Focused Beams for use in EBSD

Session

Poster Session One

Authors

Dr. Bartlomiej Winiarski (1)

Affiliations

1. Thermo Fisher Scientific

Keywords

FIB, PFIB, femtosecond Laser, SEM, EBSD, EDS, Direct Electron Detection

Abstract text

Focused beams (electrons, ions, and photons) are at the forefront of today’s and future scientific and engineering advanced research instruments. The beams are typically used for six purposes [1]: imaging, detection, deposition, implantation, milling/ablation, and polishing. There are plethora of detectable and useful signals coming from the beam irradiated matter. One of the signals is electron diffraction and scattering on a crystal planes used by Electron Backscattered Diffraction (EBSD) method [2]. This surface superficial probing technique is sensitive to surface contamination, amorphization, and lattice distortions, thus requires damage-free sample surface preparation techniques.

In the beginning these beams formed standalone research platforms. The development of FIB-SEM microscope opened up in situ, and site-specific investigation in the micro- and nano-scale, and in two- and three-dimensions. Improved beams performance, various electron detection channels and analytical detectors (EBSD, Energy-Dispersive X-ray Spectroscopy - EDS, Wavelength-Dispersive X-ray Spectroscopy - WDS, etc.) add new imaging modalities and quantitative analyses possibilities. Xenon Plasma FIB expands the application space, and increases 3D EBSD material volume analyzed with DualBeams [3]. EBSD and EDS data mapping remain the slowest part of the 3D data collection workflow, although there are exciting improvements in detector speed with direct electron detection (DeD) EBSD [4, 5] and elemental mapping [6, 7]. Multi-ion plasma beam and low keV beam performance further expands the application spaces of PFIB to (a) a broader range of life sciences applications (with oxygen beam) [8], (b) near damage-free surface preparation (with Argon and Xenon beams) [9]. The recent addition of femtosecond laser beam to the Helios 5 DualBeam microscope platforms enables the collection of high-quality 3D EBSD datasets in the mm3 volume range [10] at submicron SEM imaging resolution. Athermal femtosecond laser serial sectioning of soft polymers and biological materials, as well as integrated circuit devices, demonstrates good surface quality and finish [10]. PFIB-SEM and Laser PFIB-SEM becoming an essential part in the multi-modal Correlative microscopy (CM) workflows [11], being the essential link between the macro- and nano-scale. The envisaged advancement of CM workflows, on-the-fly data reconstruction, smart sampling, active prior knowledge analysis and instrument feedback, additional imaging modalities will expand the already broad application envelope of the focused beams.

This contribution briefly reviews the last 30 years of the development of the focused beams (electron, ion, and photon beams), and their application for the EBSD and TKD methods.

References

[1] Yao, N., Focused Ion Beam Systems, Basics and Applications 2010, Cambridge, MA: Cambridge University Press

[2] Schwarzer, R.A., et al., Present State of Electron Backscatter Diffraction and Prospective Developments. Electron Backscattered Diffraction in Materials Science, ed. A.J. Schwartz, et al.2009, New York: Springer.

[3] Burnett, T.L., et al., Large volume serial section tomography by Xe Plasma FIB dual beam microscopy. Ultramicroscopy, 2016. 161: p. 119–129.

[4] Marshall, A.L., et al., The EBSD spatial resolution of a Timepix-based detector in a tilt-free geometry. Ultramicroscopy, 2021. 226: p. 113294.

[5] Wang F., at al., Electron backscattered diffraction using a new monolithic direct detector:

High resolution and fast acquisition. Ultramicroscopy 220 (2021) 113160

[6] Marks, S. at al., Live EDS Mapping of the Precipitation and Annealing Cycle of Alloys in the TEM

Generated Through in Situ Heating. Microsc. Microanal. 25 (Suppl 2), 2019, doi:10.1017/S1431927619008304

[7] Wandrol P., at al., ChemiSEM: multimodal approach for faster quantitative elemental mapping. Microsc. Microanal. 27 (Suppl 1), 2021, doi:10.1017/S1431927621004864

[8] Wang, J., et al., Reactive oxygen FIB spin milling enables correlative workflow for 3D super-resolution light microscopy and serial FIB/SEM of cultured cells. Scientific Reports, 2021. 11(1).

[9] Jiao, C., et al. Low Energy 500 eV Focused Argon Ion Beam Provided by Multi-Ions Species Plasma FIB for Material Science Sample Preparations. in 2021 Microscopy and Microanalysis Conference. 2021. Virtual Meeting: Cambridge Press.

[10] Echlin, M.L.P., et al., Recent Developments in Femtosecond Laser-Enabled TriBeam Systems. JOM, 2021. 73(12): p. 4258-4269.

[11] Winiarski, B. and R. Geurts, Laser Xe+ Plasma FIB-SEM: Correlative microscopy of 3D microstructures from nanometers to millimeters. Microscopy and Microanalysis, 2020. July/August '20: p. S4-S8.