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

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 prot...

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Main Authors: Yang, D, Phillips, NW, Song, K, Harder, RJ, Cha, W, Hofmann, F
Formato: Journal article
Idioma:English
Publicado em: International Union of Crystallography 2021
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author Yang, D
Phillips, NW
Song, K
Harder, RJ
Cha, W
Hofmann, F
author_facet Yang, D
Phillips, NW
Song, K
Harder, RJ
Cha, W
Hofmann, F
author_sort Yang, D
collection OXFORD
description 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, non-destructive Bragg coherent X-ray diffraction imaging is used to study the in situ annealing of FIB-milled gold microcrystals. Two non-collinear reflections are simultaneously measured 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 with thermocouple readings, which are shown to be substantially affected by thermal resistance. To evaluate the annealing process, each reflection is analysed by considering facet area evolution, cross-correlation maps of the displacement field and binarized 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°C and the self-diffusion of gold above ∼280°C. The majority of FIB-induced strains are removed by 380–410°C, depending on which reflection is being considered. These observations highlight the importance of measuring multiple reflections to unambiguously interpret material behaviour.
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spelling oxford-uuid:f9f56e1a-3bfe-41b8-9ac5-585ecc964c7e2022-03-27T13:01:56ZAnnealing of focused ion beam damage in gold microcrystals: an in situ Bragg coherent X-ray diffraction imaging studyJournal articlehttp://purl.org/coar/resource_type/c_dcae04bcuuid:f9f56e1a-3bfe-41b8-9ac5-585ecc964c7eEnglishSymplectic ElementsInternational Union of Crystallography2021Yang, DPhillips, NWSong, KHarder, RJCha, WHofmann, FFocused 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, non-destructive Bragg coherent X-ray diffraction imaging is used to study the in situ annealing of FIB-milled gold microcrystals. Two non-collinear reflections are simultaneously measured 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 with thermocouple readings, which are shown to be substantially affected by thermal resistance. To evaluate the annealing process, each reflection is analysed by considering facet area evolution, cross-correlation maps of the displacement field and binarized 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°C and the self-diffusion of gold above ∼280°C. The majority of FIB-induced strains are removed by 380–410°C, depending on which reflection is being considered. These observations highlight the importance of measuring multiple reflections to unambiguously interpret material behaviour.
spellingShingle Yang, D
Phillips, NW
Song, K
Harder, RJ
Cha, W
Hofmann, F
Annealing of focused ion beam damage in gold microcrystals: an in situ Bragg coherent X-ray diffraction imaging study
title Annealing of focused ion beam damage in gold microcrystals: an in situ Bragg coherent X-ray diffraction imaging study
title_full Annealing of focused ion beam damage in gold microcrystals: an in situ Bragg coherent X-ray diffraction imaging study
title_fullStr Annealing of focused ion beam damage in gold microcrystals: an in situ Bragg coherent X-ray diffraction imaging study
title_full_unstemmed Annealing of focused ion beam damage in gold microcrystals: an in situ Bragg coherent X-ray diffraction imaging study
title_short Annealing of focused ion beam damage in gold microcrystals: an in situ Bragg coherent X-ray diffraction imaging study
title_sort annealing of focused ion beam damage in gold microcrystals an in situ bragg coherent x ray diffraction imaging study
work_keys_str_mv AT yangd annealingoffocusedionbeamdamageingoldmicrocrystalsaninsitubraggcoherentxraydiffractionimagingstudy
AT phillipsnw annealingoffocusedionbeamdamageingoldmicrocrystalsaninsitubraggcoherentxraydiffractionimagingstudy
AT songk annealingoffocusedionbeamdamageingoldmicrocrystalsaninsitubraggcoherentxraydiffractionimagingstudy
AT harderrj annealingoffocusedionbeamdamageingoldmicrocrystalsaninsitubraggcoherentxraydiffractionimagingstudy
AT chaw annealingoffocusedionbeamdamageingoldmicrocrystalsaninsitubraggcoherentxraydiffractionimagingstudy
AT hofmannf annealingoffocusedionbeamdamageingoldmicrocrystalsaninsitubraggcoherentxraydiffractionimagingstudy