(Advanced) FIB sample preparation for (high performance) TEM analysis
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1 (Advanced) FIB sample preparation for (high performance) TEM analysis Bertrand Van de Moortèle Laboratoire de Géologie de Lyon Terre, Planètes, Environnement ENS de Lyon CROSSBEAM MICROSCOPY Metz, June 12, 2013
2 (Advanced) FIB sample preparation for (high performance) TEM analysis Bertrand Van de Moortèle Laboratoire de Géologie de Lyon Terre, Planètes, Environnement ENS de Lyon CROSSBEAM MICROSCOPY Metz, June 12, 2013
3 CLYM, FED 4092, ww.clym.fr Thierry EPICIER (MATEIS INSA) JEOL 2010F déc.2012 TOPCON JEOL LEO-912 Phoenix-Varian ETEM TM commercial 2000 FEI-ESEM-XL30 ZEISS-NVision40 instruments partagés labos/clym ZEISS Supra 55VP TESCAN mira instruments 100% CLYM 2010 INL-INSA de Lyon instruments labos
4 Michael J. Stringer
5 Detectors: SESI, BSE, InLens, EsB, STEM µmanipulators: 2 KlockeNanotechnik Analytique: EDX SDD 50 mm 2 Oxford; EBSD camera NordlysF + N. BLANCHARD (LPMCN Lyon I) GIS : W, SiO x, C, H 2 0, XeF 2 Flood Gun External Scan generator : FIBICS T. DOUILLARD (MATEIS INSA) A. DESCAMPS-MANDINE (INL INSA)) B. VAN DE MOORTELE (LGL ENS Lyon)
6 Paris Lizardite dépôt C, W, SiOx assisté aux électrons Olivine + carbonate DAC sample (H. Piet, EPFL)
7 lowvoltage(1kv) highcurrent(ap.120µm,hcmode) slowscan Scheme of interactions of primary electrons generating an emitted flux of secondary electrons and backscattered electrons. All electrons can dissociate surface adsorbed molecules via electronic excitation.
8 Scheme of interactions of primary ions generating secondary electrons and a collision cascade of substrate atoms. The nonsputtered target atoms remain as excited surface atoms contributing to molecule dissociation.
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10 Lift-out view SEM SEM objective lens sin view FIB 386 µm 477 µm
11 Lift-out Gluing on copper grid Milling
12 SEM objective lens Ga + e - FIB column +V ( V) SE detector
13 Electron transparency 9 µm 280 nm θ= grey level ~ linearity lamella thickness (nm)
14 before after θ= 6 FIB Low Voltage : 2 kv over tilt deposition mode 0.5 µm
15 in-situ nano-indentation Understand the behavior of the soot particles/ aggregates on the liner surfaces without and with anti-wear tribofilm Liner Oil film Piston I. Lahouij, B. Vacher, F. Dassenoy (LTDS, ECL) B. Van de Moortèle (LGL, ENS de Lyon) Ring Soot particles Diamond tip Diamond tip Steel substrate Sliding direction Loading direction Tribofilm Steel substrate Sliding direction Liner /soot contact Liner/tribofilm/soot contact
16 in-situ nano-indentation SEM objective lens
17 in-situ nano-indentation
18 in-situ nano-indentation SEM objective lens
19 in-situ nano-indentation
20 in-situ nano-indentation 200 nm t/l θ t = 0.1 µm L = 20 µm θ nm
21 in-situ nano-indentation 90
22 in-situ nano-indentation
23 Stress Relaxation Silicate Silicate LMA : laboratoire de Matériaux avancés, univ. de Lyon 1 22
24 (1, 2) (1) from, Zeiss CrossBeam User Meeting 2012, Schulmeyer. (2) S. Chalal, Zeiss France, is thanked for giving us the opportunity to use the X2 sample holder
25 (1, 2) (1) from, Zeiss CrossBeam User Meeting 2012, Schulmeyer. (2) S. Chalal, Zeiss France, is thanked for giving us the opportunity to use the X2 sample holder
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27 E. Amiguet 1, B. Van de Moortèle 1, P. Cordier 2, N. Hilairet 2, B. Reynard 1 1 LGL, ENS de Lyon 2 Unité Matériaux et Transformation, USTL 0.2 µm 0.2 µm
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31 phase map olivine Euler map carbonate S. Peuble, thèse (en cours), lab. LGL, de 2013 Lyon crossbeam microscopy, Metz, ENS June 12,
32 31
Y. LIU 1, H. YUAN 1,2, A. BOGNER-VAN DE MOORTELE 1, B. VAN DE MOORTELE 2, T. EPICIER 1
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2012/01/20. Thierry EPICIER. MATEIS-CLYM, umr CNRS5510, Director METSA (FR 3507 CNRS) M. AOUINE, JP MILLET et al.
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