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The R&D on SiC/SiC composites under the broader approach (BA) activities between Japan and the EU for fusion DEMO developed a fundamental database of mechanical (Task-1) and physical/chemical (Task-2) properties, with a primary target of the application of SiC/SiC composites as functional structure to be used in the dual coolant breeding blanket concept. This paper aims to summarize previous 10-years activities of the R&D of Japan and to provide the key deliverables toward the DEMO design. In Task-1, good creep and fatigue durability were first demonstrated. Besides, in-plane and inter-laminar strength anisotropy maps at elevated temperatures were comprehensively identified. In parallel, the irradiation effects of SiC materials were specifically determined as input parameters of the analytical model to provide for the irradiation-induced residual stresses. In Task-2, the apparent dose-dependence of the radiation-induced electrical conductivity and the indicative radiation-induced electrical degradation was identified by various irradiation sources. In addition, good gas confinement was identified. Furthermore, no accelerated corrosion for duration of 3000 h at below 1173 K was first demonstrated. With these achievements, it is suggested that the in-vessel component technology, e.g., material corrosion database development, activated corrosion product evaluation code development, compact module tests for validation of the key functions of the components, technology integration assessment for fusion nuclear tests, etc., should be further developed toward DEMO in near-term.

Irradiation creep beyond the transient regime was investigated for various silicon carbide (SiC) materials. The materials examined included polycrystalline or monocrystalline high-purity SiC, nanopowder sintered SiC, highly crystalline and near-stoichiometric SiC fibers (including Hi-Nicalon Type S, Tyranno SA3, isotopically-controlled Sylramic and Sylramic-iBN fibers), and a Tyranno SA3 fiber–reinforced SiC matrix composite fabricated through a nano-infiltration transient eutectic phase process. Neutron irradiation experiments for bend stress relaxation tests were conducted at irradiation temperatures ranging from 430 to 1180 °C up to 30 dpa with initial bend stresses of up to ∼1 GPa for the fibers and ∼300 MPa for the other materials. Initial bend stress in the specimens continued to decrease from 1 to 30 dpa. Analysis revealed that (1) the stress exponent of irradiation creep above 1 dpa is approximately unity, (2) the stress normalized creep rate is ∼1 × 10 −7 [dpa −1 MPa −1 ] at 430–750 °C for the range of 1–30 dpa for most polycrystalline SiC materials, and (3) the effects on irradiation creep of initial microstructures—such as grain boundary, crystal orientation, and secondary phases—increase with increasing irradiation temperature.

Nuclear-grade silicon carbide (SiC) composite material was examined for mechanical and thermophysical properties following high-dose neutron irradiation in the High Flux Isotope Reactor at a temperature range of 573–1073 K. The material was chemical vapor-infiltrated SiC-matrix composite with a two-dimensional satin weave Hi-Nicalon Type S SiC fiber reinforcement and a multilayered pyrocarbon/SiC interphase. Moderate (1073 K) to very severe (573 K) degradation in mechanical properties was found after irradiation to >70 dpa, whereas no evidence was found for progressive evolution in swelling and thermal conductivity. The swelling was found to recover upon annealing beyond the irradiation temperature, indicating the irradiation temperature, but only to a limited extent. The observed strength degradation is attributed primarily to fiber damage for all irradiation temperatures, particularly a combination of severe fiber degradation and likely interphase damage at relatively low irradiation temperatures.

The irradiation creep behavior of nano-powder sintered silicon carbide was investigated using the bend stress relaxation method under neutron irradiation up to 1.9 dpa. The creep deformation was observed at all temperatures ranging from 380 to 1180 °C mainly from the irradiation creep but with the increasing contributions from the thermal creep at higher temperatures. The apparent stress exponent of the irradiation creep slightly exceeded unity, and instantaneous creep coefficient at 380–790 °C was estimated to be ∼1 × 10 −5 [MPa −1 dpa −1 ] at ∼0.1 dpa and 1 × 10 −7 to 1 × 10 −6 [MPa −1 dpa −1 ] at ∼1 dpa. The irradiation creep strain appeared greater than that for the high purity SiC. Microstructural observation and data analysis indicated that the grain-boundary sliding associated with the secondary phases contributes to the irradiation creep at 380–790 °C to 0.01–0.11 dpa.

To identify a comprehensive stress envelope, i.e., strength anisotropy map, of silicon carbide fiber-reinforced silicon carbide matrix composite (SiC/SiC composite) for practical component design, tensile and compressive tests were conducted using the small specimen test technique specifically tailored for high-temperature use. In-plane shear properties were, however, estimated using the off-axial tensile method and assuming that the mixed mode failure criterion, i.e., Tsai–Wu criterion, is valid for the composites. The preliminary test results indicate no significant degradation to either proportional limit stress (PLS) or fracture strength by tensile loading at temperatures below 1000 °C. A similarly good tolerance of compressive properties was identified at elevated temperatures, except for a slight degradation in PLS. With the high-temperature test data of tensile, compressive and in-plane shear properties, the stress envelopes at elevated temperatures were finally obtained. A slight reduction in the design limit was obvious at elevated temperatures when the compressive mode is dominant, whereas a negligibly small impact on the design is expected by considering the tensile loading case.

Silicon carbide (SiC) continuous fiber-reinforced, SiC-matrix composites (SiC/SiC composites) are industrially available materials that are promising for applications in nuclear environments. The SiC/SiC composites consisting of near-stoichiometric SiC fibers, stoichiometric and fully crystalline SiC matrices, and the pyrocarbon (PyC) or multilayered PyC/SiC interphase between the fiber and the matrix are considered particularly resistant to very high radiation environments. This paper provides a summary compilation of the properties of these composites, specifically those with the chemically vapor-infiltrated (CVI) SiC matrices, including newly obtained results. The properties discussed are both in unirradiated condition and after neutron irradiation to intermediate fluence levels (most data are for

Unidirectional silicon carbide (SiC)-fiber-reinforced SiC matrix (SiC/SiC) composites fabricated by a nano-infiltration and transient eutectic-phase (NITE) process were irradiated with neutrons at 600 °C to 0.52 dpa, at 830 °C to 5.9 dpa, and at 1270 °C to 5.8 dpa. The in-plane and trans-thickness tensile and the inter-laminar shear properties were evaluated at ambient temperature. The mechanical characteristics, including the quasi-ductile behavior, the proportional limit stress, and the ultimate tensile strength, were retained subsequent to irradiation. Analysis of the stress–strain hysteresis loop indicated the increased fiber/matrix interface friction and the decreased residual stresses. The inter-laminar shear strength exhibited a significant decrease following irradiation.

A silicon carbide fiber reinforced silicon carbide matrix (SiC/SiC) composite is a promising candidate for a fusion DEMO blanket. To develop design codes in practical use of them, strength anisotropy is an important issue to be clarified and therefore this study aimed to evaluate the failure behavior of the SiC/SiC composites to provide a strength map. For this purpose, detailed tensile, compressive and in-plane shear failure behaviors were evaluated by the acoustic emission (AE) technique for a plain–weave (P/W) chemically vapor-infiltration (CVI) SiC/SiC composite. The AE results distinguished damage accumulation processes by separately discussing localized variations of power within a time series by wavelet analysis. Of particular emphasis is that matrix cracking occurred prior to the proportional limit stress (PLS) by both tensile and compressive tests. This is because the rough-surface of SiC fibers resulted in the strong frictional stress at the fiber/matrix (F/M) interface, showing linearity in the stress–strain curve beyond the actual matrix cracking stress (i.e., possibly no sliding of the fibers at the F/M interface). In this paper, an updated failure envelope was provided by referring the true matrix cracking stresses as more realistic and reasonable failure criteria.

This paper reviews recent achievements as to "nuclear-grade" SiC composites in particular for materials-system integration. SiC composite component development are reviewed including VHTR control rod scale model and compact intermediate heat exchanger scale mode by current joining and assembly techniques. Joining methods for SiC to metal and results of characterization of joint shear strength by the torsion tests using small specimens were also reviewed. The recent results of neutron irradiation experiments were also reviewed including detailed analysis of mechanical properties, irradiation creep and preliminary results on tritium behavior in SiC.

High purity chemically vapor-deposited (CVD) silicon carbide (SiC) and near-stoichiometric SiC fiber, chemically vapor-infiltrated (CVI) SiC matrix composite were evaluated following neutron irradiation to ∼28 dpa at 300 and 650 °C and to ∼41 dpa at 800 °C, respectively. The irradiated swelling, thermal conductivity, and elastic modulus indicated no additional changes in these properties at high fluences after saturation at low fluences. With a statistically meaningful sample population, no change in flexural strength of CVD SiC was observed after 300 °C irradiation. A slight decrease in strength was observed after 650 °C irradiation but was attributed to an experimental artifact; specifically, a reaction between samples and the capsule components. The Hi-Nicalon™ Type-S, CVI SiC composite retained the pre-irradiation strength and the non-linear fracture mode. The electrical resistivity measurement revealed a relatively minor effect of irradiation. Overall, irradiation-insensitivity of the high purity SiC ceramics and composite to neutron irradiation to doses 30–40 dpa at temperatures 300–800 °C was demonstrated.

Six different composite materials of various near-stoichiometric silicon carbide (SiC) fiber reinforcements and pyrolytic carbon or SiC/pyrolytic carbon multilayer interphases were neutron-irradiated to ∼6 × 10 25 n/m 2 ( E > 0.1 MeV) at nominal temperatures of 800 °C and 1300 °C, and tested for tensile properties at room temperature. Only insignificant or very minor modifications to the tensile strength were realized. However, statistical analysis on relatively large specimen populations revealed minor but statistically significant strength degradation for some composites. From 50 to 150 nm appeared to be within the optimum PyC interphase thickness range for the SiC fibers used in terms of tensile properties. The misfit stresses present in the unirradiated samples were significantly reduced after irradiation. The change in misfit stress may be attributed to the irradiation-induced modification of coefficient of thermal expansion or potential differential swelling between the fibers and the matrix. True matrix cracking stress estimated from the proportional limit stress and misfit stress did not appear to degrade by neutron irradiation.

The microstructural evolution of SiC/SiC composites after Si{sup 2+} with/without He{sup +} ion irradiation was studied using transmission electron microscopy. The temperature, displacement damage level, and He/dpa ratio were 1273/1673K, 10/100dpa and 0/60appmHe/dpa, respectively. In 10dpa single-ion irradiation, no cavity was detected at 1273 and 1673K. But cavities were observed locally at 1673K, 100dpa. In dual-ion irradiation, cavities were observed at 1673K, 100dpa. Helium bubbles (d

Silicon carbide (SiC) matrix composites reinforced by SiC fibers is a candidate structural material of fusion gas-cooled blanket system. From the viewpoint of material designs, it is important to investigate the swelling by irradiation, which results from the accumulation of displacement damages. In the fusion environment, (n,) nuclear reactions are considered to produce helium gas in SiC. For the microstructural evolution, a dual-ion irradiation method is able to simulate the effects of helium. In the present research, 1.7 MeV tandem and 1 MeV single-end accelerators were used for Si self-ion irradiation and helium implantation, respectively. The average helium over displacement per atom (dpa) ratio in SiC was adjusted to 60 appm/dpa. The irradiation temperature ranged from room temperature to 1400C. The irradiation-induced swelling was measured by the step height method. Helium that was implanted simultaneously with displacement damages in dual-ion irradiated SiC increased the swelling that was larger than that by single-ion irradiated SiC below 800C. Since this increase was not observed above 1000C, the interaction of helium and displacement damages was considered to change above 800C. In this paper, the microstructural behavior and dimensional stability of SiC materials under the fusion relevant environment are discussed.

The authors have proposed a new divertor concept using SiC composite with directional high thermal conductivity enhanced with fiber as substrate of the divertor structure in fusion reactor. In this study, unidirectional SiC composite with pitch-based carbon fibers (UD-Cf/SiC) was fabricated as the model material. The thermal conductivity (or thermal diffusivity) in directions parallel (0°), inclined (45°), and transverse (90°) to the Cf orientation was measured by the laser flash method. The results were compared with monolithic SiC (mono-SiC) in order to evaluate the enhancement of thermal conductivity by an introduction of Cf. Although the thermal conductivity of the UD-Cf/SiC in directions of 45° and 90° was relatively lower than that of the mono-SiC, that of the UD-Cf/SiC in direction of 0° was ten times as large as that of the mono-SiC.

The effects of irradiation-induced swelling of constituents on tensile properties of advanced SiC/SiC composites were examined. After the swelling of the fiber and matrix ion-irradiated up to 1dpa at 1000°C was measured, the modified four phase model was applied in order to estimate the residual stress in each constituent. The swelling mismatch was obtained between Hi-Nicalon™ Type-S fiber (0.27%) and ICVI-matrix (0.48%), which increases the residual stresses according to the model. These increases of the residual stresses were roughly consistent with the tensile stress-strain behavior of the same SiC/SiC composites after neutron irradiation up to 1dpa at 1000°C and the behavior of the misfit stress obtained by the hysteresis loop analysis methodology, which is related with the residual stress. These results suggest that irradiation-induced residual stress caused by the differential swelling of each constituent may affect the tensile properties in this irradiation condition.

Silicon carbide composites (SiC/SiC) are attractive candidate materials for structural and functional components in fusion energy systems. The effect of neutron irradiation on damage tolerance of the nuclear grade SiC/SiC composites (plain woven Hi-Nicalon™ Type-S reinforced CVI matrix composites multilayer interphase and unidirectional Tyranno™-SA3 reinforced NITE matrix with carbon mono-layer interphase) was evaluated by means of miniaturized single-edged notched beam test. No significant changes in crack extension behavior and in the load-loadpoint displacement characteristics such as the peak load and hysteresis loop width were observed after irradiation to 5.9 × 1025 n/m2 (E > 0.1 MeV) at 800°C and to 5.8 × 1025 n/m2 at 1300°C. By applying a global energy balance analysis based on non-linear fracture mechanics, the energy release rate for these composite materials was found to be unchanged by irradiation with a value of 3±2 kJ/m2. This has led to the conclusion that, for these fairly aggressive irradiation conditions, the effect of neutron irradiation on the fracture resistance of these composites appears insignificant.

Polymer impregnation and pyrolysis (PIP) is one of the most attractive fabrication processes for silicon carbide (SiC) composites due to the shape flexibility, mass production and relatively low cost. In particular, advanced PIP SiC/SiC composite with high-crystallinity and nearstoichiometric composition is expected to have superior thermo-mechanical properties including good oxidation resistance, due to the reduction of impurities and well-organized crystal structure. Additionally, by applying a thin carbon interphase by chemical vapor infiltration (CVI), control of the crack propagation and oxidation resistance are also achieved. In this study, a CVI + PIP hybrid process based on the recently developed stoichiometric PIP process was performed. Specifically, matrix crystallization was enhanced by heat treatment in Ar, and its effect on microstructures and mechanical properties were evaluated. Stoichiometric SiC/SiC composites exhibit superior flexural strength up to 1573 K in Ar and 1273 K in air. This is because the stoichiometric composition in PIP-SiC matrix reduces inner oxidation by impurities. Also, the thin pyrolytic carbon interphase tailored by CVI process effectively controls crack propagation at fiber and matrix interphase. In a similar manner, the microstructure of the stoichiometric PIP-SiC matrix, constructed by the mixture of amorphous SiC and highly crystalline SiC, was stable against the high-temperature heat exposure up to 1773 K in Ar. In particular, stoichiometric SiC/SiC composites heated at 1773 K in Ar provides superior stability of mechanical properties up to 1573 K even in air atmosphere, although extensive crystallization, in the case of heat treatment at 1973 K in Ar, caused brittle composite fracture.