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NASA NTRS1998

Factors Affecting Fiber Design and Selection for Advanced Ceramic Composites

Structural Ceramic Matrix Composites (CMC) have the potential for application in the hot sections of a variety of advanced propulsion and power systems. It is therefore necessary to have a general understanding of the key properties of CMC and Reinforcing Fibers. This need is complicated by the wide variety of application conditions and structural requirements for which CMC's will be used, and the proprietary concerns of the design engineers. CMC's, to be successful, must display properties which are competitive with the currently used high temperature structural materials: (i.e., Iron and Nickel based superalloys, tough monolithic ceramics, and carbon/carbon composites.) Structural CMC offers several areas of competition: (1) performance, (i.e., strength and strength retention, creep resistance, and thermal conductivity), (2) reliability (i.e., environmental durability, and damage tolerance) and (3) processing (i.e., capability for varying sizes and shapes, and cost effective fabrication). The presentation further discusses, and illustrates with fiber and CMC data the key fiber properties and processes which strongly affect each CMC area of competition. The presentation further discusses the current knowledge of the important factors which control the key fiber properties. A design guidelines for the optimum fiber characteristics is developed, and the currently available fibers are compared against those guidelines.

DiCarlo, James A.↗

NASA NTRS2006

Non-Contact Measurements of Creep Properties of Refractory Materials

State-of-the-art technologies for hypersonic aircraft, nuclear electric/thermal propulsion for spacecraft, and more efficient jet engines are driving ever more demanding needs for high-temperature (>2000 C) materials. At such high temperatures, creep rises as one of the most important design factors to be considered. Since conventional measurement techniques for creep resistance are limited to about 17OO0C, a new technique is in demand for higher temperatures. This paper presents a non-contact method using electrostatic levitation (ESL) which is applicable to both metallic and non-metallic materials. The samples were rotated quickly enough to cause creep deformation by centrifugal acceleration. The deformation of the samples was captured with a high speed camera and then the images were analyzed to estimate creep resistance. Finite element analyses were performed and compared to the experiments to verify the new method. Results are presented for niobium and tungsten, representative refractory materials at 2300 C and 2700 C respectively.

Lee, Jonghyun↗

DOE OSTI2023

Review of HAYNES® 282® alloy for supercritical CO2 structural applications

In this paper, HAYNES® 282® alloy (282® alloy) properties, microstructure, high temperature oxidation resistance, weldability, and American Society of Mechanical Engineers (ASME) code case highlights are reviewed. The long term performance of high temperature, high strength, creep resistant alloys is critical to the success of supercritical carbon dioxide equipment. Several modern power generation technologies require alloys that can operate continuously at or above 700oC. 282® alloy is a precipitation strengthened nickel based super alloy that meets these requirements. The results of 282® alloy research reviewed in this paper include longterm cyclic oxidation behavior in air and sCO2, independent research and validation of 100k hour creep life, and successful welding of the alloy in the age hardened condition. The latter is critical for joining of hardened components (flanges, piping, heat exchanger internal, etc.) and field repair. Several highlights from the code case for this ASMEapproved material are also presented.

Tossey, Brett↗

DOE OSTI2025

Step-loaded creep testing of Zircaloy-4 cladding at higher temperatures in the α-phase

A refined understanding of zirconium-based cladding thermomechanical performance during rapid transients is essential for enhancing the safety and operation of light-water reactors. Traditional models for zirconium alloys under accident conditions generally assume that creep dominates fuel cladding performance. Here, these historic models have largely remained unchanged and serve as the basis for safety criteria development. As the U.S. nuclear industry pursues higher burnup levels, the increased release of fission gases during transients raises the risk of cladding failure in the low-temperature hcp α-phase, making the fidelity of these models of greater importance. Creep testing was conducted from 550–700°C with 25–120 MPa applied hoop stresses to investigate Zircaloy-4 deformation at accident-relevant temperatures in the α-phase. Step-loading was employed to capture creep behavior across a wide stress range from a single sample. The stress-strain rate data at higher temperatures (650 and 700°C) were well-described by isotropic versions of the Erbacher and Kaddour models, while the lower temperature data (550 and 600°C) were underpredicted by both anisotropic and isotropic model variants. Greater strain rates during the initial loading step at 650 and 700°C were attributed to recrystallization and grain growth of sub-micron crystallites. Yet, texture analysis revealed the basal split texture remained after testing. These observations produced results suggesting Zircaloy-4 claddings experience higher creep rates across the α-phase than previously thought, possibly related to dynamic anisotropy due to temperature dependent activation of deformation mechanisms, effects of biaxial loading, and variation in material condition between the current testing used in previous model development.

36 MATERIALS SCIENCE↗

NASA NTRS1993

The effects of stress and physical aging on the creep compliance of a polymeric composite

An experimental study was performed to determine the effects of stress and physical aging on the matrix dominated viscoelastic properties of IM7/8320, a high temperature fiber reinforced thermoplastic composite. Established creep/aging test techniques developed for polymers were adapted for testing of the composite material. The transverse and shear compliance for an orthotropic plate were found from creep compliance measurements at constant, sub-Tg temperatures. These compliance terms were shown to be effected by physical aging. Aging time shift factors and shift rates were found to be a function of applied stress.

Gates, Thomas E.↗

DOE OSTI2020

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

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

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

NASA NTRS1977

Stiffness and damping characteristics of aluminum in creep

Tensile creep tests conducted at 200 C were performed on annealed commercially pure aluminum specimens in order to measure the dominant elevated temperature dislocation processes. Testing consisted of applying small lateral loads to measure flexural stiffness, and vibrating the specimens laterally in order to measure dynamic modulus and internal damping. It was concluded that (1) the strain hardening increased static stiffness and decreased internal damping during early creep, and (2) the dynamic modulus remained essentially constant at the elastic value during creep. These results imply that primary creep may constitute a mechanism of recovery of dislocatory disorder induced by yielding the material during loading, and that the inelastic modulus utilized as a mathematical concept in several creep buckling theories is not a directly measurable material property.

Berkovits, A.↗

NASA NTRS1980

Effects of thermally induced porosity on an as-HIP powder metallurgy superalloy

The effect of thermally induced porosity on the mechanical properties of an as-hot-isostatically pressed and heat-treated pressing made from low carbon Astroloy is examined. Tensile, stress-rupture, creep, and low cycle fatigue tests were performed and the results were compared with industrial acceptance criteria. It is shown that the porous pressing has a porosity gradient from the rim to the bore with the bore having 1-1/2% greater porosity. Mechanical properties of the test ring below acceptance level are tensile reduction in area at room temperature and 538 C and time for 0.1% creep at 704 C. It is also found that the strength, ductility, and rupture life of the rim are slightly inferior to those of the rim of the sound pressings, while those of the bore are generally below the acceptable level. At strain ranges typical of commercial aircraft engines, the low cycle fatigue life of the rim of the porous pressings is slightly lower than that of the sound pressings.

Dreshfield, R. L.↗

DOE OSTI2020

Irradiation enhanced diffusion and diffusional creep in U₃Si₂

U₃Si₂ is a candidate as an advanced fuel for light water reactors (LWRs). Compared to UO₂, there are significant data gaps for the thermophysical and thermomechanical properties of U₃Si₂. Atomic scale simulations can help fill in those gaps, while also providing a more mechanistic understanding of the material properties. Creep is an important property for fuel performance as it influences the pellet-cladding gap, which in turn affects the temperature of the fuel (a key parameter in many other aspects of fuel behavior). In this work, we employed a DFT-informed cluster dynamics framework to predict point defect concentrations in U₃Si₂. The concentrations, diffusivities, and volumes of these defects were used to develop a diffusional creep model based on bulk (Nabarro-Herring) and grain boundary (Coble) diffusion processes. It was found that irradiation enhanced Nabarro-Herring creep is dominant at low temperatures, while Coble creep dominates for high temperatures. The model compares well against available experimental data and has been implemented in BISON. A demonstration case using simple power profiles has been carried out, showing that negligible creep occurs due to the low temperatures experienced by U₃Si₂, a consequence of its high thermal conductivity.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2022

H-Canyon Jumper Gasket Sealing Evaluation

H-Canyon Documented Safety Analysis approved December 2019 credits the leak integrity of H-Canyon (HCA) process tanks, piping, and jumpers in preventing the release of radioactive material in a post seismic environment. Demonstration of leak tightness capability for this equipment was achieved through substantial analytical effort. However, one potential weak point that affects leak integrity exists at the gasketed joint between Hanford Connectors (HC) and nozzles. Review of the HCA Crane Log over a three-year period indicates the HCs periodically leak. Savannah River National Laboratory (SRNL) was requested to perform gasket compression tests that evaluate gasket relaxation characteristics, i.e., creep, and provide improvements to the HC installation process that can reduce or eliminate the frequency of leaks at HCs. A HC torque value of 312 ft-lbf is the target value used because it is the minimum torque value, with 95% confidence, when an unlubricated HC is impacted for standard sealing period of 9 seconds. In the HCA pipe-jumper connections are installed remotely by using HCs. HCs inherently add to the uncertainty of a gasketed joint because a calibrated torque value cannot be applied. The gasket material is a special material made of asbestos-fiber impregnated with Teflon. This material has been used for decades and generally performs well but does leak intermittently as gaskets creep and preloaded torque is lost. Gasket types are either snap-ring (SR) or lampshade (LS). Both gasket types cover the same seating area. The SR gasket is designed to remain with the jumper when the jumper is removed leaving the nozzle faces clean of any debris. SR gaskets are initially installed when the jumper is fabricated. Changing gaskets is time consuming and the radioactive environment presents risks to personnel. When jumpers are removed LS gaskets could be used to better seal the connection to reduce down time and ALARA concerns. That is, an LS gasket would be remotely positioned over the nozzle and the HC reinstalled. Testing also included two situations not typical of plant operation. One situation was the use of the non-standard double-layered gaskets (DG), and the other situation was the use of a LS without removal of the installed SR gasket. The DG was used when the supply of LS gaskets ended, so that testing could continue. It was of interest to demonstrate this gasket’s creep response because the DG, which was two gaskets glued together, was thicker than the LS gasket and the thicker material was expected to elicit a greater creep characteristics. The second situation of using two gaskets together by installing an LS gasket without removing the installed gasket is not allowed by the ASME Codes. However, by demonstrating the creep history of such a gasket arrangement it could be considered as an option that could possibly seal a connection while significantly reducing operational down time and personnel risk. Forty tests were conducted, and the overall results demonstrate the initial applied force and how the gasket changes with time. The change in sealing force, in terms of torque, was then measured to obtain a force history as the gaskets creep. This report documents the results of those tests as well as the method used to perform the tests.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

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 OSTI2020

Mechanical Properties of Aged A709

A709 plate is in the process of being developed and qualified through a collaboration by Argonne National Laboratory (ANL), Idaho National Laboratory (INL), and Oak Ridge National Laboratory (ORNL). The goal is to qualify A709 plate in Section III, Division 5 of the American Society of Mechanical Engineers (ASME) Boiler and Pressure Vessel Code (BPVC). This would permit the construction of A709 plate for fast-reactor structural applications. A tradeoff between creep and creep-fatigue properties was established in prior work. A processing route was identified as providing the optimal balance between creep-rupture and elevated-temperature cyclic properties for the solution annealed condition. This condition, however, resulted in a shorter than desired creep-rupture life. Aging is probed to evaluate its potential at further improving mechanical properties. Aging statically precipitates the solutes in solution prior to service. The processing routes identified as providing the best creep-rupture properties and best balance in mechanical properties are investigated. This report discloses the results from tensile, creep, and elevated-temperature cyclic testing performed at INL on the aged material. The aged properties are compared to solution annealed properties. A709 offers improvement in performance compared to 316H particularly at high temperatures; 316H is a material qualified in Section III, Division 5 of the ASME BPVC. For certain high-temperature fast-reactor design conditions, 316H cannot be used while A709 can.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

FY24 Integrated Results for High-Temperature Mechanical Testing of LPBF 316H Stainless Steel

This report provides the mechanical test data of laser powder bed fusion (LPBF) 316H stainless steel (SS) collected during Fiscal Year 2024 (FY 24) under the US Department of Energy, Office of Nuclear Energy’s Advanced Materials and Manufacturing Technologies program, along with the current state of microstructural-based understandings of the behaviors. Materials with variabilities in manufacturing site, machine, laser parameters, powder chemistry, porosity, specimen geometry and heat treatment were tested in high-temperature tension, creep, fatigue and creep-fatigue. Electron microscopy and optical microscopy were performed on selected materials before and after the tests to provide microstructural-based understandings to the mechanical behavior. It was discovered that the as-built (AB) and stress-relieved (SR) materials exhibit similar behaviors in tension and creep, as do the solution-annealed (SA) and hot-isostatic pressed (HIP) materials. The AB and SR materials are softer but more ductile than the SA and HIP materials in tension. In creep, the LPBF materials have comparable rupture times but lower rupture strains compared to the wrought materials. The AB and SR materials have low creep rupture strains (<10%) when tested at 720°C and 800°C, while the SA and HIP materials are much more ductile. The LPBF materials exhibit large scatter in fatigue and creep-fatigue lives. The cyclic lives of creep-fatigue tests are lower than those of fatigue tests. In fatigue and creep-fatigue, SR materials outperform SA materials. A common observation from the cyclic tests is that, given the same post-build heat treatment, a lower initial peak stress generally results in a longer cyclic life regardless of hold time. It was also discovered that the batch variation can be more impactful than heat treatment, as demonstrated by the overall better performance of one batch of material than another, regardless of the heat treatment. The results provided insights into how different factors impact the behaviors of LPBF 316H SS. An outlook to FY 25 work scope is provided.

36 MATERIALS SCIENCE↗

NASA NTRS1987

Material characterization of superplastically formed titanium (Ti-6Al-2Sn-4Zr-2Mo) sheet

The aerospace industry has focused considerable interest on the near-alpha titanium alloy Ti-6Al-2Sn-4Zr-2Mo (Ti-6242) because of both its high-temperature properties and its superplastic forming (SPF) capabilities. This paper describes current research to characterize selected mechanical properties of Ti-6242 sheet in the SPF-strained condition, both with and without heat treatment, and compares the results with those obtained on as-received material. Tensile and creep tests were conducted, and metallographic analysis was performed to show the effect of 100 to 700 percent SPF strain on titanium properties. Analysis shows that as a result of SPF processing, both tensile and yield strengths, as well as elongation, are moderately reduced. Creep tests at 800 F and 1000 F show that the SPF processed material displays superior creep resistance compared with the as-received material. A post-SPF duplex-anneal heat treatment had no beneficial effect on tensile and creep properties.

Ossa, William A.↗

DOE OSTI2023

BISON validation to in situ cladding burst test and high-burnup LOCA experiments

The process for developing and qualifying nuclear fuels for commercial nuclear application requires fundamental material development, characterization, and design; out-of-pile testing on unirradiated materials; integral fuel rod irradiations, testing, and postirradiation examinations; and transient analyses. The historical approach depends on the generation of large empirical datasets and series of integral fuel rod irradiations, and this approach ultimately takes ~20 years—or sometimes longer—to acquire data through extensive sequential testing. Thus, the qualification and eventual deployment of new fuel systems constitute a long process. However, recent technological advancements have provided researchers the opportunity to perform out-of-cell, in situ measurements to assess material performance for the duration of the experiment. One such example of this capability is the use of digital image coordination and thermal imaging to assess Zircaloy cladding performance under a simulated loss-of-coolant accident (LOCA) transient condition. In situ measurements generally provide high-fidelity strain, strain rates, and temperature surface maps. This is critical for the US nuclear industry, which is actively developing a technical basis to support extending the peak rod average burnup from 62 to ~75 GWd/tU and the deployment of accident-tolerant fuel. However, the US Nuclear Regulatory Commission (NRC) outlined in its research information letter several technical issues that the industry must address before extending burnup. One topic of specific interest is understanding the cladding balloon and rupture geometry during the LOCA heat-up phase. By leveraging these advanced in situ capabilities, this work used in situ data generated from a simulated LOCA to better understand high-temperature creep and its effect on Zircaloy balloon and rupture performance. Here, this work used the BISON fuel performance code to assess the high-temperature creep model predictions with in situ data.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2021

AGC-4 Disassembly Report

The Advanced Reactor Terminology Graphite Research and Development program is currently measuring irradiated material property changes in several grades of nuclear graphite to predict behavior and operating performance within the core of these new high temperature reactor designs. The Advanced Graphite Creep (AGC) experiment, consisting of six irradiation capsules, will generate the irradiated graphite performance data for the Very High Temperature Reactor operating conditions. All six capsules in the experiment conducted at Idaho National Laboratory will be irradiated in the Advanced Test Reactor, disassembled in the Hot Fuel Examination Facility, and examined at the Idaho National Laboratory Research Center. This is the disassembly report describing the disassembly, shipment, post irradiation inspection, and storage of the graphite specimens contained within the AGC 4 irradiation test series capsule (the fourth irradiation capsule of the series). AGC 4 was irradiated in the Advanced Test Reactor (ATR) East Flux Trap (EFT) during ATR Cycle 157D, 158A, 162A, 162B, 164A, 164B, 166A, and Cycle 166B. Approximately 3.6 dpa was achieved. Desired experiment temperatures were exceeded by at least 100C during the second Cycle of irradiation due to the insertion of the KJRR experiment. The capsule was removed from the ATR and transferred to the Hot Fuel Examination Facility on May 15, 2020 and eventually unloaded into the Hot Fuel Examination Facility (HFEF) Decon Cell through Penetration 2D on February 26, 2021. It was moved to the HFEF Main Cell Window 3M for disassembly on March 15, 2021. Disassembly and specimen extraction began March 18, 2021, and packaging of the graphite specimens was completed on April 16, 2021. Several anomalies were noted, specifically that the radiological dose rates were nominally an order of magnitude higher than that of the previous AGC experiments. This report summarizes the disassembly of the AGC 4 experiment.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2023

AGC-4 Disassembly Report

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS1994

Creep and stress relaxation modeling of polycrystalline ceramic fibers

A variety of high performance polycrystalline ceramic fibers are currently being considered as reinforcement for high temperature ceramic matrix composites. However, under mechanical loading about 800 C, these fibers display creep related instabilities which can result in detrimental changes in composite dimensions, strength, and internal stress distributions. As a first step toward understanding these effects, this study examines the validity of a mechanism-based empirical model which describes primary stage tensile creep and stress relaxation of polycrystalline ceramic fibers as independent functions of time, temperature, and applied stress or strain. To verify these functional dependencies, a simple bend test is used to measure stress relaxation for four types of commercial ceramic fibers for which direct tensile creep data are available. These fibers include both nonoxide (SCS-6, Nicalon) and oxide (PRD-166, FP) compositions. The results of the Bend Stress Relaxation (BSR) test not only confirm the stress, time, and temperature dependencies predicted by the model, but also allow measurement of model empirical parameters for the four fiber types. In addition, comparison of model tensile creep predictions based on the BSR test results with the literature data show good agreement, supporting both the predictive capability of the model and the use of the BSR text as a simple method for parameter determination for other fibers.

Dicarlo, James A.↗