Thomas Schenk

The Samson phase, β-Mg2Al3, revisited

Co-Authors: Michael Feuerbacher, Carsten Thomas, Julien P. A. Makongo, Stefan Hoffmann, Wilder Carrillo-Cabrera, Raul Cardoso, Yuri Grin, Guido Kreiner, Jean-Marc Joubert, Thomas Schenk, Joseph Gastaldi, Henri Nguyen-Thi, Nathalie Mangelinck-Noël, Bernard Billia, Patricia Donnadieu, Aleksandra Czyrska-Filemonowicz, Anna Zielinska-Lipiec, Beata Dubiel, Thomas Weber, Philippe Schaub, Günter Krauss, Volker Gramlich, Jeppe Christensen, Sven Lidin, Daniel Fredrickson, Marek Mihalkovic, Wieslawa Sikora, Janusz Malinowski, Stefan Brühne, Thomas Proffen, Wolf Assmus, Marc de Boissieu, Francoise Bley, Jean-Luis Chemin, Jürgen Schreuer Abstract. The Al−Mg phase diagram has been reinvestigated in the vicinity of the stability range of the Samson phase, β-Mg2Al3 (cF1168). For the composition Mg 38.5 Al 61.5, this cubic phase, space group Fd-3m (no 227), a = 28.242(1) Å, V = 22526(2) Å3, undergoes at 214 °C a first-order phase transition to rhombohedral β′-Mg2Al3(hR293), a = 19.968(1) Å, c = 48.9114(8) Å, V = 16889(2) Å3, (i.e. 22519 Å3 for the equivalent cubic unit cell) space group R3m (no 160), a subgroup of index four of Fd-3m. The structure of the β-phase has been redetermined at ambient temperature as well as in situ at 400 °C. It essentially agrees with Samsons model, even in most of the many partially occupied and split positions. The structure of β′-Mg2Al3is closely related to that of the β-phase. Its atomic sites can be derived from those of the β-phase by group-theoretical considerations. The main difference between the two structures is that all atomic sites are fully occupied in case of the β′-phase. The reciprocal space, Bragg as well as diffuse scattering, has been explored as function of temperature and the β- to β′-phase transition was studied in detail. The microstructures of both phases have been analyzed by electron microscopy and X-ray topography showing them highly defective. Finally, the thermal expansion coefficients and elastic parameters have been determined. Their values are somewhere in between those of Al and Mg.

X-ray diffraction study of undercooled molten silicon

The short-range order of molten silicon was investigated in a wide temperature range from 1893 K down to 1403 K, corresponding to an undercooling of 290 K. Energy-dispersive x-ray diffraction was used in combination with electromagnetic levitation. The structure factor and the pair correlation function were determined as a function of temperature from the experimental data. A small hump on the higher wave vector side of the first peak in the structure factor was observed at all temperatures. The position of the first peak in the pair distribution function shifted to shorter distances and its height increased gradually with decreasing temperature. No discontinuous behavior was observed in the entire temperature range investigated.

Short-range order in undercooled and stable melts forming quasicrystals and approximants and its influence on nucleation

An icosahedral short-range order has been predicted to prevail in undercooled metallic melts. For melts of pure metals, this hypothesis was recently experimentally confirmed by diffraction experiments. This paper presents results of neutron scattering experiments on the short-range order of stable and undercooled liquids of alloys forming quasicrystals and polytetrahedral crystals. The studies indicate that an icosahedral topological short-range order prevails in all of the investigated melts. The influence of this icosahedral short-range order on the nucleation behaviour of solid phases from the undercooled liquid is discussed.

Short-range order in undercooled melts forming quasicrystals and approximants

Abstract For the first time, the short-range order of deeply undercooled liquids of alloys forming quasicrystalline and polytetrahedral phases (Al13Fe4 and Al74Co26) is investigated by combining the containerless processing technique of electromagnetic levitation with elastic neutron scattering. The experimentally determined structure factor, S(Q), was simulated by assuming that clusters with different structures exist in the liquid. The best fit of the experimental data is obtained under the assumption of an icosahedral short-range order. This supports the nearly 50 year-old prediction of Frank that an icosahedral short-range order prevails in undercooled metallic liquids.

Fragmentation in an Al–7 wt-%Si alloy studied in real time by X-ray synchrotron techniques

Abstract One mechanism for the formation of equiaxed grains is the detachment of dendrite fragments which is believed to be at the origin of the central equiaxed core region in casting processes. Unfortunately, the dynamics of the fragmentation phenomena cannot be revealed by classical methods. Investigation of a unrefined Al–7 wt-%Si alloy using in situ and real time synchrotron X-radiography and X-ray topography at the European Synchrotron Radiation Facility, has allowed verification of the existence of dendrite fragmentation and of cascade fragmentation during directional solidification, and to study the evolution of the growth and sedimentation of the equiaxed grains formed from these fragments. An examination of the crystallographic misorientation of dendrites as fragmentation is ongoing. These results contribute to the understanding of the characteristics of the columnar to equiaxed transition and to knowledge of the origin of new equiaxed grains in unrefined alloys.

Measurement of solute profiles by means of synchrotron X-ray radiography during directional solidification of Al - 4 wt% Cu alloys

In the present study, we report on an image analysis procedure, which enables to extract from synchrotron radiographs the long range solute profiles in the whole sample and in both phases (solid and liquid). This image analysis is based on the measurement of local density differences, and is applied to study the directional solidification of Al - 4wt% Cu alloy, from planar to onset of the initial instability. Dedicated experiments were carried out at the European Synchrotron Radiation Facility (ESRF) in Grenoble (France). In order to validate this analysis the value of a key solidification parameter, namely the partition coefficient, was experimentally determined during the planar solidification, and a very good agreement was found with value found usually in the literature. On a further step, the evolution of the microstructure and solute profile during the initial transient of solidification was analysed in detail.

Phase-specific high temperature creep behaviour of a pre-rafted Ni-based superalloy studied by X-ray synchrotron diffraction

The phase-specific high temperature creep behaviours of the γ and γ′ phases of a rafted Ni-based single crystal superalloy were investigated by a combination of in situ creep experiments and diffraction of high-energy X-ray synchrotron radiation. In situ experiments were performed at constant temperatures in a 930–1125 °C temperature range and under variable applied stress in order to study the material’s response (plastic strain, load transfer) to stress jumps. Using three crystal diffractometry in transmission (Laue) geometry, it was possible to measure the average lattice parameters of both the matrix and the rafts in the [1 0 0] direction at intervals shorter than 300 s. The absolute precision on the measurement of the constrained transverse mismatch (in the rafts’ plane) is better than 10−5. Plastic strain occurs within the γ corridors as soon as the Von Mises stress exceeds the Orowan stress. The plasticity of the γ′ rafts apparently depends on the transverse stress (i.e. perpendicular to the tensile axis) exceeding a threshold value of 60 MPa.

Short-range order of liquid Ti 72.3 Fe 27.7 investigated by a combination of neutron scattering and X-ray diffraction

Abstract In this work we report on investigations into the topological and chemical short-range order of binary Ti72.3Fe27.7 alloy melts. In order to analyse the structure, the melts were investigated by means of neutron scattering and energy dispersive diffraction of synchrotron radiation. The combination of both diffraction techniques allowed the determination of the partial Bhatia Thornton structure factors SNN(Q) and SCC(Q). The experimental results provide evidence of an icosahedral topological short-range order prevailing in the liquid that is accompanied by a pronounced chemical short-range order such that Ti-Fe nearest neighbours are preferentially formed.

Diffraction Profile, Strain Distribution and Dislocation Densities during Stage II Creep of a Superalloy

One of the major ingredients of modelling the mechanical behaviour of superalloys is the knowledge of dislocation densities and strain distribution. Both can be measured using post mortem BF TEM and CBED, but such methods do not allow following their variations during a test. The aim of the present work is to investigate the usefulness of in situ X-Ray Three Crystal Diffractometry (TCD) to measure the density and distribution of dislocations within a rafted superalloy, i.e. during stage II of high temperature creep. As the instrument contribution is very low, the two-peaked experimental profiles are representative of the lattice parameter distribution within the material. The profiles were measured within bulk specimens at the BW5 high energy beamline Hasylab (DESY), during high temperature (1050°C to 1180°C) tests under loads between 0 MPa and 300 MPa. The peak shapes were observed to change with varying experimental conditions. The peak width follows different patterns under low and high stress, i.e. with low and high strain rates. The distribution of elastic strains was calculated by assuming two main contributions: dislocation segments trapped at the γ/γ’ interfaces in a more or less regular network, and dislocations moving within the γ’ rafts. A comparison between experimental and simulated peaks shows that several features of their behaviour can be explained: the absolute magnitude of the peak width, the observed decrease of the peak width under low loads with increasing interfacial dislocation densities. The larger increase in the width of the γ’ peak under high load (and strain rate) may be attributed to a dislocation density within the 1013 m-2 range within the rafts. The present results are presently being cross-checked by post mortem TEM observations.

In situ and real-time analysis of the growth and interaction of equiaxed grains by synchrotron X- ray radiography

The phenomena involved during equiaxed growth are dynamic, so that in situ and real-time investigation by X-ray imaging is compulsory to fully analyse the microstructure formation. The experiments on Al - 10 wt% Cu alloy of this paper are carried out at the European Synchrotron Radiation Facility (ESRF) in Grenoble (France). Equiaxed growth was achieved in nearly isothermal conditions and continuously monitored from the very early stages of solidification to an asymptotic state. First, measurements of dendrite arms velocity for a same grain showed slight differences in the early stages of the growth. This effect is attributed to a gravity-related self - poisoning of the grain. Then, the propagation of primary dendrite arms was analysed and two successive growth regimes were observed. First, due to the relative distance with neighbour grains, each grain could be considered as isolated (i.e. growing freely) and tip growth rate gradually increased. In a subsequent phase, tip growth rate slowly decreased towards zero, due to the proximity of neighbouring grains. Using an image analysis technique, we were able to measure the solute profiles in the liquid phase between interacting arms. These measurements confirmed that solutal impingement is responsible for stopping the grain growth.