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Operando and real time 3D analysis of Nanomaterials

Thierry Epicier, CNRS Research Director, member of MATEIS Laboratory, Lyon, will give a lecture about "Towards Operando and real time 3D analysis of Nanomaterials in Environmental TEM", thursday 15th february
Léonard de Vinci Building, e-media amphitheater
Add to my Calendar02/15/2018 1:30pm 02/15/2018 3:00pm Operando and real time 3D analysis of Nanomaterials Léonard de Vinci Building, e-media amphitheater Europe/Paris public

In the last decade, Environmental Transmission Electron Microscopy (ETEM) has become a new sharp blade of the TEM' Swiss Army knife for studying materials at the nanoscale in almost operando conditions. Spectacular technological improvements have been made for both dedicated ETEMs and E-cells [1, 2], enabling today to follow a chemical reaction under gas and in temperature down to the atomic level.

Doing so, one of the scientific locks to be lifted is the temporal resolution required to follow the dynamic of the process to be studied. Another challenging topic is the need for 3D information during the evolution of the object when exposed to reactive conditions and more ambitiously, mechanical stimuli.

We will survey here several studies related mostly to nanocatalysts and conducted on the 80-300 kV Cs-corrected FEI-TITAN ETEM installed at CLYM in Lyon in 2013. In most of experiments, a Wildfire heating-holder (DENSsolutions) was used with 1300°C compatible Si/SiNx nanochips. Its high tilting capability of ± 72° allows in situ nano-tomography. A high speed Oneview camera from Gatan capable of acquisition rates at several hundreds frames per second (100 fps in 2K) allows fast tilting' tomography at the minute and even second level [3], which opens the way to quantitative 3D kinetics studies of nanocatalysts under operando conditions. Illustrated works concern:

- The oxidation of soot by YSZ catalysts in the contest of Diesel motors depollution [4]
- A Quantitative atomic mobility at {100} surfaces of ceria (cerium dioxide CeO2) nanocubes under different atmospheres, see figure 1 [5].
- Preliminary in situ nanocompression of nanoparticles (depending on time)
During this presentation, attention will be paid to the influence of the electron beam on the observed processes (irradiation effects). Some clues will be discussed regarding the development of routine 5-10 seconds' fast operando nanotomography in the ETEM. Big data issues (regarding storage and more importantly image processing) will also be evoked [6].

[1] J. Jinschek, Chem. Commun., 50 (2014), 2696-2706; E.D. Boyes, P. Gai, C. R. Physique 15 (2014), 200-213; P.A. Crozier, T.W. Hansen, MRS Bull. 40 (2015), 38-45; S Takeda, Y Kuwauchi, H Yoshida, Ultramicroscopy 151 (2015), 178-190.
[2] "Controlled Atmosphere Transmission Electron Microscopy", ed. T.W. Hansen, J.B. Wagner (Springer, New York), (2016), 332 p.
[3] A. Serve, T. Epicier, M. Aouine, F.J. Cadete Santos Aires, E. Obeid, M. Tsampas, K. Pajot, P. Vernoux, Appl. Catal. A, 504 (2015) 74-80.
[4] L. Roiban, S. Li, M. Aouine, A. Tuel, D. Farrusseng, T. Epicier, J. of Microscopy 269, 2 (2018), 117-126.
[5] M. Bugnet, S. H. Overbury, Z. Wu, T. Epicier, Nano Letters, 17 12 (2017), 7652-7658.
[6] This work is largely based on ongoing projects involving several colleagues at Univ. Lyon: S. Koneti, L. Roiban, M. Bugnet, L. Joly-Pottuz, K. Masenelli-Varlot from MATEIS, INSA-Lyon; M. Aouine, F.C. Santos Aires, Philippe Vernoux, Diego Lopez-Gonzalez from IRCELYON, UCBL; T. Grenier, H. Banjak, V. Maxim from CREATIS, INSA-Lyon; I. Jenei, F. Dassenoy from LTDS, ECL). The support of ANR through the project 3DCLEAN n°15-CE09-0009-01 is gratefully acknowledged. Thanks are due to CLYM ( for the access to the Environmental microscope which was founded through a CPER project funded by the Rhône-Alpes region, the Great Lyon' and the CNRS.