Microstructural Characterisation

Scanning electron microscope FEI NNS 450 with  EDS detector

Scanning Electron Microscopy (SEM) is used for the imaging and characterisation of material surfaces at the µm and nm scale. Chemical and physical information about particle topography and morphology can be provided.

The method is based on the interaction between electrons and matter. A 3-dim image is built up by scanning the materials surface point by point by means of an electronic probe.

The NOVA NanoSEM 450 was installed at ISL in the year 2013 and belongs to the last generation of high resolution scanning electron microscopes.

Technical features

  • Schottky FEG hot tip
  • Acceleration voltage: 50 V to 30 kV
  • Probe current 0.6 pA to 30 nA
  • Magnification: 35 x to 1 000 000 x
  • Resolution: 1 nm at 15 kV (SE) ; 1.4 nm at 1 kV (SE)
  • Detector EDS SDD Bruker XFlash 50 to 30 mm²
scanning electron microscope
 

High Resolution Transmission Electron Microscopy (HRTEM) JEOL JEM 2011 with EDS detector

(High Resolution) Transmission Electron Microscopy is used to realise structural and morphological analysis of solid samples at the µm scale, nm-scale and even at the atomic level.

The method is based on the interaction of electrons with matter. Detection is done underneath the sample that has been trespassed by fast electrons. Therefore the samples must be prepared in a special and specific way to be transparent to electrons (<100 nm).

Technical features

  • LaB6 Tip
  • High voltage: 80 to 200 kV
  • Resolution: 0.2 nm
  • Magnification: 50x to 500 000x
  • EDS detector: SDD Sahara Bruker
TEM microscope
 

Electronic micro probe CAMECA SX100

This in-situ analytical method is dedicated to the X-ray microanalysis and quantitative precision analysis to realize X ray cartography.

A focused electronic beam coupled with high energy is used to generate characteristic X ray beams of the elements present in the interesting zone. The emitted beams are selected by diffraction thanks to monochromatic crystals; their intensity is then measured thanks to proportional counters.

The elementary content can be deduced of the measured X intensity by comparing them with known standard elements after having corrected the matrix effects. The major and minor elements (from B to U) can be quantified within the materials. It is also possible to detect traces of elements (some ten of ppm) .

Technical features

  • 5 wavelengh dispersive X-ray spectroscopy
  • 1 Energy-dispersive X-ray spectroscopy EDS (SDD Röntec)
  • Optical camera (field from 260 µm to 1600 µm)
electronic micro probe
 

Atomic Force Microscope AIST-NT CombiScopeTM-1000SPM coupled with Confocal Raman Microscope Horiba LabRam HR Evolution

Atomic Force Microscopy – Tip Enhanced Raman Spectroscopy (AFM-TERS) enables simultaneous topographical imaging and vibrational spectroscopy on the nanoscale. In contrary to Scanning or Transmission Electron Microscopy the energy input during the measurements is relatively low. Thus chemical information and structure of organic materials, which would decompose under the electron beam of an electron microscope, can be received. AFM-TERS is especially suitable for the investigation of energetic or pharmaceutical nanostructured composites.

During a typical AFM-TERS measurement a probe equipped with a gold or silver nanoparticle at its tip apex scans the sample of interest. Meanwhile, a focused laser beam illuminates the tip apex. According to a strong field enhancement due to the gold or silver nanoparticle, Raman spectra can be recorded of small amounts of substances, such as single nanoparticles.

The AFM-TERS was installed at ISL in 2017. It is one of the latest and most modern devices of this measurement technique.

Technical features

Raman - Microscope

  • equipped with two lasers (532 nm and 633 nm)
  • two gratings (600 l/mm and 1800 l/mm)
  • high spectral and spatial resolution

AFM

  • 15 different SPM measuring modes
  • scanning range 200 μm x 200 μm x 20 μm
  • noise level:
    • 0.1 nm RMS in XY dimension
    • < 0.1 nm RMS in Z direction
 

The operation “Matériaux S3-phase1” is co-funded by the French Ministry of Higher Education, Research and Innovation, the association of greater Mulhouse (Mulhouse Alsace agglomeration), the departmental Council Haut-Rhin, the region Grand Est, and the European Union under the operational program FEDER Alsace 2014-2020.

In the context of the program “Matériaux s3 – Phase 1”, the French-German Research Institute (ISL) purchased a NanoRaman IR-microscope with the support of the departmental Council of Haut-Rhin, the Ministry of Higher Education, Research and Innovation and the European Union under the operational program FEDER Alsace 2014-2020.

 

Structural Characterisation

Bruker D8 Advance diffractometer

X-Ray Diffraction is a method to identify the nature of crystalline and semi crystalline structures.

An X ray beam is emitted by a X ray source to interact with the sample surface. The X ray emission is diffracted in a characteristic way and captured by a detector which transforms the signal into a diffraction pattern (function which represents the intensity of the reflexion depending on the diffraction angle).

Technical features

  • Geometry θ-θ Bragg-Brentano
  • Copper source
  • Sample holder, 7 sample positions for powders and bulk material
  • Linear detector high speed high resolution Lynxeye

Option : High temperature chamber MRI wide range : -195 °C to 1600 °C

diffractomètre