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Koyanagi, Takaaki

Publications and source records attributed to Koyanagi, Takaaki.

At least 19 records

Post-Irradiation Examination to Quantify Irradiation-Induced Bowing of SiGA® Silicon Carbide Composite Structures (Final CRADA Report – NFE-23-09937)

As part of the SiC-based material development at General Atomics Electromagnetic Systems (GA-EMS), this project involved the first-of-a-kind experimental post-irradiation examination of the irradiation-induced bowing response in SiC composite structures under a neutron flux gradient. The SiC composite miniature channel specimen was provided by GA-EMS for the irradiation experiment. To quantify the irradiation-induced bowing of the channel specimen, a series of visual and dimensional inspections were conducted using the unique capabilities at Oak Ridge National Laboratory (ORNL), including a custom profilometry rig. The post-irradiation examination results of this project will assist GA-EMS in validating their fuel performance model for SiC-based core structures in neutron irradiation environments.

36 MATERIALS SCIENCE↗

Comprehensive characterization of the irradiation effects of glassy carbon

Carbon materials have become increasingly diverse, finding applications in high-temperature and high-radiation environments. Glassy carbon, an allotrope known for its exceptional chemical inertness and desirable mechanical properties. However, understanding neutron irradiation effects in glassy carbon has proven challenging, primarily because of its unique nanopore structure. Here, this study presents a highly detailed microstructural characterization investigation of neutron-induced changes in glassy carbon, revealing how changes in nanopore structure and crystallinity impact the irradiation-induced shrinkage. Aberration-corrected scanning transmission electron microscopy (STEM) reveals pore closure that leads to material densification in the irradiated samples. Dimensional analysis combined with comparison to historical data suggest significant length shrinkage to occur. Neutron and in situ electron irradiation experiments suggest that glassy carbon transforms into so-called carbon onions, supporting the concept of shrinkage saturation. Investigating irradiation temperature effects using STEM, electron energy loss spectroscopy, x-ray diffraction, and Raman spectroscopy revealed partial amorphization at 210 °C–230 °C and preserved order in glassy carbon at 860 °C, coinciding with pore closure. Thermal property measurements were also conducted to assess the effects of densification and other changes in the atomic structure of glassy carbon. The results of this study have broad implications in the deployment of glassy carbon to nuclear environments, based around the observed changes in the thermal properties, and demonstrates the operational window for the onset of densification.

36 MATERIALS SCIENCE↗

Phase stability and microstructure of neutron-irradiated substoichiometric yttrium dihydrides

The impact of the neutron-displacement damage on phase stability and microstructure of substoichiometric yttrium dihydrides (YH x , x <2) were investigated to assess their use as solid moderator in high-temperature nuclear reactors. YH x specimens were, thus, subjected to neutron irradiations in the range of 0.1–2 displacements per yttrium atom (dpa-Y) in the temperature range of 536–878°C at the Oak Ridge National Laboratory's (ORNL's) High Flux Isotope Reactor (HFIR). YH x specimens were initially prepared at stoichiometry (H/Y) ratios of 1.69 and 1.83. HFIR-irradiated specimens were characterized by variety of techniques to investigate H retention characteristics including dimensional analysis, optical microscopy, scanning electron microscopy electron back scatter diffraction (EBSD), transmission electron microscopy, thermal desorption spectroscopy (TDS), and high-energy x-ray diffraction (HE-XRD) characterizations. Overall, YH x exhibited notable structural and phase stability under short-term neutron-irradiation, except for the samples with significant silicon carbide (SiC) interaction at high doses and temperatures. Basic dimensional and mass measurements were misleading for accurate assessment of H retention, as confirmed by EBSD phase maps, XRD line profiles, and TDS signals. Thus, it was discussed that a robust H retention metric is needed to assess irradiated hydrides. Further, nanoscale cavities were observed as a result of the neutron irradiation in all samples. Although no clear impact of dose and irradiation temperature was determined, the initial H/Y ratio had an impact on the cavity number density where low H/Y specimens had high-resistance to cavity formation. The Y-vacancy cluster formation at the collision stage of the displacement cascade and their stabilization by H were considered to be the likely underlying mechanisms for the observed cavity microstructure.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Response of 11 B enriched ZrB 2 ultra-high temperature ceramic to neutron irradiation at elevated temperatures

ZrB 2 , an ultra-high temperature ceramic (UHTC) is being considered for use in fusion reactor first-wall structures, yet its response to irradiation remains poorly understood. This study employed scanning/transmission electron microscopy (S/TEM), synchrotron X-ray diffraction (XRD), finite element calculations, and thermal property measurements to thoroughly investigate the neutron-irradiation effects on 11 B-enriched ZrB 2 . Neutron irradiations were conducted at 220 °C and 620 °C, with a neutron fluence of 2.2 × 10 25 neutron/m 2 (energy > 0.1 MeV), resulting in 3.9 dpa and 4200 appm He. The study revealed the unusual prevalence of prism loops and a > c anisotropic lattice swelling, likely linked to the low c/a ratio of ZrB 2 , leading to grain boundary microcracking. Reducing the grain sizes was effective in reducing intergranular cracking and macroscopic swelling. The observation of cavities in ZrB 2 irradiated at 620 °C, as opposed to 220 °C, prompts questions about the temperature at which vacancies in ZrB 2 become mobile, and the role of neutron absorption by 10 B in elevating irradiation temperatures. Isotopic enrichment in 11 B proves to be a viable strategy for mitigating helium production in transition-metal diborides, which is a critical consideration for nuclear applications. Irradiation-induced defects reduce the thermal diffusivity and conductivity of ZrB 2 by a factor of 4–9, which has important implications for its role as a plasma-facing material in fusion reactors that drive high heat fluxes through first-wall materials. Here, this comprehensive study lays the foundation for understanding ZrB 2 behavior under neutron irradiation and highlights important phenomena to consider for various material applications.

36 MATERIALS SCIENCE↗

Emerging continuous SiC fibers for high-temperature applications

Silicon carbide (SiC) fibers are responsible for the ultimate strength and toughness of SiC-fiber reinforced composites in harsh environments. The development of a new generation of continuous SiC fibers continues to advance the mechanical properties of composite materials. Tyranno™ SA4 fiber was recently released as a successor of Tyranno™ SA3 fiber. Laser-driven chemical vapor deposition (LCVD) has been adopted as an alternative fiber processing route to synthesizing high-strength SiC fiber with tailorable small diameters and chemical compositions. Both Tyranno™ SA4 and laser-driven CVD fibers show very high tensile strength, about 4 GPa in the as-fabricated condition. The degradation of thermal stability and strength due to annealing in an inert environment were similar for Tyranno™ SA3 and SA4 fibers because of their similar carbon-rich, crystalline microstructure. Silicon-rich fibers produced by LCVD possessed heterogeneous crystallinity, which was attributed to laser power distribution and showed microstructural instability at 1500 °C and above. Finally, the new SiC fibers demonstrated an increase in as-fabricated strength but faced the same challenges in environmental resistance as the traditional SiC fibers do.

36 MATERIALS SCIENCE↗

Mechanical degradation of duplex SiC-fiber reinforced SiC matrix composite tubes under a controlled high-temperature steam environment

This paper describes results from the mechanical evaluation of unirradiated SiC fiber–reinforced SiC matrix composite tubes under a controlled high-temperature steam environment. The experiments were aimed at identifying key material degradation behavior under environments relevant to loss-of-coolant accidents of light water reactors. Mechanical tests of the SiC composite tubes at 1000 °C under steam and inert environments were conducted using a unique test capability. Further, the material tested was a duplex tube with a thick monolithic SiC layer on the outer surface. The tubes were subjected to preloading at ~100 MPa in tension before exposure to high-temperature steam with up to 75% of the preload at a constant displacement. In the presence of matrix cracks, the steam exposure caused embrittlement of the SiC composite tubes and failure at a stress level below the pretest stress. The material degradation was explained by a fiber oxidation model, which can be applied to various SiC cladding concepts. The embrittlement could be a limiting factor for using SiC cladding subjected to loss-of-coolant accident conditions.

36 MATERIALS SCIENCE↗

Experimental investigation of probabilistic failure of SiC/SiC composite tubes under multiaxial loading

This paper presents an experimental investigation of the failure behavior of SiC fiber-reinforced SiC matrix (SiC/SiC) composite tubes under multiaxial loading. A new testing apparatus is designed to independently apply axial stress and internal pressure to SiC/SiC tubes. Acoustic emission (AE) is used to monitor the damage growth in the specimen. Based on the measured stress–strain response, a strain-based criterion is proposed to determine the proportional limit stress (PLS). The proposed strain-based criterion is compared with the PLS determined by the AE measurement. The PLS is determined for different loading ratios to form a multiaxial failure surface. By testing multiple replicates, the statistical variations of the PLS are determined. In conclusion, based on the experimental results, a mathematical model is developed to characterize the probability distribution of the PLS of SiC/SiC composites under multiaxial loading.

36 MATERIALS SCIENCE↗

Phase separation during the direct powder bed fusion of SiC

Powder bed fusion (PBF) is an attractive additive manufacturing option for fabrication of SiC object with complex geometries. However, the density and microstructure controls remain a challenge. This study is aimed at understanding laser–SiC interactions, with emphasis on microstructure-processing relationships, to identify potential solutions for the process improvement. SiC tubes were fabricated by PBF of pure SiC powders without sintering additives. Further, comprehensive analysis by X-ray diffraction, Raman spectroscopy, and electron microscopy indicated that binding of SiC particles was achieved by incongruent melting of SiC to a Si/C mixture containing SiC micro- and nanocrystallites. The phase evolution under laser irradiation of SiC was explained by phase diagrams. This study uncovered the PBF SiC microstructure at different length scales and the relationship between the microstructure and the processing parameters.

36 MATERIALS SCIENCE↗

Hermeticity of SiC/SiC composite and monolithic SiC tubes irradiated under radial high-heat flux

Demonstration of hermetic SiC fiber–reinforced SiC matrix composite cladding under normal operating environments has been identified as one of the most critical feasibility issues for accident-tolerant fuel cladding in light-water reactors. This study provides critical experimental data needed for understanding the effects of irradiation on hermeticity. SiC composite and monolithic tubes were neutron-irradiated to 2 displacements per atom with and without a nominal radial heat flux of 0.6 MW/m2 to produce a simulated in-pile stress state for the normal operation of a light-water reactor. The through-thickness temperature gradient under irradiation results in a gradient in swelling, which causes a significant stress buildup. Such irradiation-induced stress was modeled using a commercial finite element analysis code. The radial heat flux–irradiation synergism was experimentally investigated by constructing a special irradiation capsule and evaluating the helium hermeticity of the specimens. The simulated stress state exhibited a near equi-biaxial tensile axial and hoop stress of ~150 MPa at the inner surface of the SiC composite tube. This stress level is potentially beyond the matrix cracking stress. Degradation of hermeticity of the SiC composite tubes was observed after irradiation, indicating irradiation-induced cracking, whereas the irradiated monolithic SiC tubes remained hermetic. In conclusion, the results indicate that loss of hermeticity caused by radiation-induced microcracking is a potential issue for SiC composite cladding, depending on the magnitude of the temperature gradients. Coating the outer surface of the cladding was identified as a mitigation strategy that might overcome the cracking issue.

36 MATERIALS SCIENCE↗

Probabilistic Failure Criterion of SiC/SiC Composites Under Multiaxial Loading

Owing to its excellent mechanical properties and stability under high temperature and neutron irradiation conditions, SiC/SiC composites have emerged as a promising material for light water reactors (LWRs) in the development of accident-tolerant fuel (ATF) systems. Structural integrity and retention of hermeticity are two crucial requirements for SiC/SiC claddings during normal operations, and both of them are closely related to the proportional limit stress (PLS) of the material. Understanding the behavior of SiC/SiC composites under multiaxial stress states and developing a probabilistic approach for evaluating the structural vulnerability are of paramount importance for reliability-based analysis and design of SiC/SiC composite claddings. So far, there has been very limited effort towards experimental and analytical investigations of probabilistic failure of SiC/SiC claddings. This critical knowledge gap motivates this research. A probabilistic failure criterion for SiC/SiC composites under multi-axial loading is developed, and this criterion is incorporated into reliability analysis of the structural integrity of SiC/SiC fuel cladding. The research consists of two parts: 1) experimental investigation of multiaxial failure behavior of SiC/SiC composites, and 2) theoretical modeling of time-dependent probabilistic failure of SiC/SiC cladding. In the experimental investigation, the PLS is determined through the examination of stress-strain response, the acoustic emission measurement, as well as the X-ray computed tomography. The theoretical framework is derived by combin- ing the finite weakest-link statistical model and the subcritical damage growth model. This theoretical model captures the time-dependent failure mechanism of the material, which has a major consequence for predicting the lifetime distribution of the cladding. Meanwhile, the model also predicts that the failure statistics of the cladding depends strongly on the cladding length. The results of the multiaxial experiments reveal the level of statistical variation of the PLS of SiC/SiC materials under different stress states. The theoretical model provides a robust analytical tool for extrapolation of small-scale laboratory test results to the behavior of full-scale claddings. These findings establish a scientific foundation for the development of reliability-based design of SiC/SiC fuel claddings, which will play an essential role in improving the structural safety and integrity of LWRs.

42 ENGINEERING↗

Corrosion characteristics of monolithic SiC materials in beryllium-bearing molten fluoride salt

In this work, chemical vapor deposited SiC single crystal and polycrystals were exposed to a static beryllium-bearing molten fluoride salt, 2LiF–BeF 2 for 500 and 1000 h at 750 °C. Overall, the single crystal and polycrystalline SiC materials experienced slight weight loss and nominal surface etching regardless of the material type. Localized pitting and nonuniform Si removal from surface regions were associated with trace metal impurities and oxygen. Cross-sectional observation revealed minimal subsurface changes in the microstructure. The corrosion damage processes were similar to those reported for molten LiF–KF–NaF salt with trace impurities, indicating that the impurities significantly affect SiC corrosion.

36 MATERIALS SCIENCE↗

Heterogeneous microstructure of yttrium hydride and its relation to mechanical properties

Here, the goal of this study is to investigate the properties of yttrium hydride materials in relation to the microstructure, especially its homogeneity. High-throughput nanoindentation mapping was used to evaluate hardness distribution. Raman spectral imaging demonstrated its sensitivity to the presence of YH2 and impurities. Raman peak position maps were correlated with residual stress in the specimens. Electron backscatter diffraction mapping provided phase distributions with correlation to high-energy X-ray diffraction analysis. The experimental mapping data were combined and analyzed using unsupervised machine learning cluster procedures. The machine learning analysis revealed that yttrium hydride specimens contained a major δ-YH2 – x phase component and minor α-Y and δ-YH2 – x components with significant residual stress. The minor phase fraction decreased with increasing nominal H/Y ratio, which affected the nanoindentation and Vickers hardness. The multimodal mapping procedures described herein affect developing important microstructure–property relationships, as well as correlations in heterogeneity and mechanical properties.

36 MATERIALS SCIENCE↗

Mechanistic modeling of lifetime distribution of SiC/SiC composite claddings

Silicon carbide (SiC) fiber-reinforced SiC matrix (SiC/SiC) composites have emerged as a new material candidate for fuel claddings in light water reactors. Recent studies showed that the load capacity of SiC/SiC materials exhibits a considerable statistical variation. Therefore, reliability analysis plays a critical role in design of SiC/SiC composite claddings. Here, this paper presents a probabilistic model for the lifetime distribution of SiC/SiC composites. The model is anchored by a multiaxial stress-based failure criterion and subcritical damage accumulation mechanism. Based on the kinetics of subcritical damage growth, the lifetime distribution of a laboratory test specimen for any given loading history can be calculated. A finite weakest-link model is used to extrapolate the lifetime distribution of test specimens to full-length claddings. It is shown that the damage accumulation mechanism has a strong influence on the lifetime distribution of the cladding. This finding highlights the importance of understanding the static fatigue behavior of SiC/SiC composites. The present analysis also demonstrates an intricate length effect on the failure probability of the cladding, which is expected to play a crucial role in design extrapolation.

36 MATERIALS SCIENCE↗

Surface chemistry of neutron irradiated tungsten in a high-temperature multi-material environment

Deuterium retention was measured on neutron irradiated tungsten samples where one side of the samples had a visually clean metallic luster and the opposite side appeared to have a reacted surface film. Deuterium plasma exposure and subsequent thermal desorption from the reacted surface side produced spectra with larger total deuterium desorption at lower temperatures than from the clean surface side. For neutron irradiation, these W disk samples were installed in an irradiation capsule in such a way that one side of W sample was in contact with the surface of another W sample, and the opposite side was in contact with a SiC temperature monitor. The composition of the reacted surface was investigated using X-ray photoelectron spectroscopy and showed that SiC had interdiffused into the W samples. Neutron enhanced diffusion likely contributed to this as SiC and W are stable at temperatures exceeding the irradiation temperature. Results highlight the need to consider the surface chemistry of samples in drawing conclusions on hydrogen isotope retention of W materials and also illustrate the complexity of multi-material nuclear environments expected in fusion devices.

36 MATERIALS SCIENCE↗

Stress rupture of SiC/SiC composite tubes under high-temperature steam

SiC-fiber–reinforced SiC matrix composite cladding for light water reactor fuel elements must withstand high-temperature steam oxidation in a loss-of-coolant accident scenario (LOCA). Current composite designs include an outer monolithic SiC layer, in part, to increase steam oxidation resistance. However, it is not clear how such a structure would behave under high-temperature steam in the case when the monolithic layer cracks and carbon interphases and SiC fibers are exposed to the environment. To fill this knowledge gap, stress-rupture tests of prototypic SiC composite cladding at 1000°C under steam and inert environments were conducted. The applied stress was ~120 MPa, which was beyond the initial cracking stress. The failure lifetime under steam was 400–1300 s, while 75% of the composite specimens did not fail after 3 h of total exposure under inert gases. Microstructural observations suggest that steam oxidation activated slow crack growth in the fibers, which led to failure of the composite. The results from this study suggest that stress rupture in steam environments could be a limiting factor of the cladding under reactor LOCA conditions.

36 MATERIALS SCIENCE↗

The response of accident tolerant fuel cladding to LOCA burst testing: A comparative study of leading concepts

Accident tolerant fuel claddings seek to improve safety margins during loss-of-coolant accident (LOCA) scenarios by reducing cladding steam oxidation rates, hydrogen production, delaying or mitigating cladding burst, and reducing cladding deformation. After rapid and extensive progress in recent years, Cr coated Zr-based alloys, ferritic FeCrAl, and SiC/SiC ceramic matrix composites (CMCs) have emerged as the most promising cladding concepts, but there are few studies comparing the accident tolerance of all three concepts simultaneously. Here, in this study, LOCA burst testing has been conducted on Cr high impulse power magnetron sputtered Zry-4 (Cr/Zry-4), C26M (FeCrAl), and SiC/SiC SiGA (CMC). Experimental observations indicate Cr/Zry-4 burst at higher temperatures than Zry-4 however the effectiveness of the coating on mitigating ZrO 2 formation via Cr 2 O 3 formation depended on physical proximity to the burst opening. No dramatic improvement in diametrical strain nor opening geometry was observed. C26M burst at higher temperatures than Zry-4 at lower pressures, exhibiting small amounts of strain and smaller openings, and formed slow-growing Al 2 O 3 regardless of location. The CMCs did not burst or show any macroscopic signs of deformation, all the way up to an internal cladding pressure of 15.2 MPa. High temperature expanding Nb plug testing indicated that CMC room temperature strength may persist up to 1650°C, with an approximately 40% loss of strength at 1900°C. CMC steam oxidation was also compared to reference chemically vapor deposited SiC up to 1700°C, and CMCs were found to oxidize at slightly accelerated rates that were still orders of magnitude lower than bare Zry-4. Projected H 2 generation during LOCA burst testing showed that when accounting for cladding burst exposing inner diameters to steam, Cr coated Zry-4 reduced H 2 generation by a factor of two compared with bare Zry-4, while both C26M and SiC/SiC reduced H 2 generation by orders of magnitude relative to bare Zry-4.

36 MATERIALS SCIENCE↗

Failure evaluation of neutron-irradiated SiC/SiC composites by underwater acoustic emission

Here, understanding the statistical properties of mechanical properties of non-irradiated and neutron-irradiated SiC/SiC composites is essential for component design. This study aims to evaluate the detailed damage accumulation behavior of composites focusing on two fracture parameters: proportional limit stress (PLS) and acoustic emission (AE) onset stress. The developmental underwater AE technique, which is benefit in non-contact in-situ failure monitoring method during mechanical testing and in handle of the irradiated material, was first applied to evaluate damage accumulation behavior. Two types of chemical vapor infiltration SiC/SiC composites were used: one reinforced with Hi-Nicalon Type-S SiC fiber and one reinforced with Tyranno-SA3 SiC fiber in the form of satin-woven 2D fabrics with pyrolytic carbon interface. Neutron irradiation in the High Flux Isotope Reactor at Oak Ridge National Laboratory reached a fluence of 30 dpa at a temperature of 620–670°C. Four-point flexural tests were conducted to evaluate post-irradiation strength. Weibull statistics did not suggest marked degradation of composite strength. Detailed failure behavior evaluated by AE demonstrated no irradiation-induced change of the AE onset stress (i.e., crack initiation equivalent stress). Failure probability analysis suggests that increasing the reliability of composites (i.e., the Weibull modulus rather than strength itself) is essential to expanding the design margin and benefiting from a probabilistic design approach.

36 MATERIALS SCIENCE↗