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What is EDS?
Energy Dispersive X-Ray Spectroscopy (EDS or EDX) is a chemical microanalysis
technique used in conjunction with scanning electron microscopy (SEM). The EDS
technique detects x-rays emitted from the sample during bombardment by an electron
beam to characterize the elemental composition of the analyzed volume.
Working Principle of EDS?
When the sample is bombarded by the SEM's electron beam, electrons are ejected from
the atoms comprising the sample's surface. The resulting electron vacancies are filled
by electrons from a higher state, and an x-ray is emitted to balance the energy difference
between the two electrons' states. The x-ray energy is characteristic of the element from
which it was emitted.
The EDS x-ray detector measures the relative abundance of emitted x-rays versus their
energy. The detector is typically a lithium-drifted silicon, solid-state device. When an
incident x-ray strikes the detector, it creates a charge pulse that is proportional to the
energy of the x-ray. The charge pulse is converted to a voltage pulse (which remains
proportional to the x-ray energy) by a charge-sensitive preamplifier. The signal is then
sent to a multichannel analyzer where the pulses are sorted by voltage. The energy, as
determined from the voltage measurement, for each incident x-ray is sent to a computer
for display and further data evaluation. The spectrum of x-ray energy versus counts is
evaluated to determine the elemental composition of the sampled volume
Usage areas of EDS:
Failure analysis
Contamination identification
Unknowns identification
Stringer location and identification
User can quickly collect a full spectrum with the push of a button.
EDS is quicker in analyzing .
EDS system is inexpensive.
Disadvantages:
Low Resolution
On EDS the broad X-ray lines appear to be a single peak, which makes it
difficult to analyze individual X-ray lines.
The count rate is fewer as compared to WDS.
WDS
What is WDS?
A wavelength-dispersive spectrometer (WDS or EDS) uses the characteristic X-rays
generated by individual elements to enable quantitative analyses (down to trace element
levels) to be measured at spot sizes as small as a few micrometers. WDS can also be
used to create element X-ray compositional maps over a broader area by means of
rastering the beam. Together, these capabilities provide fundamental quantitative
compositional information for a wide variety of solid materials.
Working Principle of WDS?
The WDX operates in much the same way as EDX. Unlike the related technique of
Energy dispersive X-ray spectroscopy (EDX), WDX reads or counts only the x-rays of
a single wavelength, not producing a broad spectrum of wavelengths or energies.
Measurement of an element's abundance requires exciting an atom to produce X-rays,
focusing the X-rays through a crystal spectrometer to a detector, converting the X-rays
to photoelectrons, the crystal structure of sample diffracts the photons in principles of
Bragg's law. Which in turn generates an electrical signal whose magnitude is
proportional to the abundance of the element! This multi-step process involves many
potential breakdowns, but works reliably well to allow for routine analysis.
Usage areas of WDS:
Identification of spectrally overlapped elements
S in the presence of Pbor Mo
W or Ta in Si, or N in Ti
Advantages:
Higher Resolution
When compared to EDS, WDS exhibits superior peak resolution of elements
and sensitivity of trace elements
WDS system will have a count rate about 10x that of an EDS system
Disadvantages:
WDS
Spectral
resolution
Light
elements?
With windowless
window detector
Detection
Limits
~1000-5000 ppm
or thin With
synthetic
("crystals")
diffractors
<100-500 ppm
Specifications Cheaper, quicker but some More expensive, but with much
elements are too close better resolution giving lower
together to resolve (eg S Ka, detection limits.
Mo La, Pb Ma)
Overlapping
of Peaks
Yes
No
Advantages:
Disadvantages:
XPS
What s XPS?
X-Ray Photoelectron Spectroscopy (XPS), also known as Electron Spectroscopy for
Chemical Analysis (ESCA), is an analysis technique used to obtain chemical
information about the surfaces of solid materials. Both composition and the chemical
state of surface constituents can be determined by XPS. Insulators and conductors can
easily be analyzed in surface areas from a few microns to a few millimeters across.
Working Principle of XPS?
The sample is placed in an ultrahigh vacuum environment and exposed to a low-energy,
monochromatic x-ray source. The incident x-rays cause the ejection of core-level
electrons from sample atoms. The energy of a photoemitted core electron is a function
of its binding energy and is characteristic of the element from which it was emitted.
Energy analysis of the emitted photoelectrons is the primary data used for XPS. When
the core electron is ejected by the incident x-ray, an outer electron fills the core hole.
The energy of this transition is balanced by the emission of an Auger electron or a
characteristic x-ray. Analysis of Auger electrons can be used in XPS, in addition to
emitted photoelectrons.
The photoelectrons and Auger electrons emitted from the sample are detected by an
electron energy analyzer, and their energy is determined as a function of their velocity
entering the detector. By counting the number of photoelectrons and Auger electrons
as a function of their energy, a spectrum representing the surface composition is
obtained. The energy corresponding to each peak is characteristic of an element present
in the sampled volume. The area under a peak in the spectrum is a measure of the
relative amount of the element represented by that peak. The peak shape and precise
position indicates the chemical state for the element.
Applications:
Advantages:
Disadvantages:
References:
http://www.mee-inc.com/hamm/energy-dispersive-x-ray-spectroscopyeds/
http://www.mcswiggen.com/TechNotes/WDSvsEDS.htm
https://www.oxford-instruments.com/products/microanalysis/wavelength-dispersivesystems-wds
https://www.phi.com/surface-analysis-techniques/aes.html
http://www.mecheng.iisc.ernet.in/~bobji/mspc/assign/AES.htm
https://www.phi.com/surface-analysis-techniques/xps-esca.html
http://www.kratos.com/applications/techniques/x-ray-photoelectron-spectroscopy
http://chem.libretexts.org/Core/Physical_and_Theoretical_Chemistry/Spectroscopy/P
hotoelectron_Spectroscopy/Photoelectron_Spectroscopy%3A_Application