Dynamic study of contact damping in martensitic stainless steels using nano-indentation

The study was undertaken to gain insight into the micro-mechanisms controlling plasticity at the micrometer scale of elastic-plastic metallic alloys. Dynamic nano-indentation tests, where a small harmonic force amplitude is superimposed during loading, referred to as continuous stiffness measurement (CSM), were performed to study contact damping in martensitic stainless steels with different heat treatments. The nano-indentation experiments were analyzed according to a specific protocol developed in this study, which results from a careful dynamic characterization done over a wide range of materials with significant different plastic flow properties, to separate the effect of the instrument from those of the material. The method was then applied to the tempered martensitic steel Eurofer97 in different tempering conditions. Based on the dynamic contact analysis developed for visco-elastic materials, we propose a new interpretation of the damping coefficient for materials like Eurofer97 dominated by an elastic-plastic behavior. The loss factor and the nano-hardness were correlated with the propensity of the material to plastic deformation, characterized by the average flow stress determined from tensile tests.

Microstructure of single crystal Ni-based superalloys during blade manufacturing process and creep deformation

Stéphane Pierret

The aim of the thesis is to obtain more understanding about the influence of plastic deformation on the microstructural changes observed in single crystal (SX) Ni-based superalloys using diffraction techniques. This work was organised around two main problematics: (1) rafting in turbine blades after the manufacturing process and (2) rafting and mosaicity evolution in two SX alloys with different composition during creep deformation. SX Ni-based superalloys are first choice materials for turbine blade application in land-based gas turbines and aero-engines. Superior mechanical properties of these materials at high temperatures are achieved due to the optimisation of the alloying composition and the microstructure. SX Ni-based superalloy turbine blades solidify by dendritic solidification with dendrites aligned along the directions of lowest Young modulus (interdendritic spacing around 300μm). At the end of the manufacturing process, the microstructure consists of high volume fraction of cubic γ’ precipitates (around 500nm) coherently embedded in the γ matrix. However specific parts of engine-ready turbine blades exhibit directionally coarsened γ’ precipitates in a preferred direction (rafting) without the influence of an applied load. It is of prime importance to understand the origin of rafting prior to the introduction of the blades in the engine since rafting can alter the mechanical properties of the alloy. Chemical segregations and the introduction of plastic deformation prior to thermal treatments were identified as potential driving force for rafting during load-free high temperature annealing. Most of the SX Ni-based superalloys used in the current blade production in Alstom contain significant amount of refractory elements which are expensive and increase the density of the alloy. To answer the demand of cheaper and lighter components, Alstom launched a development program to design novel SX superalloys. One of these projects led to the production of a Re-free superalloy, so-called MD2. Extensive mechanical investigations on MD2 are on-going and compared to the behaviour of the MK4HC alloy (3wt% Re) currently used in turbine blade production. One of the major differences in terms of mechanical properties between Re-containing and Re-free SX alloys is the faster kinetics of coarsening and rafting during creep deformation at high temperature in the latter alloys. It prevented so far their application in the hottest areas in gas turbines. It is therefore of utmost importance to acquire more knowledge about the mechanisms associated with the microstructure evolution during creep of the new MD2 SX alloy in comparison with the MK4HC alloy. The evolution of the lattice parameter misfit in different directions with respect to the applied load during creep deformation was associated with the evolution of the microstructure from cubic to elongated γ’ precipitates It could be shown that rafting occurs after the cooling stage following the solution heat treatment (SHT) during the manufacturing of the blade with investigations of the microstructure. The influence of chemical segregations on rafting was excluded with the investigation of the blade alloy composition in different parts of the blade cooled from the SHT and diffraction measurements in stress-relieved combs prepared from the same blade. The formation of a rafted microstructure during the manufacturing process was associated with the formation of plastic strains during cooling after the SHT. This was confirmed after gathering results from investigations of the microstructure, simulation of the cooling stage and neutron diffraction measurements on the blade. The investigations of the microstructure performed on the engine-ready blade revealed an inversion of the γ’ raft orientation below (parallel to [001]) and above the platform of the blade (perpendicular to [001]). This was attributed to an inversion of the sign of residual strain between the previously mentioned positions as revealed by neutron diffraction measurements performed along the airfoil of the blade cooled after the SHT. Microscopy also showed that the rafted microstructure was more pronounced below the platform (long γ’ rafts) than above the platform (shorter γ’ rafts with retained cubic precipitates). The concept of the threshold plastic strain necessary to induce rafting during annealing subsequent to plastic deformation was used to describe the difference in rafted microstructure. It is suggested that plastic strains largely exceed the threshold below the platform leading to fully formed rafted microstructure. On the other side, plastic strains of the order to the threshold strain are suggested above the platform in order to explain the partially formed rafted microstructure Neutron diffraction measurements revealed that the lattice parameter misfit was larger in the MK4HC than in the MD2 alloy at 20°C in the unloaded state. The larger misfit in the MK4HC alloy was attributed to the larger concentration of elements dissolving in the γ phase and to the presence of Re. During creep deformation, coherency stresses are relieved at the γ/γ’ interface in the γ channels perpendicular to the applied load by dislocations. On the other hand, dislocations increase the internal stress at the γ/γ’ interface in the γ channels parallel to the applied load. This leads to the rafting of the γ’ precipitates perpendicular to the applied load. This was observed in the MK4HC. The absence of clear misfit evolution in the MD2 alloy was attributed to the anomalous microstructure at the beginning of the creep deformation. The mosaicity of the MK4HC and MD2 alloys revealed crystallographic misorientation between neighbouring dendrites up to 0.5°. The misorientation was associated with the presence of dislocations in the regions between the dendrites formed during the dendritic solidification of the alloys from existing work. It was shown that the composition of the SX alloys and short periods at high temperature in the unloaded state had only little influence on the misorientation between neighbouring dendrites. Upon creep loading to 180MPa, the mosaicity markedly changed in the two SX alloys independent of the creep temperature. In particular, the number of single misoriented domains measured by X-ray diffraction decreased. This was attributed to the fast propagation of the dislocations present in the interdendritic structure inducing a rotation of the individual dendrites. During creep deformation, the mosaicity increased as visible from the broadening of the maximum spread in misorientation. The formation of inhomogeneous plastic strain fields in the γ/γ’ microstructure is believed to create new mosaic blocks in the dendritic structure of the alloys leading to the observed broadening of the mosaicity. The influence of plastic deformation on the evolution of the mosaicity was demonstrated. The mosaicity significantly changed during creep of the MD2 at 1050°C/180MPa and 1000°C/180MPa whereas no significant evolution could be measured during creep at 950°C/180MPa. This was attributed to a temperature dependence of the yield strength of the MD2 alloy. It therefore induces difference in dislocation propagation at 950°C compared to 1050°C and 1000°C which retards the broadening of the mosaicity during creep at 950°C. Furthermore, the mosaicity formed during creep deformation was retained upon unloading and cooling of the SX samples to room temperature.

EPFL2012

Comportement mécanique des milieux granulaires sous sollicitations cycliques

Frédéric Mayoraz

The following work deals with the characterisation of the behaviour of road bases granular material, made of tunnel excavation material and loaded by passing vehicle axles. This granular media, don't correspond generally to the standards demanded for the construction of road pavements. The thesis is a part of the project COST 337 ("Unbound granular materials for road pavements") whose aim is to develop a guideline for the design of road pavements in Europe (material production, laboratory tests, modelling of mechanical behaviour). At the beginning, several loadings of road pavements are described (mechanical, thermal, hydric), concentrating on mechanical loading. Full-scale tests and finite element simulations led to the knowledge of the order of magnitude of stresses and deformations as well as to the understanding of the rotation of the principal stresses, due to the passing of a vehicle axle. This theoretical part is followed by laboratory cyclic tests with sand to estimate the influence of the principal stress rotation on the deformability of granular media and the importance to take this phenomenon into account for the modelling. Further laboratory tests were carried out on high diameter samples (160 and 250 mm) made of tunnel excavation material. Those tests were made by performing a large number of cycles (80'000 to 250'000 cycles) and various stress paths. The aim of the tests was to measure the evolution of elastic (stiffening of material) and plastic (accumulation of permanent deformations) material characteristics during the cycles. Tools have been developed in the framework of image analysis to assess the eventual change of morphology of this non-standard granular media. Finally the modelling of the accumulation of plastic deformations is discussed in accordance to the theory of elasto-plasticity and visco-plasticity. To remove the limits of elasto-plasticity to simulate a large number of cycles, a visco-plastic approach is developed. The elegant approach, replacing the time by the number of cycles, allows to approximate the permanent deformations of a road pavement in dependence on the stress path. It provides a tool to estimate the rutting in road pavements.

EPFL2002

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