imust Project NSTEM Nanomanipulationwith Simultaneous TEM Observation PNNL, NanoLyon, ILM INL

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1 imust Project NSTEM Nanomanipulationwith Simultaneous TEM Observation PNNL, NanoLyon, ILM INL

2 History and context of the project TEM acquisition Latest results Impact & conclusion

3 TOPCON 002B TEM acquired en 1993 New spare parts no longer available (Topcon ceased commercial activities in electron microscopy) The PNNL plateforme (Plateforme Nanotubes et Nanofils Lyonnaise) started to work on nanomanipulation in SEM et TEM.

4 Nanomanipulation under TEM P. Poncharal developed home made in-situ TEM sample holder Sample (tips) heating up to 1500 K Precision positioning via external microscrew and piezo movements (nm resolution) (mechanical drift) Electrical and piezo mechanical actuation High voltage biasing of the sample (up to 2000 V)

5 Nanomanipulation in the TEM Mechanics Field Emission

6 Nanomanipulation in the TEM Shear Force Apex modification Based on Field Evaporation First observation of Atoms by Muller in 1955

7 Apex modification SiC nanowire PECVD carbon nanotube BN nanotube opened for nanofluidic experiments Si nanowire

8 The NSTEM project In 2013 M. F. Joubert asked us to apply to the 2014 imust call to complete the financing to acquire a new TEM In order to sustain and grow our Nanomanipulation activities in the TEM. Project bringing together several teams from several laboratories The projet was proposed by two plateformes: PNNL and NanoLyon 180 k obtained to complete the TEM financing

9 The NSTEM project Jeol JEM2100, LaB 6 Global budget: euros HT - CNRS HT - UCBL CS HT - Fédération Ingénierie HT, - ILM 570 HT - LGTPE HT HT imust Project 31 % of the budget

10 New results: Electron beam assisted field evaporation. Improving the electrical contact in SEM and TEM for electrical characterization.

11 Electron beam assisted field evaporation. Why do highly insulating materials like BN desorb so easily (sometimes without DC voltage)!!! The electron beam plays a major role in inducing positive charging of the sample (for thin enough sample). I 0 I D I E I S U I 0 V DC

12 Electron beam assisted field evaporation. Why do highly insulating materials like BN desorb so easily (sometimes without DC voltage)!!! Observation of electron beam induced field evaporation of a BN nanotube Successive field evaporation of two close BN nanotubes

13 Electron beam assisted field evaporation. Interest and originality of this method? Considerable effort is currently necessary to characterize samples at the ultimate length scales (which atoms?, their position?,.) TEM et Atom Probe, réseau METSA Thomas Kelly, CAMECA Patent ANR project

14 Improving the electrical contact in SEM and TEM for electrical characterization. Main problem for electrical characterization of nanowires Glue that polymerizes under electron beam irradiation: no contact Connection via metals with low melting temperature

15 Connection via metals with low melting temperature

16 Overview Training users Project Public tender Acceptance This presentation No schematics from JEOL Administrative and customs delay New TEM sample holder with nanomanipulators??

17 Impact INL ILM - Hétéroépitaxie et Nanostructures - Photovoltaïque - Chimie et Nanobiotechnologies - Agrégats et Nanostructures - FemtoNanoOptics - Luminescence - (nano)matériaux pour l'énergie - Nanostructures Magnétiques - Physique des Nanostructures et Emission de Champ - CERA (Matériaux Céramiques et Composites) - METAL (METaux et ALliages) - SNMS (Structures, Nano- et Micro-Structures) - PVMH MATEIS ENS Lyon chimie - Matériaux Fonctionnels et Photonique - Structuration Multi-échelle des Matériaux - Couches Minces LMI GaAsnanowireswith oxidation-proof As capping for the growth of epitaxial shell, X. Guan, J. Becdelievre, A. Benali, C. Botella, G. Grenet, P. Regreny, N. Chauvin, N. P. Blanchard, X. Jaurand, G. Saint-Girons, M. Gendry, J. Penuelas, Nanoscale 8 (2016) GaAscore / SrTiO3 shell nanowiresgrown by Molecular Beam Epitaxy, X. Guan, J. Becdelievre, B. Meunier, A. Benali, G. Saint-Girons, R. Bachelet, P. Regreny, C. Botella, G. Grenet, N.P. Blanchard, X. Jaurand, M. Silly, F Sirotti, M. Gendry, J. Penuelas, Nano Letters 16 (2016)

18 Conclusion Procurement of a new JEOL 2100 microscope Trained users New sample holders with nanometric movements should be ready by the end of the year

19 Acknowledgements: INL: Jean Louis Leclerc, José Penuelas ILM: Nicholas Blanchard, Philippe Poncharal

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