Transmission Electron Microscopy of Metallic Multilayers

We give an overview of use of the transmission electron microscope (TEM) in the characterisation of metallic multilayers. The different types of structural information available from phase and diffraction contrast imaging, as well as the various diffraction modes, are described. The particular usefulness of techniques such as the Fresnel fringe method for multilayer interface characterisation is emphasised. The use of analytical TEM and scanning TEM (STEM) for chemical characterisation is also covered. Special considerations and methods applying to the study of magnetic materials are briefly considered. All points covered are illustrated with examples from the recent literature

Synthesis and microstructure of bulk nanocrystalline copper

International audienceThe synthesis of bulk nanocrystalline copper (NC-Cu) by powder metallurgy is presented, from compaction of nanocrystalline powders to sintering and differential extrusion. At each step of the process, the microstructure is characterized using X-ray diffraction (XRD) analysis, field-emission gun scanning electron microscopy (FEG-SEM), and transmission electron microscopy (TEM). Particular attention is given to the concept of grain size in nanostructured materials and the comparison of results from the different characterization techniques. The fully dense material has a grain size of 100 nm with a microstructure best described in terms of the distribution of high-angle grain boundaries (GBs), twin boundaries, and low-angle GBs. Dislocations occur in half the grains and at most of the twin boundaries. The GBs are shown to be crystalline, and no evidence is found for amorphous interfacial regions. It is proposed that the grain size be defined only in terms of high-angle GBs, excluding low-angle GBs, for the discussion of mechanical properties. In this respect, the microstructure is compared with the NC-Cu material produced by other synthesis techniques. Powder metallurgy (P/M) processing is revealed as an alternative for the production of large-size submicrocrystalline and NC materials

Mechanical Behaviour of Nanocrystalline Copper Related to Grain-boundary Structure

Understanding the mechanical behaviour of metallic nanostructures is a key issue for their development. On the one hand, knowledge of the plastic behaviour at various temperatures is essential to control the synthesis, forming, and machining of such materials. Equally, a clear understanding of atomic and mesoscopic mechanisms, involving defects and their interactions, is essential for the control of ageing and functional properties. Regarding plastic deformation at room temperature, there is now evidence for unusual behaviour in nanostructured metals. In addition to high resistance and ductility, tensile testing reveals peculiar elasto-plastic deformation. Such behaviour was initially attributed to grain-boundary sliding. However, intergranular areas (including triple junctions) may possess special properties compared to their microcrystalline counterparts. For example, low activation energies have been measured for grain-boundary diffusion and it has been observed that grain-boundaries may act as dislocation sources and nucleation sites for deformation twinning. In this paper, we report on analysis on bulk copper nanostructures. Grain-boundaries are studied, by cross-correlating information from mechanical tensile testing and structural analysis, including X-ray diffraction (XRD) and transmission electron microscopy (TEM). Macroscopic bulk specimens (with grain size of about 80 nm) are prepared by powder metallurgy techniques, modified to fit to the special properties of nanocrystalline powders. Processing includes coldisostatic pressing, sintering and differential extrusion. The powders used (grain size of 40 nm) are synthesised by evaporation and cryo-condensation of a metallic vapour within liquid nitrogen. Results on mechanical testing and structural analysis will be reported. Emphasis will be placed on the structure of grain-boundaries (type of grain-boundary, grain-boundary thickness) studied by TEM and high resolution TEM image analysed using the geometric phase technique. The nanostructure was revealed to be consist in agglomerate of nano-size grains separated by low angle grain-boundaries. Agglomerates are themselves separerated by general high angle boundaries. These observations will then be related to the unusual mechanical true stress-true strain curves of the metallic nanostructures

Optimization of off-axis electron holography performed with femtosecond electron pulses

International audienceWe report on electron holography experiments performed with femtosecond electron pulses in an ultrafast coherent Transmission Electron Microscope based on a laser-driven cold field emission gun. We first discuss the experimental requirements related to the long acquisition times imposed by the low emission/probe current available in these instruments. The experimental parameters are first optimized and electron holograms are then acquired in vacuum and on a nano-object showing that useful physical properties can nevertheless be extracted from the hologram phase in pulsed condition. Finally, we show that the acquisition of short exposure time holograms assembled in a stack, combined with a computer-assisted shift compensation of usual instabilities encountered in holography, such as beam and biprism wire instabilities, can yield electron holograms acquired with a much better contrast paving the way to ultrafast time-resolved electron holography

Quantitative analysis of strain field in thin films from HRTEM micrographs

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