Annealing of focused ion beam damage in gold microcrystals: An in situ Bragg coherent X-ray diffraction imaging study

TL;DR

This study uses in situ Bragg coherent X-ray diffraction imaging to analyze how annealing reduces FIB-induced damage in gold microcrystals, revealing temperature-dependent strain evolution and the importance of multiple reflection measurements.

Contribution

It demonstrates the effectiveness of non-destructive in situ X-ray imaging for tracking FIB damage annealing in gold microcrystals and highlights the need to measure multiple reflections for accurate interpretation.

Findings

FIB-induced strains are largely removed at 380-410°C.

Multiple reflections provide clearer insights into strain evolution.

Gallium diffusion occurs below ~280°C, gold self-diffusion above.

Abstract

Focused ion beam (FIB) techniques are commonly used to machine, analyse and image materials at the micro- and nanoscale. However, FIB modifies the integrity of the sample by creating defects that cause lattice distortions. Methods have been developed to reduce FIB-induced strain, however these protocols need to be evaluated for their effectiveness. Here we use non-destructive Bragg coherent X-ray diffraction imaging to study the in situ annealing of FIB-milled gold microcrystals. We simultaneously measure two non-collinear reflections for two different crystals during a single annealing cycle, demonstrating the ability to reliably track the location of multiple Bragg peaks during thermal annealing. The thermal lattice expansion of each crystal is used to calculate the local temperature. This is compared to thermocouple readings, which are shown to be substantially affected by thermal resistance. To evaluate the annealing process, we analyse each reflection by considering facet area evolution, cross-correlation maps of displacement field and binarised morphology, and average strain plots. The crystal's strain and morphology evolve with increasing temperature, which is likely to be caused by the diffusion of gallium in gold below ~280{\deg}C and the self-diffusion of gold above ~280{\deg}C. The majority of FIB-induced strains are removed by 380-410\degree C, depending on which reflection is being considered. Our observations highlight the importance of measuring multiple reflections to unambiguously interpret material behaviour.