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At least 613 records · Page 34

First-of-a-Kind Fuel-bearing Molten Chloride Irradiation Experiment

Molten salt reactors (MSRs) have garnered increasing attention recently with several demonstration efforts on the way. A key challenge to the licensing basis for these reactors is the lack of experimental data on fueled salts. This is expected to be crucial to the safety evaluation and licensing basis of reactors of this type deployed in the future. While capability for irradiating molten salts has been reestablished in the recent decade, no enriched fuel irradiation capability has been developed and tested as of yet. A new experiment vehicle under development at Idaho National Laboratory (INL) is presented here. The Molten-salt Research Temperature-controlled Irradiation (MRTI) experiment was developed to host enriched uranium bearing salt samples to be irradiated at a test reactor within the lab complex. One of the key scientific objectives is to provide irradiated salt samples for post-irradiation examination (PIE) to study the impact of fission product generation and neutron/gamma radioactivity on the salt solution and salt-facing wall material. This paper provides a detailed overview of the mechanical design of the experiment, followed by an overview of the fabrication and assembly of an initial prototype vehicle (with non-fuel-bearing salt). A summary of the key analyses conducted as a part of the performance and safety evaluation is then provided. Lastly, an overview of the test conducted in prototypic out-of-pile (non-neutron) environment are shown. These evaluations provide the foundation for a planned irradiation of an enriched uranium-bearing chloride salt sample in the near term. The upcoming irradiation will contain 13 cm3 of UCl3-NaCl salt (93% enrichment) generating around 20 W/cm3 of fission energy during irradiation and a temperature range that can be contained between bounds of 525-900°C.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Atom Probe Tomography Characterization of High-Dose Ion Irradiated MA957

This paper presents a comprehensive characterization study of the microstructural responses to ion irradiation of the oxide dispersion strengthened (ODS) ferritic alloy MA957 using atom probe tomography (APT). The MA957 specimens were irradiated by 1.8 MeV Cr3+ ions to doses and temperatures relevant to advanced fast reactors (100 and 500 dpa at 400-500 °C). The average sizes of the YTiO particles decreased slightly after irradiation at all temperatures, with the most pronounced change at 400 °C. The particle number densities for 400 and 500 °C were slightly below number densities for the unirradiated condition, while the values were slightly higher at 420 and 450 °C. This behavior is consistent with the Nelson-Hudson-Mazey rate theory model that considers the competing effects between recombination and dissolution. An increase in the Y/Ti ratio of the YTiO particles was observed at the two lower temperatures. The formation of Cr-rich precipitates (a') was observed in specimens irradiated at temperatures up to 450 °C. Irradiation-induced segregation on grain boundaries was also investigated. Grain boundary element concentration profiles and ion maps demonstrate differences among the irradiation temperatures, with most datasets differing from the unirradiated condition. A key focus of this ion irradiation study is the high-dose response, and this quantitative assessment revealed relatively small but distinct effects of irradiation on microstructure evolution. Overall, these results showing minor second phase evolution suggest that MA957 should retain mechanical performance generally well up to 500 dpa for the irradiation temperatures studied.

Wang, Jing↗

The microstructure effects on irradiation response of ferritic – martensitic steels

Microstructural optimization to achieve greater mechanical strength has been one of the focuses in ferritic–martensitic steels development. However, these optimized microstructures’ effects on the radiation response are not well known. In this work, two ferritic–martensitic steels (9Cr-NbMo and 9Cr-Ta) underwent neutron irradiation in the High Flux Isotope Reactor, and their room-temperature post-irradiation tensile properties and microstructure evolutions were investigated and compared. These two steels exhibit similar pre-irradiation tensile behavior, and their yield strengths are higher than that of other ferritic–martensitic steels by about 200–250 MPa. Microstructural characterization on pre-irradiated materials reveals a smaller grain size in 9Cr-Ta (2.8 ± 0.3 μm in 9Cr-Ta versus 4.3 ± 0.5 μm in 9Cr-NbMo) but higher dislocation density and precipitate density in 9Cr-NbMo. As is common for ferritic–martensitic steels at low irradiation temperatures (less than about 0.45T m ), irradiation-induced hardening at 400 °C was observed for both alloys. Irradiation at 490 °C causes the two alloys to exhibit different tensile behavior: 9Cr-Ta softens by 208 MPa in yield stress, whereas 9Cr-NbMo maintains strength. Additionally, microstructural characterizations were performed, including precipitate growth, dislocation, and defect formation. Using the barrier hardening model for microstructure–property correlation, the softening in irradiated 9Cr-Ta is primarily attributed to the significant dislocation recovery, while the strength lost from the slight dislocation recovery in 9Cr-NbMo was compensated by the additional strength from the irradiation-induced cavities. The microstructure effect (primarily precipitate, dislocation and boundary) on the radiation response is discussed herein.

36 MATERIALS SCIENCE↗

Status of the NGNP graphite creep experiments AGC-1 and AGC-2 irradiated in the advanced test reactor

The United States Department of Energy's Next Generation Nuclear Plant (NGNP) Program will be irradiating six nuclear graphite creep experiments in the Advanced Test Reactor (ATR) located at the Idaho National Laboratory (INL). The graphite experiments will be irradiated over the next six to eight years to support development of a graphite irradiation performance data base on the new nuclear grade graphites now available for use in high temperature gas reactors. The goals of the irradiation experiments are to obtain irradiation performance data, including irradiation creep, at different temperatures and loading conditions to support design of the next generation nuclear plant (NGNP) very high temperature gas reactor, as well as other future gas reactors. The experiments will each consist of a single capsule that will contain six peripheral stacks of graphite specimens, with half of the graphite specimens in each stack under a compressive load, while the other half of the specimens will not be subjected to a compressive load during irradiation. The six peripheral stacks will have three different compressive loads applied to the top half of three diametrically opposite pairs of specimen stacks, while a seventh stack will not have a compressive load. The specimens will be irradiated in an inert sweep gas atmosphere with on-line temperature and compressive load monitoring and control. There will also be sampling the sweep gas effluent to determine if any oxidation or off-gassing of the specimens occurs during irradiation of the experiment.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Neutron irradiation induced defects in oxides and their impact on the oxide properties

Understanding the irradiation-induced defects in oxides is of interest for a wide range of applications. ZnO is an interesting oxide with mixed ionic and covalent bonding that contains a variety of point defect structures—making it an excellent model for studying irradiation-induced defects and their impact on properties. Here, we investigate the effects of neutron irradiation on the formation of defects and on the structural, optical, and electrical properties of ZnO single crystals. We observe the formation of vacancies and voids via positron annihilation spectroscopy. Neutron irradiation led to a significant deterioration of the ZnO structure and formed a high concentration of point defects, vacancy clusters, and voids with large disparities in their structure across variable irradiation times. It also led to significant changes in the optical properties and sample color. Irradiation for 444 h induced a high concentration of Cu acceptors as well as a high concentration of Ga donors. Additionally, temperature-dependent Hall effect measurements revealed the competing production of donors and acceptors and showed an increase in the slope of the carrier freeze-out curve with increasing irradiation dose. This work demonstrates the combined effects of neutron irradiation in producing a wide range of structural defects, impurities, and dopants in oxides and their enormous impact on modifying the oxide structure and both the optical and electronic properties. It particularly emphasizes the importance of considering the production of new impurities and dopants during the neutron irradiation of oxides.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Comparative RNA-Seq transcriptome analyses reveal dynamic time-dependent effects of 56 Fe, 16 O, and 28 Si irradiation on the induction of murine hepatocellular carcinoma

One of the health risks posed to astronauts during deep space flights is exposure to high charge, high-energy (HZE) ions (Z > 13), which can lead to the induction of hepatocellular carcinoma (HCC). However, little is known on the molecular mechanisms of HZE irradiation-induced HCC. We performed comparative RNA-Seq transcriptomic analyses to assess the carcinogenic effects of 600 MeV/n 56 Fe (0.2 Gy), 1 GeV/n 16 O (0.2 Gy), and 350 MeV/n 28 Si (0.2 Gy) ions in a mouse model for irradiation-induced HCC. C3H/HeNCrl mice were subjected to total body irradiation to simulate space environment HZE-irradiation, and liver tissues were extracted at five different time points post-irradiation to investigate the time-dependent carcinogenic response at the transcriptomic level. Our data demonstrated a clear difference in the biological effects of these HZE ions, particularly immunological, such as Acute Phase Response Signaling, B Cell Receptor Signaling, IL-8 Signaling, and ROS Production in Macrophages. Also seen in this study were novel unannotated transcripts that were significantly affected by HZE. To investigate the biological functions of these novel transcripts, we used a machine learning technique known as self-organizing maps (SOMs) to characterize the transcriptome expression profiles of 60 samples (45 HZE-irradiated, 15 non-irradiated control) from liver tissues. A handful of localized modules in the maps emerged as groups of co-regulated and co-expressed transcripts. The functional context of these modules was discovered using overrepresentation analysis. We found that these spots typically contained enriched populations of transcripts related to specific immunological molecular processes (e.g., Acute Phase Response Signaling, B Cell Receptor Signaling, IL-3 Signaling), and RNA Transcription/Expression. A large number of transcripts were found differentially expressed post-HZE irradiation. These results provide valuable information for uncovering the differences in molecular mechanisms underlying HZE specific induced HCC carcinogenesis. Additionally, a handful of novel differentially expressed unannotated transcripts were discovered for each HZE ion. Taken together, these findings may provide a better understanding of biological mechanisms underlying risks for HCC after HZE irradiation and may also have important implications for the discovery of potential countermeasures against and identification of biomarkers for HZE-induced HCC.

59 BASIC BIOLOGICAL SCIENCES↗

AGR-5/6/7 Irradiation Test Predictions using PARFUME

PARFUME, (PARticle FUel ModEl) a fuel performance modeling code used for high temperature gas-cooled reactors (HTGRs), was used to model the Advanced Gas Reactor (AGR)-5/6/7 irradiation test using predicted physics and thermal hydraulics data. The AGR-5/6/7 test consists of the combined fifth, sixth, and seventh planned irradiations of the AGR Fuel Development and Qualification Program. The AGR-5/6/7 test train is a multi-capsule, instrumented experiment that is designed for irradiation in the 133.4-mm diameter north east flux trap (NEFT) position of Advanced Test Reactor (ATR). Each capsule contains compacts filled with uranium oxycarbide (UCO) unaltered fuel particles. This report documents the calculations performed to predict the failure probability of tristructural isotropic (TRISO)-coated fuel particles during the AGR-5/6/7 experiment. In addition, this report documents the calculated source term from the driver fuel. The calculations include modeling of the AGR-5/6/7 irradiation that is scheduled to occur from October 2017 to April 2021 over a total of 13 ATR cycles, including nine normal cycles and four Power Axial Locator Mechanism (PALM) cycle for a total between 500 – 550 effective full power days (EFPD). The irradiation conditions and material properties of the AGR-5/6/7 test predicted zero fuel particle failures in Capsules 1, 2, and 4. Fuel particle failures were predicted in Capsule 3 due to internal particle pressure. These failures were predicted in the highest temperature compacts. Capsule 5 fuel particle failures were due to inner pyrolytic carbon (IPyC) cracking causing localized stresses concentrations in the SiC layer. This capsule predicted the highest particle failures due to the lower irradiation temperature. In addition, shrinkage of the buffer and IPyC layer during irradiation resulted in formation of a buffer-IPyC gap. The two capsules at the two ends of the test train, Capsules 1 and 5 experienced the smallest buffer-IPyC gap formation due to the lower irradiation fluences and temperatures. Capsule 3 experienced the largest buffer-IPyC gap formation of just under 24 µm. The release fraction of fission products Ag, Cs, and Sr silver (Ag), cesium (Cs), and strontium (Sr) vary depending on capsule location and irradiation temperature. The maximum release fraction of Ag occurs in Capsule 3, reaching up to 84.8% for the TRISO fuel particles. The release fraction of the other two fission products, Cs and Sr are much smaller and, in most cases, less than 1%. The notable exception is again in Capsule 3, where the release fraction for Cs and Sr reach up to 9.7% and 19.1%, respectively.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Assembly and Delivery of Rabbit Capsules for Irradiation of Silicon Carbide Cladding Tube Specimens in the High Flux Isotope Reactor

Neutron irradiation of silicon carbide (SiC)-based fuel cladding under a high radial heat flux presents a critical challenge for SiC cladding concepts in light water reactors (LWRs). Fission heating in the fuel provides a high heat flux through the cladding, which, combined with the degraded thermal conductivity of SiC under irradiation, results in a large temperature gradient through the thickness of the cladding. The strong temperature dependence of swelling in SiC creates a complex stress profile in SiCbased cladding tubes as a result of differential swelling. The Nuclear Science User Facilities (NSUF) Program within the US Department of Energy Office of Nuclear Energy is supporting research efforts to improve the scientific understanding of the effects of irradiation on SiC cladding tubes. Ultimately, the results of this project will provide experimental validation of multi-physics models for SiC-based fuel cladding during LWR operation. The first objective of this project is to irradiate tube specimens using a previously developed design that allows for irradiation testing of miniature SiC tube specimens subjected to a high radial heat flux. The previous “rabbit” capsule design uses the gamma heating in the core of the High Flux Isotope Reactor (HFIR) to drive a high heat flux through the cladding tube specimens. A compressible aluminum foil allows for a constant thermal contact conductance between the cladding tubes and the rabbit housing despite swelling of the SiC tubes. To allow separation of the effects of irradiation from those due to differential swelling under a high heat flux, a new design was developed under the NSUF program. This design allows for irradiation of similar SiC cladding tube specimens without a high radial heat flux. This report briefly describes the irradiation experiment design concepts, summarizes the irradiation test matrix, and reports on the successful delivery of six rabbit capsules to the HFIR. Rabbits of both low and high heat flux configurations have been assembled, welded, evaluated, and delivered to the HFIR along with a complete quality assurance fabrication package. These rabbits contain a wide variety of specimens including monolith tubes, SiC fiber SiC matrix (SiC/SiC) composites, duplex specimens (inner composite, outer monolith), and specimens with a variety of metallic or ceramic coatings on the outer surface. The rabbits are targeted for insertion during HFIR cycle 475, which is scheduled for September 2017.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

High Fidelity Ion Beam Simulation of High Dose Neutron Irradiation

The objective of this proposal is to demonstrate the capability to predict the evolution of microstructure and properties of structural materials in-reactor and at high doses, using ion irradiation as a surrogate for reactor irradiations. “Properties” includes both physical properties (irradiated microstructure) and the mechanical properties of the material. Demonstration of the capability to predict properties has two components. One is ion irradiation of a set of alloys to yield an irradiated microstructure and corresponding mechanical behavior that are substantially the same as results from neutron exposure in the appropriate reactor environment. Second is the capability to predict the irradiated microstructure and corresponding mechanical behavior on the basis of improved models, validated against both ion and reactor irradiations and verified against ion irradiations. Taken together, achievement of these objectives will yield an enhanced capability for simulating the behavior of materials in reactor irradiations.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Analysis and Design of Ex-Service Garter Spring Irradiation Capsules in the High Flux Isotope Reactor

Nickel-based super alloys such as Inconel X-750 are used to fabricate internal components for various reactor systems. Recent efforts to research and understand the effects of long-term neutron radiation damage on this material are crucial for quantifying the performance (radiation-induced creep and embrittlement) of such materials under extended use. The CANDU® ex-service garter spring irradiation program was instituted to investigate such effects on various types of Inconel X-750 garter springs, tensile specimens, and fatigue specimens. Conventional irradiation programs use rabbits, which are capsules that are generally loaded with non radioactive irradiation specimens. These rabbits are designed to realize various specimen temperatures while irradiated to high neutron fluences in the Oak Ridge National Laboratory (ORNL) High Flux Isotope Reactor (HFIR). To accelerate the irradiation schedule of this program, two types of material — unirradiated and previously irradiated ex-service garter spring material — were both included in the irradiation program test matrix. These two material conditions are expected to provide intermediate and end-of-life neutron dose experimental results concurrently to accelerate the overall irradiation program schedule. This document describes the B8J18 garter spring design and the supporting work required to successfully fabricate, assemble, and qualify subsequent irradiation capsules.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

First Annual Progress Report on the Procurement and Post-Irradiation Examination of the Selected Samples of Alloy 800H and Grade 92 and 91 Steels

Ferritic-martensitic steel Grade 92, with Grade 91 as a reference, together with austenitic stainless steel (or Incoloy Alloy) 800H and its grain-boundary-engineered version 800H-TMP (Thermo-Mechanical Processing), is investigated in this project. A total of fifteen Grade 92 samples from two or three heats, four T91 samples from two heats, and six 800H and six 800H-TMP samples from one heat were selected, which were primarily irradiated in the Advanced Test Reactor (ATR) of Idaho National Laboratory (INL), with the rest in the High Flux Isotope Reactor (HFIR) of Oak Ridge National Laboratory (ORNL), BOR-60 of Russia, and Phénix reactor of France. The samples were irradiated in the temperature range of 241 to 720°C and a dose range of 1.28 to ~70 displacements per atom. All the INL and ORNL samples and part of the LANL (Los Alamos National Laboratory) samples have been received at the Irradiated Materials Examination and Testing (IMET) hot cell facility. The selected ORNL samples include six Grade 92 and two 800H samples, which were irradiated in the HFIR to 0.46–14.66 dpa at 400 to ~720°C. The Grade 92 is an optimized heat and named as G92-2b. The two 800H samples have one sample as the standard solution-annealed condition and the other sample as a TMP condition with a maximized fraction of low-Σ coincidence site lattice (CSL) boundaries. Tensile test of the G92-2b samples were conducted at room temperature in the IMET hot cell. The lower temperature irradiation at 400–496.7°C to 0.52–14.66 dpa resulted in minimal changes in tensile properties. However, the higher temperature irradiation at ~683.3–720°C to 0.46–14.63 dpa tended to reduce yield and tensile strength by about –136 to –311 MPa and plastic elongation by –1 to –3% with the increasing dose. The 800H and 800H-TMP samples were tensile-tested at their irradiation temperature 580°C in the IMET hot cell, which showed >40% increase in yield and tensile strength with nearly 9% reduction in elongation for 800H-TMP compared with 800H. Three of the G92-2b samples, i.e., GB04 (7.44 dpa at ~490°C), GB05 (14.66 dpa at 496.7°C), and GB12 (14.63 dpa at ~720°C), were examined at the LAMDA for Vickers hardness measurements and microstructural characterization by SEM and TEM. Vickers hardness was successfully measured on GB12, which was reduced by is – (112.4 ± 12.3) HV1 from the control sample. However, the Vickers hardness measurements were failed on GB04 and GB05 because the samples were polished too thin to prevent the interference from the substrate (epoxy). The other half of the GB04 and GB05 will be polished for the hardness measurements, as well as nanoindentation studies. Fractography by SEM indicated increased numbers of ductile dimples (or voids) with the increasing irradiation dose, while significantly increased numbers and sizes of dimples with the increasing irradiation temperature. TEM characterization exhibited the presence of Cr 23 C 6 , VN, and Laves precipitates at boundaries and matrix, which showed pronounced precipitate-dislocation interactions (pinning effect). Dense dislocations but limited dislocation loops were observed in the samples, which noticeably reduced in GB12. Additionally, some tiny partially amorphized spherical domains were observed in GB12, which had a normal body-centered cubic lattice parameter of 9Cr steels at the surround regions but ~11% smaller than the lattice parameter of the matrix away from the amorphized spherical domains. Further characterization will be pursued to clarify the new findings.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Recovery of Silicon Carbide monitor irradiation temperature via continuous resistance measurement during annealing (Pt. II)

Silicon carbide (SiC) monitors provide a means of measuring peak irradiation temperature of experiment capsules in nuclear irradiation experiments. Neutron irradiation of a SiC monitor causes permanent lattice changes that are removed by annealing via heating to a temperature that exceeds the peak irradiation temperature. The annealing process results in changes to SiC physical characteristics that can be observed during the annealing process. This paper presents results of a method aimed at using electrical resistance, measured during a two-pass heating – cooling cycle as a means of recovering the irradiation temperature of a SiC monitor. Results indicate that the relationship between resistance and temperature of a SiC monitor shows a significant change in slope when the peak irradiation temperature is reached. This demonstrates the potential for this method to replace the current manual, and lengthy, process of post irradiation examination used to extract the peak irradiation temperature from irradiated SiC monitors.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Mechanical and Thermophysical Properties of 3D-Printed SiC before and after Neutron Irradiation – FY21

This report presents the mechanical and thermophysical properties of 3D-printed SiC before and after neutron irradiation that have been evaluated to assess the fuel matrix material for the Transformational Challenge Reactor (TCR). The TCR fuel form consists of an additively-manufactured silicon carbide (SiC) matrix and uranium nitride tristructural isotropic (UN TRISO) fuel particles, which is manufactured through a newly developed processing route combining binderjet 3D printing, TRISO fuel particle loading, and chemical vapor infiltration (CVI). Because the fuel matrix is a primary component of the TCR core and its response to mechanical and thermal loads during operation is one of the most influential factors on the integrity of TCR core, testing and evaluation have focused on producing mechanical and thermophysical properties data for the binderjet/CVI SiC. Baseline mechanical and thermophysical properties were measured from the disk specimens printed for different and sizes orientations, which included equibiaxial flexural failure strength, elastic constants, thermal diffusivity and conductivity, density, and the coefficient of thermal expansion. Flexural failure strength datasets showed similar Weibull distributions regardless of sample variants including different orientations. The mean failure strengths of the 3D-printed SiC variants were in the range of 280–310 MPa, which are slightly lower than that of the chemical vapor deposition (CVD) SiC. Thermophysical test results showed that specific heat and thermal expansion are not sensitive to the build direction of SiC samples, while thermal conductivity is highly dependent on the build direction and can be correlated to the anisotropic character of the 3D-printed SiC. Neutron irradiation tests were carried out on the 3D-printed 6-mm diameter SiC disk specimens. Irradiation was carried to 2.3 dpa over a temperature range of 360–880°C. No significant degradation in strength was observed in SiC after irradiations in various conditions and with different orientations. Anisotropy that had been observed in the thermal conductivity of 3D-printed SiC prior to irradiation vanished after irradiation as the irradiation defect thermal resistivity accumulated in the material. Electron microscopy of the microstructure after neutron irradiation showed distinct defect morphologies in the heterogenous material, but no evidence for irradiation-induced cracking or degradation in the microstructure was observed.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Irradiation of Sintered Mo Disks with Presence of Organic Impurities in He Gas Flow

Argonne National Laboratory (Argonne) is assisting NorthStar Medical Technologies in the development of a domestic supply of 99 Mo. Specifically, the present study focuses on the production of 99 Mo-feed solution used by the RadioGenix™ 99m Tc generator. During the target-irradiation phase of production, impurities can potentially be introduced into the feed, and can lead to disturbance of ligand- 99m Tc complexation chemistry and contamination of the final radiopharmaceutical that directly interacts with the patient. To address this issue, Argonne performed irradiations and chemical processing to identify whether the potential contamination of He flow with hydrocarbon oil during irradiation affects the radiochemical purity of the final K 2 MoO 4 (K 2 TcO 4 ) in 5M KOH solution. To mimic the conditions of real irradiation at NorthStar, Argonne used its electron linear accelerator and Van de Graaff facilities, heated the target and oil source to >800°C, and controlled oxygen in the presence of He during irradiation. Following irradiation, scanning electron microscopy (SEM) and carbon analysis (CA) were used to detect carbon contamination on the solid targets. The radiochemical purity of the dissolved targets was studied via thin-layer paper chromatography (TLC). As a result of these experiments, small regions of the surface of some irradiated disks were found to be high in carbon, but the total carbon content was still negligible in comparison to the reference sample, which had experienced no irradiation or contact with oil. The summarized results from the SEM, CA, and TLC tests lead to the conclusion that even an excess of oil and heating during irradiation do not affect the radiochemical purity of the final product.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

Experimental Evaluation of Deformation and Fracture Mechanisms in Highly Irradiated Austenitic Steels

The present report documents recent experimental results of analysis using scanning electron microscopy/electron backscatter diffraction (SEM-EBSD) of plastic deformation mechanisms and strain localization phenomena in austenitic steels irradiated by neutrons. Experiments were performed with specimens irradiated to 125 dpa and, additionally, with specimens that experienced radiation-induced swelling up to 3%. Section 1 briefly analyzes the deformation localization in irradiated steels and its consequences on the material performance. The section describes the advantages and importance of the SEM-EBSD approach combined with in situ mechanical testing capability. Section 2 briefly introduces the experimental tools and methods (i.e., SEM/EBSD in situ tensile frame, electric discharge machine to manufacture irradiated specimens) and describes the investigated materials (i.e., element composition, irradiation conditions, and general microstructure). Section 3 describes the key experimental results and provides a brief analysis and comparison with the datasets obtained earlier within the same task (i.e., low-dose specimens). The discussion focuses on EBSD microstructure maps with strain localization features, misorientation evolution as a function of strain, and observed deformation mechanisms. Section 4 evaluates data collected in recent years on highly irradiated steel and estimates the possible misorientation evolution under irradiation. The section introduces and discusses the concept of in-service-induced damage as an irradiation-assisted stress-corrosion cracking precursor. Section 5 summarizes the work performed. As expected, the present work results are beneficial for exploring and understanding degradation mechanisms in highly irradiated in-core materials found in light water reactors after long-term in-service life.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

The Recovery of Medical Isotope 188 W from Irradiated W Metal Target - A New Approach

Tungsten-188 is in widespread use in 188 W(t 1/2 = 69 d )/ 188 Re(t 1/2 = 16.9 h ) biomedical generators. Oak Ridge National Laboratory has been providing this product to the world since 1999. At ORNL, 188 W is produced via irradiation in ORNL’s High Flux Isotope Reactor (HFIR). Enriched 186 W targets in the form of sintered metallic pellets or rings achieve a compact loading in the irradiation vessel, providing a high yield per unit target. The enrichment of the target is >90% 186 W, and this isotope undergoes double neutron capture to produce the desired 188 W product. While 188 W is produced by neutron bombardment, 191 Os(t 1/2 = 15.4 d ) is simultaneously produced as a by-product and expected to be separated from 188 W by postirradiation treatment.In the current processing pathway, the irradiated W metal rings are first converted into an oxide form of WO 3 by heating the irradiated W metal target at 750°C in a quartz reaction vessel inside a vertical furnace under a constant flow of air. During heating, W metal reacts with oxygen in the air to produce WO 3 , which is soluble in 6 M NaOH for preparation of 188 W product. This oxidation process also converts 188 Os (the decay daughter of 188 W) and 191 Os (15.4 d , the irradiation produced byproduct) into OsO 4 , a highly volatile and toxic gas. The gaseous effluents driven from the quartz reaction vessel are passed through a scrubbing array to remove OsO 4 before the air is discharged from the process. This heterogeneous oxidation method simultaneously achieves goals of (1) converting metal target to a soluble oxide form and (2) removing volatile OsO 4 away from the solid WO 3 product by air flow and absorbing the harmful Os species by the scrubbing array. But this method has two potential problems as well: (1) O 2 reacts with only W metal at high temperatures, not with W alloyed with other elements. The O 2 –W reaction will be retarded when formation of WRe or WC occurs, or even when a layer of non-W materials on the surface of the irradiated W rings.; (2) 100% absorption of OsO 4 of high yield (>90%) from the reaction of Os + O 2 is a strict requirement to the OsO 4 scrubbing system--so NaOH scrubbers of a redundant size (2x 1.5 L) are in use for safety reasons.To resolve above two potential problems, direct dissolution of the irradiated W metal target by a selected reagent is a preferred pathway to avoid heating step with generation of tremendous amount of volatile OsO 4 . Hydrogen peroxide (H 2 O 2 ) is such a candidate to dissolve W in forms of either metal or alloys, although literature lacks information of solubilities of Re or Os in H 2 O 2 . With experimental results of dissolving non-radioactive W, Re and Os in H 2 O 2 under various conditions, this report illustrates a method of H 2 O 2 dissolution for irradiated W target, with a complete dissolution of W and Re, but ≤10% dissolution of Os (converted into gaseous OsO 4 and carried out into a scrubbing for absorption) during processing irradiated W target. The portion of undissolved Os can be separated from W solution by a follow up filtration step. Solubilities of W, Re and Os in H 2 O 2 at a temperature range from 14° to 50°C are presented. And a dissolution rate of W metal per surface area of W metal in H 2 O 2 is calculated based on results of dissolving a W metal cylinder of known surface area in H 2 O 2 at room temperature without stirring.

07 ISOTOPE AND RADIATION SOURCES↗

AGC-1 Specimen Post Irradiation Data Report

Here we report the results of the Post Irradiation Examination (PIE) of the creep, control, and piggyback specimens from the irradiation creep capsule AGC-1. This is the first (prototype) of a series of six capsules planned as part of the Advanced Graphite Creep (AGC) experiment to fully characterize the neutron irradiation effects and radiation creep behavior of current nuclear graphites. The data reported include: specimen dimensions and hence the dimensional change upon irradiation (a comparison of these data for specimen matched pairs will yield the creep strain); mass and volume, hence density; elastic constants (Young’s modulus, shear modulus and Poisson’s ratio) from ultrasonic time of flight (TOF) and velocity measurements; Young’s modulus from the fundamental frequency of vibration; electrical resistivity; and thermal expansion from 100-550°C (hence coefficient of thermal expansion). Over 8500 individual physical measurement have been made and the data are reduced and reported here. The AGC-1 capsule was irradiated in the Advanced Test Reactor (ATR) at INL at approximately 700°C and to a peak dose of 7 dpa (displacements per atom). The specimen’s final dose, temperature and stress conditions have been reported by INL and are also tabulated here. Additionally the analysis of the SiC temperature monitors is reported. These temperature monitors were located along the center of the AGC-1 capsule and provide an independent assessment of the capsules final irradiation temperature. While all the PIE testing is reported (with the exception of the glued-end tensile strength specimens) additional analysis of the AGC data will be required to allow: 1. Improved fits to the existing models of graphite irradiation induced creep strain. 2. With the eventual advent of temperature dependency data from the additional AGC series of capsules, and microstructural data from piggy back specimens in AGC capsules, the development of new and improved models for the development of irradiation induced creep strain in graphite are anticipated. 3. An Investigation into the effects of creep strain on the physical properties of irradiated graphite.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

In-situ and ex-situ characterization of irradiated AM materials

This study investigates the irradiation performance of laser powder bed fusion (LPBF) 316L and 316H stainless steels (SS), and their wrought counterparts. While LPBF 316L has been more studied, LPBF 316H is relatively new, with little prior data on its irradiation behavior. The research involved fabricating, preparing, irradiating, and characterizing six materials: LPBF 316L (two variants), LPBF 316H (two variants), and wrought 316L and 316H. LPBF materials were subjected to various heat treatments, including solution annealing and stress relief, and were irradiated using in-situ and ex-situ ion techniques at temperatures of 300°C and 600°C, with doses ranging from 0.2 dpa to 25 dpa. Under ex-situ irradiation with 4 MeV Ni 2+ ions at 600°C, the dislocation cell structures in LPBF316L-1 and LPBF316H-1 gradually evolved into a uniform dislocation network. At a low irradiation dose (0.2 dpa), the cell structures were still partially visible. At 2 dpa, a uniform dislocation network formed, though remnants of the original cell structure were still discernible as contrast domains. At 5 dpa and 10 dpa, even the contrast domains vanished. For irradiation at 300°C, the cell structure was still clearly visible at 0.2 dpa for LPBF316L-1. For LPBF316H-1, the dislocation cell structure was less apparent at the same dose but was still recognizable. With further increase in dose at 300°C, the dislocation cell walls were completely replaced by irradiation-induced defects and no longer visible. Void formation was observed for irradiation at 600°C. At 2 dpa, no evident voids were observed in either LPBF316L-1 or LPBF316H-1.

36 MATERIALS SCIENCE↗