Energy-dispersive X-ray spectroscopy

1 Equipment
Four primary components of the EDS setup are
1. the excitation source (electron beam or x-ray beam)
2. the X-ray detector
3. the pulse processor
4. the analyzer.
EDS spectrum of the mineral crust of the vent shrimp Rimicaris
exoculata[1] It shows peaks caused by X-rays given o as electrons return to the K electron shell and one peak resulting from
the L shell of iron.

Electron beam excitation is used in electron microscopes,

scanning electron microscopes (SEM) and scanning
transmission electron microscopes (STEM). X-ray beam
excitation is used in X-ray uorescence (XRF) spectrometers. A detector is used to convert X-ray energy into
voltage signals; this information is sent to a pulse processor, which measures the signals and passes them onto an
analyzer for data display and analysis. The most common
detector now is Si(Li) detector cooled to cryogenic temEnergy-dispersive X-ray spectroscopy (EDS, EDX, peratures with liquid nitrogen; however newer systems
or XEDS), sometimes called energy dispersive X-ray are often equipped with silicon drift detectors (SDD) with
analysis (EDXA) or energy dispersive X-ray micro- Peltier cooling systems.
analysis (EDXMA), is an analytical technique used for
the elemental analysis or chemical characterization of a
sample. It relies on an interaction of some source of X- 2 Technological variants
ray excitation and a sample. Its characterization capabilities are due in large part to the fundamental principle
M
that each element has a unique atomic structure allowing unique set of peaks on its X-ray emission spectrum.[2]
L
To stimulate the emission of characteristic X-rays from a
specimen, a high-energy beam of charged particles such
K
L
as electrons or protons (see PIXE), or a beam of X-rays,
is focused into the sample being studied. At rest, an atom
K
atomic nucleus
within the sample contains ground state (or unexcited)
K
electrons in discrete energy levels or electron shells bound kicked-out
electron
to the nucleus. The incident beam may excite an electron
in an inner shell, ejecting it from the shell while createxternal
ing an electron hole where the electron was. An electron
radiation
stimulation
energy
from an outer, higher-energy shell then lls the hole, and
the dierence in energy between the higher-energy shell
and the lower energy shell may be released in the form of
an X-ray. The number and energy of the X-rays emitted Principle of EDS
from a specimen can be measured by an energy-dispersive
spectrometer. As the energies of the X-rays are charac- The excess energy of the electron that migrates to an inner
teristic of the dierence in energy between the two shells shell to ll the newly created hole can do more than emit
and of the atomic structure of the emitting element, EDS an X-ray. Often, instead of X-ray emission, the excess
allows the elemental composition of the specimen to be energy is transferred to a third electron from a further
outer shell, prompting its ejection. This ejected species is
measured.[3]
1

5 SEE ALSO

called an Auger electron, and the method for its analysis

is known as Auger electron spectroscopy (AES).
X-ray photoelectron spectroscopy (XPS) is another close
relative of EDS, utilizing ejected electrons in a manner similar to that of AES. Information on the quantity
and kinetic energy of ejected electrons is used to determine the binding energy of these now-liberated electrons,
which is element-specic and allows chemical characterization of a sample.

5. Ability to be stored and operated at relatively high

temperatures, eliminating the need for liquid nitrogen cooling.
Because the capacitance of the SDD chip is independent
of the active area of the detector, much larger SDD chips
can be utilized (40 mm2 or more). This allows for even
higher count rate collection. Further benets of large area
chips include:

EDS is often contrasted with its spectroscopic counter1. Minimizing SEM beam current allowing for optipart, WDS (wavelength dispersive X-ray spectroscopy).
mization of imaging under analytical conditions,
WDS diers from EDS in that it uses the diraction of X2. Reduced sample damage and
rays on special crystals to separate its raw data into spectral components (wavelengths). WDS has a much ner
3. Smaller beam interaction and improved spatial resspectral resolution than EDS. WDS also avoids the probolution for high speed maps.
lems associated with artifacts in EDS (false peaks, noise
from the ampliers, and microphonics). In WDS, only
one element can be analyzed at a time, while EDS gath- Where the X-ray energies of interest are in excess of ~
ers a spectrum of all elements, within limits, of a sample. 30 keV, traditional silicon-based technologies suer from
poor quantum eciency due to a reduction in the detector stopping power. Detectors produced from high density semiconductors such as cadmium telluride (CdTe)
3 Accuracy of EDS
and cadmium zinc telluride (CdZnTe) have improved
eciency at higher X-ray energies and are capable of
Accuracy of EDS spectrum can be aected by various room temperature operation. Single element systems,
factors. Many elements will have overlapping peaks (e.g., and more recently pixelated imaging detectors such as
Ti K and V K, Mn K and Fe K). The accuracy of the the HEXITEC system, are capable of achieving energy
spectrum can also be aected by the nature of the sample. resolutions of the order of 1% at 100 keV.
X-rays can be generated by any atom in the sample that
is suciently excited by the incoming beam. These X- In recent years, a dierent type of EDS detector, based
rays are emitted in any direction, and so they may not all upon a superconducting microcalorimeter, has also beescape the sample. The likelihood of an X-ray escaping come commercially available. This new technology comthe specimen, and thus being available to detect and mea- bines the simultaneous detection capabilities of EDS
sure, depends on the energy of the X-ray and the amount with the high spectral resolution of WDS. The EDS
and density of material it has to pass through. This can microcalorimeter consists of two components: an abresult in reduced accuracy in inhomogeneous and rough sorber, and a superconducting transition-edge sensor
(TES) thermometer. The former absorbs X-rays emitted
samples.
from the sample and converts this energy into heat; the
latter measures the subsequent change in temperature due
to the inux of heat. The EDS microcalorimeter has his4 Emerging technology
torically suered from a number of drawbacks, including
low count rates and small detector areas. The count rate
There is a trend towards a newer EDS detector, called is hampered by its reliance on the time constant of the
the silicon drift detector (SDD). The SDD consists of a calorimeters electrical circuit. The detector area must be
high-resistivity silicon chip where electrons are driven to small in order to keep the heat capacity small and maxia small collecting anode. The advantage lies in the ex- mize thermal sensitivity (resolution). However, the count
tremely low capacitance of this anode, thereby utilizing rate and detector area have been improved by the impleshorter processing times and allowing very high through- mentation of arrays of hundreds of superconducting EDS
put. Benets of the SDD include:
microcalorimeters, and the importance of this technology
is growing.
1. High count rates and processing,
2. Better resolution than traditional Si(Li) detectors at
high count rates,
3. Lower dead time (time spent on processing X-ray
event),
4. Faster analytical capabilities and more precise X-ray
maps or particle data collected in seconds,

5 See also
Elemental mapping
Transmission electron microscopy
Wavelength dispersive X-ray spectroscopy

3
X-ray uorescence
X-ray microtomography
Scanning electron microscopy

References

[1] Corbari, L; et al. (2008). Iron oxide deposits associated with the ectosymbiotic bacteria in the hydrothermal
vent shrimp Rimicaris exoculata (PDF). Biogeosciences
5: 12951310. doi:10.5194/bg-5-1295-2008.
[2] Joseph Goldstein (2003). Scanning Electron Microscopy
and X-Ray Microanalysis. Springer. ISBN 978-0-30647292-3. Retrieved 26 May 2012.
[3] Joseph Goldstein (2003). Scanning Electron Microscopy
and X-Ray Microanalysis. Springer. ISBN 978-0-30647292-3. Retrieved 26 May 2012.

External links
MICROANALYST.NET Information portal with
X-ray microanalysis and EDX contents
-EDS on the SEM: Primer discussing principles, capabilities and limitations of EDS with the SEM

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