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Development of an Open-source Alloy Selection and Lifetime Assessment Tool for Structural Components in CSP

Lack of sufficient data on high temperature mechanical and corrosion behavior of structural materials is a huge barrier in the technological maturity of current and future Concentrating Solar Power (CSP) technologies. Rapid development and selection of materials cannot be achieved by expensive and time-consuming acquisition of experimental data. The goal of the proposed work is development of an open-source alloy selection and lifetime prediction tool that will integrate validated physics-based models to describe influence of temperature, alloy composition, environment and component geometry (thickness) on mechanical and corrosion behavior of Ni and Fe-based alloys employed in molten salts/sCO 2 heat exchangers. This one-year project leveraged the extensive dataset on the creep\corrosion behavior of candidate materials generated at ORNL through past projects and input from current collaborations with industrial partners. Based on previous experience and the feedback provided by industry (Brayton Energy and Echogen), three candidate materials of interest, Ni-based alloys 740H, 282 and 625 and application-specific operating conditions (max. temperature of 730 °C and stress of 150 MPa) were identified for the heat exchanger. An extensive corrosion and creep dataset was assimilated for the relevant operating conditions and was supported by detailed characterization of about 100 metallographic cross-sections. The corrosion dataset consisted of scanning electron microscopy images (secondary electron and backscatter electron), measured concentration profiles of alloying elements using energy dispersive X-ray spectroscopy (EDS), widths of denuded zones (dissolution of strengthening phases) and depths of attack in molten KCl-MgCl 2 mixtures using image analyses. The creep dataset comprised of creep rupture data and creep strain curves (for 740H and 282). Coupled thermodynamic-kinetic microstructure-based models were employed to predict the stress-corrosion induced compositional and phase evolutions in the alloy during operation under the identified operating conditions. Reduced order models were developed from advanced physics-based models and were integrated in a user-friendly alloy selection tool. The corrosion model was able to predict the time to a critical Cr concentration at the oxide/alloy interface (chemical lifetime) within ±10% (1 standard deviation) of typical statistical variation in corrosion tests and EDS measurement errors (±0.5 wt%). The initial scope of the project was limited to predict creep rupture times (Larson-Miller parameter). Based on the input provided by industry, the mechanical lifetime of the heat exchanger is governed by accumulated creep strains (2%) rather than creep rupture. To be able to predict the times to specific creep strains, a more extensive creep model development was undertaken largely beyond the initial scope of the project. The continuum damage mechanics creep model was able to predict times to 2% creep strain, t 2% with an accuracy of ±500h. Ultimately, a screening protocol for SiC was generated to demonstrate the pathway for integration of one of the currently immature materials from a commercial adoption standpoint in the current material evaluation tool. The modeling tool developed here is accessible to the science community and stakeholders and lays the foundation for methods that will enable a rapid evaluation of optimum materials for CSP applications and reliable prediction of material degradation thereby considerably reducing operational costs, improving reliability and increasing overhaul intervals. However, the complete potential of such a tool to include a wider range of materials and test conditions can only be realized with a more concentrated combined experimental-characterization-computation effort.

14 SOLAR ENERGY↗

AGC-1 Irradiation Induced Proprerty Changes Analysis Report: Electrical Resistivity and Coefficient of Thermal Expansion

Here we report the analysis of some of the test property data from the AGC-1 creep capsule. Specifically, we report analysis of the electrical resistivity (ER) and coefficient of thermal expansion (CTE). AGC-1 was operated at ~640°C and we measured the irradiated specimen CTE (α) over the temperature range 25°C to 550°C. Consequently, we have analyzed the mean CTE value for the temperature rage 25°C – 500°C. Both the ER and α(25-500°C) have been examined as a function of specimen dose (control specimens) and creep strain, %, (creep specimen). A direct comparison of the property changes has been made for the creep and control specimens by plotting their respective fractional changes as a function on neutron dose. Statistical “t” testing has been applied to any observed differences in property (ER or CTE) as a function of dose for the creep and control specimens of each graphite grade in the AGC-1 capsule. For electrical resistivity the irradiated value was shown to be greater than the unirradiated value for all graphite grades. However, the additional change due to creep strain was not found to be statistically significant. The coefficient of thermal expansion was seen to increase with dose for both the creep and control specimens. This increase was clearly seen in the fractional changes in CTE plot. The creep specimens were seen to increase their CTE above that noted for the control samples. The values of α(25-500°C) was statistically “t” tested and the differences between the creep and control CTE increases were shown to be statistically significant. Thus, creep strain is shown to have no additional effect upon ER but does increase the CTE over that observed from dose alone. The additional increase of CTE due to creep, is attributed to the closure of a larger fraction of the aligned porosity by compressive creep.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Progress report on the incorporation of lower lengthscales into polycrystal plasticity models - Part 2

Creep is the time-dependent, irreversible deformation that occurs at a low rate, at stresses below the ultimate stress of the material. Non-hydrostatic stresses (i.e. shear stresses) are required for creep. The kinds of creep relevant in cladding materials are (1) thermal creep, and (2) irradiation creep. These deformation processes require elevated temperatures, and applied stresses. Both processes are mediated by the motion of dislocations. Dislocations preferentially absorb either vacancies or interstitials, causing them to climb over obstacles. In thermal creep, the higher temperature causes high mobility of point defects, leading to a significant absorption rate of point defects by dislocations, leading to dislocation motion. In irradiation creep, the high radiation flux causes a supersaturation of point defects, that in turn leads to point defect absorption, and consequently dislocation motion. Irradiation growth is defined as the irradiation induced dimensional changes that take place in the absence of applied stresses, and is caused by the partitioning of vacancies and interstitials among two or more kinds of sinks. Each kind of sink produces strain in a different crystallographic direction, such that the final deformation is anisotropic, and is volume conserved. In this phenomenon, the high radiation flux causes the supersaturation of point defects. These point defects then tend to aggregate into dislocation loops (either interstitial of vacancy). These loops then absorb more point defects, thereby growing in size, and leading to macroscopic strain. The two phenomena of creep and growth become coupled in polycrystalline materials. Growth in a single grain is opposed by stresses caused by interaction of the growing grain with its neighbors (that are also growing, but it in different directions). These stresses initiate and/or potentiate irradiation creep. In extreme cases, such as accident scenarios, thermal creep becomes important. Internal stresses in turn affect the diffusive characteristics of point defects within a grain, and consequently affecting the phenomenon of growth. In this report, we examine the coupling between creep and growth in a polycrystalline materials, and also look at the atomistic mechanisms that contribute to these phenomena.

36 MATERIALS SCIENCE↗

Progress Report on Alloy 617 Time Dependent Allowables

Time dependent allowable stresses are required in the ASME Boiler and Pressure Vessel Code for design of components in the temperature range where time dependent deformation (i.e., creep) is expected to become significant. There are time dependent allowable stresses in Section IID of the Code for use in the non-nuclear construction codes, however, there are additional criteria that must be considered in developing time dependent allowables for nuclear components. These criteria are specified in Section III NH. St is defined as the lesser of three quantities: 100% of the average stress required to obtain a total (elastic, plastic, primary and secondary creep) strain of 1%; 67% of the minimum stress to cause rupture; and 80% of the minimum stress to cause the initiation of tertiary creep. The values are reported for a range of temperatures and for time increments up to 100,000 hours. These values are determined from uniaxial creep tests, which involve the elevated temperature application of a constant load which is relatively small, resulting in deformation over a long time period prior to rupture. The stress which is the minimum resulting from these criteria is the time dependent allowable stress St. In this report data from a large number of creep and creep-rupture tests on Alloy 617 are analyzed using the ASME Section III NH criteria. Data which are used in the analysis are from the ongoing DOE sponsored high temperature materials program, form Korea Atomic Energy Institute through the Generation IV VHTR Materials Program and historical data from previous HTR research and vendor data generated in developing the alloy. It is found that the tertiary creep criterion determines St at highest temperatures, while the stress to cause 1% total strain controls at low temperatures. The ASME Section III Working Group on Allowable Stress Criteria has recommended that the uncertainties associated with determining the onset of tertiary creep and the lack of significant cavitation associated with early tertiary creep strain suggest that the tertiary creep criteria is not appropriate for this material. If the tertiary creep criterion is dropped from consideration, the stress to rupture criteria determines St at all but the lowest temperatures.

36 MATERIALS SCIENCE↗

Demonstrate new plasticity models for doped UO 2 that capture dislocation mechanisms

In light water reactors, fuel vendors are investigating the use of dopants to modify the properties of UO 2 pellets, with the goal of improving pellet-cladding mechanical interactions during operation. Dopants are expected to ‘soften’ the pellets; that is, the doped pellets have higher plastic deformation than conventional UO 2 . This leads to a reduction in the severity of mechanical pellet-cladding interactions, helping to reduce the hoop strain on the cladding. By minimizing the strain exerted by the pellet on the cladding, it is anticipated that cladding performance under accident conditions can be enhanced (i.e., lowering the risk of burst during a LOCA). Dopants such as chromium (Cr) promote grain growth during pellet fabrication, leading to larger grains; therefore, understanding the link between chemistry, microstructure and mechanical deformation (enhanced creep rates) behavior of UO 2 is critical to helping operators further substantiate the benefits of doping UO 2 . Historically, the nuclear energy industry has relied on empirical models to make assessments of performance. Compared to empirical models, mechanistic physics-based models provide benefits, such as, fewer data points for validation and better extrapolation where experimental data is scarce or non-existent. In this report, Bayesian inference techniques have been applied to a previously developed lower length-scale-informed diffusional creep model. The objective is to i) infer lower-length-scale parameter distributions from available experiment and then ii) determine the uncertainties in the measurable quantity (in this case creep rates) after propagating the inferred lower length scale parameter uncertainties. The approach requires many evaluations of the model, which becomes computationally insurmountable; therefore, a neural-network model is trained to data obtained by sampling the full model over the most important parameters. This neural-network is then used in the Bayesian inference approach to determine probability distributions in the parameter values that represent the uncertainty in the model given what is known from the experiments (posterior). A significant reduction compared to conservative initial (prior) uncertainties is achieved through inference against the experimental data, demonstrating the efficacy of this approach. Furthermore, by accounting for uncertainties in the experimental conditions and sample non-stoichiometry, it is possible to resolve apparent discrepancies in experimental measurements within a self-consistent grain boundary (Coble) creep model that is sensitive to chemistry. This work has been written up and submitted to Nuclear Technology for a special issue on accelerated fuel qualification (AFQ). This uncertainty quantification (UQ) work not only improves the diffusional model, while accounting for uncertainty, but also establishes a framework which can readily be applied to the mechanistic models of dislocation deformation developed in this study. The most likely values from the Bayesian analysis are incorporated into our UO 2 diffusional creep model and a lower length scale-informed irradiation UO 2 creep mechanistic model to generate a dataset. This dataset has been provided to our INL collaborators for training an artificial neural network surrogate model, which will be implemented in the BISON fuel performance code to assess how the results differ from those currently obtained using a fully empirical model and that of using the nominal (uncalibrated) atomic scale parameters in our mechanistic model. Plastic deformation (creep and glide) in UO 2 is a complex phenomenon, governed by multiple underlying processes such as local defect concentrations, applied stresses, and microstructural characteristics. Consequently, there is a need for a meso-scale model with polycrystalline resolution capable of extrapolating to large grain sizes applicable to doped UO 2 , where data is limited and the model can help bridge the knowledge gap. By integrating atomistic data into the polycrystal LApx code, it becomes possible to predict dislocation climb and glide plasticity that simple analytical models cannot accurately represent. The application of atomic-scale data within LApx demonstrated the importance of climb and glide mechanisms in reproducing high-stress UO 2 behavior. Behaviors such as this are crucial to capture and implement in BISON, as parts of the fuel pellet can reach temperatures where glide can occur before pellet cracking. This model which captures dislocation based mechanisms for UO 2 is then used to stand up the doped model accounting for larger grain sizes. It was found that larger grain sizes can lead to enhanced deformation rates in the glide regime, and therefore can help with the pellet cladding mechanical interaction. Therefore if the fuel pellet reaches conditions (stress/temperature) where glide is active, the enhanced creep rates for larger grains in the glide regime (doped UO 2 ) can help with pellet cladding mechanical interactions. Plastic deformation in UO 2 involves multiple mechanisms, including diffusional creep, dislocation climb, and glide. This milestone contains two parts: (1) UQ of a pre-existing lower length scale informed mechanistic diffusional creep model, and (2) development of a new LApx based model for dislocation-mediated creep mechanisms in UO 2 , with application to large-grain doped UO 2 .

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

The International Space Station Assembly on Schedule

As engineers continue to prepare the International Space Station (ISS) for in-orbit assembly in the year 2002, ANSYS software has proven instrumental in resolving a structural problem in the project's two primary station modules -- Nodes 1 and 2. Proof pressure tests performed in May revealed "low temperature, post-yield creep" in some of the Nodes' gussets, which were designed to reinforce ports for loads from station keeping and reboost motion of the entire space station. An extensive effort was undertaken to characterize the creep behavior of the 2219-T851 aluminum forging material from which the gussets were made. Engineers at Sverdrup Technology, Inc. (Huntsville, AL) were responsible for conducting a combined elastic-plastic-creep analysis of the gussets to determine the amount of residual compressive stress which existed in the gussets following the proof pressure tests, and to determine the stress-strain history in the gussets while on-orbit. Boeing, NASA's Space Station prime contractor, supplied the Finite Element Analysis (FEA) model geometry and developed the creep equations from the experimental data taken by NASA's Marshall Space Flight Center and Langley Research Center. The goal of this effort was to implement the uniaxial creep equations into a three dimensional finite element program, and to determine analytically whether or not the creep was something that the space station program could live with. The objective was to show analytically that either the creep rate was at an acceptable level, or that the node module had to be modified to lower the stress levels to where creep did not occur. The elastic-plastic-creep analysis was performed using the ANSYS finite element program of ANSYS, Inc. (Houston, PA). The analysis revealed that the gussets encountered a compressive stress of approximately 30,000 pounds per square inch (psi) when unloaded. This compressive residual stress significantly lowered the maximum tension stress in the gussets which decreased the creep strain rate. The analysis also showed that the gussets would not experience a great deal of creep from future pressure tests if braces or struts proposed by Boeing were installed to redistribute stress away from them. Subsequent analysis of on-orbit station keeping and reboost loads convinced Boeing that the gussets should be removed altogether.

Source record↗

Effect of moderate magnetic annealing on the microstructure, quasi-static and viscoelastic mechanical behavior of a structural epoxy

In this study the effect of moderate magnetic fields on the microstructure of a structural epoxy system was investigated. The changes in the microstructure have been quantitatively investigated using wide angle x-ray diffraction (WAXD) and pole figure analysis. The mechanical properties (modulus, hardness and strain rate sensitivity parameter) of the epoxy system annealed in the magnetic field were probed with the aid of instrumented nanoindentation and the results are compared to the reference epoxy sample. To further examine the creep response of the magnetically annealed and reference samples, short 45 min duration creep tests were carried out. An equivalent to the macro scale creep compliance was calculated using the aforementioned nano-creep data. Using the continuous complex compliance (CCC) analysis, the phase lag angle, tan (δ), between the displacement and applied force in an oscillatory nanoindentation test was measured for both neat and magnetically annealed systems through which the effect of low magnetic fields on the viscoelastic properties of the epoxy was invoked. The comparison of the creep strain rate sensitivity parameter , A/d(0), from short term(80 ), creep tests and the creep compliance J(t) from the long term(2700 s) creep tests with the tan(δ) suggests that former parameter is a more useful comparative creep parameter than the creep compliance. The results of this investigation reveal that under low magnetic fields both the quasi-static and viscoelastic mechanical properties of the epoxy have been improved.

36 MATERIALS SCIENCE↗

Fuel Performance Modeling Results for Representative FCRD Irradiation Experiments: Projected Deformation in the Annular AFC-3A U-10Zr Fuel Pins and Comparison to Alternative Designs

The objective of the present study was to predict the outcome of the AFC-3A annular U-10Zr fuel irradiation experiment. Specifically, the study attempted to predict whether the annular fuel will swell inward and fill the annulus, or swell outward resulting in an undesirable cladding deformation. It was predicted that both 55% and 75% annular fuels operating at 350 W/cm for 201 days will swell inward and partially fill the annulus which signifies a positive outcome of the experiment. The driving mechanism for such behavior is the fuel creep under the compressive stress exerted on the fuel by the cladding as a result of the fuel cladding mechanical interaction. Comparison with the solid fuel revealed that the annular fuel is expected to swell less early in life due to the mechanical constraint provided by the cladding. Furthermore, mechanical constraint is expected to yield a marked reduction of the axial elongation of the annular fuel as compared to the solid fuel. The prediction is based on the assumption that the annular fuel is not capable of moving axially relative to the cladding after the two come in contact. Post irradiation examination results would be very useful to assess the validity of this assumption. Specifically, underprediction of the axial growth would point to the fact that some slippage of the fuel relative to the cladding occurs after the onset of the FCMI. As fuel creep plays the major role in the deformation of the annular fuel, the contributions from the thermal and irradiation induced creep to the total creep rate of fuel were examined to provide guidance for possible creep testing experiments of the fuel (separate effect tests). It was found that irradiation induced creep dominates deformation of the fresh fuel at low temperatures. At high temperatures, and in the case of porous fuel, the thermal creep of the fuel becomes dominant and irradiation induced creep can be neglected. Fission gas induced porosity seems to accelerate fuel creep drastically. Recognizing the sensitivity of the fuel creep to the porosity, additional studies exploring this phenomenon and verifying published equations either experimentally or through computation may benefit the understanding of the annular fuel behavior.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Assessment of a Grade 91 Steel Forging and Seamless Pipe Section After 141,000-Hours of Operation in a Superheat Outlet Header

In this work, two unique heats of 9Cr creep strength enhanced ferritic (CSEF) steels extracted from a retired superheat outlet header after 141,000 hours of service were evaluated. These two CSEF steels were a forging manufactured to SA-182 F91 (F91) reducer and a seamless pipe produced to SA-335 P91 (P91) pipe. Their creep deformation and fracture behavior were assessed using a lever arm creep frame integrated with in-situ high-temperature digital image correlation (DIC) system. Critical metallurgical and microstructure factors, including composition, service damage, grain matrix degradation, precipitates, and inclusions were quantitatively characterized to link the performance of the two service aged F91 and P91 CSEF steels. The creep test results show the F91 and P91 steels exhibit a large variation in creep strength and creep ductility. The F91 steel fractured at 572 hours while P91 steel fractured at 1,901 hours when subjected to a test condition of 650 °C and 100 MPa. The nominal creep strains at fracture were 12.5% (F91) and 14.5% (P91), respectively. The high-resolution DIC strain measurements reveal the local creep strain in F91 was about 50% while the local creep strain in P91 was >80%. The characterization results show that the F91 steel possessed pre-existing creep damage from its time in service, a higher fraction of inclusions, and a faster matrix grain coarsening rate. These features contribute to the observed reduction in performance for the F91 steel. The context for these findings, and the importance of metallurgical risk in an integrated life management approach will be emphasized.

Wang, Yiyu↗

Methods for structural design at elevated temperatures

A procedure which can be used to design elevated temperature structures is discussed. The desired goal is to have the same confidence in the structural integrity at elevated temperature as the factor of safety gives on mechanical loads at room temperature. Methods of design and analysis for creep, creep rupture, and creep buckling are presented. Example problems are included to illustrate the analytical methods. Creep data for some common structural materials are presented. Appendix B is description, user's manual, and listing for the creep analysis program. The program predicts time to a given creep or to creep rupture for a material subjected to a specified stress-temperature-time spectrum. Fatigue at elevated temperature is discussed. Methods of analysis for high stress-low cycle fatigue, fatigue below the creep range, and fatigue in the creep range are included. The interaction of thermal fatigue and mechanical loads is considered, and a detailed approach to fatigue analysis is given for structures operating below the creep range.

Ellison, A. M.↗

Superplastic Deformation of ice: Experimental Observations

Creep experiments on fine-grained ice reveal the existence of three creep regimes: (1) a dislocation creep regime; (2) a superplastic flow regime in which grain boundary sliding is an important deformation process; and (3) a basal slip creep regime in which the strain rate is limited by basal slip. Dislocation creep in ice is likely climb-limited, is characterized by a stress exponent of 4.0, and is independent of grain size. Superplastic flow is characterized by a stress exponent of 1.8 and depends inversely on grain size to the 1.4 power. Basal slip limited creep is characterized by a stress exponent of 2.4 and is independent of grain size. A fourth creep mechanism, diffusional flow, which usually occurs at very low stresses, is inaccessible at practical laboratory strain rates even for our finest grain sizes of approximately 3 micrometers. A constitutive equation based on these experimental results that includes flow laws for these four creep mechanisms is described. This equation is in excellent agreement with published laboratory creep data for coarse-grained samples at high temperatures. Superplastic flow of ice is the rate-limiting creep mechanism over a wide range of temperatures and grain sizes at stresses less than or equal to 0.1 MPa, conditions which overlap those occurring in glaciers, ice sheets, and icy planetary interiors.

Goldsby, D. L.↗

Characterization of long-term extension of isolated cell walls from growing cucumber hypocotyls

Walls from frozen-thawed cucumber (Cucumis sativus L.) hypocotyls extend for many hours when placed in tension under acidic conditions. This study examined whether such "creep" is a purely physical process dependent on wall viscoelasticity alone or whether enzymatic activities are needed to maintain wall extension. Chemical denaturants inhibited wall creep, some acting reversibly and others irreversibly. Brief (15 s) boiling in water irreversibly inhibited creep, as did pre-incubation with proteases. Creep exhibited a high Q10 (3.8) between 20 degrees and 30 degrees C, with slow inactivation at higher temperatures, whereas the viscous flow of pectin solutions exhibited a much lower Q10 (1.35). On the basis of its temperature sensitivity, involvement of pectic gel-sol transitions was judged to be of little importance in creep. Pre-incubation of walls in neutral pH irreversibly inactivated their ability to creep, with a half-time of about 40 min. At 1 mM, Cu2+, Hg2+ and Al3+ were strongly inhibitory whereas most other cations, including Ca2+, had little effect. Sulfhydryl-reducing agents strongly stimulated creep, apparently by stabilizing wall enzyme(s). The physical effects of these treatments on polymer interactions were examined by Instron and stress-relaxation analyses. Some treatments, such as pH and Cu2+, had significant effects on wall viscoelasticity, but others had little or no apparent effect, thus implicating an enzymatic creep mechanism. The results indicate that creep depends on relatively rugged enzymes that are firmly attached to or entangled in the wall. The sensitivity of creep to SH-reducing agents indicates that thiol reduction of wall enzymes might provide a control mechanism for endogenous cell growth.

NASA Program Space Biology↗

Quarterly Management Document – FY22, 1st Quarter, Multi-pass Hybrid Laser Arc Welding of Alloy 740H

This report summarizes the progress made on the project during the first quarter of FY22. The model for deep penetration laser welding continues to be developed to understand and mitigate cracking issues associated with laser welding Alloy 740H. The effects of laser wobble on laser welding of this alloy are also being developed. Additionally, the short-term creep behavior of welds made by various hybrid laser arc parameters has been obtained and the results indicate they are comparable to welds made by conventional gas tungsten arc welding which is a factor 2 slower than the hybrid welds. Additionally, the creep behavior of laser-only welds is also consistent with conventional gas tungsten arc welds as well as the hybrid laser arc welds made under this project. However, the creep rate of the laser-only welds is much higher than that observed in the hybrid laser arc welded specimens. This is most likely due to the narrower weld produced by laser-only welding compared to hybrid laser arc welding and, thus, the higher creep rate of laser-only welded creep specimens is likely a result of the increased fraction of base metal (which exhibits a higher creep rate than weld metal) contained within the gage section of the creep specimen. Creep rupture lifetimes were all about the same for both laser-only and hybrid laser arc welded specimens and consistent with the creep rupture lifetime of conventional gas tungsten arc welded creep specimens.

36 MATERIALS SCIENCE↗

AGC-4 Graphite Preirradiation Data Analysis Report

The Advanced Reactor Technology (ART) Graphite R&D program is conducting an extensive graphite irradiation program to provide data for licensing of a high temperature reactor (HTR) design. In past applications, graphite has been used effectively as a structural and moderator material in both research and commercial high temperature gas cooled reactor (HTGR) designs. Nuclear graphite H 451, used previously in the United States for nuclear reactor graphite components, is no longer available. New nuclear graphite grades have been developed and are considered suitable candidates for new HTR reactor designs. To support the design and licensing of new HTR core components within a commercial reactor, a complete properties database must be developed for these current grades of graphite. Quantitative data on in service material performance is required for the physical, mechanical, and thermal properties of each major graphite grade with a specific emphasis on data accounting for the life limiting effects of irradiation creep on key physical properties of the HTR candidate graphite grades. Further details on the research and development activities and associated rationale required to qualify nuclear grade graphite for use within the HTR are documented in the graphite technology research and development plan. Based on experience with previous graphite core components, the phenomenon of irradiation induced creep within the graphite has been shown to be critical to the total useful lifetime of graphite components. Irradiation induced creep occurs under the simultaneous application of high temperatures, neutron irradiation, and applied stresses within the graphite components. Significant internal stresses within the graphite components can result from a second phenomenon—irradiation induced dimensional change—where the graphite physically changes (i.e., first shrinking and then expanding with increasing neutron dose). This disparity in material volume change can produce significant internal stresses within graphite components. Irradiation induced creep relaxes these large internal stresses, thus reducing the risk of crack formation and component failure. Obviously, higher irradiation creep levels tend to relieve more internal stress, thus allowing the components longer useful lifetimes within the core. Determining the irradiation creep rates of nuclear grade graphite is critical for determining the useful lifetime of graphite components and is a major component of the Advanced Graphite Creep (AGC) experiment. The AGC experiment is currently underway to determine the in service behavior of these new graphite grades for HTR and molten salt reactor designs. This experiment will examine properties and behavior of nuclear grade graphite over a large spectrum of temperatures, irradiation fluencies and applied stress levels that are expected to cause irradiation creep strains within a HTR graphite component. Irradiation data are provided through the AGC test series, which is comprised of six planned capsules irradiated in the Advanced Test Reactor (ATR) in a large flux trap located at Idaho National Laboratory (INL). Each irradiation capsule consists of over 400 graphite specimens that are characterized before and after irradiation to determine the irradiation induced material properties changes and life-limiting irradiation creep rate for each graphite grade.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Resolution of Qualification Issues for Existing Structural Materials

This report gives a detailed assessment of several key technical issues that needs resolution for the existing structural materials with emphasis on application in liquid metal reactors (LMRs), in particular, sodium cooled fast reactors. The work is a combined effort between Argonne National Laboratory (ANL) and Oak Ridge National Laboratory (ORNL) with ANL as the technical lead, as part of Advanced Structural Materials Program for the Advanced Fuel Cycle Initiative (AFCI) Reactor Campaign. The report is the second deliverable in FY09 (M2505050201) under the work package “Advanced Materials Code Qualification”. The overall objective of the Advanced Materials Code Qualification project is to evaluate the key technical requirements for the qualification of currently available and future advanced materials for application in sodium reactor systems and the resolution of issues that the U.S. Nuclear Regulatory Commission (NRC) has raised in the past on structural materials in support of the design and licensing of the LMR. Advanced materials are a critical element in the development of sodium reactor technologies. Enhanced materials performance not only improves safety margins and provides design flexibility, but also is essential for the economics of future advanced sodium reactors. Qualification and licensing of advanced materials are prominent needs for developing and implementing advanced sodium reactor technologies. However, the development of sufficient database and qualification of these materials for application in LMRs require considerable amount of time and resources. In the meantime, the currently available materials will be used in the early development of fast reactors. Nuclear structural component designs in the U.S. comply with the ASME Boiler and Pressure Vessel Code Section III (Rules for Construction of Nuclear Facility Components) and the NRC grants licensing. As the LMR will operate at higher temperatures than the current light water reactors (LWRs), the design of elevated-temperature components must comply with ASME Section III Subsection NH (Class 1 Components in Elevated Temperature Service). Assessment of materials performance issues and high temperature design methodology issues pertinent to the LMR were presented in an earlier report (Natesan et al. 2008). In a subsequent report (Majumdar et al. 2009), we addressed the needs in high temperature methodologies for design of various high temperature components in sodium cooled fast reactor. The present report addresses several key technical issues for the currently available structural materials such as Type 304 and 316 austenitic stainless steels and ferritic steels such as 2.25Cr-1Mo and modified 9Cr-1Mo. The 60-year design life for the LMR presents a significant challenge to the development of database, extrapolation/prediction of long-term performance, and high temperature structural design methodology. The current Subsection NH is applicable to the design life only up to 34 years. No experimental data contain test durations of 525,000 hours, and it is impractical to conduct such long-term tests in any types of testing. So far the longest creep tests for Grade 91 and Grade 92 steels have run up to 100,000 hours. It has been noted that there is a large drop in creep rupture strength in long-term tests for these high-Cr creep-resistant steels, which may result in overestimation of the long-term creep strength and allowable stress. The report addresses in detail the need for a mechanistic understanding of the structural materials, from the standpoint of the effects of thermal aging, creep deformation, creep fracture, fatigue and creep-fatigue, creep-fatigue predictive models, fatigue and creep crack growth, and fracture toughness. Based on an in-depth assessment of the available data and mechanistic understanding, key technical issues are identified and discussed for each of the property areas. Furthermore, we have proposed viable approaches to resolve the issues and prioritized our recommendations.

Natesan, K.↗

Effect of the Addition of a Low Equivalent Stress Mechanism to the Analysis of Geomechanical Behavior of the SPR West Hackberry Site

Sandia National Laboratories has long used the Munson-Dawson (M-D) model to predict the geomechanical behavior of salt caverns used to store oil at the Strategic Petroleum Reserve (SPR). Salt creep causes storage caverns to deform inward, thus losing volume. This loss of volume affects the salt above and around the caverns, puts stresses and strains on borehole casings, and creates surface subsidence which affects surface infrastructure. Therefore, accurate evaluation of salt creep behavior drives decisions about cavern operations. Parameters for the M-D model are typically fit against laboratory creep tests, but nearly all historic creep tests have been performed at equivalent stresses of 8 MPa or higher. Creep rates at lower equivalent stresses are very slow, such that tests take months or years to run, and the tests are sensitive to small temperature perturbations (<0.1°C). A recent collaboration between US and German researchers, recently characterized the creep behavior at low equivalent (deviatoric) stresses (<8 MPa) of salt from the Waste Isolation Pilot Plant. In addition, the M-D model was recently extended to include a low stress creep “mechanism”. This paper details new simulations of SPR caverns that use this extended M-D model, called the M-D Viscoplastic model. The results show that the inclusion of low stress creep significantly alters the prediction of steady-state cavern closure behavior and indicate that low stress creep is the dominant displacement mechanism at the dome scale. The implications for evaluating cavern and well integrity are demonstrated by investigating three phenomena: the extent of stress changes around the cavern; the predicted vertical strains applied to wellbore casings; and the evaluation of oscillating stress changes around the cavern due to oil sale cycles and their potential effect on salt fatigue.

58 GEOSCIENCES↗

Complete Optimization of LPBF Ni-Based Alloys Down-Selected from FY23 Candidate Materials Including, Thermodynamic Modeling, Sample Fabrication and Microstructure Characterization

The goal of the Advanced Materials and Manufacturing Technologies (AMMT) program is to accelerate the incorporation of new materials and manufacturing technologies into advanced nuclear-related systems. Although 316H stainless steel fabricated by laser powder bed fusion (LPBF) has already been identified as an alloy that could have a significant effect on various reactor technologies, many other materials and manufacturing techniques are being evaluated. Nickel-based alloys typically offer higher-temperature capabilities compared with advanced stainless steels, and previous reports looked at three Ni-based alloy categories: low-Co alloys with a potential use close to the reactor core; high-temperature, high-strength alloys; and molten salt–compatible alloys. In the first category, alloy 718 was studied in 2023, and creep testing at 600°C and 650°C revealed that the alloy exhibited great creep strength after the appropriate annealing but had low ductility. Advanced characterization was recently conducted to highlight the presence of strengthening γ' and γ" precipitates after creep testing and to show that brittle phases at grain boundaries might explain the low ductility of LPBF 718 compared with wrought 718. For the high-temperature, high-strength alloys, previously purchased powders of alloys 617, 230, and 625 were used to assess the printability of these three solution-strengthened alloys. Hot cracking could not be suppressed for alloy 617 and 230, and it was shown that these cracks, which were elongated along the build direction (BD), had a drastic effect on the ductility of alloy 230 at room temperature when specimens were machined perpendicular to the BD. On the contrary, LPBF printing of crack-free alloy 625 was achieved using similar printing parameters, and the alloy looked like a promising candidate for various reactor technologies. The fabrication of alloy 282 by LPBF, a γ'-strengthened alloy with great creep strength up to 800°C, was performed in 2023, and x-ray computed tomography (XCT) scans of the alloy before and after creep testing at 750°C were carried out to assess the effect of flaws on the alloy’s creep behavior. Correlation between the flaws’ volume fraction, creep ductility, and creep lifetime could be established, and future work on LPBF 625 will take full advantage of in situ printing data and ex situ XCT scans to accelerate the alloy qualification. Finally, single track experiments were performed on the two alloys previously identified as good molten salt–resistant, Ni-based candidates: Hastelloy N and 244. Various laser parameters were considered, and cracking was not observed for either of the two alloys. Wrought 244 offers better creep strength and molten salt compatibility than alloy 625, and future work will aim to establish the alloy LPBF processing window.

36 MATERIALS SCIENCE↗

The Combined Influence of Molecular Weight and Temperature on the Aging and Viscoelastic Response of a Glassy Thermoplastic Polyimide

The effect of molecular weight on the viscoelastic performance of an advanced polymer (LaRC-SI) was investigated through the use of creep compliance tests. Testing consisted of short-term isothermal creep and recovery with the creep segments performed under constant load. The tests were conducted at three temperatures below the glass transition temperature of five materials of different molecular weight. Through the use of time-aging-time superposition procedures, the material constants, material master curves and aging-related parameters were evaluated at each temperature for a given molecular weight. The time-temperature superposition technique helped to describe the effect of temperature on the timescale of the viscoelastic response of each molecular weight. It was shown that the low molecular weight materials have higher creep compliance and creep rate, and are more sensitive to temperature than the high molecular weight materials. Furthermore, a critical molecular weight transition was observed to occur at a weight-average molecular weight of M (bar) (sub w) 25000 g/mol below which, the temperature sensitivity of the time-temperature superposition shift factor increases rapidly. The short-term creep compliance data were used in association with Struik's effective time theory to predict the long-term creep compliance behavior for the different molecular weights. At long timescales, physical aging serves to significantly decrease the creep compliance and creep rate of all the materials tested.

Nicholson, Lee M.↗