STUDY ON HIGH TEMPERATURE DEFORMATION CHARACTERISTICS OF Cu-0.23%Al2O3 DISPERSION-STRENGTHENED COPPER ALLOY

In order to deeply understand the high temperature deformation behaviors of Cu-0.23%Al2O3 (volume fraction) alloy, the changes of flow stress and microstructure for this alloy after deformation at high temperatures were investigated by using the Gleeble-1500 hot simulator, metallographic microscope and transmission electron microscope. The results show that the flow stress will change significantly with the thermal compression conditions and is mainly divided into three different stages. In addition, the average activation energy and other material parameters of this alloy deformed at high temperatures were obtained, based on them, the constitutive equation of the peak value yield stress-strain rate-temperature was also established. With increasing of compression temperature, the size and number of dynamic recrystallization grains are increased. However in the case of isothermal compression, with increasing of strain rates, the evolution of metallographical microstructures becomes disequilibrium, the size of subgrain is gradually decreased to about 0.5-1 mu m, and the dislocation density is increased at first, and then decreased.

On the relationship between the microstructure and the mechanical properties of an ODS ferritic/martensitic steel

Amuthan Ramar

In the quest of materials for the first wall of the future fusion reactor, it has been shown that oxide dispersion strengthened (ODS) ferritic / martensitic (F/M) steels appear to be promising candidates. The inherent good mechanical properties supported by a good thermal conductivity, swelling resistance and low radiation damage accumulation of the base material, such as EUROFER97, are further enhanced by the presence of a fine dispersion of nanometric oxide particles. They would allow in principle for a higher operating temperature of the fusion reactor, above 550°C, which improves its thermal efficiency. In effect, their strength remains higher than the base material at high temperatures. There are however limitations to their application in the reactor, which relate to the intimate link between the microstructure and the mechanical properties. These limitations, such as an increased ductile to brittle transition temperature above room temperature relative to the base material, come directly from the role played by the oxide particles but also from their indirect impact on the overall microstructure, stemming from the procedure of elaboration of these materials. In addition, there is a lack of knowledge on their response to irradiation, which, even though it appears to be promising with a reduced irradiation induced hardening, is not very well understood. In this work we have developed and evaluated ferritic/martensitic steel, EUROFER97, strengthened by a dispersion of yttria particles. (1) The powder metallurgical process used to obtain it was optimized, (2) the basic mechanisms of hardening were identified and (3) the impact of irradiation on its microstructure and mechanical properties were investigated. In order to understand the behaviour of this class of material other oxide dispersion strengthened (ODS) ferritic/martensitic steels based on EUROFER97 and model alloys were also investigated. For the elaboration of the ODS steel the powders of atomized EUROFER97 and yttria are ball milled in a planetary ball mill and the material is compacted by hot isostatic pressing (HIP). The mechanical properties are evaluated by uniaxial tensile test, Charpy test and micro-indentation while the microstructure is investigated by optical microscopy, scanning electron microscopy and transmission electron microscopy. The focused ion beam (FIB) technique is also used. In the study of the ball milling it appears that the optimal time is 20 hours, as the X-ray peak broadening, crystallite size and hardness of the particles remain unchanged at longer times. Yttria nanoparticles clusters are no more detectable by X-ray after 2 hrs of milling, which is attributed here to their incorporation in the matrix, as opposed to dissolution in the matrix as is often suggested in the open literature. HR-TEM performed on the yttria particles before and after incorporation in the steel by ball milling shows that the yttria maintain its bcc equilibrium structure throughout the process. This could suggest that they are not dissolved during ball milling. We have clarified this point by a cross sectional examination of the EUROFER97 ball milled particles with 0.3wt% of yttria in an FIB. By X-ray EDS analysis it shows nanometric regions reach in yttrium and oxygen, which are the yttria particles embedded in the EUROFER97 particles, proving that they are not dissolved by ball milling. The mechanism at the origin of the alloy compaction during HIP was elaborated. The alloy compaction was done through HIPing at 1150°C for 2.5 hrs at a pressure of 190 MPa. This condition is shown to provide the highest bulk density, to a value close to 99.9%. In the optimization process, it is found that temperature plays a larger role than pressure for alloy compaction. The compaction appears to be mainly due to diffusion. Also, it appears that the ball milled particle size plays a major role in the alloy compaction. It is shown that smaller particles size induces better compaction, provided that the densification proceeds through diffusion flow. This further suggests to terminate the ball milling process by 20 hrs as the particles size reaches its minimum. The impact of the ball milling process on the mechanical properties was evaluated. EUROFER97 with and without ball milling, with and without oxide addition presents an average density around 99.8%. In the as received state, casted EUROFER97, atomized EUROFER97, ball milled EUROFER97 and ODS Yttria present microstructure morphology typical of tempered martensite, whereas ODS Ti presents a nano sized grain microstructure with an average grain size of 200 nm. Ball milling and HIPping does have a slight influence up to 400°C, due to the higher dislocation density induced by ball milling relative to casted EUROFER97. It becomes negligible above 400°C, since both casted and ball milled EUROFER97 present similar hardness and microstructure. In ODS Yttria, yttria presents an average particle size of 25 nm. In ODS Ti, Y-Ti-O presents an average particle size of 7 nm. In the following the identification of the hardening mechanisms in ODS F/M steels. A new model was developed to quantify the collective hardening due to different obstacles, assuming that they provide independent hardening mechanisms. The model helped identifying the dominating source of hardening in ODS F/M steels. The base of the model is the dispersion barrier strengthening model, which is given by Δσsparticle or defects = Mαμb(Nd)1/2 for the hardening due small defects or oxide particles and is given by Δσd-d = Mαμb(ρ)1/2 for the hardening due to dislocations. In this approximation, the total hardening is then given by Δσtotal = {(Δσd-d)2 + (Δσparticle or defects)2}1/2 . The model is used to explain the hardening due to oxides, dislocations and irradiation induced defects. It appears that dispersed oxides is dominating hardness up to 800°C, while following a heat treatment at 1000°C it is the dislocations that then dominate the hardness. Deformation mechanisms were investigated using differential strain rate experiments. The activation parameters, i.e. the activation volume and activation energy, were calculated. It appears that there is a decrease in the activation volume from room temperature to 400°C, which is less than 3%. At about 500°C there is a sudden drop in the activation volume that reaches a minimum at 600°C. With further increase in temperature, there is a significant raise in the activation volume. This abrupt decrease between 400°C and 600°C hints at a change in dislocation-rate controlling mechanism, marking two regimes, a low temperature one and a high temperature one. In situ TEM observations show that at low temperature the deformation is mainly due to the formation of the Orowan loops around the particle. At high temperature the activation energy is about 3.4 eV for ODS, whereas it is 1.3 eV for EUROFER97. The calculated activation energy corresponds well to the one of dislocation climb mechanism. This indicates that at high temperature the yttria particles could be overcome by climb, while at low temperature they are overcome by the Orowan mechanism. The peculiar response of the yield stress to irradiation for this class of material was rationalized using the total hardening model we developed. At a dose of 2 dpa, irradiation induced defects are higher in number density than the dispersed yttria particles, which although they are weaker than the yttria particles they can explain the significant hardening observed in the material. Conversely, the shallow impact of irradiation on ODS F/M steels at low doses, relative to base F/M steels, is explained by the fact that the amount of dispersoid is found to be higher than the density of irradiation induced defects.

EPFL2008

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

Deformation behaviour and microstructure of nanocrystalline electrodeposited and high pressure torsioned nickel

Florian Dalla Torre, Robin Schäublin, Philippe Spätig

Microstructural analysis and mechanical testing have been performed on two types of nanocrystalline (NC) Ni samples and compared to coarse-grained (CG) Ni. The NC electrodeposited (ED) Ni is characterized by a mean grain size of 21 nm, a narrow grain size distribution and the absence of dislocations observed in undeformed conditions. NC high pressure torsioned (HPT) Ni shows a mean grain size of 105 nm with a broad grain size distribution. Grains observed in transmission electron microscopy exhibit dislocations and dislocation cells. The mechanical properties deduced from tensile and indentation tests of NC ED Ni show a significantly higher strength than the one of NC HPT Ni. Both materials show a limited total plastic deformation of less than 5% and a quasi-linear decrease in the work hardening rate with increasing stress. Strain rate jump tests have shown for both materials similar strain rate sensitivities, which are one order of magnitude higher than in CG Ni. A significantly smaller apparent activation volume V,p has been measured for NC Ni as compared to CG Ni. NC ED Ni shows a decrease in Vap with increasing stress, while an increase of V-ap was measured for NC HPT Ni. Using the repeated stress relaxation technique, an effective activation volume and associated parameters describing the change in the mobile dislocation density have been estimated for NC ED Ni and CG Ni and are discussed in terms of the possible deformation kinetics. Results have shown that the apparent activation volume of NC ED Ni deduced from relaxation tests is more than three times higher than the one deduced from jump tests, while in CG Ni both methods give consistently similar values. This can be taken as an indication for a breakdown in the application of such analysis to 20 nm grain sized metals. (c) 2005 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

2005