Plastic flow mechanisms in microcast aluminium wires

Jérôme Krebs, Andreas Mortensen, Suzanne Godelieve Alphonsine Verheyden
2015
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Résumé

A microcasting process is developed to produce microwires of pure or alloyed aluminium. These wires have a diameter ranging between five and twenty micrometers and have a high aspect ratio, on the order of 50. The wires furthermore are monocrystalline and have a surface roughness around 30 nm. Their monotonic plastic flow, in uniaxial tension, has features similar to those of larger single crystals; however, deformation progresses in these crystals by a series of sudden strain bursts of stochastically distributed intensity. We study the distribution of these strain bursts, and also present results from relaxation tests conducted on such wires, in which we probe the role of thermal activation on the initiation and cessation of dislocational plasticity within samples. Mechanical tests are supplemented with microscopic investigations of the metal substructure evolution that accompanies deformation of the wires.

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Chargement

Plasticity of microcast aluminium wires

Jérôme Krebs, Andreas Mortensen, Suzanne Godelieve Alphonsine Verheyden

A microcasting process is developed for the production of monocrystalline microwires of pure and alloyed aluminium. The process is based on pressure infiltration of single-crystalline salt moulds; it is capable of producing wires with a diameter between 6 and 100 µm and a length in excess of 1000 µm. The wire has a surface roughness around 30 nm and an initial dislocation density that is roughly 1011 m-2 when the wire diameter is 20 µm. We present results from classical tensile testing on these wires, and also on relaxation testing. Tests aim to probe the initiation and cessation of dislocational plasticity in different ways, which is observed to proceed to a significant extent in the form of large sudden strain bursts. The mechanical tests are supplemented with microscopic investigations of the metal substructure evolution that accompanies the deformation of the wires.

2015

Chargement

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

Chargement

Intermetallic phases formation is one of the phenomena, which when coupled to thermal and mechanical strains leads to the premature wear of aluminium die casting tools made out of steel. This work focuses on two aspects of this wear problem. The first and major part investigates a simplified chemical system Fe(s)–Al(l) at 700 °C in order to study the formation of the intermetallic compounds. The second part focuses on the limitations of the tool wear by testing different coatings on the steel currently used for die casting. Experiments are performed on two sample types, differentiated by their interface orientation between the two initial phases (vertical and horizontal). Observation are also of two types. Post mortem observations are performed by light microscopy and both scanning and transmission electron microscopy. In situ observation are performed by X-ray tomography, that allows to follow the evolution of the intermetallic layer with time. In the Fe(s)–Al(l) system, one main phase, namely Fe2Al5 , forms with a particular morphology called tongue-like feature in the iron matrix. Tongue tips are generally single crystals. It is also observed that these exhibit a periodical contrast at the nanometre scale. This contrast is found to be due to a slight chemical variation within the existence domain of Fe2Al5. This splitting is linked to the spinodal decomposition of the phase observed at higher temperature. At the interface between tongues and the iron matrix, a layer of about hundred nanometres that surrounds the tongues is observed. It corresponds to the Æ2 FeAl phase. Iron matrix, due to the tongue growth, suffers a plastic deformation that is observed by recrystallisation of the direct tongue surrounding. The induced strain field also leads to porosity formation at the interface between the tongues and the matrix. Pores are then trapped in the Fe2Al5 phase and partially disappear near from the liquid interface. At this interface, a layer of the order of 10μm of Fe4Al13 is observed. The thickness of this layer is stable in the explored time range of 0-4 h. However, intermetallic blocks that detach from the layer are observed in the liquid. This is interpreted as mainly due to the dissolution of the formed layer in the bath to achieve its saturation in Fe. Intermetallic thicknesses and tongue density measurements as functions of time allow to highlight the presence of three main growth regimes. The first at the beginning of the contact corresponds to rapid emergence of the tongues in the matrix. The second is linked to their progressive slow down while they start to thicken. Both thickening and tip growth are in competition from the beginning of this regime. A third regime is however defined and corresponds to a more stable growth during which thickening and tip growth still act in parallel is but their effect is less visible as they vary with the square root of time. The tongue growth observed at the beginning of the reaction is explained by a growth front destabilisation, similarly to the destabilisation of a planar front that leads to dendritic solidification described by Mullins and Sekerka. A calculation based on their model is proposed and confirms the effect of the law aluminium diffusion in iron but is limited by assumptions made for its development. Technological investigation proceeds by modification of the studied system and comparison with the fundamental one. Two ferrous materials and one aluminium alloy are studied. In addition, different coatings deposited by electroless plating on one of the ferrous substrates are tested. A quality coefficient is proposed in order to compare the result of the contact between coating and liquid aluminium. One Co-based coating is revealed as the most promising material that allows to limit the wear of the ferrous part by liquid aluminium.

EPFL2013

Chargement

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

Stéphane Pierret

EPFL2012

EPFL2013