Nanomechanical testing study of the elementary deformation mechanisms in the Ti2AlN and Cr2AlC MAX phases

Abstract: Deformation mechanisms in MAX phases are still not well understood. The complex mechanical behavior of these materials, including mechanical hysteresis, arises both from their crystallography, with a nanolayered structure alternating nitride or carbide layers with metal atoms layers, and from their macroscopic polycrystalline structure, composed of platelets-like grains. In order to distinguish from these two contributions, we focused our study at the sub-micrometer scale, in order to probe the mechanical response of individual grains. Please click Additional Files below to see the full abstract

Deformation twinning in Cr2AlC MAX phase single crystals: A nanomechanical testing study

In a recent study [1], we observed and characterized for the first time deformation twinning in the Ti2AlN MAX phase deformed at high temperature (800°C) by Berkovich nanoindentation. Since plastic deformation in these nanolayered materials was believed to be governed only by basal plane dislocations involved in kink band mechanisms, this result has shed a new light on the mechanical behavior of MAX phases. In order to go further in the understanding of twinning deformation mechanisms in MAX phases, we performed a study in Cr2AlC single crystal, deformed at room temperature by spherical nanoindentation and by micropillar compression tests, in such an orientation that the basal plane was edge on, to inhibit basal dislocations and to promote twinning. Please click Download on the upper right corner to see the full abstract

Portevin‐Le Chatelier effect in AlMg3% studied using elevated temperature nanoindentation

The Portevin-Le Chatelier (PLC) is a plastic instability observed in different alloys, and particularly in aluminum alloys, which is characterized by a serrated flow during plastic deformation. The PLC effect originates from the competition between gliding of mobile dislocations and pinning of these dislocations by diffusing solute atoms. This dynamic strain hardening leads to a negative strain rate sensitivity which is often used to characterize or quantify the PLC effect. The PLC effect has been widely investigated in the case of stress-strain curves obtained in macroscopic uni-axial tests. However, in the case of the aluminum matrix composites Al/AlCuFe, it has been observed that copper atoms diffuse during the material synthesis form the reinforcement particles to the aluminum matrix. The aluminum matrix thus presents a heterogeneous concentration of copper atoms leading to local PLC effect. Nanoindentation test is the best way to characterize locally this mechanical effect. However, strain rate is not a convenient parameter for nanoindentation tests since the complex strain field below the indent, as well as the increase of the contact area during the test, makes difficult the definition a single strain value. Another way to investigate a local PLC effect would be thus the perform nanoindentation tests at different temperatures rather than different strain rates. This poster will present experimental results from elevated temperature nanoindentation studies on an AlMg3% alloy, used as a model material for easy comparison with uniaxial tests, in the temperature range from 25-300°C. The experiments were performed in displacement controlled mode in a recently developed vacuum high temperature nanoindenter based on active surface referencing and non-contact tip and sample heating. In this configuration, the PLC effect appears as successive load drops on the loading curves. The temperatures of the tip and the sample surface were calibrated and matched in order to minimize thermal drift. With increasing temperature, the magnitude of load drop decreased whereas its occurrence frequency increased. The load drop magnitude and its occurrence frequency were statistically analyzed for different temperatures of testing. The results will be discussed in terms of an expanding plastic volume beneath the indenter interacting with the solute atoms in the complex stress field of the indenter

Mechanical hysteresis of the MAX phase Ti2AlN: A nano-mechanical testing study

MAX phases are nano-lamellar ternary carbides and nitrides, with a hexagonal crystallographic structure. These materials combine several properties of metals and ceramics, which give them a high potential for technological applications. Their mechanical properties are characterized by a high stiffness and a relatively low yield strength More surprisingly, deformation tests on MAX phases reveal a mechanical hysteresis. At a macroscopic scale, in polycrystalline samples, several studies have shown that this behavior could be related to load transfers from grain to grain. However, a mechanical hysteresis is also observed in single crystals. In this work, the mechanical hysteresis and the plasticity of the MAX phase Ti2AlN has been studied at small scale by using nanoindentation tests with a spherical tip and micro-pillar compression tests. In both cases, cyclic loadings have been applied in single grains, for different crystallographic orientations, previously determined by EBSD. These cyclic loadings, with partial unloadings (cf. figure 1), have revealed a same behavior in nanoindentation tests and in micro-pillars compression test. In both cases, the unloading curves show an elastic behavior followed by a plastic recovery at low load. Furthermore, this mechanical hysteresis is related to the crystallographic orientation since the energy dissipated during the cycles is shown to be minimum when the basal plane is perpendicular or parallel to the indentation (or compression) axis. Please click Additional Files below to see the full abstract

Mécanismes de déformation des phases MAX (une approche expérimentale multi-échelle)

Il est couramment admis que la déformation plastique des phases MAX est dueau glissement de dislocations dans les plans de base s'organisant en empilements et murs. Cesderniers peuvent former des zones de désorientation locale appelées kink bands. Cependant, lesmécanismes élémentaires et le rôle exact des défauts microstructuraux sont encore mal connus. Cemanuscrit présente une étude expérimentale multi-échelle des mécanismes de déformation de laphase MAX Ti2AlN. A l'échelle macroscopique, deux types d'expériences ont été menés. Des essaisde compression in-situ à température et pression ambiantes couplés à la diffraction neutroniqueont permis de mieux comprendre le comportement des différentes familles de grains dans le Ti2AlNpolycristallin. Des essais de compression sous pression de confinement ont également été réalisés dela température ambiante jusqu'à 900 C. À l'échelle mésoscopique, les microstructures des surfacesdéformées ont été observées par MEB et AFM. Ces observations complétées par des essais denanoindentation ont montré que la forme des grains et leur orientation par rapport à la directionde sollicitation gouvernent l'apparition de déformations intra- et inter-granulaires ainsi que lalocalisation de la plasticité. Finalement à l'échelle microscopique, une étude détaillée par METdes échantillons déformés sous pression de confinement a révélé la présence de configurations dedislocations inédites dans les phases MAX, telles que des réactions entre dislocations, des dipôleset des dislocations hors plan de base. À la vue de ces résultats nouveaux, les propriétés mécaniquesdes phases MAX sont rediscutées.It is commonly believed that plastic deformation mechanisms of MAX phases consistin basal dislocation glide, thus forming pile-ups and walls. The latter can form local disorientationareas, known as kink bands. Nevertheless, the elementary mechanisms and the exact role ofmicrostructural defects are not fully understood yet. This thesis report presents a multi-scale experimentalstudy of deformation mechanisms of the Ti2AlN MAX phase. At the macroscopic scale,two kinds of experiments were performed. In-situ compression tests at room temperature coupledwith neutron diffraction brought new insight into the deformation behavior of the different grainfamilies in the polycrystalline Ti2AlN. Compression tests from the room temperature to 900 Cunder confining pressure were also performed. At the mesoscopic scale, deformed surface microstructureswere observed by SEM and AFM. These observations associated with nanoindentationtests showed that grain shape and orientation relative to the stress direction control formationof intra- and inter- granular strains and plasticity localization. Finally, at the microscopic scale,a detailed dislocation study of samples deformed under confining pressure revealed the presenceof dislocation configurations never observed before in MAX phases, such as dislocation reactions,dislocation dipoles and out-of-basal plane dislocations. In the light of these new results, mechanicalproperties of MAX phases are discussed.POITIERS-SCD-Bib. électronique (861949901) / SudocSudocFranceF

Room temperature deformation in the Fe7_7Mo6_6 μ\mu-Phase

The role of TCP phases in deformation of superalloys and steels is still not fully resolved. In particular, the intrinsic deformation mechanisms of these phases are largely unknown including the active slip systems in most of these complex crystal structures. Here, we present a first detailed investigation of the mechanical properties of the Fe7Mo6 {\mu}-phase at room temperature using microcompression and nanoindentation with statistical EBSD-assisted slip trace analysis and TEM imaging. Slip occurs predominantly on the basal and prismatic planes, resulting also in decohesion on prismatic planes with high defect density. The correlation of the deformation structures and measured hardness reveals pronounced hardening where interaction of slip planes occurs and prevalent deformation at pre-existing defects.Comment: Accepted manuscript in International Journal of Plasticit

Nanoindentation cartography in Al/Al-Cu-Fe composites: Correlation between chemical heterogeneities and mechanical properties

During the last two decades, nanoindentation testing has become a commonly used technique for measuring surface mechanical properties such as hardness or elastic modulus. With devices equipped with a motorized X-Y table, it is now possible to perform large regular nanoindentation arrays in order to make an accurate statistics of the mechanical properties. This method is particularly interesting to study heterogeneous materials. The statistical analysis, associated to mathematical deconvolution methods allows identifying the properties of each individual phase. Furthermore, hardness or elastic modulus maps can be then established and compared to other local properties such as microstructure, crystallographic orientation or chemical composition. The nanoindentation cartography method has been used to study the mechanical properties of a metal matrix composite (Aluminum matrix with ω-Al-Cu-Fe reinforcement particles, synthesized by sparking plasma sintering) (cf. figure 1). Emphasize has been placed on the Aluminum matrix properties, where the detailed analysis of the individual nanoindentation curves shows serrated behavior characteristic of Portevin-Le Chatelier effect associated to dislocation pinning by solute atoms. The comparison between chemical (SEM – EDXS analysis) and hardness maps as well as the quantitative analysis of the deformation curves gives evidence of a strong correlation between the chemical heterogeneities and mechanical properties of the Aluminum matrix

Etude par AFM et TEM des premiers stades de plasticité induits par un essai de nanoindentation sur une face (001) d'un monocristal d'oxyde de magnésium

POITIERS-BU Sciences (861942102) / SudocSudocFranceF

Evidence of dislocation cross-slip in MAX phase deformed at high temperature

International audienceTi2AlN nanolayered ternary alloy has been plastically deformed under confining pressure at 900 degrees C. The dislocation configurations of the deformed material have been analyzed by transmission electron microscopy. The results show a drastic evolution compared to the dislocation configurations observed in the Ti2AlN samples deformed at room temperature. In particular, they evidence out-of-basal-plane dislocations and interactions. Moreover numerous cross-slip events from basal plane to prismatic or pyramidal planes are observed. These original results are discussed in the context of the Brittle-to-Ductile Transition of the nanolayered ternary alloys