Precipitation of T₁ and θ′ Phase in Al-4Cu-1Li-0.25Mn During Age Hardening: Microstructural Investigation and Phase-Field Simulation

Experimental and phase field studies of age hardening response of a high purity Al-4Cu-1Li-0.25Mn-alloy (mass %) during isothermal aging are conducted. In the experiments, two hardening phases are identified: the tetragonal θ′ (Al2Cu) phase and the hexagonal T1 (Al2CuLi) phase. Both are plate shaped and of nm size. They are analyzed with respect to the development of their size, number density and volume fraction during aging by applying different analysis techniques in TEM in combination with quantitative microstructural analysis. 3D phase-field simulations of formation and growth of θ′ phase are performed in which the full interfacial, chemical and elastic energy contributions are taken into account. 2D simulations of T1 phase are also investigated using multi-component diffusion without elasticity. This is a first step toward a complex phase-field study of T1 phase in the ternary alloy. The comparison between experimental and simulated data shows similar trends. The still unsaturated volume fraction indicates that the precipitates are in the growth stage and that the coarsening/ripening stage has not yet been reached

Quantitative Shape-Classification of Misfitting Precipitates during Cubic to Tetragonal Transformations: Phase-Field Simulations and Experiments

The effectiveness of the mechanism of precipitation strengthening in metallic alloys de-pends on the shapes of the precipitates. Two different material systems are considered: tetragonal γ′′ precipitates in Ni-based alloys and tetragonal θ′ precipitates in Al-Cu-alloys. The shape formation and evolution of the tetragonally misfitting precipitates was investigated by means of experiments and phase-field simulations. We employed the method of invariant moments for the consistent shape quantification of precipitates obtained from the simulation as well as those obtained from the experiment. Two well-defined shape-quantities are proposed: (i) a generalized measure for the particles aspect ratio and (ii) the normalized λ2, as a measure for shape deviations from an ideal ellipse of the given aspect ratio. Considering the size dependence of the aspect ratio of γ′′ precipitates, we find good agreement between the simulation results and the experiment. Further, the precipitates’ in-plane shape is defined as the central 2D cut through the 3D particle in a plane normal to the tetragonal c-axes of the precipitate. The experimentally observed in-plane shapes of γ′′-precipitates can be quantitatively reproduced by the phase-field model. © 2021 by the authors. Licensee MDPI, Basel, Switzerland

An Artificial SEI Layer Based on an Inorganic Coordination Polymer with Self-Healing Ability for Long-Lived Rechargeable Lithium-Metal Batteries

Upon immersion of a lithium (Li) anode into a diluted 0.05 to 0.20 M dimethoxyethane solution of the phosphoric-acid derivative (CF$_{3}$CH$_{2}$O)$_{2}$P(O)OH (HBFEP), an artificial solid-electrolyte interphase (SEI) is generated on the Li-metal surface. Hence, HBFEP reacts on the surface to the corresponding Li salt (LiBFEP), which is a Li-ion conducting inorganic coordination polymer. This film exhibits – due to the reversibly breaking ionic bonds – self-healing ability upon cycling-induced volume expansion of Li. The presence of LiBFEP as the major component in the artificial SEI is proven by ATR-IR and XPS measurements. SEM characterization of HBFEP-treated Li samples reveals porous layers on top of the Li surface with at least 3 μm thickness. Li−Li symmetrical cells with HBFEP-modified Li electrodes show a three- to almost fourfold cycle-lifetime increase at 0.1 mA cm$^{-2}$ in a demanding model electrolyte that facilitates fast battery failure (1 M LiOTf in TEGDME). Hence, the LiBFEP-enriched layer apparently acts as a Li-ion conducting protection barrier between Li and the electrolyte, enhancing the rechargeability of Li electrodes

Local texture measurements with high-energy synchrotron radiation on NiAl deformed in torsion

Plastic deformation leads to crystallographic preferred orientations (texture) of the grains in a polycrystalline sample. Therefore, the study of these textures gives informations about the slip systems activated during the deformation. In this study the deformation of polycrystalline NiAl was done by torsion under confining pressure leading to crack-free samples with a well-defined strain gradient. NiAl, an ordered intermetallic alloy with B2 structure, is a potential material candidate for high-temperature applications. Polycrystalline NiAl cylindrical samples with two different initial textures were deformed in torsion tests at 1000 K and 1273 K, respectively, in a Paterson-type rock deformation machine [1] under 400 MPa argon confining pressure. The diameter and height of the samples were 10 mm. The applied torsion leads to a simple shear in the tangential direction in a plane normal to the torsion axis. The shear strain and the shear strain rate in the samples increase linearly from zero at the torsion axis to a maximum ( ) at the sample edge. To investigate the local textures between the torsion axis and the edge, small pins with a diameter of 1 mm were prepared in the radial direction for each of the four deformed samples Quantitative texture measurements were performed with high-energy (100 keV) synchrotron radiation at the beamline BW5 [2], The incident monochromatic beam was defined by a slit system to 1 mm x 2 mm. The small pins were mounted in the Eulerian cradle parallel to the rotation axis ω. An image plate detector was positioned perpendicularly to the diffracted beam at a distance from the sample of about 1.3 m. Thus, the Debye-Scherrer rings with the indices (100), The texture was measured as a function of the shear strain at five different positions between γ = 0 and 3. The samples deformed at 1273 K showed a poor grain statistics due to a large grain size. The corresponding pole figures are not shown here. The torsion deformation at 1000 K leads to much smaller grains. The corresponding (100) pole figures are shown for γ = 1.5; 2.3 and 3 and two different initial texture

Hall-plot of the phase diagram for Ba(Fe₁₋ₓCoₓ)₂As₂

The Hall effect is a powerful tool for investigating carrier type and density. For single-band materials, the Hall coefficient is traditionally expressed simply by , where e is the charge of the carrier, and n is the concentration. However, it is well known that in the critical region near a quantum phase transition, as it was demonstrated for cuprates and heavy fermions, the Hall coefficient exhibits strong temperature and doping dependencies, which can not be described by such a simple expression, and the interpretation of the Hall coefficient for Fe-based superconductors is also problematic. Here, we investigate thin films of Ba(Fe₁₋ₓCoₓ)₂As₂ with compressive and tensile in-plane strain in a wide range of Co doping. Such in-plane strain changes the band structure of the compounds, resulting in various shifts of the whole phase diagram as a function of Co doping. We show that the resultant phase diagrams for different strain states can be mapped onto a single phase diagram with the Hall number. This universal plot is attributed to the critical fluctuations in multiband systems near the antiferromagnetic transition, which may suggest a direct link between magnetic and superconducting properties in the BaFe₂As₂ system

Nanomaterials by severe plastic deformation: review of historical developments and recent advances

International audienceSevere plastic deformation (SPD) is effective in producing bulk ultrafine-grained and nanostructured materials with large densities of lattice defects. This field, also known as NanoSPD, experienced a significant progress within the past two decades. Beside classic SPD methods such as high-pressure torsion, equal-channel angular pressing, accumulative roll-bonding, twist extrusion, and multi-directional forging, various continuous techniques were introduced to produce upscaled samples. Moreover, numerous alloys, glasses, semiconductors, ceramics, polymers, and their composites were processed. The SPD methods were used to synthesize new materials or to stabilize metastable phases with advanced mechanical and functional properties. High strength combined with high ductility, low/room-temperature superplasticity, creep resistance, hydrogen storage, photocatalytic hydrogen production, photocatalytic CO2 conversion, superconductivity, thermoelectric performance, radiation resistance, corrosion resistance, and biocompatibility are some highlighted properties of SPD-processed materials. This article reviews recent advances in the NanoSPD field and provides a brief history regarding its progress from the ancient times to modernity