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

J Appl Crystallogr. 2023 Feb 28;56(Pt 2):381-390. doi: 10.1107/S1600576723000493. eCollection 2023 Apr 1.

Abstract

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.

Keywords: InSb; coherent X-ray Bragg diffraction; compression; in situ; micropillars.

Grants and funding

This project has received funding from the European Union’s Horizon 2020 research and innovation programme under the Marie Skłodowska-Curie grant agreement No. 701647, as well as SNSF grant No. 200021L_169753, and from ANR grant Nos. ANR-16-CE93-0006 and ANR-19-CE08-0007, ‘Investissement d’Avenir’ (LABEX INTERACTIFS, ANR-11-LABX-0017-01), and Nouvelle Aquitaine Region/European Structural and Investment Funds (ERDF No. P-2016-BAFE-94/95).