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Communication Dans Un Congrès Année : 2023

3D in situ and environmental TEM studies of nanomaterials in action

Résumé

Environmental Transmission Electron Microscopy (ETEM) aims at studying nano-objects in a liquid or gaseous atmosphere in the TEM. Nanomaterials exposed to such conditions at a given temperature generally experience phase transitions, crystallographic and compositional changes. These processes induce a morphological evolution which may be fast or very fast. When classical 2D imaging is possible since a few decades even at atomic resolution during such reactions [1], following them in situ in three dimensions (3D) is a difficult challenge since rapid data acquisition is required. The term ‘3D’ here is preferred to ‘tomography’: indeed, Electron Tomography (ET) in TEM does not refer to a ‘slice’ ('tomos' in Greek) method as, for example, the slice-and-view approach in FIB (see e.g. [2]), but rather to an algorithmic reconstruction of 2D projections acquired during tilt series over a large angular amplitude or using a collection of randomly oriented identical objects [3]. This contribution will present recent ETEM (FEI/TFS Titan ETEM 60-300 kV) experiments on nanomaterials, essentially nanocatalysts, exposed to gases at high temperature using a DENSsolutions Wildfire heating holder, or during cooling experiments under water vapor. We first illustrate simple ways to obtain a pertinent 3D information in real space without undertaking complete tilt series, in order to speed up the acquisition and, incidentally, reduce the possible beam irradiation effects. We will then focus on ‘classical’ but fast ET. If diffraction acquisitions on the fly while continuously rotating the sample is now frequently used in biology (e.g. the ‘microED’ technique, extending the capabilities of earlier methods for automated diffraction tomography - see references within review [4]), few works have been published on nanomaterials imaged in real space and in real time, meaning faster than one minute or so down to a few seconds. For single nanoparticles under dynamic conditions, STEM tomography can be employed, and possibly successfully accelerated even at atomic resolution [5,6], but the 3D characterization of large populations of objects remains more efficient in conventional TEM imaging (see examples from our group [7]) owing to the speed and sensitivity of modern cameras at several fps. Acknowledgements The support of the French National Research Agency ANR through projects 3DCLEAN n°15-CE09-0009-01 and WATEM n°20-CE42-0008 is gratefully acknowledged. Thanks are due to CLYM (www.clym.fr, a member of the French METSA network www.metsa.fr) for the access to the ETEM. The author is indebted to several contributors to some of the reported experiments: Benlekbir S. (Toronto, CA), Koneti S., Roiban L., Grenier T., Ndaya-Cibaka C., Santos Aires F.C., Ehret E. (Univ. Lyon, F). [1] Boyes E.D, Gai P.L., (2014) doi.org/10.1016/j.crhy.2014.01.002 [2] Yuan H. et al., (2021) doi.org/10.1016/j.ultramic.2021.113265 [3] Frank J. (ed.), Electron Tomography, Springer New York, (2010) 456 p., ISBN 978-1-4419-2172-7 [4} Nannenga B.L., Gonen T., (2019) doi.org/10.1038/s41592-019-0395-x [5] Altantzis T. et al., (2019) doi.org/10.1021/acs.nanolett.8b04303 [6] Zhou J. et al., (2019) doi.org/10.1038/s41586-019-1317-x [7] Roiban L. et al., (2017) doi.org/10.1111/jmi.12557; Banjak H. et al., (2018) doi.org/10.1016 /j.ultramic.2018.03.022; Epicier T. et al., (2019) doi.org/0.1016/j.cattod.2019.01.061; Koneti S. et al., (2019) doi.org/10.1016/j.matchar.2019.02.009; Monpezat A. et al., (2019), http://doi.org/10.1021/ acsanm.9b01407
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hal-04229765 , version 1 (05-10-2023)

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  • HAL Id : hal-04229765 , version 1

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T. Epicier. 3D in situ and environmental TEM studies of nanomaterials in action. IMC20, Sep 2023, Busan, South Korea. ⟨hal-04229765⟩
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