Daniel Kiener

In situ nanocompression testing of irradiated copper

Increasing demand for energy and reduction of CO2 emissions has revived interest in nuclear energy. Designing materials for radiation environments necessitates fundamental understanding of how radiation-induced defects alter mechanical properties. Ion beams create radiation damage efficiently without material activation, but their limited penetration depth requires small-scale testing. However, strength measurements of nano-scale irradiated specimens have not been previously performed. Here we show that yield strengths approaching macroscopic values are measured from irradiated ~400 nm diameter copper specimens. Quantitative in situ nano-compression testing in a transmission electron microscope reveals that the strength of larger samples is controlled by dislocation-irradiation defect interactions, yielding size-independent strengths. Below ~400 nm, size-dependent strength results from dislocation source limitation. This transition length-scale should be universal, but depend on material and irradiation conditions. We conclude that for irradiated copper, and presumably related materials, nano-scale in situ testing can determine bulk-like yield strengths and simultaneously identify deformation mechanisms.

Source Truncation and Exhaustion: Insights from Quantitative in situ TEM Tensile Testing

A unique method for quantitative in situ nanotensile testing in a transmission electron microscope employing focused ion beam fabricated specimens was developed. Experiments were performed on copper samples with minimum dimensions in the 100–200 nm regime oriented for either single slip or multiple slip, respectively. We observe that both frequently discussed mechanisms, truncation of spiral dislocation sources and exhaustion of defects available within the specimen, contribute to high strengths and related size-effects in small volumes. This suggests that in the submicrometer range these mechanisms should be considered simultaneously rather than exclusively.

Decomposition pathways in age hardening of Ti-Al-N films

The ability to increase the thermal stability of protective coatings under work load gives rise to scientific and industrial interest in age hardening of complex nitride coating systems such as ceramic-like Ti1−xAlxN. However, the decomposition pathway of these systems from single-phase cubic to the thermodynamically stable binary nitrides (cubic TiN and wurtzite AlN), which are essential for age hardening, are not yet fully understood. In particular, the role of decomposition kinetics still requires more detailed investigation. In the present work, the combined effect of annealing time and temperature upon the nano-structural development of Ti0.46Al0.54N thin films is studied, with a thermal exposure of either 1 min or 120 min in 100 °C steps from 500 °C to 1400 °C. The impact of chemical changes at the atomic scale on the development of micro-strain and mechanical properties is studied by post-annealing investigations using X-ray diffraction, nanoindentation, 3D-atom probe tomography and high-resolution...

Crystal rotation in Cu single crystal micropillars : In situ Laue and electron backscatter diffraction

In situ microdiffraction experiments were conducted on focused ion beam machined single crystal Cu pillars oriented for double slip. During deformation, the crystal undergoes lattice rotation on both the primary and critical slip system. In spite of the initial homogeneous microstructure of the Cu pillar, rotation sets in already at yield and is more important at the top of the pillar than at the bottom, demonstrating the inhomogeneous stress state during a microcompression experiment. The rotation results are confirmed by electron backscatter diffraction measurements.

Reversible cyclic deformation mechanism of gold nanowires by twinning-detwinning transition evidenced from in situ TEM

Mechanical response of metal nanowires has recently attracted a lot of interest due to their ultra-high strengths and unique deformation behaviours. Atomistic simulations have predicted that face-centered cubic metal nanowires deform in different modes depending on the orientation between wire axis and loading direction. Here we report, by combination of in situ transmission electron microscopy and molecular dynamic simulation, the conditions under which particular deformation mechanisms take place during the uniaxial loading of [110]-oriented Au nanowires. Furthermore, by performing cyclic uniaxial loading, we show reversible plastic deformation by twinning and consecutive detwinning in tension and compression, respectively. Molecular dynamics simulations rationalize the observed behaviours in terms of the orientation-dependent resolved shear stress on the leading and trailing partial dislocations, their potential nucleation sites and energy barriers. This reversible twinning-detwinning process accommodates large strains that can be beneficially utilized in applications requiring high ductility in addition to ultra-high strength.

Overview on established and novel FIB based miniaturized mechanical testing using in-situ SEM

Abstract Probing mechanical properties in the micrometer regime is of current interest in materials science. A focused ion beam microscope was employed to fabricate miniaturized specimens, while an indenter installed in a scanning electron microscope was utilized to actuate the samples and record the load and displacement data during the deformation. Examples for miniaturized compression, tension, bending, as well as newly developed bending fatigue and bending fracture experiments are presented, demonstrating the unique flexibility of in-situ mechanical testing in the scanning electron microscope at small length scales.

Advanced nanomechanics in the TEM: Effects of thermal annealing on FIB prepared Cu samples

The effect of focused ion beam (FIB) fabrication on the mechanical properties of miniaturized mechanical tests has recently been realized, but is not well documented. In this study, the effect of post thermal annealing on the plastic properties of FIB fabricated micro- and nanometer-sized Cu samples was studied by means of advanced analytic and in situ transmission electron microscopy. In situ heating experiments on thin films and pillars revealed a reduction of the initially high dislocation density, but never a recovery of the bulk dislocation density. Aberration-corrected atomic imaging documented the recovery of a pristine crystalline surface structure upon annealing, while electron energy-loss spectroscopy showed that the remaining contamination layer consisted of amorphous carbon. These structural observations were combined with the mechanical data from in situ tests of annealed micro- and nanometer-sized tensile and compression samples. The thermal annealing in the micron regime mainly influences the initial yield point, as it reduces the number of suited dislocation sources, while the flow behavior is mostly unaffected. For the submicron samples, the annealed material sustains significantly higher stresses throughout the deformation. This is explained by the high stresses required for surface-mediated dislocation nucleation of the annealed material at the nanoscale. In the present case, the FIB affected the surface near defects and facilitated dislocation nucleation, thereby lowering the material strength.

Dislocation storage in single slip-oriented Cu micro-tensile samples: new insights via X-ray microdiffraction

Synchrotron X-ray microdiffraction was used to characterize the deformation structure of single crystalline Cu micro-tensile specimens which were oriented for single slip. The 3-µm thick samples were strained in situ in a scanning electron microscope (SEM). Electron microscopy observations revealed glide steps at the surface indicating single slip. While the slip steps at the surface must have formed by the predominant activation of the primary glide system, analysis of Laue peak streaking directions revealed that, even at low strains, dislocations had been activated and stored on an unpredicted slip system. Furthermore, the µLaue scans showed that multiple slip takes over at a later state of deformation.

Towards predictive modelling of near-edge structures in electron energy loss spectra of AlN based ternary alloys

Although electron energy loss near edge structure analysis provides a tool for experimentally probing unoccupied density of states, a detailed comparison with simulations is necessary in order to understand the origin of individual peaks. This paper presents a density functional theory based technique for predicting the N K-edge for ternary (quasi-binary) nitrogen alloys by adopting a core hole approach, a methodology that has been successful for binary nitride compounds. It is demonstrated that using the spectra of binary compounds for optimising the core hole charge (

Influence of external and internal length scale on the flow stress of copper

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