technique to achieve highly purified metal resources.

Shi, Fan↗

DOE OSTI2024

Particle-wall heat transfer in narrow-channel bubbling fluidized beds for thermal energy storage

Robust metal oxide particles can provide low-cost and stable thermal energy storage (TES) to temperatures up to 1200 °C or higher. The transfer of heat into and out of the particles in cost-effective high-temperature particle heat exchangers remains a principal challenge to implementing particle-based TES. The present work expands on prior studies of particle-wall heat transfer in narrow-channel fluidized beds operated in the bubbling fluidization regime. Batch-mode experiments with various oxide particles over a range of temperatures and airflow rates indicate that particle-wall heat transfer increases with higher bed temperature and decreasing particle size. Measured particle-wall heat transfer coefficients in a 12 mm deep channel are fit to a Nusselt number correlation proportional to a non-monotonic function of excess fluidization velocity. Particle-wall heat transfer coefficients rise rapidly with excess fluidization velocities until reaching a maximum at intermediate air velocities due to a trade-off between enhanced transverse particle mixing and decreasing particle volume fraction with increased fluidization velocity. The heat transfer coefficient reaches a maximum of ≈ 400% of values without fluidization for oxide particles ranging in diameter d p from 159 to 408 μm. For the smallest particles tested, composed of olivine sand, particle-wall heat transfer coefficients peak above 1100 Wm –2 K –1 at 450 °C. 100-h tests at 500 °C and near-optimal heat transfer fluidization velocities indicated minimal wall wear or oxide scaling. Furthermore, high particle-wall heat transfer coefficients suggest narrow channel fluidized beds as a potential pathway for reducing the required surface area and cost of high-temperature particle heat exchangers, as needed in large-scale thermal energy storage applications.

14 SOLAR ENERGY↗

DOE OSTI2023

Influence of carbon nanotubes on microstructure and corrosion performance of additively manufactured 316L stainless steel

For this study, laser powder bed fusion (LPBF) was performed on feedstock-modified 316L stainless steel powder with 1 and 2 vol% carbon nanotubes (CNT). The corrosion resistance was evaluated following cyclic potentiodynamic polarization tests conducted in 0.6 M NaCl at room temperature, 35 and 50 °C, and immersion tests in 6 % FeCl 3 . The CNT addition has increased the pitting potential and decreased number of pits formed during immersion in FeCl 3 solution, which could be attributed to Mn-Si-O nano inclusions refinement and segregation of chromium around the inclusions. The observed corrosion behavior was correlated with the altered microstructure due to CNT addition.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Temperature-responsive smart tracers for field-measurement of inter-well thermal evolution: Heterogeneous kinetics and field demonstration

Temperature-responsive smart tracers enable advanced warning of a “premature thermal breakthrough” and may therefore improve reservoir management and reduce financial risk. A successful calculation of inter-well fluid temperatures requires that temperature-dependent kinetics are known, which typically result from homogeneous batch reactor experiments. However, recent meso-scale field experiments at the Altona Field Laboratory involving fluid flow in a discretely-fractured reservoir suggest that silica-fluid interfaces may accelerate hydrolysis kinetics. Here, the Arrhenius parameters of phenyl acetate hydrolysis are investigated under heterogeneous reaction conditions in packed-bed column experiments. The breakthrough curve of the reaction product is compared to an inert reference tracer (carbon-cored nanoparticles). Temperatures experienced during field testing ranging from 10 to 40 °C were studied using a phosphate buffer solution to maintain a near-neutral pH, as found in the reservoir. The empirically-determined pre-exponential factor and activation energy values are subsequently used in a first-order kinetic model to improve calculations of effective reservoir temperatures for these meso-scale field tests. Here, the results suggest that hydrolysis reactions can directly monitor inter-well reservoir temperatures, but only if the influence of solid-fluid interactions are carefully accounted for.

15 GEOTHERMAL ENERGY↗

DOE OSTI2020

Progress Report on the Assessment of the Material Performance for TCR Applications

The objective of Argonne’s materials research activities for the Transformational Challenge Reactor (TCR) program is to improve the understanding of material properties from additive manufacturing with the focus on understanding the creep and fatigue properties of additively manufactured materials. The material work conducted by Argonne provides support in developing and qualifying advanced materials and manufacturing processes to allow for innovative reactor design and licensing for the TCR. In this report, we present the creep data at temperatures of 550, 600 and 650°C and stresses between 175 and 300 MPa for 316L stainless steel produced by a laser powder bed fusion process. We conducted five different post-build heat treatments, namely 650°C/1h, 750°C/1h, 800°C/1h, 900°C/1h and 1050°C/1h. Creep tests of the heat-treated specimens were performed under the same test condition, 550°C/275 MPa to evaluate and understand the effect of post-build heat treatment on the creep behavior of additively-manufactured 316L SS. Creep tests were conducted to ASME NQA-1 or its lab equivalent for quality assurance.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2020

Catalytic Removal of Oxygen and Pollutants in Exhaust Gases from Pressurized Oxy-Combustors

The primary goal of this project was to develop and validate advanced catalytic materials and systems for purifying the flue gas generated from pressurized oxy-combustors in an effort to achieve the purity specifications of carbon dioxide (CO 2 ) streams required by the U.S. Department of Energy (USDOE) for application in enhanced oil recovery. The technology has shown great potential for improving energy efficiency, simplifying process complexity, and lowering costs compared with current state-of-the-art oxy-combustion flue gas purification technologies. Laboratory studies were conducted for the development, characterization, and screening of metal catalysts for residual oxygen (O 2 ) reduction with methane (CH 4 ) and multifunctional carbon catalysts for combined nitrogen oxides (NO x ), sulfur oxides (SO x ), and mercury (Hg) removal. A bench-scale reverse-flow fixed-bed (RFFB) reactor and a trickle-bed direct-contact cooler (DCC) reactor capable of treating 15 standard liters per min of pressurized oxy-combustion flue gas were fabricated and tested with both a simulated flue gas in the laboratory and a slipstream of actual flue gas at a 100 kW th Staged, Pressurized Oxy-Combustion (SPOC) pilot facility. Process simulation and techno-economic studies were performed to evaluate the energy efficiency and cost of the developed catalytic flue gas purification process integrated into a conceptual 550-MWe SPOC power plant. The goal and objectives of the project have been successfully accomplished. A cobalt-manganese (CoMn) oxide catalyst was developed and demonstrated in the bench-scale RFFB reactor in either a reverse-flow or one-direction flow mode of operation that met the success criterion of performance for residual O 2 reduction. A carbon catalyst was developed and demonstrated in the bench-scale DCC reactor that met the success criterion of performance for combined NO x /SO x /Hg removal. Slipstream testing of the integrated DCC-RFFB system at the SPOC pilot facility demonstrated stable operation and verified the superior performance obtained in the laboratory. The techno-economic analysis showed that a 550-MWe SPOC plant integrated with the catalytic flue gas purification process would result in costs of electricity of $\$$96.94/MWh and $\$$80.27/MWh in two assessed cases compared with $\$$91.07/MWh reported for the USDOE’s Current Technology Case, which generated only a partially pure CO 2 stream. On the basis of the results and findings from this project, scale-up studies of materials production and system demonstration and optimization studies of reactors and processes are recommended at the next stage of technology development.

20 FOSSIL-FUELED POWER PLANTS↗

DOE OSTI2024

Report on technical development in ANL for innovative creep testing and measurement

This report summarizes a research effort undertaken by Argonne National Laboratory to accelerate the development of creep data package for ASME code qualification. Progress on the fabrication of a 3-sample load train and the application of a direct current potential drop (DCPD) technique to measure large creep strains are reported. Specifically: (1) The 3-sample load train, with three sets of Linear Variable Differential Transformers (LVDT), has been fabricated and assembled. (2) A DCPD method for creep-strain measurement up to 50% has been demonstrated. The DCPD data matches very well to LVDT results, suggesting its potential application in future creep testing. The technical developments contribute towards shortening the time needed to generate a creep data package for an ASME code case of the laser powder bed fusion 316H stainless steel, an effort under the US Department of Energy’s Advanced Materials and Manufacturing Technologies (AMMT) program.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2025

Scaled-up fabrication of durable and porous adsorbent-coated minichannels on aluminum for CO 2 separation

A method was developed to fabricate zeolite 13X adsorbent-coated minichannels on aluminum for CO₂ adsorption applications in this study. It emphasizes the innovative use of aluminum as a substrate, which offers airtight assembly, paving the way for highly efficient adsorption systems. An optimized coating process was developed using a slurry of Zeolite 13X, yeast, sugar, and xanthan gum, resulting in durable and highly porous layers that enhance CO₂ capture performance. A PETG peeler was designed to remove the top layer of the yeast-engineered adsorbent coatings, revealing a super porous and foamy structure. The teeth of the peeler were designed and fabricated for high repeatability and rapid prototyping. Breakthrough experiments were conducted on the scaled-up adsorbent bed using gas mixtures of 80% CO₂, 20% N₂, and 20% CO₂, 80% N₂ to represent different industrial scenarios. The performance of the bed was evaluated at flow rates of 160 and 190 cm³ min -1 using a Raman Laser Gas Analyzer (RLGA), demonstrating stable adsorption without degradation across multiple cycles. Computational modeling of integral transport phenomena under the chosen experimental conditions was pursued using gPROMS ProcessBuilder™, and the modeling results were compared with those from the tests for adsorption time, which resulted in an error margin of 2% to 9% for the breakthrough time, confirming the easy reproducibility of the design through modeling. This research advances CO₂ capture technologies by providing an effective and scalable solution for producing aluminum-based adsorbent coated beds, supporting industrial carbon capture efforts.

CO2 capture↗

DOE OSTI2020

Testing of UV Oxidation Process for Acetonitrile Destruction

The Hanford Site Effluent Treatment Facility (ETF) currently treats aqueous waste streams that include condensates from the 242-A evaporator, leachate from the Environmental Restoration Disposal Facility (ERDF), as well as laboratory wastes and, in the future, will treat liquid effluents from the Hanford Waste Treatment and Immobilization Plant (WTP) and Integrated Disposal Facility (IDF) leachate. Liquid effluents from the WTP will have significant concentrations of acetonitrile. Acetonitrile is formed by reaction of nitrates and sugar in the WTP low activity waste (LAW) melters and is prevalent in the submerged bed scrubber (SBS) and wet electrostatic precipitator (WESP) liquid effluents from WTP off-gas treatment. When these liquids are concentrated in the WTP Effluent Management Facility (EMF) evaporator in the direct feed low activity waste (DFLAW) flow-sheet, testing has shown that the majority of the acetonitrile partitions to the evaporator condensate. Since the evaporator condensate is directed to the ETF, this creates a potential issue with the ETF waste acceptance criteria and, specifically, the ETF Delisting Modification treatability envelope limits. Consequently, there is a need to assess possible mitigation approaches, one of which involves identification and assessment of potential treatment processes to destroy the acetonitrile, which is the subject of the present report.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2023

Sensitization of 316L Stainless Steel made by Laser Powder Bed Fusion Additive Manufacturing

Additively manufactured (AM) 316L stainless steel (SS) manufactured by laser powder bed fusion (L-PBF) and wrought 316L SS were subjected to sensitization heat treatments at 700°C up to 100 h. Using two evaluation methods, double-loop electrochemical potentiokinetic reactivation (DL-EPR) and ditching tests, degree of sensitization (DOS) and intergranular corrosion (IGC) susceptibility was evaluated. It was found that the wrought samples showed slightly lower IGC susceptibility compared to their AM counterpart. DOS and IGC attacks increased with sensitization time for all samples. Dislocation cellular structures were found to have little to no impact on DOS and IGC for the AM samples. Sensitized at 100 h, the AM sample showed significant Cr depletion along high-angle grain boundaries (12.35 wt% on average) and exhibited Cr carbide precipitation. Mo-rich particles along grain boundaries were also observed. The DL-EPR test attacks the surface oxide film and grain boundaries while the ditching test attacks the melt pool boundaries and grain boundaries (IGC and pitting). Changes to the DL-EPR and ditching standards for AM application have been proposed in this work.

316L stainless steel↗

DOE OSTI2024

Very high cycle fatigue characteristics of laser beam powder bed fused AlSi10Mg: A systematic evaluation of part geometry

This study explores the influence of geometry and part size on defect distribution, melt pool size, and mechanical characteristics in laser beam powder bed fused (LB-PBF) AlSi10Mg. Five distinct geometries—hourglass, small rod, small block, large block, and large rod—were fabricated under identical process parameters. Fully reversed ultrasonic fatigue testing, operating at a frequency of 20 kHz, was conducted to assess the very high cycle fatigue properties. The findings indicated that part geometry had a major impact on the fatigue properties of the material in the very high cycle fatigue regime. Specimens machined from large rods and large blocks had the lowest porosity and highest fatigue resistance. Microstructural analysis indicated that hourglass, small rod, and small block specimens had shallower melt pools and overlap depths compared to other geometries. This observation suggests a higher cooling rate in specimens with smaller cross-sectional areas, leading to the increased presence of entrapped gas pores and a lack of fusion defects. Understanding the relationship between part geometry and fatigue properties in LB-PBF components offers insights for optimizing design and manufacturing processes in additive manufacturing applications.

AlSi10Mg↗