Investigations and numerical modeling of mechanical properties of tempered martensitic steel Eurofer97 at various loading rates, temperatures and after spallation irradiation

The reduced activation tempered martensitic steel Eurofer97 is a reference steel for a structural applica-tions in fusion reactors. The first-wall and blanket materials will be subjected to high thermal and neutron fluxes and will experience very complex, time-dependent mechanical loading. Owing to impinging neutrons in materials, points defects and gasesous impurities (hydrogen and helium) are created and accummulated in the form of small defect clusters in the microstructure altering the mechanical properties. Notably, fracture toughness decreases as strength increases. Eurofer97, being a body centered cubic alloy, presents a ductile-to-brittle transition temperature T0 that shifts to higher temperatures after irradiation. The main objective was to study the loading rate and irradiation effects on plastic flow and fracture properties of Eurofer97. Tensile and fracture tests were performed at temperatures in the transition region, at low and high loading rates on unirradiated material. Tensile properties of irradiated material were assessed after irradiation in the Swiss neutron spallation source SINQ to a dose of about 11 dpa and helium content of 500 appm at about 250 Â°C. The information gathered from the mechanical tests was used either as input in finite element models of fracture specimens, or as benchmark data to calibrate and verify the predictions of the models. Fractographic observations were also conducted. The tensile tests on unirradiated Eurofer97 showed a strong temperature dependence and strain rate sensitivity of the stress at low temperature, consistent with a mechanism of nucleation and propagation of double kink on screw dislocation. At high loading rate, the strain rate hardening was partially compensated by thermal softening due to quasi-adiabatic heating. The tensile properties after irradiation showed strong irradiation hardening (increase of the yield stress) accompanied by a drastic decrease of uniform elongation. The constitutive behavior at large strains, representative of those at crack tip, was obtained with an inverse method, based on finite element (FE) models of tensile specimens, developed to derive the true stress-strain curves from the load-displacement ones. These curves were used as input for the FE models of fracture specimens. Comparative fractographic observations on unirradiated and irradiated specimens did not reveal any strong effect of irradiation or helium on fracture mechanism, which remains transgranular cleavage. This observation indicates that higher helium concentration than 500 appm is necessary to initiate intergranular cleavage by helium bubble precipitation on grain boundaries. Dynamic fracture tests were performed on unirradiated Eurofer97. A shift of about 10 Â°C of T0 by one order of magnitude in loading rate was determined, which was in good agreement with results obtained on different ferritic steels. Static fracture toughness tests were also performed on disk compact tension specimens that can be accommodated in irradiation tubes of SINQ. Different FE models of fracture specimens were developed to include strain-rate sensitivity of flow stress, heating resulting from the plastic work in the fracture process zone and loading rate. The structure of the stress field at the crack tip was studied and the temperature dependence of a lower bound to toughness data in the transition was reconstructed using a calibrated criterion of local approach to brittle fracture.

Constitutive behavior and fracture properties of tempered martensitic steels for nuclear applications

Raul Alejandro Bonadé

In this study, the tensile and fracture properties and the microstructure of the reduced-activation tempered martensitic steel Eurofer97 have been investigated. This technical alloy is a 9%Cr steel developed within the European fusion material research program. To a lesser extend, the plastic flow properties of a equiaxed ferritic Fe9%Cr model alloy were also studied for comparison with those of the tempered martensitic structure. The main objectives of this work are described hereafter: to correlate the microstructural features with the plastic flow properties measured by the tensile tests for both the Eurofer97 steel and the model alloy. The correlation established should be reflected in a physically-based model of plastic flow. to study the fracture properties of the Eurofer97 steel in details in the lower ductile-to-brittle transition region. to calculate with finite element modeling the stress fields at the crack tip. This information is further used in conjunction with a local approach model for quasi-cleavage to reconstruct the fracture toughness-temperature curve. Tensile tests were carried out at different imposed nominal strain rate at several temperatures from 77K up to 473K, on both the Eurofer97 steel and the Fe9%Cr model alloy. The temperature dependence of the yield stress was precisely determined. As expected for body-centered cubic (BCC) materials, a strong increase of the yield stress by decreasing temperature, below 200 K, was observed. At higher temperatures, the temperature dependence of the yield stress was found much weaker, being associated with the temperature dependence of the shear modulus. Efforts were made to analyze in details the post-yield behavior (strain-hardening) as a function of temperature. The post-yield behavior was modeled using the Kocks phenomenological model based on the competition of storage and annihilation of dislocations. While this model was originally developed for face-centered cubic (FCC) metals where the rate-controlling mechanism of dislocation motion is the dislocation-dislocation interaction, we used is model in the high temperature domain (T>200K) of BCC materials, to model the strain-hardening evolution of the Eurofer97 steel and the model alloy. The values obtained for the key parameters of the model, namely the dislocation mean free path and annihilation coefficient, were found consistent with the microstructural features. The parameters temperature-dependence observed was also consistent with the physics of two basic mechanisms of dislocation storage and annihilation (dynamical recovery). For the low temperature domain, the strain-hardening model was modified to account for the strong Peierls lattice friction, based on an original idea of Rauch. Transmission electron microscopy observations were done to characterize the undeformed microstructures and their evolution with strain. A clear correlation was established between the stress-dependence of the strain-hardening and the microstructures. Fracture toughness tests on the Eurofer97 steel were performed with 0.2T C(T) and 0.4T C(T) specimens in the lower transition. Five temperatures were selected at which many tests were repeated to determine the amplitude of the inherent scatter of quasi-cleavage. The temperature were chosen in such a way that the measure fracture toughness remain below 150 MPa m1/2, which correspond for the 0.4T C(T) at a M value larger than 70 at the highest temperature. Such a M value for 0.4T C(T) specimens is known to ensure enough constraint. An attempt to analyze the experimental data in the framework of the master-curve approach by following the ASTM E-1921 standard was done. It was clearly demonstrated that the assumed shape of the toughness-temperature curve as described in the ASTM E-1921 standard for the reactor pressure vessel steels is not adequate for the tempered martensitic Eurofer97 steel, which present a particularly steep transition. Our Eurofer97 fracture database was then compared to the existing one on another similar steel, the F82H. Differences in the amplitude of the scatter of both steels was found while the lower bound of the toughness-temperature curve, describing the 1% failure probability was shown to be the same. 2D finite element simulations of the compact tension specimens were performed at various temperatures using the constitutive laws determined previously. The stress field around the crack tip were calculated and used to determine a local criterion of quasi-cleavage. The criterion is defined by the attainment of a critical stress encompassing a critical area. The lower bound of the toughness-temperature curve was then successfully reconstructed by using this local criterion. Finally, the relationship between the critical area and the applied stress intensity factor for the C(T) specimen was shown to follow a power law whose coefficients are dependent on the real dimensions of the specimen. Such a relationship allows scaling the C(T) toughness data from one size to another in case of in-plane constraint loss.

EPFL2006

Finite element modeling and experimental study of brittle fracture in tempered martensitic steels for thermonuclear fusion applications

Pablo Federico Mueller

In this work we have studied brittle fracture in high-chromium reduced activation tempered martensitic steels foreseen as structural materials for thermonuclear fusion reactors. Developing the adequate materials that can withstand the severe irradiation conditions of the burning plasma in a future fusion reactor is one of the major challenges to be solved in order to make profit from the great advantages of thermonuclear fusion as an energy source. High-chromium tempered martensitic steels such as F82H and the most advanced version Eurofer97 are among the main candidate materials for structural applications in future fusion power plants due to low irradiation-induced swelling, good mechanical and thermal properties, and reasonably fast radioactive decay. The most concerning drawback of these kind of steels is irradiation embrittlement, which is manifested by a ductile-to-brittle transition temperature shift to higher temperatures after irradiation whose amplitude depends on the irradiation conditions (temperature, neutron flux, neutron fluence, etc). The aim of this work was to study and model brittle fracture in the ductile-brittle transition region of this kind of steels in the as-received unirradiated conditions. It is necessary to be able to transfer laboratory specimen fracture data to real components and structures in order to assess the performance of these steels in the different operating and transient conditions they could find during the operation life of a fusion reactor. In order to do so, the specimen geometry effects and specimen size effects on measured fracture toughness need to be properly understood, taken into account and predicted with an appropriate model. In particular, specimen size effect on measured toughness is a major concern for the nuclear materials research community owing to the limited irradiation volume in current and planed materials irradiation facilities. The main results of this PhD work are summarized below. The microstructure of Eurofer97 and F82H has been characterized and compared by means of optical microscopy, scanning electron microscopy, transmission electron microscopy and energy-dispersive X-ray spectroscopy in order to identify microstructural features that could play a role in the measured fracture toughness. Both steels have similar but slightly different chemical composition and final heat-treatments but the prior austenitic grain size measured in F82H is approximately 8 times larger than in Eurofer97. It was shown that the alloying element Tantalum, added to stabilize the austenite grain size, played a different role in both steels. After a careful analysis of the particles present in both steels, it was found that Tantalum in Eurofer97 formed carbides of an average size around 100 nanometers. In contrast in F82H it did not form small carbides but formed big oxide inclusions with a size up to 30 µm. These large particles do not effectively pin the grain boundaries. The different behavior of Tantalum in these steels is believed to be mainly a consequence of the larger content of Oxygen present and the smaller amount of Aluminum in F82H compared to Eurofer97. The Master-Curve ASTM-E1921 standard is a method initially developed to determine the ductile-to-brittle transition reference temperature, T0, in fission reactor ferritic steels from a small number of experiments. In this work the applicability of the Master-Curve method to reduced activation tempered martensitic steels such as Eurofer97 and F82H was studied in detail. Fracture tests with pre-cracked sub-sized compact tension specimens (three different sizes, 0.18T, 0.35T and 0.87T of Eurofer97) were carried out in the temperature range [-196 °C, -40 °C]. The toughness-temperature behavior and scatter were shown to deviate from the ASTM-E1921 standard predictions near the lower shelf. Using the method of maximum likelihood, the athermal component of the Master-Curve was calculated to better fit our fracture toughness data from the lower to the middle transition region. We showed that these Master-Curve adjustments are necessary to make the T0 values obtained near the lower shelf with 0.35T size C(T) specimens consistent with those obtained in the middle transition region with 0.87T C(T) specimens. The ASTM-E1921 specimen size limitations, setting the maximum toughness measurable with a given specimen size, were found to be too lenient for this kind of steels. This problem was especially evident in fracture toughness data of Eurofer97 and F82H obtained in the upper transition temperature range with two different specimen sizes. Thus a more stringent specimen size requirement was proposed to avoid inconsistent transition temperature determinations. A promising local fracture model with the potential of predicting cleavage fracture toughness was studied. Finite element simulations were undertaken for compact specimens, notched specimens and tensile specimens of Eurofer97 steel tested from 20 °C down to -197 °C. Three and two dimensional as well as axisymmetric simulations were run in order to calculate the stress and strain fields at the onset of brittle fracture. For each tested temperature, the calculated load-displacement curves were found to reproduce very well those of the experiments. A local approach fracture criterion was studied. This criterion states that when the maximum principal stress is larger than a critical stress within a critical volume ahead of the crack tip, notch or neck, cleavage is triggered leading to macroscopic fracture of the specimen. It was shown that this model is able to predict the minimum fracture load of the notched specimens with the same values of critical stress and critical volume that were calibrated to predict the lower bound of fracture in compact specimens. This local approach model was also successfully used to predict the strong size effect observed experimentally in pre-cracked compact tension specimens in the upper transition region. The critical fracture stress determined in the standard tensile specimens was found higher than that of the fracture specimens. It was suggested that this difference stems from a significant difference in the stress state between the different specimens (triaxiality). Finally, the comparison between the overall fracture behavior in the transition between F82H and Eurofer97 steels indicated that these two materials are quite similar. A difference in the reference temperature T0 of about 20 °C was found, with a nominal value of -100 °C and -80 °C for F82H and Eurofer97 respectively. However, some excessive scatter in the toughness data was found in F82H with more data points than expected lying below the 1% tolerance bound; this was not observed in Eurofer97. From an engineering point of view, the entire fracture databases of these two steels are encompassed practically by the same lower tolerance bound.

EPFL2009

Assessment of mechanical properties in unirradiated and irradiated zircaloys and steels with non-standard tests and finite element calculations

Emiliano Campitelli

Nuclear materials have been successfully employed in commercial fission reactors for many decades. Research and material development for advanced fission system and future thermo-nuclear fusion reactors have acquired maturity while great challenges remain to be taken up. The goal of the material scientist is to understand the way neutron irradiation and aggressive reactor environment alter the original material properties and to safely manage the operation conditions for each particular reactor component. In the framework of surveillance programme, the need has arisen to design experimental methods to be used with a limited amount of material for Post Irradiation Examination (PIE) of reactor components to test the integrity of those on a regular time basis. Having to deal with radioactive material, it is particularly important to devise experimental testing procedures as simple as possible but from which reliable information can be drawn. Within materials development programme, irradiations have continuously been performed either in reactors or with particle accelerators. In both cases, the irradiation volumes are usually limited. The concern was to optimize the volume of the irradiated samples in order to increase their number to obtain a good statistical representation of their mechanical behavior after irradiation, and to have a very definite and homogeneous damage dose and irradiation temperature. The concerns explained above originated the development of small-scale specimen testing methods. Advantage is taken of the fact that, within size and geometry limitations, some mechanical properties of a sample are independent of its absolute size. In this way it is possible to perform mechanical tests on samples of reduced volume that represents big advantages to face the aforementioned challenges. Non-standard test on very small specimen have also been proposed to extract mechanical properties of the bulk. If these non-standard testing methods are to be employed for PIE, it becomes necessary to develop modeling tool to understand under what circumstances they can provide useful information and specially how to obtain it. Finite element modeling (FEM) of the non-standard tests has played a key role in this sense, providing a link between standard test analysis and that of the non-standard ones. The goal of this work was to implement finite element models for non-standard tests to ultimately study the mechanical properties of Zircaloy cladding tube and tempered martensitic steels in the unirradiated and irradiated condition. One model was developed for ring tensile tests. It was first validated with a quite ductile iron-chromium ferritic alloy, for which ring and uniaxial tensile test were performed at room temperature. Using the constitutive behavior determined from the uniaxial tensile tests, the load – displacement curves of the ring tensile tests were very well reproduced. Another model was developed for the so-called small ball punch test, which consists in deforming a 3 mm diameter disk clamped between two dies with a ball puncher and to record the load – displacement curve. In order to validate the model, a series of ball punch tests and of tensile tests were carried out on the austenitic steel 316L at room temperature. In this last case, the ball punch test curves were also well reconstructed with the model. Based upon a simple analysis and simulation results, we showed that it is possible to obtain, by ring tensile tests, a quick and accurate assessment of the constitutive behavior of an unknown material, simply by processing the experimental force-elongation data in the same way as for uniaxial tests, taking half the ring perimeter as initial length and twice the ring cross section as the sample cross section. The ring tensile test method was used to determine the hoop mechanical properties of Zircaloy tubes used in fission reactors. Tensile tests were also performed in the axial direction of the Zircaloy tubes. Differences between the yield stress as well as the post-yield behaviors in the axial direction and those in the circumferential direction of the tube could be measured reflecting some component of the anisotropy of the tube. Ball punch specimens were cut also out of the tube in the radial direction and tested. Using the FE model for punch test, in which the anisotropy of the mechanical properties are taken into account through the Hill's theory, the values of the Hill's yield function parameters were estimated. The irradiation hardening of neutron irradiated Zircaloy tube was finally determined. The ball punch test model was extensively used for numerical investigations, to determine how the constitutive behavior of the materials (uniaxial true stress – true strain) employed as input acts in combination with other experimental factors (specimen thickness, friction coefficient) in mediating the shape of the experimental curves. In the light of the results, we derived calibrations between parameters of the non-standard and standard tests. For instance we proposed a new approach to determine the yield stress from the ball punch test. We also showed how the slope of the punch tests scales with the average flow stress of the material. The calibrations proposed in the past by authors and published in the open literature have been revisited and critically reviewed. Based upon the findings of the numerical studies, we propose a given methodology to unambiguously evaluate the material constitutive behavior of a material in a case where the only available data comes from various non-standard tests. Experimental ball punch test results obtained on proton-irradiated specimen (0.5 dpa and Tirr = 523 K), of the tempered martensitic steel, EUROFER97, have been obtained. The irradiation hardening was found equal to about 150 MPa, consistently with previous data on similar steels and irradiation conditions. From the simulations of the ball punch test curves of the irradiated specimens, it was concluded that the irradiation does not affect the strain hardening at relatively low fluence.

EPFL2005