Feb. 2010

Instrumentation

Pôle Instrumentation: Sébastien PAIRIS, Christiane CAPPOEN, Stéphanie GARAUDEEConsortium de Recherche pour l’Emergence de Technologies Avancées, Laboratoire de Géophysique Interne et de Tectonophysique

NEXANS - IMPHY (FUI-Superfacts), Schneider-Electric-TEC38

Physical and Chemical Characterization byScanning Electron Microscopy

Morphological observations of conductive... and non conductive nano objects

Secondary electron image of a non conductive luminescent silica sphere with CMONS active component obtained at low voltage (1kV) - A. IBANEZ, C. PHILPPOT (MatONLP)-ZEISS ultra+

Secondary electron image of a hanging carbon nanotubeobtained at low voltage (1 kV) - JP CLEUZIOU (NanoSpin)

ZEISS ultra+

Hanging carbon nanotube

Electrode (Pt)

Electrode (Pt)

EBSD measurements of phase and/or orientation rely on detecting and analyzing electron backscattered patterns generated in the SEM from a polycrystalline sample. A little part of Backscattering electrons undergoes Bragg reflexion on crystallographic planes and form bands (Kikuchi) on a pattern. This pattern is recorded on a phosphor screen behind a CDD camera. Theirs width, positions, intensities and symmetry in the pattern are due to the nature and the orientation of the crystal. Software determines the 3 Euler angles of the orientation in the Bunge definition repair.

Non-textured Nickel with twins Textured Nickel Substrate La2Zr2O7 layer on textured Ni Substrate

Map of the three Euler’s angles shows the grains

Off-line Calculation shows only the Σ3 twins boundaries <111> (60°)Random orientation is shown on

the pole figure

Electron BackScatter Diffraction – FUI Superfacts 2009-2011P. ODIER, JL. SOUBEYROUX (SupraMIT), S. GARAUDEE, S. PAIRIS (Pôle Instrumentation)

Crystallographic relationship between

Ni substrate and La2Zr2O7 epitaxial layer

50 µm 100 µm50 µm

Preferential orientation on textured Nickel is clearly shown on the pole figure

Epitaxial La2Zr2O7 follows crystallographic orientation of the substrate with 45° angle rotation

Actual spectral resolution

Electron Probe Microanalyser (EPMA)N. CAILLAULT, L. CARBONE - SCHNEIDER-ELECTRIC / 38TECD. BOURGAULT (SupraMIT), S. PAIRIS (Pôle Instrumentation)

An Electron Probe Microanalyser (EPMA) will be installed in January 2010. Quantitativeanalyses for heavy and lights elements ( Z > 5 ) will be performed thanks to very accurate high resolution measurements.

Equipment: 5 wavelength dispersive x-ray spectrometers (WDS) carrying each two crystals.

= EPMA

Spectra of EDS (yellow) and EPMA (blue) explain gain in spectral resolution and in

the ratio Peak versus background

The EPMA JEOL JXA-8800 on Schneider-Electric laboratory 38TEC

Localization of atoms species in hyperaccumulation plants

G. SARRET et al (LGIT), S. PAIRIS (Pôle Instrumentation)

Elemental EDX profile (170 µm) along a trichome of Arabidopsis Halleri to explain Zn accumulation capacity - G. SARRET & al (LGIT), S. PAIRIS (PôleInstrumentation) – JEOL840

Research and chemical analysis of phasesP. LEJAY, J. BALAY, A. HADJ-AZZEM,– (Pôle Cristaux Massifs), S. PAIRIS (Pôle Instrumentation)

Backscattered electron image of BaCo2V2O8 polish sample (20 kV) – P. LEJAY – ZEISS ultra+

Co-Kα

Ba-lα

V-Kα

O-Kα

EDX Spectra of the matrix and of the light phases on BaCo2V2O8 polish sample (20 kV) – P. LEJAY – ZEISS ultra+

EDX mapping of BaCo2V2O8 polish sample (20 kV)– P. LEJAY – ZEISS ultra+

Cobalt oxide

Matrix BaCo2V2Ox

Scanning Electron Microscopes Facilities

Field Emission Gun Scanning Electron Microscope (FESEM) - ZEISS ULTRA+ - (2008)

Energy Dispersive X-ray Spectrometry (SDD) – (2008)

Scanning Electron Microscope JEOL 840A (1989)

Energy Dispersive X-ray Spectroscopy (EDX- Si [Li] ) (1999)

Electron BackScatter Diffraction (EBSD) – (2009)

ANR PNano2006 - T. Fournier

FUI Superfacts 2009 - P. ODIER, JL SOUBEYROUX

Changing the energy of the incident electrons varies the volume of the electron-matter interaction in the sample : at low beam voltage for example, the upper layers are favoured compared to buried layers and the substrate. A multi-layer sample is characterized by doing x-ray analyses at different beam voltages. The results are treated by off-line calculation software packages (STRATAgem). The calculations use the nominal layer architecture as starting point, estimating fluorescence and absorption for its geometry. At the end of an iteration process, curves of predicted relative intensities corresponding to the chemical compositions and thicknesses found are drawn and compared with the experimental points to validate the analysis.

Thin films analysis based on EDX measurements

Results after iteration : the sample is composed by a Nb2O5 passive film of 5nm at the surface and a Nb86,3O13,7 layer of 302 nm on a silicon substrate.

The backscattered electron in-lens image (left) shows the chemical contrast between the layer and the silicon substrate. Morphological measurement confirms the thickness of the layer. On the right, experimental points which are resulting of EDX analysis at several energies and curves fits based of the iteration results are shown and confirm the process. E. COLLIN (ULT) , S. PAIRIS (PôleInstrumentation) – ZEISS ultra+

300 nm