Electron beam microanalysis (ESMA)

  • Models SXFive FE Electron Probe MicroAnalyser and SX100 Electron Probe MicroAnalyser from CAMECA , each with energy dispersive (EDS) and wavelength dispersive X-ray spectroscopy (WDS)
  • including equipment for recording SE and BSE images
  • Highly spatially resolved geochemical analysis of element concentrations in solids
  • Results are usually given for each measuring point in wt.% of oxides

Contact person

  • Dietlind Nordhausen
  • Dr. Thomas Schirmer

configuration

CAMECA SXFive FE:

Excitation:30 kV, field emitter
Spectrometer:5 x vertical and Bruker-EDS (Peltier cooling)
Counters:5 x Ar/Me flow counters (WDS),
SDD semiconductor (EDS, Peltier cooling; resolution 136 eV)
Optics (WDS):LTAP, LPC1 (extended θ-range for OKa to TLAP);
LiF, TAP, PC0, PC1;
LLiF, LPET (large area crystals);
TAP, PET, PC2, PCX;
LLiF, LPET (large area crystals)
Element range:Be (PC3) - U (LIF)
Optical microscope:Incident light with polarizer and CCD camera;
Magnification variable 150 µm - 1700 µm
Instrument software:PeakSight (WDS, PC/Win7), Quantax (EDS)

Evaluation:

  • MinIdent (Prof. Dorian G.W. Smith & David Peirre Leibovitz; mineral identification)

applications

  • Qualitative and quantitative element analysis (minerals, rocks, technical products)
  • Applicable for thin sections and polished sections
  • Analysis depending on application and matrix topography/element mapping (minerals, rocks, technical products)
  • Extensive range of international reference materials for calibration of most applications in the field of geology and materials science

Energy dispersive X-ray spectroscopy (EDS)

  • EDS is used for the rapid qualitative identification of all minerals or components contained in the sample and the subsequent selection of measuring points for WDS
  • well suited for the determination and differentiation of accessory minerals (zircon, apatite, rutile, etc.)
  • only suitable for quantitative analyses to a limited extent, as the detection limit for most elements is 0.1% by weight at best
  • measurement inaccuracies and unresolvable line interferences possible
  • excited atoms emit X-rays with an energy specific to the respective element (characteristic radiation)
  • Detector measures the energy of each incoming X-ray photon

Wavelength dispersive X-ray spectroscopy (WDS)

  • WDS requires significantly longer measurement times, but provides much more accurate measurement results and has a detection limit of around 100 ppm.
  • Decomposition of X-rays into their spectral components by diffraction from natural or synthetic crystals
  • Characteristic X-rays of an element are analyzed
  • The different wavelength ranges are scanned one after the other for a complete spectrum

BSE images

  • Acquisition of high-resolution BSE images by detecting backscattered electrons on the sample surface
  • Material contrast images provide a grayscale image that can be used to identify individual minerals according to their different mean atomic numbers and to visualize the microstructures

Preparation of thin sections

  • Bal-Tec MED 020 (coating with C, Ag, Au etc.)
  • Vaporization of uncovered thin sections with a carbon layer a few nanometers thick to prevent negative charging of the sample
  • Electrons are conducted away from the sample surface during the analysis via a carbon strip that connects the thin section to the stainless steel sample carrier