In situ compression of micropillars under coherent X-ray diffraction: a case study of experimental and data-analysis constraints.

Micropillar compression is a method of choice to understand mechanics at small scale. It is mainly studied with electron microscopy or white-beam micro-Laue X-ray diffraction. The aim of the present article is to show the possibilities of the use of diffraction with a coherent X-ray beam. InSb micropillars in epitaxy with their pedestals (i.e. their support) are studied in situ during compression. Firstly, an experiment using a collimated beam matching the pillar size allows determination of when the sample enters the plastic regime, independently of small defects induced by experimental artefacts. A second experiment deals with scanning X-ray diffraction maps with a nano-focused beam; despite the coherence of the beam, the contributions from the pedestal and from the micropillar in the diffraction patterns can be separated, making possible a spatially resolved study of the plastic strain fields. A quantitative measurement of the elastic strain field is nevertheless hampered by the fact that the pillar diffracts at the same angles as the pedestal. Finally, no image reconstructions were possible in these experiments, either in situ due to a blurring of the fringes during loading or post-mortem because the defect density after yielding was too high. However, it is shown how to determine the elastic bending of the pillar in the elastic regime. Bending angles of around 0.3° are found, and a method to estimate the sample's radius of curvature is suggested.

Size-induced twinning in InSb semiconductor during room temperature deformation.

Room-temperature deformation mechanism of InSb micro-pillars has been investigated via a multi-scale experimental approach, where micro-pillars of 2 µm and 5 µm in diameter were first fabricated by focused ion beam (FIB) milling and in situ deformed in the FIB-SEM by micro-compression using a nano-indenter equipped with a flat tip. Strain rate jumps have been performed to determine the strain rate sensitivity coefficient and the related activation volume. The activation volume is found to be of the order of 3-5 b3, considering that plasticity is mediated by Shockley partial dislocations. Transmission electron microscopy (TEM) thin foils were extracted from deformed micro-pillars via the FIB lift-out technique: TEM analysis reveals the presence of nano-twins as major mechanism of plastic deformation, involving Shockley partial dislocations. The presence of twins was never reported in previous studies on the plasticity of bulk InSb: this deformation mechanism is discussed in the context of the plasticity of small-scale samples.