Spatial control of heavy-fermion superconductivity in CeIrIn5

Although crystals of strongly correlated metals exhibit a diverse set of electronic ground states, few approaches exist for spatially modulating their properties. In this study, we demonstrate disorder-free control, on the micrometer scale, over the superconducting state in samples of the heavy-fermion superconductor CeIrIn5. We pattern crystals by focused ion beam milling to tailor the boundary conditions for the elastic deformation upon thermal contraction during cooling. The resulting nonuniform strain fields induce complex patterns of superconductivity, owing to the strong dependence of the transition temperature on the strength and direction of strain. These results showcase a generic approach to manipulating electronic order on micrometer length scales in strongly correlated matter without compromising the cleanliness, stoichiometry, or mean free path.

Pulsed laser deposition of (SrBa)Nb2O6 thin films and their properties

Anna Infortuna

Strontium barium niobate (SrxBa1-xNb2O6, shortly SBN) is a solid solution system with tetragonal tungsten bronze crystal structure. It exhibits a ferroelectric phase with only one polar axis and a transition temperature depending on the Sr/Ba ratio. This thesis studies the growth of SBN thin films, in order to obtain a ferroelectric thin film model system for the study of 180° domain switching close to the ferroelectric phase transition. SBN has been chosen not only because uniaxial, but because it is possible to tune the temperature of phase transition varying the Sr/Ba ratio. It is thus possible to study electric properties of the phase transition close to room temperature, where conduction phenomena related to defects are normally lower. Thin films of SBN were grown by Pulsed Laser Deposition in a vacuum system constructed during this thesis work. For the formulation of a model it is desirable to have a system as close as possible to a single crystal. Therefore deposition parameters have been optimized to grow SBN thin films with the polar axis oriented perpendicular to the film plane. The films are integrated in parallel plate capacitor structures, in order to measure dielectric properties. The stability of the ferroelectric phase is found to be sensitive to impurities; contaminants with concentration below 1% induce a lowering of the transition temperature of about 100°C. Strain as well has influence on the phase transition; in the case of substrate with thermal expansion coefficients different from the SBN ones, the SBN film is under stress. A 0.6% tensile strain induces a lowering of the transition temperature of about 100°C, this is the case of silicon single crystal substrate. Grown on strontium titanate single crystals (STO), whose thermo-mechanical properties are close to the one of SBN, the films exhibit a phase transition temperature compatible with the one measured on single crystals. The obtained films suffer from leakage that is reduced by thermal treatment in oxygen rich atmosphere. The oxygen vacancies, created during the deposition process, are considered to be responsible of leakage. Vacancies recovery upon annealing does not eliminate the problem, and measurement of polarization at room temperature is difficult. However, piezoelectric measurements performed on individual grains, with atomic force microscope, prove that these have ferroelectric properties; by these experiment has been proved that it is possible to switch the polarization. Films with a disordered structure of grains are much less leaky than the ones with columnar grains spanning the whole cross section. These observations lead to the conclusion that conduction goes trough the grain boundaries. On STO single crystals, SBN grows epitaxial in Volmer-Weber mode. With a suitable preparation of the substrate surface, it is possible to induce the growth of films with different orientations of the polar axis: in the film plane, perpendicular to it or inclined of 45°. A model is proposed, explaining the epitaxial relation with the substrate on the basis of the perovskite kernel contained in the unit cell of the tetragonal tungsten bronze structure. The film grows from the nucleation of the perovskite structure that rules the orientation of the film; the high temperature at which the substrate is kept during the deposition, assure the necessary mobility for the arriving atoms to organize in the SBN structure around these nuclei. The study of literature data allows to state that such a model is valid not only for substrates with perovskite structure, but can be extended to substrates with a cubic crystal structure, like magnesium oxide.

EPFL2005

In-situ Laue Diffraction During Compression of Directionally Solidified Mo Micropillars

Julien René André Zimmermann

With recent developments in micro and nano-technologies, mechanical components such as those used in medicine or electronics tend to be miniaturized, requiring a new set of testing techniques to study their reliability and performance. One of the new methods is micro-pillar compression testing, which allows the study of mechanical properties of confined volumes precisely shaped by focused ion beam (FIB) milling from sometimes complex microstructures. This technique has garnered a great deal of interest in recent years; on one hand because of its apparent simplicity, on the other hand because it revealed an unexpected size dependence in the flow stress of single crystals when the pillar diameter was reduced below a few tenths of a micrometre. The flow stress of FIB milled face centred cubic (fcc) micro-pillars appears to follow a power law as a function of their size. In contrast, non-FIB milled, body centred cubic (bcc) eutectic Molybdenum (Mo) alloy pillars prepared by directional growth exhibit, in their pristine state, whisker-like behaviour without a size effect. Furthermore, after FIB milling or moderate pre-deformation, the whisker character is lost and the typical scatter of the flow stress usually observed for FIB milled pillars is reproduced. After large pre-deformation the scatter vanishes and the pillars exhibit no size effect. These findings show that 1) the deterministic parameter in the size effect can be correlated with the initial microstructure of the pillar, and 2) FIB milling influences this microstructure. This study aims to link the deformation modes occurring in small-scale pillars with their initial microstructure by studying directionally solidified eutectic Mo-alloy pillars with a diameter of 1 micrometre. In-situ Laue diffraction experiments during the compression of such defect-free pillars show that with readily-available dislocation sources from a concave pillar top, the {112}[111] slip system with the highest Schmid factor is initially activated and not the allegedly assumed {110}[111] slip system that is typical for bcc metals. Post-mortem slip trace analysis and TEM observations confirm this finding. Moreover, 3D atom probe measurements and TEM images show that this behaviour can be linked to the presence of both alloying elements and fcc nano-precipitates found in the bcc Mo-alloy. Both can lead to a decrease of the critical temperature and the observation of an fcc-like deformation. Additionally, it is shown that both FIB milling and pre-deformation introduce defects in the initially dislocation-free pillars. In addition to this, pillars prepared under similar conditions yield quite different microstructures. The angle between the focused ion beam and the crystal orientation is found to play an important role in the creation of defects. It can also be shown that pillars with high initial dislocation density deform bulk-like and exhibit strain hardening, while pillars with low initial dislocation content demonstrate a large scatter in the flow and yield stress and exhibit large strain burst at later deformation stages. Furthermore several slip systems are activated before the flow stress is reached for pillars containing initially low dislocation content. Interestingly the first activated slip system can be linked to the initial streaking direction; slip is observed on the {112} plane that contains excess dislocations. For both the as-prepared pillars and the pillars with low initial dislocation content, the yield seems to be source limited, which is not the case for pillars with high initial dislocation content.

EPFL2011

Irreversible Degradation in Nb3Sn Cable in Conduit Conductors

Ciro Calzolaio

One of the biggest goals for the international thermonuclear experimental reactor (ITER) is the steady state operation. For this reason all its coils will be superconducting and Nb3Sn material is used for both the toroidal field (TF) and the central solenoid (CS) coils. The primary current carrying unit in a coil is the cable, which contains hundreds of superconducting strands. The ITER coils will be made using a kind of cable called cable in conduit conductor (CICC). Both CS and TF magnets have to withstand several electromagnetic (EM) cycles in their lifetime. This has been discovered to cause a severe reduction of the magnet performances. Nb3Sn is a brittle material, therefore it is very strain sensitive. The knowledge of the strain state in a CICC allows the explanation of the performances of the cable itself, providing also information regarding the permanent damaging of the Nb3Sn structure. The measurement of the Nb3Sn strain state in a CICC is a very challenging task because it is not possible to make it directly. An indirect technique that allows the measurement of the thermal strain through the measurement of the magnetic susceptibility vs. temperature (χ(T )) for a CICC has been developed. A CICC is a complex system and as such it behaves in a way which is not directly predictable studying the single components. The elastic deformation of the superconducting layers produces reversible phenomena which interact with irreversible phenomena due to Nb3Sn fractures and to plastic deformations of the matrix surrounding the superconducting layers. Reversible and irreversible phenomena occurs together and are deeply shuffled such that it is not straightforward the explanation of the cable performance. The magnetic susceptibility measurements, via an appropriate data analysis, allow to quantify and to separate the thermal strain from the jumble of parameters necessary to describe the cable performance. Several TF and CS samples have been measured with this technique in the SULTAN test facility. Each cable behaves differently from the others but at least it is possible to identify common features. For some samples, the evolution of the performance with the EM cycles is dominated by reversible rearrangements of the strand position in the cable and consequently by the change of the strain distribution during the EM load, for others it is dominated by breakages and irreversible phenomena.

EPFL2013