Microscopy

Support staff

Hamza BOUHRIZ
Maria KONSTANTAKOPOULOU

The electron microscopy service provides the laboratory, but also neighboring laboratories and teaching components of the University of Paris 13, with the tools necessary for the qualitative and quantitative characterization of materials at the mesoscopic and microscopic scales; for the past twenty years, it has been constantly enriched through the acquisition or development of new equipment.
The department has three SEMs and a TEM; they are equipped with their own devices for characterization and in situ thermomechanical tests.

Fleet of electron microscopes

MEB S360 (LEO brand, operational since 1990)

EBSD system adjustable in height

This conventional scanning electron microscope with tungsten filament is equipped with many accessories:

An automatic acquisition and analysis system of local crystallographic orientations (EBSD system: second generation HJELEN CCD camera, automatic indexing and TSL analysis software); the maximum EBSD indexing speed is 43 points per second.
A tensile machine for in situ tests up to 10000 N load and 800 °C temperature (machine developed in the laboratory, patent and CNRS license); the device, which also allows the realization of compression tests, cold or hot, or bending (4 points system), is also used for the realization of annealing in the framework of the studies on recrystallization
A shearing machine (monotonic or alternating test) up to 5000 N load
Two computers allowing the piloting of the SEM and its peripheral equipment (high resolution image acquisition, realization of microgrids and nanostructures by electronic lithography, automatic analysis of EBSD diagrams) and the piloting of the mechanical and thermal test devices in situ.
A fast and high resolution image acquisition system (Digiscan from GATAN).

MEB S440 (LEO, 1995)

EDX microanalysis

This conventional tungsten filament microscope was acquired in partnership with the LIMHP (Laboratory of Materials and High Pressure Engineering), the LEEC (Laboratory of Experimental and Comparative Ethology), and several teaching components of the Galileo Institute. It is equipped with an EDS microanalysis system (PGT) with an ultra-thin window for the detection of light elements (a new SDD detector operating without liquid nitrogen was installed in early 2011).

MEB FEG SUPRA 40VP (ZEISS, 2007)

Height adjustable EBSD system and other detectors

This high-resolution field emission gun microscope (Schottky type) can also operate in controlled pressure mode; it was acquired within the framework of a SESAME funding granted to the Ile-de-France Federation of Mechanics (F2MSP) for the acquisition of 3 FEG SEMs. Located on three different sites (LMS-X, LIM-ENSAM and LPMTM), they have specific characteristics in order to respond to the specific themes of each laboratory; additional funding has been granted by the CNRS and the P13 university.

The FEG SEM is equipped with a new generation of fast EBSD camera (HJELEN UF300, 305 points/s) and a high temperature heating furnace (GATAN, 1250 °C).
This set allows, among other things, the characterization of materials with very fine microstructure (ultra fine grain materials, nanostructured materials, etc.) and the realization of dynamic studies (microstructural characterization at high temperature for example).

MET 200 KV JEM 2011 (JEOL, 2004)

This microscope, acquired under a SESAME funding, with the support of the CNRS, the university and the general council of Seine-Saint-Denis, is operational since 2004 (initially common to the LPMTM and the LIMHP (which became LSPM in early 2011).
It is equipped with filtered imaging (GIF from GATAN) and beam scanning (STEM) systems. Two digital cameras allow image acquisition (1000*1000 resolution), one (GATAN dual Vision) is placed in the wide angle port for low magnification observations (dislocation microstructures) and indexing of diffraction patterns, the other (Multi Scan) at the GIF filter output for filtered imaging and high resolution. It can be equipped with several specimen holders (rotation-tilt, traction, heating, etc.).
The preparation of the thin slides is performed either with an electrochemical polishing equipment associating a STRUERS TENUPOL III polishing unit with a LAUDA cryostat, or with an ion thinning apparatus (PIPS from GATAN).

Les équipements périphériques

Instrumented in situ testing machines

Tensile testing machine (10 kN and 800 °C capacities); additional modules allow compression (5 kN, 600 °C) and bending (2.5 kN) tests.

Heating device
Compression and bending modules

Shearing machine allowing monotonic or alternated tests (5 kN).

Specific devices for characterization and fabrication of microstructures

2 EBSD systems for the acquisition and processing of backscattered electron diffraction patterns (maximum acquisition speeds of 43 and 305 points per second respectively).
4 EBSD analysis licenses (OIM Analysis from TSL and HKL CHANNEL5 from Oxford Instruments).
1 Si-Li diode EDX microanalysis (PGT).
1 RAITH ELPHY QUANTUM electron lithography system.

Additional equipment (metallographic preparation)

Ion etching and metallization system (PECS by GATAN, 2003) This system meets the needs of sample preparation for their characterization by EBSD; it also allows the etching of thin slides for TEM (but not their thinning) and the controlled deposition of all types of materials (e.g. for the realization of magnetic nanolayers).
Ion thinning system for TEM (PIPS from GATAN, 2004) This system allows the preparation of non-conductive samples; it is completed by a mechanical pre-thinning device (Dimple Grinder type from GATAN).
The preparation of thin metal slides is ensured by an electrochemical polishing equipment associating a STRUERS TENUPOL III polishing unit with a LAUDA cryostat and allowing the realization of thin slides up to 2.5 mm in diameter and in a temperature range between -80 and + 50 °C.
EDWARDS evaporation bench and POLARON sputtering apparatus for the metallization of samples