imust Project NSTEM Nanomanipulationwith Simultaneous TEM Observation PNNL, NanoLyon, ILM INL
History and context of the project TEM acquisition Latest results Impact & conclusion
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.
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)
Nanomanipulation in the TEM Mechanics Field Emission
Nanomanipulation in the TEM Shear Force Apex modification Based on Field Evaporation First observation of Atoms by Muller in 1955
Apex modification SiC nanowire PECVD carbon nanotube BN nanotube opened for nanofluidic experiments Si nanowire
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
The NSTEM project Jeol JEM2100, LaB 6 Global budget: 548 070 euros HT - CNRS 250 000 HT - UCBL CS 40 000 HT - Fédération Ingénierie 80 000 HT, - ILM 570 HT - LGTPE 5 000 HT - 172 500 HT imust Project 31 % of the budget
New results: Electron beam assisted field evaporation. Improving the electrical contact in SEM and TEM for electrical characterization.
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
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
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
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
Connection via metals with low melting temperature
Overview Training users 2013 2014 2015 2016 2017 11 4 5 9 Project Public tender Acceptance This presentation No schematics from JEOL Administrative and customs delay New TEM sample holder with nanomanipulators??
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)
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
Acknowledgements: INL: Jean Louis Leclerc, José Penuelas ILM: Nicholas Blanchard, Philippe Poncharal