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All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

An initial framework for the rapid qualification of long-term creep rupture strength via microstructural modeling

This report describes the development and testing of a new method for extrapolating short-term creep rupture test data to predict long-term rupture strength. The goal of this work is to reduce the time required to qualify new materials for nuclear service by reducing the lead time required for dedicated, long-term material testing to establish key long-term material properties. The new approach described here uses a physics-based model to predict the long-term creep rupture strength of 316H stainless steel using only short-term test data. The key idea is to use Bayesian inference to find the statistical distribution of the model parameters that best explain the short-term rupture data. Because the model is physics-based these parameters are all microstructural quantities that can be measured through detailed material characterization experiments. The Bayesian prior distributions provide a means for incorporating this characterization data into the final model to improve the accuracy of the long-term model predictions. However, where such data is not available the process still produces an accurate model based on an uniformed prior. Our hypothesis is that this approach more accurately extrapolates the short-term test data when compared to current, empirical methods. The report proves this hypothesis using actual long-term rupture data available for 316H, including tests with rupture times greater than 200,000 hours. The general approach developed here could be applied to other materials and other time-dependent material properties. Applying this new technique to develop long-term qualified material properties, potentially in conjunction with other accelerated qualification approaches like staggered qualification test programs, could greatly reduce the time required to qualify new materials for nuclear service.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

KOMPASS-II: Compaction of Crushed salt for Safe Containment – Phase 2

Long-term stable sealing elements are a basic component in the safety concept for a possible repository for heat-emitting radioactive waste in rock salt. The sealing elements will be part of the closure concept for drifts and shafts. They will be made from a welldefinied crushed salt in employ a specific manufacturing process. The use of crushed salt as geotechnical barrier as required by the German Site Selection Act from 2017 /STA 17/ represents a paradigm change in the safety function of crushed salt, since this material was formerly only considered as stabilizing backfill for the host rock. The demonstration of the long-term stability and impermeability of crushed salt is crucial for its use as a geotechnical barrier. The KOMPASS-II project, is a follow-up of the KOMPASS-I project and continues the work with focus on improving the understanding of the thermal-hydraulic-mechanical (THM) coupled processes in crushed salt compaction with the objective to enhance the scientific competence for using crushed salt for the long-term isolation of high-level nuclear waste within rock salt repositories. The project strives for an adequate characterization of the compaction process and the essential influencing parameters, as well as a robust and reliable long-term prognosis using validated constitutive models. For this purpose, experimental studies on long-term compaction tests are combined with microstructural investigations and numerical modeling. The long-term compaction tests in this project focused on the effect of mean stress, deviatoric stress and temperature on the compaction behavior of crushed salt. A laboratory benchmark was performed identifying a variability in compaction behavior. Microstructural investigations were executed with the objective to characterize the influence of pre-compaction procedure, humidity content and grain size/grain size distribution on the overall compaction process of crushed salt with respect to the deformation mechanisms. The created database was used for benchmark calculations aiming for improvement and optimization of a large number of constitutive models available for crushed salt. The models were calibrated, and the improvement process was made visible applying the virtual demonstrator.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2021

Compaction of crushed salt for safe containment – overview of the KOMPASS project

Abstract. In Germany, rock salt formations are possible host rock candidates for a repository for heat-emitting radioactive waste. The safety concept of a repository in salt bases on a multibarrier system consisting mainly of the geological barrier salt and geotechnical seals ensuring safe containment. Crushed salt will be used for backfilling of cavities and sealing measures in drifts and shafts due to its favourable properties and its easy availability (mined-off material). The creep of the rock salt leads to crushed salt compaction with time. Thereby, the crushed salts' porosity is reduced from the initial porosity of 30 %–40 % to a value comparable to the porosity of undisturbed rock salt (≤1 %). In such low porosity ranges, technical impermeability is assumed. The compaction behaviour of crushed salt is rather complex and involves several coupled THM processes (Kröhn et al., 2017; Hansen et al., 2014). It is influenced by internal properties like humidity and grain size distribution, as well as boundary conditions such as temperature, compaction rate or stress state. However, the current process understanding has some important gaps referring to the material behaviour, experimental database and numerical modelling. It needs to be extended and validated, especially in the low porosity range. The objective of the KOMPASS project was development of methods and strategies for the reduction of deficits in the prediction of crushed salt compaction leading to an improvement of the prognosis quality. Key results are as follows (KOMPASS Phase 1, 2020): selection of an easily available and permanently producible synthetic crushed salt mixture, acting as a reference material for generic investigations; development and proof of different techniques for producing pre-compacted samples for further investigations; establishment of a tool of microstructure investigation methods to demonstrate the comparability of grain structures of pre-compacted samples with in-situ compacted material for future investigations; execution of various laboratory experiments using pre-compacted samples, e.g. long-term creep tests which deliver reliable information about time- and stress-dependent compaction behaviour; development of a complex experimental investigation strategy to derive necessary model parameters considering individual functional dependencies. Its technical feasibility was successfully verified; benchmarking with various existing numerical models using datasets from three different triaxial long-term tests. The result was not entirely satisfactory; however, the number of influencing factors is small and further validation work has to be done. Overall, the KOMPASS project has made significant progress in the approaches to solving the outstanding question, building the basis for further investigations.

Friedenberg, Larissa↗
DOE OSTI2023

A617 Notch Effect and Crack Growth Testing Status

This is an update on the Alloy 617 notched specimen creep testing and crack growth rate testing performed in FY23. Long-term notch testing continues, with some new results on double V-notch specimens. Creep-fatigue crack growth rate testing has begun and some preliminary results are shown.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Long-Term Evaluation of Remedial Technology Performance in the Laboratory: Multi-year Experimental Test Plan

An understanding of the long-term effectiveness of remediation technologies is central to sustainable environmental cleanup. Long-term experiments are valuable for reducing uncertainty and predicting remediation outcomes at scales required for regulatory compliance. However, these types of tests can be costly and challenging to interpret. Therefore, contaminated sites often rely on short-term laboratory experiments that may not account for the potentially significant effects of gradual, time- dependent processes governing contaminant retention, release, and species transformation. For example, short-term lab experiments (from months to a year) conducted with sediments from the unsaturated and saturated zones at the Hanford Site play an important role in initial evaluations of remediation technologies but cannot capture the full extent of time-dependent reactions, leaving uncertainties in field-scale deployment. Here, long-term testing will be conducted on select technologies based on their performance in short-term testing. The overall objective is to directly address the challenges described above by generating and analyzing data on long-term (2–10 years) efficacy of selected remediation technologies, integrating this understanding into models, and providing critical input for remediation planning, monitoring, and 5-year review cycles for field-implemented remedies. Specific objectives include: 1. Evaluating long-term efficiency of promising remedies under site-specific conditions. 2. Generating robust parameters for modeling, reducing uncertainty in predictive simulations. 3. Advancing integrated monitoring by combining geochemical and geophysical observations. 4. Informing field-scale implementation by incrementally advancing technologies, identifying failure mechanisms early, and prioritizing robust, cost-effective remedies. Through systematic evaluation of technologies in laboratory-scale column experiments, integrated monitoring, and modeling support, this project is designed to bolster confidence in the long-term robustness of selected technologies. The ultimate outcome is the identification and deployment of more reliable, cost-effective remedies that safeguard human health and the environment while reducing the uncertainties that have historically hindered cleanup progress at Hanford Site. An experimental approach was developed and initiated for long-term testing potentially up to 10 years. The table below summarizes the experimental approach developed for testing select technologies and presented in this multi-year experimental test plan.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2023

Compaction of crushed salt for safe containment – a summary of the KOMPASS projects

Abstract. For the underground disposal of high-level nuclear waste in rock salt formations, the safety concept includes the backfilling of open cavities with crushed salt. For the prognosis of the sealing function of the backfill for the safe containment of the radioactive waste, it is crucial to have a comprehensive process understanding of the crushed-salt compaction behavior. The crushed-salt compaction process is influenced by internal properties (e.g., grain size, mineralogy, and moisture content) and boundary conditions (e.g., temperature, stress state, and compaction rate) and, therefore, involves several coupled thermal–hydro–mechanical (THM) processes (Hansen et al., 2014; Kröhn et al., 2017). With the paradigm shift from the limited release of radionuclides to safe containment due to the German Repository Site Selection Act passed in 2017, the importance of crushed salt as geotechnical barrier has increased, with a focus on the evolution of its hydraulic properties. Based on the knowledge gaps in the current process understanding, the “Compaction of crushed salt for safe containment” (KOMPASS) projects were initiated to improve the scientific basis behind using crushed salt for the long-term isolation of high-level nuclear waste within rock salt repositories. The efforts to improve the prediction of crushed-salt compaction begun during the first phase of the KOMPASS projects (Czaikowski et al., 2020) and were followed up in a second phase ending in June 2023. The primary achievements of the projects are as follows (Czaikowski et al., 2020; Friedenberg et al., 2022): specification of the KOMPASS reference material, an easily available and reproducible synthetic crushed-salt material, for generic investigations; development of pre-compaction methods and successful production of samples in the short term and under in situ loading conditions; formulation of an extended laboratory program addressing the isolated investigation of known relevant factors influencing the compaction behavior of crushed salt (Düsterloh et al., 2022); execution of long-term compaction tests addressing isotropic and deviatoric load changes, temperature, and compaction state; construction of a backfill body using the KOMPASS reference material in the Sondershausen mine through collaboration with the SAVER (Entwicklung eines salzgrusbasierten Versatzkonzepts unter der Option Rückholbarkeit) project (Schaarschmidt and Friedenberg, 2022); advancement of the tools for microstructure investigation methods (Svensson and Laurich, 2022); generation (first stages) of a microphysical process list combining literature research with our own findings; benchmarking of long-term compaction test for model development and optimization of various existing models as well as the development of new models; application of a virtual demonstrator (2D model representing a backfilled drift in rock salt) for the visualization of developments and the quantification of the models (Rabbel, 2022). In summary, the KOMPASS projects contributed to the reduction of uncertainties and the strengthening of the safety case for using crushed salt within rock salt repositories.

Friedenberg, Larissa↗
DOE OSTI2021

The EGS Collab Project: Status and Accomplishments

The EGS Collab project, supported by the US Department of Energy, is addressing challenges in implementing enhanced geothermal systems (EGS). This includes improving understanding of the stimulation of crystalline rock to create appropriate flow pathways, and the ability to effectively simulate both the stimulation and the flow and transport processes in the resulting fracture network. The project is performing intensively monitored rock stimulation and flow tests at the 10-m scale in an underground research laboratory. Data and observations from the field test are compared to simulations to understand processes and to build confidence in numerical modeling of the processes. In Experiment 1, we examined hydraulic fracturing an underground test bed at the Sanford Underground Research Facility (SURF) in Lead, South Dakota, at a depth of approximately 1.5 km. We drilled eight sub-horizontal boreholes in a well-characterized phyllite. Six of the boreholes were instrumented with many sensor types to allow careful monitoring of stimulation events and flow tests, and the other two boreholes were used for water injection and production. We performed a number of stimulations and flow tests in the testbed. Our monitoring systems allowed detailed observations and collection of numerous data sets of processes occurring during stimulation and during dynamic flow tests. Long-term ambient temperature and chilled water flow tests were performed in addition to many tracer tests to examine system behavior. Data were rapidly analyzed, allowing adaptive control of the tests. Numerical simulation was used to answer key experimental design questions, to forecast fracture propagation trajectories and extents, and to analyze and evaluate results. Many simulations were performed in near-real-time in conjunction with the field experiments, with more detailed process study simulations performed on a longer timeframe. Experiment 2 will examine hydraulic shearing in a test bed being built at the SURF at a depth of about 1.25 km in amphibolite under a different set of stress and fracture conditions than Experiment 1. Five sets of fracture orientations were considered in design, and three orientations seem to be consistently observed.

EGS Collab↗
DOE OSTI2021

A study on the creep behavior of alloy 709 using in-situ scanning electron microscopy

In this research, an experimental evaluation of creep properties of Alloy 709 in the temperature range of 750–850 °C was undertaken. Alloy 709 is a novel austenitic stainless steel with 20% Cr and 25% Ni by wt% that was developed for application in structural components of nuclear power plants. Creep rupture tests were conducted in an in-situ heating-loading and Scanning Electron Microscope (SEM) unit equipped with Electron Backscatter Diffraction (EBSD) detector and Energy Dispersive Spectroscopy (EDS). “Real-time” creep damage mechanisms of Alloy 709 at various stresses and temperatures using a flat, un-notched sample with continuously reducing cross-section is studied so that the failure and maximum creep damage occurred at the center of the sample where the in-situ SEM imaging could be focused. Accelerated creep tests at temperatures and stresses above service conditions were performed by employing multiple blocks of constant loads where the loads were increased once the sample attained constant creep rate, indicating a secondary creep regime. This technique ensures multiple data points can be obtained from the same test, saves the time required for an otherwise long-term creep test and usage of SEM. Further, Coincident Site Lattice (CSL) boundary maps were collected as control maps before testing, and the grain boundaries were observed during the creep test to understand the effect of grain boundary character on the creep damage mechanism. Void growth, grain boundary separation, and sliding were found to be the main creep mechanisms whose rate is dependent on stress and temperature. Failure mechanisms studied on the fracture surface using SEM fractography were correlated to the sample surface observations to create complementary information to better understand the underline creep mechanism of Alloy 709.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Accelerated Materials Deployment in Advanced Nuclear Power Plants

The purpose of this report is to begin the development of a maximally efficient process for licensing and deploying new materials in Advanced Non-Light-Water Reactors (ANLWRs). Some new materials that are to be used in some new plants are seen as possibly introducing risks, because our understanding of those new materials’ behavior in the conditions generated by some novel plant designs is less complete than our understanding of the behavior of materials with long use histories in existing designs. In these cases, an approved code/standard or a code case to support the use of these materials in the novel design’s safety case may not exist for the regulator to utilize as part of the licensing determination. This circumstance creates the potential for an extremely long licensing process for new designs using new materials. The present strategy is to show how to manage these risks proactively, in such a way as to permit licensing decisions to be made in a timely manner, based on this risk management process. The present report outlines the gaps in the current codes to support deployment and use of novel materials and begins the development of the necessary risk management framework that is focused on the subject materials issues; it is based on risk-informed in-service surveillance practices, carried out in such a way as to compensate for current limitations in our state of knowledge. This development will enable licensing and deployment of the subject materials, conditional on the proactive surveillance process to be established. While this report is occasioned by limitations in our knowledge of certain materials issues that may arise in advanced designs, in-service surveillance is always done in order to compensate for a lack of knowledge: if we knew that components were not already failed and not trending toward failure, we would not perform surveillance, even in current-generation plants (except that prescriptive requirements would force us to do so). What is different about the surveillance program discussed here is that the issues are newer and the relevant experience base is less complete, so the surveillance presently contemplated may need to measure new things and/or measure them more often than has been traditional for surveillance coupons. The present report is devoted to the risk management framework and applies American Society of Mechanical Engineers Boiler and Pressure Vessel Code Section XI, Division [1] to establish the structure of a protocol for carrying out the necessary surveillance. These documents are generic: they do not tell us how often to surveille, or what to surveille, or what to measure, but rather how to determine those things, given certain technical inputs. The Regulatory Development R&D Program [2] is currently developing the companion supporting technical basis for the materials surveillance technology that, when completed and validated, can be used by owner/operator and NRC to implement a materials degradation management program for ANLWRs. This report also outlines salient points of discussion, positive potential outcomes, and potential concerns from industry and the USNRC. These aspects of the report intend to inform future work to develop a proposed technical process for adoption by the industry and endorsement by the USNRC to allow developers to propose a risk informed and conservative approach for the use of materials where operating experience/data and codes and standards may not exist for use of a novel material in an operating reactor environment. Additionally, such a technology could be leveraged to potentially reduce part of the upfront materials data requirements from ongoing long-term materials testing so that early action on license application could be undertaken by NRC, in parallel with the continuation of long-term data collection. This could accelerate the schedule for a first-of-a-kind ANLWR deployment or a nth-of-a-kind new materials insertion for established ANLWR designs.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2025

Creep Property of Intermetallic Dispersive Steels for Nuclear Applications

To meet the materials performance demands of next-generation nuclear and high-temperature energy systems, a new class of intermetallic-dispersive steels (IDS) has been designed through integrated computational thermodynamics and alloy design strategies. The IDS alloys incorporate coherent L1₂ (γ′-Ni₃Al) nanoprecipitates within an Fe–Ni–Cr austenitic matrix, engineered to achieve both high temperature strength and thermodynamic stability while suppressing the formation of detrimental δ-Ni₃Nb and η-Ni₃Ti phases. Initial creep testing of Ti-IDS and TiTa-IDS alloys demonstrates rupture lives comparable to or exceeding those of Inconel 718 and ODS steels, despite being fabricated through conventional ingot metallurgy. Step-load creep tests identified a stress threshold near 300–350 MPa for the onset of tertiary creep, and in-situ neutron diffraction experiments on Ti-IDS revealed clear load partitioning between the matrix and γ′ precipitates: elastic strain is shared by both phases, while plastic strain localizes in the matrix. These results confirm that stable γ′–matrix interfaces play a dominant role in retarding dislocation motion and enhancing creep resistance. In FY26, the program will conduct repeat creep rupture testing of TiTa-IDS at 650 °C/400 MPa, initiate long-term rupture testing of TiNb-IDS, and perform TEM-based microstructural characterization to elucidate dislocation–precipitate interactions and microstructural stability. Collectively, these efforts will establish the mechanistic foundation for next-generation high-temperature structural materials based on the IDS concept.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2024

Design, Fabrication and Testing of Surveillance Test Articles for MSR Materials Degradation Management

This report details the design, fabrication, and testing of surveillance test articles aimed at assessing material damage in reactor-relevant environments for effective degradation management. Two types of surveillance test articles with reduced sizes were developed based on design algorithms and finite element modeling: welded design and interlocking design. A furnace heating setup was adopted to apply multiple thermal cyclic loading profiles on the test articles with a temperature range of 500°C - 700°C, while the strain response was monitored using a digital image correlation technique. The testing results demonstrated the successful capturing of expected strain range for welded design while machining tolerance should be improved to engage strain coupling in the interlocking design. Mid-term (500 hours) and long-term (1500 hours) cyclic tests were conducted on welded test articles. A constant strain range of ~0.6% was observed at the specimen with testing under 500 hours, while a gradual decrease of strain at specimen was observed after 500 hours. Non-destructive evaluation through X-ray computed tomography confirmed the microcracks in the welds at specimen-driver joints after cyclic test that caused the strain change. Creep testing of the specimen after long-term cyclic test revealed a short creep life than expected. A multi-profile cyclic test was also conducted on a test article and demonstrated consistent strain response under different temperature ramp rates. The report also briefly discussed the challenges and future research efforts to advance test article development for material surveillance.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Embedded High-Temperature Sensors: Enhancing Thermoelectrical Performance with Refractory Composites Gradient Layers

To monitor the stability of various energy and manufacturing systems, sensors capable of operating at temperatures exceeding 1000 °C in diverse environments for extended durations are essential. However, under harsh conditions, degradation of sensing materials is a concern that can be controlled by embedding the sensors into refractory oxides. Doped-LaCrO3 based composites are excellent candidates for high-temperature sensing applications due to their good thermoelectrical properties. However, chemical reactivity between the conductive phase and the refractory oxides can decrease the performance of the sensors. In this work, it was devised gradient-type protective layers safeguarding conductive phases within embedded thermocouples, which were fabricated and characterized by X-Ray Diffraction for phase development analysis, Scanning Electron Microscopy and Energy-dispersive X-ray spectroscopy for microstructure and cationic interdiffusion kinetics, long-term thermoelectric testing was completed up to 1400 °C. The enhanced performance of these novel sensors addresses a critical limitation, rendering them viable for long-term high-temperature applications.

20 FOSSIL-FUELED POWER PLANTS↗
DOE OSTI2022

Innovative Method for Welding in Generation 3 CSP to Enable Reliable Manufacturing of Solar Receivers to withstand Daily Cycling at Temperatures Above 700°C (Final Technical Report)

Inconel® Alloy 740H® (alloy 740H) was the first age-hardenable nickel-based alloy approved by the ASME Boiler & Pressure Vessel Code for use in pressure-boundary applications. Over the past ~20 years the alloy has been optimized for weldability and high-temperature stability, approved for use in different applications. Development of a supply chain combined with the advantageous properties of the alloy (high-temperature creep strength, oxidation and corrosion resistance, etc.) have resulted in the alloy being applied to new high-temperature power cycle demonstration projects, and of particular interest are applications to concentrating solar power (CSP) to enable higher-efficiency Generation 3 CSP systems and the corresponding supercritical CO 2 (sCO 2 ) power cycle components (heat exchangers, piping, etc.). The high allowable stresses of alloy 740H also make it a desirable material for current Generation 2 CSP solar power receivers to improve cyclic capability and/or reduce receiver height. Recent experiences in demonstration projects utilizing alloy 740H identified cracking issues during welding and fabrication. In this project, a detailed study was done to confirm and clarify the Stress Relaxation Cracking (SRxC) mechanism, also known as stress relief cracking or strain-age cracking (SAC), during post-weld heat-treatment (PWHT). This involved detailed microscopy and advanced characterization to understand the root cause(s) of three failures obtained from industry. Based in-part on these findings, a targeted laboratory based SRxC test method was utilized to evaluate variables such as heat-to-heat variations, strain level, PWHT temperature, and starting material condition on three heats of alloy 740H. Industrial shop welding of cold-worked plates was also conducted. The research showed the following: SRxC was confirmed as the cracking mechanism for all field failures; Stress state (from residual stresses, constraint, deformation, and local stress concentrations) was playing a significant role in field failures and laboratory testing confirmed increasing susceptibility for all heats with increasing strain levels. High levels of microstructural strain were identified at crack initiation locations, in some cases leading to local recrystallization; Precipitate free zones (PFZs) at grain boundaries were found at relaxation cracks and crack initiation locations uniquely associated with SRxC in alloy 740H. Laboratory testing reproduced this microstructural feature which had only previously been reported in long-term creep testing of weldments. Advanced nano-scale characterization confirmed the presence of a moving boundary leading to coarsening of precipitates and PFZs where damage accumulated; The research suggested heat-to-heat variations due to local chemistry and processing may influence SRxC susceptibility, but more work is needed to fully clarify these effects. To disseminate the key learnings from this research to the scientific and engineering communities and alloy 740H end users, multiple technical publications and presentations were made, an industrial alloy 740H users meeting was held, and a new industry guideline specification document which can be directly implemented by end-users of alloy 740H was produced.

14 SOLAR ENERGY↗
DOE OSTI2024

Rapid assessment of the creep rupture life of metals: A model enabling experimental design

Prediction of the creep rupture life of engineering metals is critical for qualification and design of new materials. The use of long-term creep tests and the need to quantify the performance variability in a priori similar systems hinder the rapid creep assessment of a given material. Therefore, it is essential to develop methods that can extrapolate the long-term performance of alloys and the associated variability from short-term experiments. To this end, this study introduces a new model which enables the estimation of the rupture life of a material for a given stress and temperature. This model relies on two components. First, a new relation for the minimum creep rate (MCR) of materials is introduced. It includes a stress dependent stress exponent allowing the model to capture the variation of MCR across a wide range of temperatures and stresses. Second, employing the Monkman-Grant (MG) law, we establish a relation between stress, temperature and creep rupture life. Together, these two elements yield a new closed-form mathematical expression for the Larson Miller parameter as a function of stress and temperature. This expression captures the creep rupture time for many metals (Gr91, Copper, Gr122 and 347H) and compares favorably with alternate empirical approaches. The model is then used to assess the minimum duration of creep rates necessary to qualify the material up to 100000h. Furthermore, it is found that depending on the material system, creep tests as few as five limited to 5000 h for steels (Gr91, Gr122, 347H) and 100 h for copper are sufficient to model creep lifetimes. Finally, using a Bayesian inference-based approach to calibrate the model, we demonstrate that variability in rupture life can be captured via the quantification of the uncertainty in the model parameters and extrapolated from a limited number of short to moderately short creep tests; thereby paving the way for accelerated creep testing.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Understanding the effect of salt concentrations on fast charging performance of Li-ion cells

Here, different lithium salt (lithium bis(fluorosulfonyl) imide (LiFSI)/LiPF 6 9/1 mol ratio) concentrations in carbonate electrolyte were studied on the fast charging performance of LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622)/graphite pouch cells. The cells with electrolyte concentration from 0.75 M to 1.50 M showed similar fast charging capabilities. Further increase of the concentration to 1.75 M and 2.00 M decreased the attainable capacity in fast charging. In the long-term cycling test, the capacity retention after 200 fast charging cycles increased with the increase of salt concentration in electrolyte. Cells with 1.5 M electrolyte showed the best overall performance in fast charging capacity and long-term cycling. Li platings were observed in the cells with 0.75 M, 1.00 M and 1.25 M electrolyte. It was improved with greatly reduced Li plating area in 1.50 M, and no Li plating at all in 1.75 M and 2.00 M electrolyte. Post-mortem analysis such as neutron powder diffraction (NPD) and X-ray photoelectron spectroscopy (XPS) were used to characterize the electrode after cycling. It suggests that electrolyte concentration needs to be optimized for a given cell configuration with specific electrode and loading.

25 ENERGY STORAGE↗
DOE OSTI2023

Hanford Double Shell Waste Tank Corrosion Studies (Final Report)

For fiscal year (FY) 2022, the Savannah River National Laboratory (SRNL) focused on two experimental tasks related to Hanford Double Shell Tank (DST) chemistry and integrity. The first task focused on understanding risk of corrosion due to formation of either continuous layers or discrete patches of solids on the tanks' inner sidewalls and bottoms. The tank bottom solids contact corrosion testing focused on studying the effects of forming a dry adherent solids layer on a carbon steel substrate. Long-term exposure tests and electrochemical tests were performed to investigate the effect of drying (i.e., removing water) from the solids phase. The second task focused on corrosion of the exterior of the secondary liner. In previous years, vapor corrosion inhibitors (VCIs) were investigated as a means of mitigating corrosion of the exterior of the secondary liner. During FY22 the utilization of nitrogen was explored as a means of corrosion mitigation. The corrosion test results with nitrogen were compared with the corrosion mitigation performance of the VCIs.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2022

Development and performance of INCONEL® alloy 740H® seam-welded piping

INCONEL® alloy 740H® is an age-hardenable nickel-based alloy approved for pressure vessels and piping within ASME Section I, VIII, and B31.1. Currently, the code applies a weld strength reduction factor (WSRF) of 0.7 to the allowable stresses for longitudinal seam welds in the time dependent creep regime. In this work, a full-scale seam weld was successfully produced using typical industrial practices. The component was solution heat-treated and aged after fabrication to improve the performance of the weldment. Tensile, bend, impact, and low-cycle fatigue tests showed the component met all the specification requirements and elevated temperature properties were within base metal expectations with failures predominately in the weld metal. Long-term creep tests, including large samples more representative of the entire weldment, were fabricated and tested to times in excess of 10,000 h at multiple temperatures. Analysis of the creep data supports a WSRF of 0.9 for the solution annealed + aged weldments in contrast to the WSRF of 0.7 currently applied to welded + aged weldments. Metallurgical analysis shows that the solution annealing causes recrystallization of the weld metal and reduces the chemical compositional and microstructural gradients in the weldments resulting in acceptable short-term performance. In long-term creep, evidence for coarsened zones in the weldments due to discontinuous coarsening reactions were identified as the mechanism leading to accelerated creep damage formation in the weld metal and sample failure.

14 SOLAR ENERGY↗
DOE OSTI2024

A high-performance intermediate temperature reversible solid oxide cell with a new barrier layer free oxygen electrode

The best solution to address the critical durability issue of solid oxide electrolytic cells (SOECs) for high-efficiency and high-rate H 2 production is to lower the operating temperature without sacrificing the performance. Developing high performance oxygen electrodes (OEs) is a key to capitalizing this solution. Here, in this paper, we report on a highly active OE for intermediate temperature ZrO 2 -based SOECs without a CeO 2 barrier layer. The new barrier-layer-free (BLF) OE is a composite of two materials, (Bi 0.75 Y 0.25 ) 0.93 Ce 0.07 O 1.5±δ (BYC) that exhibits high oxide-ion conductivity and La 0.8 Sr 0.2 MnO 3 (LSM) that possesses a high electronic conductivity to enable fast oxygen reduction/evolution reactions (ORR/OER). Featuring a microscale porous BYC scaffold decorated with high surface area LSM nanoparticles (NPs), the new BLF-OE exhibited a low area specific resistance (ASR) of 0.10 Ω cm 2 at 650 °C in air. With 50%H 2 -50%H 2 O as a feed to hydrogen electrode (HE) and air to OE, the single cell performance achieved 588 mA cm -2 at 0.80 V in the fuel cell mode and 688 mA cm -2 at 1.30 V in the electrolytic mode at 650 °C. Our in-house testing showed that this level of performance was ~3.5x higher than the cell with the benchmark La 0.6 Sr 0.4 Co 0.2 Fe 0.8 O 3-δ -Ce 0.9 Gd 0.1 O 2-δ OE. The long-term durability testing under alternating fuel cell and electrolytic modes showed a low degradation rate of 0.10 mA cm -2 h -1 over 550 hours. These encouraging results showed the great promise of the newly developed BYC-LSM to be an excellent OE candidate for intermediate temperature SOECs.

25 ENERGY STORAGE↗