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Energy-Dispersive X-Ray Spectroscopy (EDS)

John Goodge, University of Minnesota-Duluth

Interaction of an electron beam with a sample target produces a variety of emissions, including x-rays. An energy-dispersive (EDS) detector is used to separate the characteristic x-rays of different elements into an energy spectrum, and EDS system software is used to analyze the energy spectrum in order to determine the abundance of specific elements. EDS can be used to find the chemical composition of materials down to a spot size of a few microns, and to create element composition maps over a much broader raster area. Together, these capabilities provide fundamental compositional information for a wide variety of materials.

How it Works - EDS

Photo of an EDS detector.

EDS systems are typically integrated into either an SEM or EPMA instrument. EDS systems include a sensitive x-ray detector, a liquid nitrogen dewar for cooling, and software to collect and analyze energy spectra. The detector is mounted in the sample chamber of the main instrument at the end of a long arm, which is itself cooled by liquid nitrogen. The most common detectors are made of Si(Li) crystals that operate at low voltages to improve sensitivity, but recent advances in detector technology make availabale so-called "silicon drift detectors" that operate at higher count rates without liquid nitrogen cooling.

An EDS detector contains a crystal that absorbs the energy of incoming x-rays by ionization, yielding free electrons in the crystal that become conductive and produce an electrical charge bias. The x-ray absorption thus converts the energy of individual x-rays into electrical voltages of proportional size; the electrical pulses correspond to the characteristic x-rays of the element.

Strengths

  • When used in "spot" mode, a user can acquire a full elemental spectrum in only a few seconds. Supporting software makes it possible to readily identify peaks, which makes EDS a great survey tool to quickly identify unknown phases prior to quantitative analysis.
  • EDS can be used in semi-quantitative mode to determine chemical composition by peak-height ratio relative to a standard.

Limitations

  • There are energy peak overlaps among different elements, particularly those corresponding to x-rays generated by emission from different energy-level shells (K, L and M) in different elements. For example, there are close overlaps of Mn-Kα and Cr-Kβ, or Ti-Kα and various L lines in Ba. Particularly at higher energies, individual peaks may correspond to several different elements; in this case, the user can apply deconvolution methods to try peak separation, or simply consider which elements make "most sense" given the known context of the sample.
  • Because the wavelength-dispersive (WDS) method is more precise and capable of detecting lower elemental abundances, EDS is less commonly used for actual chemical analysis although improvements in detector resolution make EDS a reliable and precise alternative.
  • EDS cannot detect the lightest elements, typically below the atomic number of Na for detectors equipped with a Be window. Polymer-based thin windows allow for detection of light elements, depending on the instrument and operating conditions.

Results

A typical EDS spectrum is portrayed as a plot of x-ray counts vs. energy (in keV). Energy peaks correspond to the various elements in the sample. Generally they are narrow and readily resolved, but many elements yield multiple peaks. For example, iron commonly shows strong Kα and Kβ peaks. Elements in low abundance will generate x-ray peaks that may not be resolvable from the background radiation.

X-ray energy spectrum of glass.
EDS spectrum of multi-element glass (NIST K309) containing O, Al, Si, Ca, Ba and Fe (Goldstein et al., 2003). Details
X-ray energy spectrum of biotite.
EDS spectrum of biotite, containing detectable Mg, Al, Si, K, Ti and Fe (from Goodge, 2003). Details

References

  • Severin, Kenneth P., 2004, Energy Dispersive Spectrometry of Common Rock Forming Minerals. Kluwer Academic Publishers, 225 p.--Highly recommended reference book of representative EDS spectra of the rock-forming minerals, as well as practical tips for spectral acquisition and interpretation.
  • Goldstein, J. (2003) Scanning electron microscopy and x-ray microanalysis. Kluwer Adacemic/Plenum Pulbishers, 689 p.
  • Reimer, L. (1998) Scanning electron microscopy : physics of image formation and microanalysis. Springer, 527 p.
  • Egerton, R. F. (2005) Physical principles of electron microscopy : an introduction to TEM, SEM, and AEM. Springer, 202.
  • Clarke, A. R. (2002) Microscopy techniques for materials science. CRC Press (electronic resource)

Related Links

  • Petroglyph--An atlas of images using electron microscope, backscattered electron images, element maps, energy dispersive x-ray spectra, and petrographic microscope-- Eric Chrisensen, Brigham Young University
  • SEM/EDX webpage from Indiana University - Purdue University Fort Wayne
  • Dmitry Dolivo-Dobrovolsky Webpage
    • MSearch: a program for searching minerals by their qualitative chemical composition and by the presence of specified text fragments in their names and formulae.  You can use this small freeware program for fast filtration of known minerals by qualitative chemical composition and/or by presence/absence of specified substrings in their names and/or formulae. For example, it can help you to select minerals that may correspond to problematic microprobe analyses. The present database version contains records for 4858 minerals and cover all known minerals (approved by IMA)

Teaching Activities

  • Argast, Anne and Tennis, Clarence F., III, 2004, A web resource for the study of alkali feldspars and perthitic textures using light microscopy, scanning electron microscopy and energy dispersive X-ray spectroscopy, Journal of Geoscience Education 52, no. 3, p. 213-217.