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Thermal Performance of Common Bulk-Fill Cryogenic Insulation Materials in Helium and Hydrogen Background Gases

Maritime shipping of vast quantities of liquid hydrogen (LH 2 ) will be necessary to facilitate a global hydrogen ecosystem; with some studies estimating volumes up to 172,000 m 3 for individual tanker ships, and requiring stationary storage tanks at terminals of 50,000 m 3 to 100,000 m 3 —ten to fifteen times larger than the current largest tank, located at launch pad B at NASA Kennedy Space Center (KSC). Such a radical scale-up will push the boundary of traditional, vacuum-insulated tank designs. Hence, a potential need exists for non-vacuum solutions, which necessitates exploring the thermal performance of insulation materials in non-condensable background gasses at LH 2 temperatures, namely helium and hydrogen. Testing of two bulk-fill insulation materials common to large LH 2 storage tanks, perlite and glass bubbles, in helium and hydrogen was recently conducted by the Cryogenics Test Laboratory at KSC using the Cryostat-100 liquid nitrogen boiloff calorimeter per the ASTM C1774 standard methodology. Effective thermal conductivity (k e ) and heat flux (q) results for each insulation/gas combination are presented across the full vacuum range, as well as thermal profiles through the insulation thickness between 78 K and 293 K.

A M Swanger

Distillable amine-based solvents for effective pretreatment of multiple biomass feedstocks

Exploring the potential of advanced distillable solvents as efficient biomass pretreatment agents is critical for biorefineries, enhancing fermentable sugar yields while enabling solvent recovery and recycling without suffering significant losses. Here, we employ distillable amine-based solvents for pretreating a wide range of lignocellulosic feedstocks, aiming to facilitate the industrial release of fermentable sugars from diverse feedstocks through enzymatic hydrolysis. Twenty-two diverse feedstocks, sourced from different geographical regions and representing various biomass categories, were surveyed for chemical (mainly carbohydrates and lignin) and lignin (S, G, and H units) profiles. Several solvents, including ethanolamine, ethanolammonium acetate, butylamine, butylammonium acetate, and triethylamine, were tested for the pretreatment of eight selected biomasses. Among these solvents, butylamine emerged as the most effective due to its favorable sugar release, excellent solvent removal rate, and low boiling point, facilitating solvent recovery and recycling. Extending butylamine pretreatment to all 22 feedstocks demonstrated desirable sugar yields and highly efficient solvent removal in the majority of the biomass sources tested. Agricultural residues and their mixtures showed particularly favorable sugar release. Despite minimal changes in cellulose crystallinity, XRD characterization of sorghum, poplar, and pine before and after butylamine pretreatment showed a decrease in intensity and a slight shift of certain peaks, indicating alterations in cellulose structure. Fourier-transform infrared spectroscopy and thermogravimetric analysis analyses suggested disruption of biomass linkages in hemicellulose and lignin, enhancing enzymatic digestibility. Scale-up experiments of the mixed agricultural feedstocks in a 1 L Parr reactor achieved over 90% glucose liberation and more than 99% butylamine removal, highlighting the scalability of the method. The resulting hydrolysates supported the growth of diverse bacterial and fungal strains, indicating downstream compatibility with commercial fermentation processes. This study presents butylamine as an effective, recoverable pretreatment solvent for a wide range of lignocellulosic feedstocks, offering a promising solution to key biorefinery challenges. The demonstrated scalability and compatibility with various biomass types and blends underscore its potential for industrial application, advancing sustainable biofuel and biochemical production.

biomass composition

Science of Scale-Up: Accelerating chemical manufacturing technology development workshop report

The Science of Scale-Up: Accelerating chemical manufacturing technology development workshop report outlines key insights and actionable recommendations for accelerating the scale-up of disruptive chemical manufacturing technologies. Convened in October 2024, the workshop brought together approximately fifty experts from academia, industry, national laboratories, and government agencies to address the barriers and solutions for maturing technologies from proof-of-concept to commercialization. The report identifies seven critical themes for enabling faster scale-up. These themes were explored through general discussions and breakout sessions focused on three specific chemical manufacturing technologies—electrochemical, thermochemical, and biological conversion processes. The findings emphasize the importance of interdisciplinary collaboration, robust funding mechanisms, and shared resources to overcome technical barriers and accelerate technology deployment. The report also highlights technology-specific challenges and opportunities, including the need for advanced materials, scalable manufacturing processes, and integrated testing environments. For electrochemical manufacturing processes, durability and material optimization are key priorities, while thermochemical processes require novel reactor designs and better supply chain integration. Biological conversion processes face hurdles in strain engineering, reactor design, and process integration. Across all technologies, the workshop emphasized the importance of leveraging computational tools, standardized protocols, and collaborative networks to address knowledge gaps and technical barriers. By acting on these insights, stakeholders can reduce the timeline for scaling up critical chemical manufacturing technologies, ensuring their timely impact on manufacturing competitiveness, and environmental sustainability.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH

Addressing the Safety of Next-Generation Batteries

Owing to increasing demand for low-cost energy storage with secure material supply chains, the battery community is approaching a pivotal shift beyond conventional lithium-ion (Li-ion) towards next-generation cells. Technologies that include alkali-metal anodes, solid electrolytes and earth-abundant materials such as sodium (Na) and sulfur (S) are reaching commercialization in cells. The abuse tolerance and thermal runaway hazards of such technologies diverge from conventional Li-ion cells. Consequently, designing safe batteries with next-generation materials requires a holistic approach to characterize cells and to understand their responses to abuse conditions from the beginning to the end of life. Here we provide a Perspective on how the safety and abuse tolerance of cells are likely to change for up-and-coming technologies; challenges and opportunities for reimagining safe cell and battery designs; gaps in our knowledge; capabilities for understanding the hazards of thermal runaway and how to address them; how standard abuse tests may need to adapt to new challenges; and how research needs to support affected professionals, from pack designers to first responders, to manage hazards and ensure safe roll-out of next-generation cells into applications like electric vehicles (EVs). Finally, given the large number of next-generation technologies being explored, we encourage giving priority to safety-focused research in proportion to the rate of manufacturing scale-up of each specific technology.

25 ENERGY STORAGE

Design of Novel Hot Gas Component for Gas Turbine Engines Enabled by Materials and Additive Manufacturing Process Development

This CRADA project was the result of a project award under FOA-DOE-0001980. The overarching FOA project team consisted of researchers from Carpenter Technology Corporation (CTC), Solar Turbines Incorporated (Solar), Pennsylvania State University (PSU), University of California-Santa Barbara (UCSB), and Oak Ridge National Laboratory (ORNL). Evaluations were conducted on two high-γ’ superalloys that were designed by CTC and the UCSB. One alloy named GammaPrint-700 (GP-700) is a cobalt-base superalloy. The other alloy named GammaPrint-1100 (GP-1100) is a nickel-base (Ni-base) superalloy. PSU provided expertise and experimental testing of the thermal performance of AM micro-cooling architectures. ORNL provided expertise with the AM superalloy materials characterization and AM processing science. Solar provided turbine component design expertise. The focus of this CRADA report is to document the efforts between ORNL and CTC towards the development of superalloys designed for AM. The project goal was to use an AM processable high-temperature superalloy and design for Additive Manufacturing (DfAM) techniques to design an efficient turbine component (i.e. a turbine tip shoe) with enhanced cooling features that can only be fabricated through additive manufacturing (AM). The efficiencies of existing combined heat and power (CHP) engines are capped by both component design and materials limitations. However, AM of a tip shoe component from a γ’strengthened superalloy offers the design flexibility to increase the efficiency and power of an industrial gas turbine. This project brought about advancements in the DfAM tip shoe design space and in the area of high temperature superalloys processable through laser powder bed fusion (LPBF) AM. State of art computation design tools were utilized to optimize unique cooling features into a tip shoe component design. A two-prong materials development approach was taken to support development of the AM tip shoe geometry. The first approach centered on investigating the processability and the appropriate process science for the industry standard high-γ’ nickel-base (Ni-base) superalloy Mar-M247. This superalloy is typically cast and considered non-weldable by traditional welding standards. In the course of this work, the alloy was not deemed feasible for process scale-up due to significant cracking issues during printing. The second approach focused on the development and evaluation of a novel cobalt-base superalloy, GammaPrint™-700 (GP-700 and a Ni-base superalloy, GammaPrint™-1100 (GP-1100) designed to mitigate the significant AM processing issues with Mar-M247. The processability of these two alloys were investigated through electron beam melting (EBM) binder-jet AM (BJAM), and LPBF as a risk mitigation for manufacturability. To be considered a candidate material for down-selection to proceed to fullscale AM tip shoe engine testing trials, the high temperature creep rupture strength was required to achieve at a minimum, a Larsen Miller Parameter (LMP) increase of 10.9% over the baseline material LPBF AM Hastelloy X.

36 MATERIALS SCIENCE

Testing and Validation of Wireless Communication Architecture for Heliostat Fields: SIPS Final Report

This work focuses on the development and testing of a low-cost wireless communication system for heliostat fields, enabling significant capital costs reductions for concentrating solar thermal systems. Outputs of this work include a working demonstration of a multi-node communication system, clear reporting of system performance, and technical documentation of system development and architecture for reproducibility. Through this process, an open-source repository was created for manufacturing hardware at ~$30/heliostat. The system includes software for cybersecurity, achieving sub-second communication latencies and derisking of hardware for eventual scale-up to tens of thousands of heliostats. While the system is not currently off-the-shelf ready, there is now a clearly defined pathway for scaling up and completing the commercial development process.

14 SOLAR ENERGY

Highly Efficient Regeneration Module for Carbon Capture Systems in NGCC Applications

The objective of this project is to design, fabricate, and test a highly efficient regeneration module capable of providing an ultra-lean absorption solution that is required for capturing CO 2 from dilute sources at 95% or better efficiency. By integrating this advanced regenerator module with SRI International’s Mixed Salt Process (MSP) absorption modules, SRI expects to demonstrate significant progress toward a reduction in cost of capture versus the DOE reference natural gas combined cycle (NGCC) plant with carbon capture. SRI designed, built, and tested an advanced stripper to enhance the performance of SRI’s MSP for CO 2 capture – a transformational ammonia-based solvent technology – for natural gas (NG) power sources. The testing of the advanced stripper for MSP was conducted at an SRI site using a simulated flue gas stream equivalent to about 10 kWe. The research work included modeling of the advanced stripper and integrating it with the MSP absorbers; studying the strategies for producing very highly alkaline lean solvent with minimized emissions; operating the stripper with advanced heat integration to improve process efficiencies; and collecting critically important data for a detailed techno-economic analysis (TEA). The project tasks were designed to address concerns relating to scale-up and integration of the technology to NG power plants—more specifically, to maximize the carbon capture efficiency achievable with MSP and identify pathways to achieve higher capture efficiencies and ultimately zero net carbon emissions. SRI teamed up with a process modeling company (OLI Systems), a process and chemical engineering company (Trimeric Corporation), and a cost-sharing commercial partner (Baker-Hughes – a leading multinational company that designs, manufactures, and services transformative energy technologies) to execute the project. The research findings will accelerate the MSP development and pave the way for the technology to reach the DOE’s goal, and ultimately commercialization of the MSP technology for low-cost CO 2 capture from NGCC flue gas and other dilute CO 2 sources.

03 NATURAL GAS

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

HIV drug resistance during antiretroviral therapy scale-up in Uganda, 2012–19: a population-based, longitudinal study

Background With scale-up of antiretroviral therapy (ART) in sub-Saharan Africa, increasing pretreatment HIV drug resistance has been reported; however, the broader effect of ART expansion on population-level resistance patterns remains insufficiently quantified. We aimed to estimate the longitudinal prevalence of drug resistance and resistance-conferring mutations. Methods This study used data collected as part of the Rakai Community Cohort Study (RCCS), an open population-based census and cohort study conducted in southern Uganda. At each survey round, residents aged 15–49 years are invited to participate and receive a structured questionnaire that obtains sociodemographic, behavioural, and health information, including self-reported past and current ART use. Voluntary HIV testing is conducted using a rapid test algorithm and a venous blood sample. People with HIV provide samples for viral load quantification and deep sequencing. We analysed RCCS survey, HIV viral load, and deep sequencing (which was used to predict resistance) data from five survey rounds. The key outcomes were the population prevalence of viraemic people with HIV with non-nucleoside reverse transcriptase inhibitor (NNRTI), nucleoside reverse transcriptase inhibitor (NRTI), protease inhibitor, or multiclass resistance among all participants (regardless of HIV serostatus) in the 2015 and 2017 surveys. Prevalence of class-specific resistance and resistance-conferring substitutions were estimated using robust log-Poisson regression. Findings Between Aug 10, 2011, and Nov 4, 2020, there were 43 361 participants in the RCCS and 7923 (18·27%) people with HIV. Over five survey rounds, 93 622 participant visits occurred, among which 17 460 (18·65%) were from people with HIV. Over the analysis period, the median age of study participants remained similar (28 years [22–35] in 2012 and 29 years [21–38] in 2019). Sufficient data were available to reliably genotype 4072 (90·03%) of 4523 participant visits from 3407 people with HIV for at least one drug. Overall population prevalence of resistance contributed by viraemic pretreatment people with HIV decreased between 2012 and 2017 from 0·56% (95% CI 0·42–0·75) to 0·25% (0·18–0·33) for NNRTI and from 0·24% (0·15–0·37) to 0·05% (0·02–0·10) for NRTI (prevalence ratio 0·44 [0·29–0·68] for NNRTI and 0·21 [0·09–0·47] for NRTI). Between 2012 and 2017, NNRTI resistance among viraemic pretreatment people with HIV increased from 4·86% (3·69–6·42) to 9·61% (7·27–12·7; prevalence ratio 1·98 [1·34–2·91]). The prevalence of NNRTI and NRTI resistance was substantially higher among viraemic treatment-experienced people with HIV (51·49% [46·24–57·34] for NNRTI and 36·46% [30·06–44·22] for NRTI in 2017) than among pretreatment people with HIV. NNRTI and NRTI resistance was predominantly attributable to rtK103N and rtM184V. inT97A was observed at a similar prevalence among viraemic treatment-experienced (9·96% [6·41–15·48]) and viraemic pretreatment (10·56% [8·01–13·93]) people with HIV; no major dolutegravir resistance mutations were observed. Interpretation Despite rising NNRTI resistance among pretreatment people with HIV, overall population prevalence of pretreatment HIV drug-resistant viraemia decreased due to increasing ART uptake and viral suppression. This finding underscores the crucial role of achieving and maintaining high ART coverage in reducing transmission of drug-resistant HIV. The high prevalence of mutations conferring resistance to components of first-line ART regimens among viraemic people with HIV is potentially concerning. Funding National Institutes of Health, Johns Hopkins University Center for AIDS Research, Bill & Melinda Gates Foundation, and the US Centers for Disease Control and Prevention.

59 BASIC BIOLOGICAL SCIENCES

Degradable Biocomposite Thermoplastic Polyurethanes

In this project, the team developed tough and degradable biocomposite thermoplastic polyurethanes (TPUs) by incorporating bacterial spores into TPUs as a biofunctional living filler. The team screened various bacteria and selected the Bacillus subtilis ATCC 6633 strain as the final candidate, primarily due to its genomic availability, sporulation ability and TPU assimilation activity. The heat-shock tolerance of ATCC 6633 spores was further improved through evolutionary engineering via Adaptive Laboratory Evolution (ALE), demonstrating a 17.7-fold enhanced germination efficiency post heat-shock treatment compared to the wild-type strain (WT). The team fabricated biocomposite TPUs by incorporating lyophilized powder of heat-shock tolerized (HST) spores during the hot melt extrusion (HME) of TPU at 135 °C. The baseline TPU used in this project is a commercially available soft-grade TPU (BCF45) manufactured by BASF. Colony forming unit (CFU) assays quantified that WT and HST spores in the TPU matrix retained approximately 20% and 100% survivability, respectively, after HME. Tensile testing demonstrated that the spores behaved as a polymer-reinforcing filler, positively affecting the overall tensile properties of the biocomposite TPU. For example, biocomposite TPU with WT and HST spores (BC TPU WT and BC TPU HST , respectively) exhibited up to 25% and 37% improved toughness, respectively, compared to TPU without spores. BC TPU HST showed remarkably improved disintegration in autoclaved compost (92% mass loss in 5 months), which simulated a microbially poor environment for TPU degradation. When compared to TPU without spores (44% mass loss in 5 months) the acceleration of degradation is marked. Respirometry confirmed that 72% of BC TPU HST was biomineralized into CO2 within 6 months, indicating that spores in the biocomposite TPU were germinated by utilizing nutrients in the autoclaved compost, facilitating TPU degradation at the end of the material's life. The team demonstrated the scale-up of biocomposite TPU fabrication using continuous extrusion and injection molding techniques. Processing conditions optimized in a lab-scale microcompounder were successfully transferred to a continuous extruder with a 30-fold increased throughput. Biocomposite TPUs prepared using these industry-relevant processes showed comparable toughness improvements to samples prepared in the lab-scale extruder. Excitingly, following compounding in the pilot-extruder the composite material could be injection molded, while retaining high spore viability and similar toughness improvements. The team also found that spores in biocomposite TPU served as antioxidants, preventing toughness decay during the recycled extrusion of BC TPU HST . Long-term storage tests over one year showed that the addition of spores had no negative effect on the longevity of the TPU. Furthermore, the team demonstrated the fabrication of spore-bearing biocomposite polymers with other polyesters such as PBAT, PLA, and PCL. We obtained promising preliminary data that showed overall toughness improvements for all polymers with spore addition. Finally, life cycle assessment (LCA) and techno-economic analysis (TEA) were carried out, which indicated minimal additional cost of fabrication. Overall, a tough and degradable biocomposite thermoplastic was successfully developed through this project, with all tasks completed successfully, achieving >100% of the objectives.

36 MATERIALS SCIENCE

Scale-Up of Electrode Coating and Flow-Field for Commercial Hydrogen Peroxide Electrolyzer: Cooperative Research and Development Final Report, CRADA Number CRD-17-00687

Hydrogen peroxide is currently produced at central chemical plants via the anthraquinone oxidation process. This process produces environmental pollutants that are costly to remediate, requires hazardous long distance shipping of highly concentrated peroxide (50% or 70%), and necessitates extra handling costs related to storage and dilution. Peroxygen Systems, Inc. (PSi) is developing breakthrough technology for on-site hydrogen peroxide production. PSi’s on-site on-demand electrolyzer can reduce the cost of producing hydrogen peroxide by 50%, while also completely eliminating the cost and safety issues associated with shipping and handling of high concentration hydrogen peroxide. The challenge for PSi is scaling. To support the next step toward commercialization (customer pilot tests), scaling the prototype into larger single cells and 20-40 cell stacks is required. In addition to internal hardware and flow-field design efforts at PSi, NREL will address three critical problems for this scale-up effort: (1) demonstrating a large scale roll-to-roll (R2R) process to coat uniform electrode materials for 100 cm2 and 500 cm2 stack testing, (2) demonstrating an in-line diagnostic to achieve better electrode quality control, and (3) performing in situ cell/stack testing to better understand and optimize the performance of the flow field design.

28 EE - Advanced Manufacturing Office (EE-5A)

A Note to Reviewers Suggesting Post-reaction Catalyst Characterization: Know What You’re Asking For

Here, we highlight examples of post-reaction characterization in thermo- and electrocatalysis to present the challenges in obtaining reliable data to answer specific questions about the true identity of the active site and/or catalyst deactivation/degradation. We use this editorial to suggest to reviewers that, when formulating comments to authors that involve materials characterization after reaction testing, they should consider what specific, meaningful information can be attained or what targeted question can be answered that adds value to the individual paper and to the field in general, and how to reasonably obtain that data. In contrast, reviewers should avoid vague, open-ended comments that suggest unguided post-reaction characterization that would not add significant value to the report and, similarly, avoid comments that are substantial enough that they could form the basis of an entirely separate report.

36 MATERIALS SCIENCE

Design of Novel Hot Gas Component for Gas Turbine Engines Enabled by Materials and Additive Manufacturing Process Development

This CRADA project was the result of a project award under FOA-DOE-0001980. The overarching FOA project team consisted of researchers from Carpenter Technology Corporation (CTC), Solar Turbines Incorporated (Solar), Pennsylvania State University (PSU), University of California-Santa Barbara (UCSB), and Oak Ridge National Laboratory (ORNL). Evaluations were conducted on two high-γ’ superalloys that were designed by CTC and the UCSB. One alloy named GammaPrint-700 (GP-700) is a cobalt-base superalloy. The other alloy named GammaPrint-1100 (GP-1100) is a nickel-base (Ni-base) superalloy. PSU provided expertise and experimental testing of the thermal performance of AM micro-cooling architectures. ORNL provided expertise with the AM superalloy materials characterization and AM processing science. Solar provided turbine component design expertise. The focus of this CRADA report is to document the efforts between ORNL and CTC towards the development of superalloys designed for AM. The project goal was to use an AM processable high-temperature superalloy and design for Additive Manufacturing (DfAM) techniques to design an efficient turbine component (i.e. a turbine tip shoe) with enhanced cooling features that can only be fabricated through additive manufacturing (AM). The efficiencies of existing combined heat and power (CHP) engines are capped by both component design and materials limitations. However, AM of a tip shoe component from a γ’strengthened superalloy offers the design flexibility to increase the efficiency and power of an industrial gas turbine. This project brought about advancements in the DfAM tip shoe design space and in the area of high temperature superalloys processable through laser powder bed fusion (LPBF) AM. State of art computation design tools were utilized to optimize unique cooling features into a tip shoe component design. A two-prong materials development approach was taken to support development of the AM tip shoe geometry. The first approach centered on investigating the processability and the appropriate process science for the industry standard high-γ’ nickel-base (Ni-base) superalloy Mar-M247. This superalloy is typically cast and considered non-weldable by traditional welding standards. In the course of this work, the alloy was not deemed feasible for process scale-up due to significant cracking issues during printing. The second approach focused on the development and evaluation of a novel cobalt-base superalloy, GammaPrint™-700 (GP-700 and a Ni-base superalloy, GammaPrint™-1100 (GP-1100) designed to mitigate the significant AM processing issues with Mar-M247. The processability of these two alloys were investigated through electron beam melting (EBM) binder-jet AM (BJAM), and LPBF as a risk mitigation for manufacturability. To be considered a candidate material for down-selection to proceed to full-scale AM tip shoe engine testing trials, the high temperature creep rupture strength was required to achieve at a minimum, a Larsen Miller Parameter (LMP) increase of 10.9% over the baseline material LPBF AM Hastelloy X.

99 GENERAL AND MISCELLANEOUS

Rapid Bayesian High Entropy Alloy Designs Fabricated via Wire Arc Additive Manufacturing

Purpose: This project seeks to demonstrate a new high-throughput (rapid) alloy design technique applied to creating new high entropy alloys (HEAs) for extreme environments. High entropy alloys shift the design paradigm from being focused on a single principal element (e.g. nickel-based alloys) to target alloys that include high atomic fractions (X >10%) of multiple elements. These HEA materials can exhibit sluggish diffusion and enhanced corrosion resistance, ideal for potential applications in advanced ultra supercritical (A-USC) steam cycles for power generation. Scope: The addition of multiple elements in high atomic fractions creates an enormous design space that cannot easily be investigated by traditional material design strategies such as designed of experiments (DOE). This project utilizes a Bayesian machine learning algorithm that has been modified to work with calculation of phase diagrams (CALPHAD) software. This Bayesian algorithm reduces manual inputs and increase the likelihood of achieving an optimal solution. Compositional inputs to this algorithm will be assessed using existing material property models for high temperature strength and corrosion resistance. The target for alloy performance will be a 15% (~100 ⁰C) increase in allowable service temperature beyond heat-resistant stainless steels while maintaining or improving alloy cost and corrosion resistance. Haynes 230 was selected as a baseline, which is 57 wt% Ni with 22 wt% Cr 14 wt% W, and 2 wt% Mo as solid solution strengtheners. In addition to rapid design via Bayesian machine learning, the alloys were rapidly fabricated using a multi-wire arc additive manufacturing (mWAAM) technique which allows for precise control of alloy composition and assessing of alloy design “windows” to study composition effects. Build speeds for wire-arc additive processes are among the highest for additive technologies enabling rapid and reliable sample fabrication when compared to conventional methods such as arc button melting. The mWAAM samples will be rapidly characterized via instrumented indentation for room temperature modulus and strength and for elevated temperature strength via hot hardness tests. After being screened with hardness testing, potential alloys will be further evaluated with conventional microscopy techniques including scanning electron microscopy (SEM) and transmission electron microscopy (TEM) to assess agreement with modeling results. The most promising compositions will also be evaluated by printing full sized tensile specimens for mechanical behavior tests at elevated temperatures. Results: Bayesian machine learning of a single performance function was initially used to optimize five performance metrics: 1) single phase stability, 2) yield strength, 3) creep resistance (low diffusion coefficient), 4) freezing range (weldability), and 5) material cost. The single performance function was suboptimal as assumptions had to be made about the results while formulating the optimization. A goal-oriented Bayesian optimization strategy (Hanaoka, 2021) was implemented with CALPHAD for use with the five metrics above. This multi-objective Bayesian optimization (MOBO) enabled the design of NiCrCoFe alloys with V and W additions. A base composition of NiCoCr was selected as Ni provides a stable FCC matrix, Cr aids corrosion/oxidation resistance, and Co is a solid-solutions strengthener that also improves creep by increasing the activation energy. Fe helps reduce diffusion coefficients and cost. Finally, V and W were selected for their reasonable solubility and high atomic misfit to aid in solid solution strengthening. Cracking of the mWAAM specimens was an early issue, and the Easton solidification cracking model (Easton et al., 2014a) was selected for addition to the MOBO function. High performing alloys fabricated by mWAAM included Ni 28 Cr 25 Co 26 Fe 15 V 8 and Ni 62 Cr 18 Co 1 Fe 3 W 15 . It was observed that even after adapting the mWAAM process for W, the W did not fully dissolve. To fully evaluate the Ni 62 Cr 18 Co 1 Fe 3 W 15 composition, a cored wire (80-20 NiCr sheath/powder core) was manufactured and printed via WAAM, and HIP’ing was utilized to homogenize and densify the printed alloy. The V and W alloys produced met metrics 1 (solid solution), 4 (solidification cracking), and 5 (cost). However, an unmodeled mechanism of thermal stress cracking was identified in the WAAM produced materials, perhaps exacerbated by the lack of grain boundary strengthening elements (B, C). Conclusions & Recommendations: A high-throughput (rapid) alloy design technique was applied to designing and manufacturing new high entropy alloys (HEAs) for extreme environments utilizing MOBO and mWAAM. The developed process was rapid and effective in addressing the mechanisms included in the model. The lack of grain boundary strengthening element additions (e.g., B, C) was a simplification that likely produced thermal stress cracking that turned into a large part of the investigation. Additions on the order of 0.005 wt% B and 0.05 wt% C likely would have minimized thermal stress grain boundary cracking. Overall, the high throughput design strategy is promising for rapid design of metrics-driven alloys for advanced ultra supercritical (A-USC) steam cycles for power generation. The MOBO and mWAAM process could be commercialized to accelerate metrics-driven alloy design. In addition, the cored-wire process utilized for scale-up is a promising high-volume process for WAAM alloy development and scale-up.

36 MATERIALS SCIENCE

Microchannel-based Membrane-less Extraction of Li from Unconventional Lithium Sources & the Separation of REE

This final report provides an overview of the Project's entire duration, covering July 1, 2021 to December 31, 2023. It primarily focuses on the achievements, technological developments, and unique challenges the team faced while working on separating and extracting Lithium from produced waters. The project's primary aim was to create an integrated, high-throughput, membrane-less, and modular microfluidic platform that could extract Lithium from unconventional sources. We have successfully met all goals and milestones envisioned in the SOPO document. The most critical primary milestones, including the Go-No-Go milestone (refer to the Gantt chart in the Appendices), were successfully accomplished. We demonstrated phase separation (>90%) and extraction (>85%) performance in the MPSE using synthetic, and representative produced water composition feed at 50 ml/min total flow through MPSE 36. We have also performed a parametric study of the MPSE operations, beyond the scope of SOPO, exploring operating conditions of current and broader interest. The extended investigation of operational parameters is concurrent with our efforts to seek further development of the MPSE technology beyond the scope of the Project. Along these lines of development, we have made efforts to be responsive to DOE calls for technological developments of other types of resources (beyond PW) for the recovery of Critical Materials and higher TRL development (beyond TRL 4). During the work on this Project, we developed and implemented three innovative technical approaches that emerged from our efforts to successfully meet the Project milestones. The innovative & original technical approaches developed and implemented in this Project are now the contributions to process engineering that could be clearly credited to the Project. First, Convergent Design Approach is a comprehensive feedforward & feedback loop of four design phases: i) design for functionality, ii) design for manufacturing, iii) design for sustainability, and iv) design for market. Next was Process Intensification. A major aim of this Project was to create an innovative phase separation & extraction microscale-based technology for Li separation – thus the words microchannel-based in the Project title. A microscale-based technology is intrinsically in the center of the Process Intensification domain as defined by its unique principles. Therefore, Process Intensification was implicitly envisioned in the Project’s SOPO. Lastly, Time Scale Analysis is a novel tool for discovering the needs and directions of Process Intensification implementations in any process technology. This Project is fully credited for developing and implementing the three novel technical approaches mentioned above. These are general contributions to process engineering that emerged from this Project. Beyond the original SOPO scope, the OSU-U.Pitt research group utilized a Convergent Design methodology, integrating first-principles mathematical modeling with experimental validation on the Minimum Development Vehicle. By creating these Digital Twins, the team rapidly assessed manufacturing iterations to support TEA analysis. This framework further enabled the development of advanced Surface Modification Techniques, where hydrophobic and oleophobic coating strategies were optimized via Digital Twin tools and validated through rigorous 100-hour longevity testing. TEA Analysis: The closing efforts of this Project were focused on the TEA analysis. TEA analysis had two primary functions: i) enabling critical assessments of design variations withing 10 the Concurrent Design Approach, thus enabling evolution of the MPSE design to reach faster- better-cheaper alternatives; and ii) to create a bridge between the accomplishments of this Project and future projects of higher TRL, beyond TRL 6 level. It is important to note that the TEA model created in the Project stirred the technological solutions for the recovery of critical materials toward a vision of a very profitable modular plant that has unique zero-waste water discharge signature. More importantly, thanks to our experimental performance data and conservative assumptions, the TEA model predicts minimal technological and investment risks. Low cost of a modular unit of a nominal capacity of [1000 tons of Li 2 CO 3 /year] positions the MPSE based technology within the reach of community investors, thus offering a paradigm shift in the development of critical technologies. The project successfully navigated two primary challenges: solvent selection and manufacturing adaptation. Restricted by the SOPO to existing literature for lithium recovery, the team identified a critical need for a "material excellence program" to develop next-generation solvents, eventually concluding with a preliminary investigation into promising Ionic Liquids (ILs). Simultaneously, COVID-19 supply chain disruptions forced a pivot from traditional manufacturing to advanced additive methods at ATAMI-OSU. By transitioning from stainless steel to 3D-printed polymer substrates, the team achieved a transformative three-order-of- magnitude reduction in manufacturing costs and compressed prototyping timelines from several months to just two days. The MPSE technology offers significant energy, environmental, and economic advantages by overcoming the traditional bottlenecks of phase-separation hardware and contactor size. Unlike conventional mixer-settlers or membrane-based systems, MPSE operates without moving parts or fouling-prone membranes, achieving robust performance even with challenging, viscous, or particulate-heavy feeds. Key performance metrics include an energy intensity reduction of 5–50x (3–40 kJ/m 3 ) compared to incumbent technologies and a dramatic reduction of processing time to under 60 seconds, which drastically reduces the physical plant footprint. These technical efficiencies translate into superior economic outcomes; for a 100 t/year Li 2 CO 3 facility, implementing MPSE is projected to nearly halve contactor CAPEX (from $\$$6.08M to $\$$3.01M) and significantly increase the project's Net Present Value (NPV), derisking new investment and enabling distributed critical-mineral processing configurations. The commercialization of MPSE technology is being spearheaded by Vigsur Dynamics Inc., which has adopted a structured, parallel approach to technical and business development since its formation in January 2026. Following extensive customer discovery and engagement with the Oregon State University accelerator, Vigsur Dynamics is working to establish a business model that transitions from pilot demonstrations to modular hardware sales, ultimately aiming for a "build-own-operate" service strategy. Current technical milestones—including 100 hours of continuous operation, superior energy efficiency, and successful 6-unit modular scale-up— provide a foundation for this transition. Backed by ongoing IP licensing and a growing network of industrial and venture advisors, the company is actively de-risking the platform to replace conventional mixer-settler systems in the critical minerals market.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH

Field Validation of Thermoelectric Generation System at Holcim Cement Plant in Alpena, Michigan

Executive Summary Project Background The Industrial Technology Validation (ITV) program aims to identify and demonstrate the performance of new, emerging, and underutilized energy-saving technologies in the industrial sector to help inform decisions to help accelerate their commercialization and deployment, as well as to help make industries more competitive. This ITV demonstration evaluated a thermoelectric generation (TEG) technology at a cement plant, aiming to reduce energy demand in the cement industry. A median cement plant consumes 5.73 million British thermal units per ton of clinker production (resulting in 0.838 metric tons of carbon dioxide [CO₂] emissions per ton of clinker) (Boyd and Zhang 2011, EPA 2021), equivalent to approximately 6.9 trillion British thermal units (TBtu) per year in energy consumption at a cement plant producing 3,300 tons of clinker per day.¹ Collaborating with Holcim, Advanced Thermovoltaic Systems (ATS) developed and deployed a pilot-scale thermoelectric power system to efficiently capture and convert waste heat to electricity. The system leverages the Seebeck effect to convert temperature differences on two sides of semiconductor cartridges into electrical power (ScienceDirect, n.d.). This generation is realized with minimal moving parts compared to existing waste-heat-to-generation solutions and allows capture from heat sources with temperatures as low as 150°C. This project aimed to validate a scalable solution applicable for capturing medium-temperature waste heat, including ambient losses from other high-temperature processes, and high-temperature sources less suitable for other waste-heat-to-power solutions. By recovering this otherwise wasted heat, this project intends to validate improvements to overall process efficiency through reduction in purchased electricity, thereby reducing operational costs while enhancing resiliency and competitiveness. Description and Scope This study evaluated the performance of a TEG system from ATS as a solution to convert waste heat into useful power at a Holcim cement plant in Alpena, Michigan. This plant is a fully integrated cement plant that has been operating since 1907. The facility operates continuously (24/7/365) with approximately 250 employees and five long dry kilns, yielding a total production capacity of 7,852 tons of cement per day (EPA 2023). Currently, the Alpena plant uses waste heat boilers to convert waste heat from the exhaust of each kiln into steam, which drives steam turbine generators. The ATS TEG is being evaluated for its potential to supplement the steam turbines by capturing the remaining lower grade heat. This technology is also being considered for other Holcim plants where steam turbines are not a viable option. ATS installed a pilot-scale TEG unit with an array of 582 individual thermoelectric semiconductor cartridges, of which 573 were operational. The cartridges are sandwiched between 48 hot plates and 49 cold plates. Each cartridge is designed to generate 20 watts (W) of gross power at a hot-side temperature of 240°C and cold-side temperature of 20°C. As such, the total gross generation capacity of the installed system is 11.5 kilowatts (kW) at design conditions. The system configuration for the evaluation was designed to prioritize convenience of installation and minimize disruption to production at the site, while ensuring that the heat required can be obtained for evaluating the TEG system at various operational conditions. To accomplish this, a portion of the steam supplied to Alpena’s steam turbine generation system was diverted to be used as the heat source for the TEG system, while water was supplied to the cold side of the system from nearby Lake Huron. This configuration was designed for the evaluation of the pilot-scale system to assess the performance at different conditions. A commercial-scale system will likely vary from the pilot system depending on typical configurations, including both scale and application. Future commercial applications of the ATS system would involve integrating the system into the exhaust from kiln preheaters, clinker coolers, or radiant heat capture from kiln shells for the heat source. For the cold source, a range of cooling solutions can be considered, including a mechanical cooling system, depending on the location and the application. To increase the generation capacity for commercial applications, the technology provider is working toward developing a commercial-scale TEG system, which would combine multiple TEG units (each similar in design to the pilot system) together. The scope of this evaluation includes the pilot-scale TEG system and all impacted equipment including pumps, controllers, and power handling equipment. Study Objectives The evaluation's goal was to assess the potential of the ATS TEG system to generate useful electrical power by capturing waste heat from cement production kilns. The objectives of this study are to evaluate and verify the following claims made by ATS regarding the pilot-scale system installed at the Holcim Alpena plant. The following design parameters and claims are also outlined in Table ES- 1 and Table ES- 2: • Gross Power: The thermoelectric system converts heat into power to create gross power, the total measured power generated by the system. The 573 active cartridge pilot-scale system is expected to generate 11.5 kW of gross power at the designed hot-side temperature of 240°C and cold-side temperature of 20°C. Power production is dependent on the temperature difference between the heat source (ultimately from the waste heat) and cold temperature supply source. • Net Power: The net power is the total usable power provided to the site by the TEG system after deducting parasitic power loads from the gross generated power. Supplementary equipment is required to operate the TEG system including pumps, controllers, and, in certain anticipated applications, mechanical cooling, which introduce parasitic loads to system operation. After deducting the parasitic loads from the gross power generation, ATS anticipates achieving a net power generation of 7.5 kW from the pilot-scale system. • Thermal Efficiency: The thermal efficiency is the percent of the total heat transferred to the TEG system that is converted to gross power. Historically, TEGs have a thermal efficiency of 2%–5% (DOE 2008). Prior industrial-scale TEG systems, such as the E1 TEG offered by Alphabet Energy, operated at an efficiency of 2.5% (Lamonica, 2014). ATS anticipates achieving an average efficiency of 4.8% or higher in converting heat energy to usable electricity. • Cartridge Performance: The TEG system comprises 573 active individual semiconductor cartridges, each of which generates a portion of the total power. Cartridge optimization and selection is an important design consideration for potential future TEG system design performance. Therefore, understanding the distribution of gross power and efficiency within the pilot system is vital to understanding what is achievable. At a design hot-side temperature of 240°C and cold-side temperature of 20°C, ATS anticipates a cartridge performance of 20 W of gross power per cartridge at an efficiency of 4.8% per cartridge. In addition to evaluating the claimed performance of the TEG pilot-scale unit, the study estimated the potential annual impacts of a scaled-up commercial system used to capture kiln waste heat over annual operations. The evaluation estimated the gross and net annual electric generation achievable by capturing heat from the two proposed tap-in points: the kiln exhaust and the clinker cooler exhaust; see Section 2.1 for details. Two use cases were examined: • Holcim Alpena: The Holcim Alpena site consists of long dry kilns with superheater boilers, which differs from the rest of Holcim’s cement plant portfolio and results in lower waste heat temperatures. The study estimates gross and net annual generation using the superheater boiler exhaust and clinker cooler exhaust, based on 2023 operational data. • Typical Installation: Common cement plants have preheater kilns with higher exhaust temperatures than Holcim Alpena across a range of production rates. The study estimates gross and net annual generation using the preheater exhaust and clinker cooler exhaust, with a sensitivity analysis to account for the typical range of preheater exhaust temperatures, clinker cooler exhaust temperatures, and clinker production rates. Methodology The evaluation methodology followed a measurement and verification (M&V) strategy based on the International Performance Measurement and Verification Protocol Option B through comprehensive measurements and analyses of the affected systems. Evaluation data was collected from March 9 to March 11, 2024, the test period of the pilot TEG system. During the test period, in coordination with the ITV team, the ATS team adjusted system operations to capture the range of variability expected for each of the variables pertinent to performance of the system. The methodology consisted of two parts: evaluating the performance of the pilot unit's TEG system and estimating the annual TEG impact in terms of gross and net power based on a given waste heat profile. First, the evaluation of the thermoelectric generation performance of the pilot unit relative to the claims was performed by analyzing the collected test data. Gross power of the pilot TEG system was directly measured. Net power was determined by deducting the measured parasitic power from the gross power. The gross power generation was compared to heat transferred to the system by the working fluid (which was heated by steam generated from the kiln waste heat) to calculate the thermal efficiency achieved by the system. Performance of individual semiconductor cartridges within the pilot array was also assessed in terms of measured gross cartridge power and calculated cartridge thermal efficiency. The second part of the evaluation estimated the annual TEG impacts in terms of gross power and net power (calculated from the difference between gross power and parasitic power). This analysis comprised development of mathematical regression models for gross power and parasitic power, with assessment of each model’s goodness-of-fit characteristics to ensure satisfaction of statistical requirements. The models predicted the gross power generation, the parasitic load based on the temperature difference between the hot working fluid and the cold-side fluid (cold water from Lake Huron) entering the system, the volumetric flow rate of the cold-side fluid at the inlet, and the volumetric flow rate of the hot working fluid at the inlet. The annual impact analysis considered a theoretical commercial-scale system sized to capture the available waste heat at a cement plant, consisting of linked pilot-scale units that receive heat from a theoretical gas-to-working-fluid heat exchanger. To estimate annual impacts at the Alpena plant, the gross power and parasitic power regression models were applied to the arrays in the theoretical commercial-scale system. The heat supplied to the unit was calculated based on the kiln run time, annual production, kiln exhaust waste heat, and clinker cooler waste heat derived from 2023 Holcim Alpena kiln operational data. Net power impacts were calculated by deducting the resulting parasitic power from the estimated gross power. Inputs for the model were generated from a combination of hourly data, assumed design considerations for TEG system scale-up from the pilot-scale unit, and assumptions regarding TEG system operations. This analysis was then used as the basis for estimating annual impacts of typical TEG installation at cement plants, by applying sensitivity analyses to key kiln operational characteristics including kiln preheater exhaust temperatures, cooler clinker exhaust temperatures, and plant daily production rates across a range of expected values. Project Results/Findings Table ES- 2 and Table ES- 2 provide a summary of the operating conditions and evaluation results compared to the stated claims from the technology provider. Key takeaways include: • Gross Power: The peak gross power achieved during the testing period was 10.0 kW, compared to the 11.5 kW expected for 573 active cartridges. The claimed gross power was associated with a target hot side of 240°C; however, the system only received a maximum hot-side mean plate temperature of 212°C during the testing period. • Net Power: The pilot-scale unit exceeded the claims for net power, achieving a peak of 7.7 kW net compared to a claim of 7.5 kW. One factor contributing to the higher achieved net power is the relatively high water pressure available through Lake Huron. The pilot TEG system did not require cold-side pumps during the test, whereas most installations would. This reduced the parasitic loads on the system, ultimately contributing to higher net power relative to the gross power. • Thermal Efficiency: The pilot-scale unit outperformed the claimed efficiency, achieving a peak system efficiency of 5.0% thermal efficiency compared to the stated 4.8%. • Cartridge Performance: To compare cartridge performance against claims, the study focused on the third day of testing, which aimed for conditions closest to the design specifications, with a hot side of 240°C and cold-side exit temperature of 6.4°–30°C. On this day, the mean gross power observed in the cartridges within the TEG array was 18.1 W/cartridge, and the peak performance was 34.7 W/cartridge. The estimated mean cartridge efficiency was 5.2%, and the estimated efficiency at peak gross cartridge power was 10%. The regression models developed for gross power generation and parasitic loads were used to estimate the generation impact for given heat input to the TEG from the working fluid (captured from the waste heat) and from the cold loop (Lake Huron) on an hourly basis for a year of operation. Based on this analysis, installation of a commercial-scale TEG system at the Holcim cement plant in Alpena, Michigan, with a waste heat exchanger of 0.85 effectiveness, would generate up to 391 kW of net power, translating to between 920,000 and 1,800,000 kilowatt-hours (kWh) in net electricity per year. Based on typical grid emissions for Alpena, this would avoid estimated net emissions by 752 metric tons of CO₂ annually.² The sensitivity analysis estimated that typical TEG system installations at cement plants could generate an average of 56–1,040 kW of net power, or between 488,000 and 9,110,000 kWh of net energy. This generation potential is most significantly affected by plant production rates and also influenced by preheater and clinker cooler exhaust temperatures. Applying the national average emission rate, typical commercial-scale installations at Holcim plants are projected to avoid between 182 and 3,401 metric tons of CO₂ annually per site. Table ES- 3 shows a summary of the estimated annual impacts.³ While parasitic loads are significant and vary by application, this analysis assumed the use of heating loop pumps and access to Lake Huron as a cold sink. This setup assumed no need for cooling loop pumps due to the available water pressure at the test site. Applications that require cooling towers or additional equipment are likely to experience higher parasitic loads. Therefore, the study’s estimates are most applicable to scenarios with similar parasitic load configurations—namely, access to a high-pressure cold sink. Applicability to other locations may be limited, as differing conditions could necessitate additional pumps and cooling systems, potentially impacting performance significantly.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI

Fabrication and Testing of Solid-Solution Strengthened Corrosion Resistant Alloys For Service in Molten Fluoride Environments

The demand for higher system thermal efficiencies requires the operation of power generation cycles and heat conversion systems at progressively higher temperatures. As the system operating temperature increases, existing materials may not provide adequate mechanical properties or environmental compatibility or both. There is an increasing commercial interest in the development and deployment of liquid-fueled Molten Salt Reactors (MSRs). Hastelloy®N, the highest performing candidate MSR structural alloy, is not capable of operations at temperatures above 700°C, thus limiting the performance of these systems. Using an Integrated Computational Materials Engineering (ICME)-approach and small laboratory scale heats, ORNL developed a class of patented alloys covered by U.S. Patent 9, 435, 011 B2, “Creep-resistant, Cobalt-free alloys for high temperature, liquid-salt heat exchanger systems,” similar to Hastelloy®N in that they are primarily solid solution strengthened. In contrast to precipitation strengthened alloys, the microstructure of solid solution alloys and hence the high temperature mechanical properties are stable for extended periods of time allowing long reactor operating life. The new alloys have shown to possess good resistance to liquid fluorides at temperatures up to 850°C and have significantly improved creep properties when compared to Hastelloy®N. The purpose of the CRADA project was for ORNL to collaborate with Haynes International- a materials producer, MetalTek International- a foundry, and Kairos Power – an advanced reactor developer – to scale-up selected alloys, evaluate their properties, and identify one solid solution strengthened alloy that can meet the property requirements for the reactor being developed by Kairos Power and other similar liquid fluoride-salt cooled reactors. As part of the project, eight alloys were down-selected and fabricated in larger industrial scale heats by Haynes International. Resistance to molten salt was evaluated in flowing FLiNaK and FLiBe by Kairos Power using their Rotating Cage Loop (RCL) system. Accounting for iron deposition during these tests, the new alloys displayed very low net mass change showing excellent corrosion performance in molten salt. Creep properties evaluated at ORNL were found to be better than that of Hastelloy®N and 316 stainless steel. Long-term stabilities of the alloys evaluated by Haynes International showed that these alloys have excellent thermal stability in the temperature range 704.4-815.6°C, with the change in strength and ductility being less than 10-15% after a 4000-hour exposure at 815.6°C. Autogenously Gas Tungsten Arc Welding (GTAW) welded samples showed less than 10% change in yield strength / ultimate tensile strength / total elongation compared to the basemetal, indicating that the alloys have excellent weldability. Three parts were successfully investment-cast using one alloy with very little voiding showing feasibility of fabricating parts using the casting process. This project enabled extensive interaction between the material producer Haynes International, casting supplier MetalTek, and reactor developer Kairos Power. This facilitated testing of materials and components produced using the newly developed alloys by the end-user. This allowed the generation of critical dataset required for down-selection of a few promising alloys for further development. This data is also currently being shared with other reactor designers for them to evaluate the suitability of this alloy for their reactor design. The availability of this alloy will ultimately enable the design and development and deployment of MSRs with increased temperature of operation and thus, improved efficiencies.

99 GENERAL AND MISCELLANEOUS

Fabrication and Testing of Solid-Solution Strengthened Corrosion Resistant Alloys For Service in Molten Fluoride Environments

The demand for higher system thermal efficiencies requires the operation of power generation cycles and heat conversion systems at progressively higher temperatures. As the system operating temperature increases, existing materials may not provide adequate mechanical properties or environmental compatibility or both. There is an increasing commercial interest in the development and deployment of liquid-fueled Molten Salt Reactors (MSRs). Hastelloy®N, the highest performing candidate MSR structural alloy, is not capable of operations at temperatures above 700°C, thus limiting the performance of these systems. Using an Integrated Computational Materials Engineering (ICME)-approach and small laboratory scale heats, ORNL developed a class of patented alloys covered by U.S. Patent 9,435,011 B2, “Creep-resistant, Cobalt-free alloys for high temperature, liquid-salt heat exchanger systems,” similar to Hastelloy®N in that they are primarily solid solution strengthened. In contrast to precipitation strengthened alloys, the microstructure of solid solution alloys and hence the high temperature mechanical properties are stable for extended periods of time allowing long reactor operating life. The new alloys have shown to possess good resistance to liquid fluorides at temperatures up to 850°C and have significantly improved creep properties when compared to Hastelloy®N. The purpose of the CRADA project was for ORNL to collaborate with Haynes International- a materials producer, MetalTek International- a foundry, and Kairos Power – an advanced reactor developer – to scale-up selected alloys, evaluate their properties, and identify one solid solution strengthened alloy that can meet the property requirements for the reactor being developed by Kairos Power and other similar liquid fluoride-salt cooled reactors. As part of the project, eight alloys were down-selected and fabricated in larger industrial scale heats by Haynes International. Resistance to molten salt was evaluated in flowing FLiNaK and FLiBe by Kairos Power using their Rotating Cage Loop (RCL) system. Accounting for iron deposition during these tests, the new alloys displayed very low net mass change showing excellent corrosion performance in molten salt. Creep properties evaluated at ORNL were found to be better than that of Hastelloy®N and 316 stainless steel. Long-term stabilities of the alloys evaluated by Haynes International showed that these alloys have excellent thermal stability in the temperature range 704.4-815.6°C, with the change in strength and ductility being less than 10-15% after a 4000-hour exposure at 815.6°C. Autogenously Gas Tungsten Arc Welding (GTAW) welded samples showed less than 10% change in yield strength / ultimate tensile strength / total elongation compared to the basemetal, indicating that the alloys have excellent weldability. Three parts were successfully investment-cast using one alloy with very little voiding showing feasibility of fabricating parts using the casting process. This project enabled extensive interaction between the material producer Haynes International, casting supplier MetalTek, and reactor developer Kairos Power. This facilitated testing of materials and components produced using the newly developed alloys by the end-user. This allowed the generation of critical dataset required for down-selection of a few promising alloys for further development. This data is also currently being shared with other reactor designers for them to evaluate the suitability of this alloy for their reactor design. The availability of this alloy will ultimately enable the design and development and deployment of MSRs with increased temperature of operation and thus, improved efficiencies.

36 MATERIALS SCIENCE