A global investigation into in situ nanoindentation experiments on zirconia: from the sample geometry optimization to the stress nanolocalization using convergent beam electron diffraction

Nanoindentation experiments inside a transmission electron microscope are of much interest to characterize specific phenomena occuring in materials, like for instance dislocation movements or phase transformations. The key points of these experiments are (i) the sample preparation and the optimization of its geometry to obtain reliable results and (ii) the choice of the transmission electron microscope observation mode, which will condition the type of information which can be deduced from the experiment. In this paper, we will focus on these two key points in the case of nanoindentation of zirconia, which is a ceramic material well known to be sensitive to stress because it can undergo a phase transformation. In this case, the information sought is the stress localization at the nanometre scale and in real time. As far as the sample preparation is concerned, one major drawback of nanoindentation inside a transmission electron microscope is indeed a possible bending of the sample occurring during compression, which is detrimental to the experiment interpretation (the stress is not uniaxial anymore). In this paper, several sample preparation techniques have been used and compared to optimize the geometry of the sample to avoid bending. The results obtained on sample preparation can be useful for the preparation of ceramics samples but can also give interesting clues and experimental approaches to optimize the preparation of other kinds of materials. The second part of this paper is devoted to the second key point, which is the determination of the stress localization associated to the deformation phenomena observed by nanoindentation experiments. In this paper, the use of convergent beam electron diffraction has been investigated and this technique could have been successfully coupled to nanoindentation experiments. Coupled nanoindentation experiments and convergent beam electron diffraction analyses have finally been applied to characterize the phase transformation of zirconia.     

Piezoelectric field around threading dislocation in GaN determined on the basis of high-resolution transmission electron microscopy image

A new method of determining the piezoelectric field around dislocations from high‐resolution transmission electron microscopy images is presented. In order to determine the electrical potential distribution near a dislocation core, we used the distortion field, obtained using the geometrical phase method and the non‐linear finite element method. The electrical field distribution was determined taking into account the inhomogeneous strain distribution, finite geometry of the sample and the full couplings between elastic and electrical fields. The results of the calculation for a transmission electron microscopy thin sample are presented.     

High-angle triple-axis specimen holder for three-dimensional diffraction contrast imaging in transmission electron microscopy

Electron tomography requires a wide angular range of specimen-tilt for a reliable three-dimensional (3D) reconstruction. Although specimen holders are commercially available for tomography, they have several limitations, including tilting capability in only one or two axes at most, e.g. tilt-rotate. For amorphous specimens, the image contrast depends on mass and thickness only and the single-tilt holder is adequate for most tomographic image acquisitions. On the other hand, for crystalline materials where image contrast is strongly dependent on diffraction conditions, current commercially available tomography holders are inadequate, because they lack tilt capability in all three orthogonal axes needed to maintain a constant diffraction condition over the whole tilt range. We have developed a high-angle triple-axis (HATA) tomography specimen holder capable of high-angle tilting for the primary horizontal axis with tilting capability in the other (orthogonal) horizontal and vertical axes. This allows the user to trim the specimen tilt to obtain the desired diffraction condition over the whole tilt range of the tomography series. To demonstrate its capabilities, we have used this triple-axis tomography holder with a dual-axis tilt series (the specimen was rotated by 90° ex-situ between series) to obtain tomographic reconstructions of dislocation arrangements in plastically deformed austenitic steel foils.