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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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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Analytical Facilities
Chemistry and Material Sciences
Earth and Environmental 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.
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.
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).
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.
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.