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French Alternative Energies and Atomic Energy Commission
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Address:
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Gif-sur-yvette cedex, PO: 91191 (Undefined)
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French National Center for Scientific Research / Centre National de la Recherche Scientifique (CNRS)
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Address:
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3 Michel-Ange street, CNRS, Paris, PO: 75794, Ile-de-France (France)
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Micro- and Nanotechnology facilities
Engineering and Energy
Chemistry and Material Sciences
METSA supports actions regarding training on electron microscopy and atom probe from both theoretical and experimental points of views; it further correlates its action with the French Society of Microscopies (SFµ).
METSA provides access to 'state-of-the-art' electron microscopes and atom probe to the scientific community through experiment requests evaluated twice a year by a Program committee constituted by independent experts.
This category concerns 6 instruments with specific developments or accessories (commercial and/or home-made) dedicated to in situ experiments or various metrology approaches (heating / straining / environmental cell / cathodoluminescence / precession).1) JEOL 2010 200 kV (CEMES Toulouse): conventional TEM for in situ straining experiments (tensile testing, nanocompression at room and high temperature).2) JEOL 3010 300 kV (CINAM Marseille): conventional TEM equipped with an environmental cell (up to 4 mbar and up to 350°C - non oxidizing atmospheres).3) JEOL 2010F 200 kV (IRMA-CRISMAT Caen): dedicated for in situ 'temperature' experiments (heating / cooling liquid helium - nitrogen stages).4) JEOL 2011UHR 200 kV (LPS Orsay): dedicated for cryo-microscopy (sample preparation: cryo-ultramicrotomy, filmification liquid helium, cryo-fracture), lose dose illumination, heating/cooling 100°C and liquid nitrogen stage.5) FEI Tecnai G2 30 UT 60 - 300 kV (IRMA-CRISMAT Caen): HRTEM 0.18 nm, precession (dedicated to electron crystallography).6) STEM VG HB501 40 - 100 kV (LPS Orsay): dedicated STEM, HR EELS 0.27 eV (low temperature), cathodoluminescence.
The infrastructure offers an access to Advanced instruments based on TEMs or Scanning TEMs equipped with analytical accessories (EDX, EELS and imaging filters), optical correctors (probe and/or objective lens aberration correctors), monochromator, environmental configurations, biprisms, specific specimen holders (straining / heating / e-cells / tomography / cryo).1) JEOL ARM 80 - 200 kV (MPQ Paris): cold field emission, image Cs-corrector (0.075 nm), STEM (0.136 nm), EDX-SDD, GIF Quantum ER (0.26 eV), tomography, heating 1000°C / cooling liquid nitrogen stages, environmental cell (gas and liquid).2) FEI Tecnai 60 - 200 kV "SACTEM" (CEMES Toulouse): image Cs-corrector, STEM mode, GIF Tridiem, biprism for holography, Lorentz mode.3) FEI TITAN "Ultimate" 60 - 300 kV (PFNC CEA/LETI Grenoble): XFEG, monochromator for HR EELS (0.18 eV), probe and image Cs-correctors, STEM (0.07 nm), HREM (0.05 nm), GIF Quantum ultra-fast Dual EELS, corrected Lorentz lens, biprism for holography.4) FEI TITAN ETEM 80 - 300 kV (CLYM Lyon): image Cs-corrector (0.085 nm), environmental column (Pmax 25 mbar),Residual Gas Analyzing (RGA) system, heating stages 1000°C, STEM (0.136 nm), tomography, EDX-SDD Oxford Instruments, GIF Tridiem ERs (0.7 eV).5) Hitachi HF3300C "I2TEM" 60 - 300 kV (CEMES Toulouse): cold field emission, image Cs-corrector, biprisms for holography, Lorentz mode, STEM mode, Gatan Imaging Filter (GIF) Quantum ER (0.3 eV).6) JEOL 2100F 100 - 200 kV (IPCMS Strasbourg): probe Cs-corrector (0.11 nm), HRTEM (0.21 nm), GIF Tridiem, EDX-SDD, biprism for holography, heating 800°C / cooling liquid nitrogen stages, tomography.7) STEM NION USTEM 200 60 - 200 kV (LPS Orsay): dedicated STEM, ultra-stable stage, probe Cs-corrector, HR STEM (0.06 nm), HR EELS (0.27 eV).
FIBs are a recent class of characterization tools made of the association of a scanning electron microscope (or column) with an ionic column. The ionic column delivers a beam of ions which allows to 'nano-machine' the matter for (i) preparation of dedicated samples for TEM or atom probe studies, (ii) nano-manipulation of nano-objects (contacting / straining experiments, (iii) tomography by serial abrasion of micrometric volumes. 6 FIBs or SEM are available (listed as they appear on accompanying pictures):1) FEI Helios 600 FIB (IM2NP Marseille): for preparation of atom probe tips.2) ZEISS NVision40 FIB (CLYM, Lyon): cross beam instrument; floodgun, two micro-manipulators, FIBICS generator, 3D-EDX and 3D-EBSD; Resolution SEM 1.1 nm, FIB 4 nm.3) FEI Helios 600i NanoLab FIB - Focused Ion Beam - (CEMES Toulouse): double column instrument equipped with a micro-manipulator for TEM lamellae preparation.4) ZEISS NVision40 FIB (IRMA-GPM, Rouen): cross beam instrument for preparation of atom probe tips; EBSD.5) FEI Strata FIB (PFNC Grenoble): double column instrument equipped with a micro-manipulator for TEM lamellae preparation.6) FEI XL30 Environmental SEM (CLYM, Lyon): for in situ heating (stages 1000°C and 1500°C) and environmental experiments (pressure up to 10 Torr; resolution 2 nm at 7 Torr); tensile stage up to 250 daN; low voltage STEM tomography ± 180°, wet-STEM.
Atom probes are based on the field ion microscopy where atoms from a "needle" cut into a given material are analyzed one by one by mass spectrometry and collected on a 2D detector allowing a tomographic reconstruction of the explored volume to be reconstructed at a nanometric and atomic level from both morphological and chemical points of view. Laser-assisted instruments allow non-ideally conducting materials to be studied. 3 atom probes are available:1) CAMECA LEAP 4000 HR (IRMA-GPM, Rouen): electric mode for metals, detection limit about 50 ppm, typical analyzed volume 150x150x500 nm3, mass resolution 1000 (FWHM), acquisition speed > 2 M atoms/min, T° 25K.2) CAMECA Lawatap + / Flextap (IRMA-GPM, Rouen): laser-assisted 1030/532/343 nm, ion microscopy; high voltage 15 kV, detection limit 4 1017 at/cm3, typical analyzed volume 80x80x200 nm3, mass resolution 2500 (FWHM).3) Imago LEAP 3000 XHR (IM2NP, Marseille): electric (250 kHz) and laser (532 nm) modes, detection limit 1018 at/cm3 typical analyzed volume 150x150x500 nm3, high voltage 15 kV, T+ 20K.



