3D nanostructural characterisation of grain boundaries in atom probe data utilising machine learning methods.

Boosting is a family of supervised learning algorithm that convert a set of weak learners into a single strong one. It is popular in the field of object tracking, where its main purpose is to extract the position, motion, and trajectory from various features of interest within a sequence of video frames. A scientific application explored in this study is to combine the boosting tracker and the Hough transformation, followed by principal component analysis, to extract the location and trace of grain boundaries within atom probe data. Before the implementation of this method, these information could only be extracted manually, which is time-consuming and error-prone. The effectiveness of this method is demonstrated on an experimental dataset obtained from a pure aluminum bi-crystal and validated on simulated data. The information gained from this method can be combined with crystallographic information directly contained within the data, to fully define the grain boundary character to its 5 degrees of freedom at near-atomic resolution in three dimensions. It also enables local atomic compositional and geometric information, i.e. curvature, to be extracted directly at the interface.

Quantifying and observing viscoplasticity at the nanoscale: highly localized deformation mechanisms in ultrathin nanocrystalline gold films.

This study unveils the stress relaxation transient deformation mechanisms in 100 nm-thick, nanocrystalline Au films thanks to a robust quantitative in situ TEM MEMS nanomechanical testing approach to quantify stress relaxation and to perform in situ observations of time-dependent deformation in ultrathin nanocrystalline films. The relaxation is characterized by a decrease in plastic strain rate of more than one order of magnitude over the first ∼30 minutes (from 10(-4) to less than 10(-5) s(-1)). For longer relaxation experiments, the plastic strain rate decreases down to 10(-7) s(-1) after several hours. The power-law exponent n, relating plastic strain rate and stress, continuously decreases from initial large values (n from 6 to 14 at t = 0) down to low values (n ∼ 1-2) after several hours. In situ TEM observations reveal that the relaxation behavior is initially accommodated by highly localized, sustained, intergranular and transgranular dislocation motion. Over time, the dislocation sources become less operative or exhausted, leading to a transition to grain-boundary-diffusion based mechanisms. The results also highlight a promising technique for nanoscale characterization of time-dependent deformation.

Shape and Effective Spring Constant of Liquid Interfaces Probed at the Nanometer Scale: Finite Size Effects.

We investigate the shape and mechanical properties of liquid interfaces down to nanometer scale by atomic force microscopy (AFM) and scanning electron microscopy (SEM) combined with in situ micromanipulation techniques. In both cases, the interface is probed with a cylindrical nanofiber with radius R of the order of 25-100 nm. The effective spring constant of the nanomeniscus oscillated around its equilibrium position is determined by static and frequency-modulation (FM) AFM modes. In the case of an unbounded meniscus, we find that the effective spring constant k is proportional to the surface tension γ of the liquid through k = (0.51 ± 0.06)γ, regardless of the excitation frequency from quasi-static up to 450 kHz. A model based on the equilibrium shape of the meniscus reproduces well the experimental data. Electron microscopy allowed to visualize the meniscus profile around the fiber with a lateral resolution of the order of 10 nm and confirmed its catenary shape. The influence of a lateral confinement of the interface is also investigated. We showed that the lateral extension L of the meniscus influences the effective spring constant following a logarithmic evolution k ∼ 2πγ/ln(L/R) deduced from the model. This comprehensive study of liquid interface properties over more than 4 orders of magnitude in meniscus size shows that advanced FM-AFM and SEM techniques are promising tools for the investigation of mechanical properties of liquids down to nanometer scale.

In situ deformation of thin films on substrates.

Metallic thin-film plasticity has been widely studied by using the difference between the coefficients of thermal expansion of the film and the underlying substrate to induce stress. This approach is commonly known as the wafer curvature technique, based on the Stoney equation, which has shown that thinner films have higher yield stresses. The linear increase of the film strength as a function of the reciprocal film thickness, down to a couple hundred nanometers, has been rationalized in terms of threading and interfacial dislocations. Polycrystalline films also show this kind of dependence when the grain size is larger than or comparable to the film thickness. In situ TEM performed on plan-view or cross-section specimens faithfully reproduces the stress state and the small strain levels seen by the metallic film during wafer curvature experiments and simultaneously follows the change in its microstructure. Although plan-view experiments are restricted to thinner films, cross-sectional samples where the film is reduced to a strip (or nanowire) on its substrate are a more versatile configuration. In situ thermal cycling experiments revealed that the dislocation/interface interaction could be either attractive or repulsive depending on the interfacial structure. Incoherent interfaces clearly act as dislocation sinks, resulting in a dislocation density drop during thermal cycles. In dislocation-depleted films (initially thin or annealed), grain boundaries can compensate for the absence of dislocations by either shearing the film similarly to threading dislocations or through fast diffusion processes. Conversely, dislocations are confined inside the film by image forces in the cases of epitaxial interfaces on hard substrates. To increase the amount of strain seen by a film, and to decouple the effects of stress and temperature, compliant substrates can also be used as support for the metallic film. The composite can be stretched at a given temperature using heating/cooling straining holders. Other in situ TEM methods that served to reveal scaling effects are also reviewed. Finally, an alternate method, based on a novel bending holder that can stretch metallic films on rigid substrates, is presented.

In situ observation of dislocation nucleation and escape in a submicrometre aluminium single crystal.

'Smaller is stronger' does not hold true only for nanocrystalline materials but also for single crystals. It is argued that this effect is caused by geometrical constraints on the nucleation and motion of dislocations in submicrometre-sized crystals. Here, we report the first in situ transmission electron microscopy tensile tests of a submicrometre aluminium single crystal that are capable of providing direct insight into source-controlled dislocation plasticity in a submicrometre crystal. Single-ended sources emit dislocations that escape the crystal before being able to multiply. As dislocation nucleation and loss rates are counterbalanced at about 0.2 events per second, the dislocation density remains statistically constant throughout the deformation at strain rates of about 10(-4) s(-1). However, a sudden increase in strain rate to 10(-3) s(-1) causes a noticeable surge in dislocation density as the nucleation rate outweighs the loss rate. This observation indicates that the deformation of submicrometre crystals is strain-rate sensitive.

Observation of giant diffusivity along dislocation cores.

Diffusion of atoms in a crystalline lattice is a thermally activated process that can be strongly accelerated by defects such as grain boundaries or dislocations. When carried by dislocations, this elemental mechanism is known as "pipe diffusion." Pipe diffusion has been used to explain abnormal diffusion, Cottrell atmospheres, and dislocation-precipitate interactions during creep, although this rests more on conjecture than on direct demonstration. The motion of dislocations between silicon nanoprecipitates in an aluminum thin film was recently observed and controlled via in situ transmission electron microscopy. We observed the pipe diffusion phenomenon and measured the diffusivity along a single dislocation line. It is found that dislocations accelerate the diffusion of impurities by almost three orders of magnitude as compared with bulk diffusion.