Automation of Simultaneous 4DSTEM-EDX Acquisition and Data Analysis for Beam-sensitive Materials

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Automation of Simultaneous 4DSTEM-EDX Acquisition and Data Analysis for Beam-sensitive Materials

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Author(s): Jinseok Ryu ¹ , Alexandra A. Sheader ² , Mohsen Danaie ¹ , David G. Hopkinson ¹ , Katherine E. MacArthur ³ , Nakita K. Noel ² , Christopher S. Allen ¹ ^, ⁴ ^,

Publication date (Electronic): 21 January 2025

Conference name: 13th Asia Pacific Microscopy Congress 2025 (APMC13)

Conference date: 2-7 Febuary 2025

Keywords: 4DSTEM, EDX, automation, beam-sensitive materials, machine learning

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Abstract

The electron beam for scanning transmission electron microscopy (STEM) provides rich information about the atomic structure and chemical composition of materials from micron to atomic scale. However, the electron probe can also damage the materials of interest, as the high-energy electrons are often focused on very small sample regions [ 1]. These effects limit the quality of information which can be extracted from experiments on beam-sensitive materials, such as Li-ion battery materials and metal halide perovskites used in solar cell devices [ 2]. However, with the increasing interest in these materials to address environmental and societal concerns, a detailed understanding of their microstructure and chemical composition at high spatial resolution is needed to improve their performance and stability.

For these materials, the correlation between processing and nanoscale structure-property relationships has been difficult to firmly establish. As shown in Fig. 1a- 1c, phase change or amorphisation in beam-sensitive materials can be easily caused by a focused electron probe. Fortunately, this problem can be solved through combined scanning electron nano-diffraction (SEND) [3] and energy dispersive X-ray spectroscopy (EDX) with low electron dose conditions, providing nanoscale crystallographic and chemical information from the specimen. However, the signal-to-noise (SNR) of the EDX data is very poor - with just a few counts in any individual scan prohibiting comprehensive materials characterisation (Fig. 1d).

To address this, we perform automated SEND-EDX data acquisition under low dose conditions utilising our automated data analysis workflow. By communicating with two different modalities, i.e., Aztec ^®; Oxford Instruments and MerlinEM; Quantum Detectors, and using our Python-based software, many SEND-EDX data pairs were simultaneously acquired from a metal halide perovskite.

Fig. 1

(a) Virtual annular dark-field image of a metal halide perovskite; (b, c) sum of diffraction patterns for the green square area of 2×2 pixels in (a) for the 1 ^st and the 7 ^th frames, respectively; after multiple scans with the dwell time of 1 millisecond for the same area, some diffraction peaks, marked with white circles, disappeared or were weakened due to the beam damage; (d) sum of energy dispersive X-ray spectra for a spectrum image of 128×127 pixels

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Publication date (Electronic): 21 January 2025

Electronic Location Identifier: e197

Affiliations

[1 ]electron Physical Science Imaging Centre, Diamond Light Source Ltd., Didcot, Oxfordshire, United Kingdom

[2 ]Department of Physics, University of Oxford, Oxford, Oxfordshire, United Kingdom

[3 ]Oxford Instruments Materials Analysis, High Wycombe, Buckinghamshire, United Kingdom

[4 ]Department of Materials, University of Oxford, Oxford, Oxfordshire, United Kingdom

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*Corresponding author: christopher.allen@ 123456diamond.ac.uk

Author information

Jinseok Ryu https://orcid.org/0000-0002-9558-3469

Mohsen Danaie https://orcid.org/0000-0002-9325-7571

David G. Hopkinson https://orcid.org/0000-0003-4259-7450

Katherine E. MacArthur https://orcid.org/0000-0002-5024-2054

Nakita K. Noel https://orcid.org/0000-0002-8570-479X

Christopher S. Allen https://orcid.org/0000-0002-6353-6000

Article

DOI: 10.14293/APMC13-2025-0197

SO-VID: 1a71a611-fdf3-4eab-bb1c-f1c4c62b1404

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Published under Creative Commons Attribution 4.0 International ( CC BY 4.0). Users are allowed to share (copy and redistribute the material in any medium or format) and adapt (remix, transform, and build upon the material for any purpose, even commercially), as long as the authors and the publisher are explicitly identified and properly acknowledged as the original source.

Conference name: 13th Asia Pacific Microscopy Congress 2025

Conference acronym: APMC13

Conference number: 13

Conference location: Brisbane, Australia

Conference date: 2-7 Febuary 2025

History

Funding

Funded by: Physical Science Imaging Centre

Award ID: MG38966

J. Ryu acknowledges funding from the InFUSE Prosperity Partnership.

References

1. N. Jiang, Reports on Progress in Physics 79.1 (2015), p.016501. https://doi.org/10.1088/0034-4885/79/1/016501
2. Q. Chen et al., Advanced Materials 32.16 (2020), p.1907619. https://doi.org/ 10.1002/adma.201907619
3. TAS. Doherty et al., Science 374.3575 (2021), p.1598. https://doi.org/10.1126/science.abl4890
4. Y. An et al., Energy & Environmental Science 14.12 (2021), p.6638. https://doi.org/10.1039/D1EE02691G

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[1] 1. N. Jiang, Reports on Progress in Physics 79.1 (2015), p.016501. https://doi.org/10.1088/0034-4885/79/1/016501

[2] 2. Q. Chen et al., Advanced Materials 32.16 (2020), p.1907619. https://doi.org/ 10.1002/adma.201907619

[3] 3. TAS. Doherty et al., Science 374.3575 (2021), p.1598. https://doi.org/10.1126/science.abl4890

[4] 4. Y. An et al., Energy & Environmental Science 14.12 (2021), p.6638. https://doi.org/10.1039/D1EE02691G

Automation of Simultaneous 4DSTEM-EDX Acquisition and Data Analysis for Beam-sensitive Materials

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