EDX (Energy Dispersive X-ray analysis)

Introduction:
EDX Analysis stands for Energy Dispersive X-ray analysis. It is sometimes referred to also as
EDS or EDAX analysis. It is a technique used for identifying the elemental composition of the
specimen, or an area of interest thereof. The EDX analysis system works as an integrated feature
of a scanning electron microscope (SEM).
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.

Principle:
During EDX Analysis, the specimen is bombarded with an electron beam inside the scanning
electron microscope. The bombarding electrons collide with the specimen atoms' own electrons,
knocking some of them off in the process. A position vacated by an ejected inner shell electron
is eventually occupied by a higher-energy electron from an outer shell. To be able to do so,
however, the transferring outer electron must give up some of its energy by emitting an X-ray.

The amount of energy released by the transferring electron depends on which shell it is
transferring from, as well as which shell it is transferring to. Furthermore, the atom of every
element releases X-rays with unique amounts of energy during the transferring process. Thus, by
measuring the amounts of energy present in the X-rays being released by a specimen during
electron beam bombardment, the identity of the atom from which the X-ray was emitted can be
established.

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EDX (Energy Dispersive X-ray analysis)

EDX spectrum :
The output of an EDX analysis is an EDX spectrum (see Figure 2 on Page 2). The EDX
spectrum is just a plot of how frequently an X-ray is received for each energy level. An EDX
spectrum normally displays peaks corresponding to theenergy levels for which the most X-rays
had been received. Each of these peaks are unique to an atom, and therefore corresponds to a
single element. The higher a peak in a spectrum, the more concentrated the element is in the
specimen.

An EDX spectrum plot not only identifies the element corresponding to each of its peaks, but
the type of X-ray to which it corresponds as well. For example, a peak corresponding to the
amount of energy possessed by X-rays emitted by an electron in the L-shell going down to the
K-shell is identified as a K-Alpha peak. The peak corresponding to X-rays emitted by M-shell
electrons going to the K-shell is identified as a K-Beta peak shown in the figure below.

Figure . Elements in an EDX spectrum are identified based on the energy content of the X-rays emitted
by their electrons as these electrons transfer from a higher-energy shell to a lower-energy one.

When performing EDX analysis, the following must be observed:

1) The probe current must be adjusted such that data collection is just between 10%-30% dead.
2) Spot Mode operation must be used for contaminants suspected to be concentrated in very
small regions.
3) The EHT level used during the analysis must be higher than the energy peaks corresponding
to the elements of interest.

Failure Mechanisms/Attributes Tested for by EDX Analysis:

Inorganic Contamination
Elemental Composition

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EDX (Energy Dispersive X-ray analysis)
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.

Figure . Example of an EDX Spectrum

Strengths Of EDX:

 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.

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EDX (Energy Dispersive X-ray analysis)

SEM/EDX analysis:
A Scanning electron microscope (SEM) can be utilized for high magnification imaging of almost
all materials. With SEM in combination of EDX it is also possible to find out that different parts
of the sample contains which elements.
This means the SEM/EDX instrument is a powerful and flexible tool for solving a wide range of
product and processing problems for a diverse range of metals and materials.
SEM/EDX analysis carried out in many industrial sectors including electronics and
semiconductors, pharmaceutical, petrochemicals, plastics and polymers, aerospace,
automotive, medical devices, engineering, chemicals, materials and metallurgy .

APPLICATIONS OF EDX:
Typical Applications include:-

 Identification of metals and materials

 Particle contamination identification and elimination
 Classification of materials
 Product and process failure and defect analysis
 Examination of surface morphology (including stereo imaging)
 Analysis and identification of surface and airborne contamination
 Powder morphology, particle size and analysis
 Cleaning problems and chemical etching
 Welding and joining technology quality evaluation and failure investigation
 Paint and coating failure and delamination investigation
 Identification and elimination of corrosion and oxidisation problems
 Contamination or stain investigation
 Structural analysis
 Reverse engineering of products and processes

The SEM/EDS is the ultimate tool for:

 Deposits and Wear Debris Analysis

 Particle Sizing and Characterization
 Failure Analysis
 Contaminant Analysis
 Metallurgical Studies

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EDX (Energy Dispersive X-ray analysis)
Range of Materials for Invesigation by SEM/EDX:-

 Metals, Glass and Ceramics

 Semiconductors
 Plastics and polymers
 Powders and Dust
 Composite Materials
 Fibres (Textile, fabric , man-made, natural, carbon fibres, glass fibres, kevlar)

Some Applications of EDX are explained below:

EDX ANALYTICAL CAPABILITIES:

Viewing three dimensional images of microscopic areas only solves half the problem in an
analysis. It is often necessary to identify the different elements associated with the a specimen.
This is accomplished by using the “built-in” spectrometer called an Energy Dispersive X-ray
Spectrometer. EDS is an analytical technique which utilizes x-rays that are emitted from the
specimen when bombarded by the electron beam to identify the elemental composition of the
specimen. To explain further, when the sample is bombarded by the electron beam of the SEM,
electrons are ejected from the atoms on the specimens surface.
A resulting electron vacancy is filled by an electron from a higher shell, and an x-ray is emitted
to balance the energy difference between the two electrons. The EDS x-ray detector measures the
number of emitted x-rays versus their energy. The energy of the x-ray is characteristic of the
element from which the x-ray was emitted. A spectrum of the energy versus relative counts of
the detected x-rays is obtained and evaluated for qualitative and quantitative determinations of
the elements present as shown in Image below

Figure 1 EDS spectrum of elements detected in sample . The order of abundance is Fe, Cr, and Ni suggest stainless
steel.

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EDX (Energy Dispersive X-ray analysis)

Analysis of Thin Films:

EDX analysis was carried out on a thin evaporated layer on top of a nickel / iron alloy.

The layer contained a mixture of barium, strontium and oxygen, with a small amount of
magnesium. The thickness of the layer was calculated to be ~ 38 nm.

Identification of the Type and Source of Particulate

Contamination in a Ceramic Component Using SEM / EDX:

Figure 2 Optical image of dark specks of contamination in sintered glass ceramic

A ceramic preform is used not only to hold together several metal components in a holder for
thermionic cathodes but also to provide an electrically insulating barrier. The ceramic is white,
and in-line optical inspection is used to look for the presence of contamination on the
preform.This inspection rejected holders for the presence of dark specks on the surface of the
glass that could lead to later insulation or poisoning problems for the cathode at the customer.
The preform is produced from a glass powder, which is pressed into shape and sintered.The
metal components are then assembled together with the preform and thermally processed to first
melt the glass around the metal and then re-crystallise it to form a rigid ceramic.The
contamination appeared to be within the surface, therefore some samples were fracture sectioned

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EDX (Energy Dispersive X-ray analysis)
to look for the presence of contamination inside the ceramic.Backscatter electron imaging was
used to look for particles of a different chemical composition to
that of the surrounding ceramic.

SEM and EDX Investigations:

The scanning electron microscope (SEM) was used to examine the contamination at a higher
magnification to determine whether the contamination was lying on the surface of the ceramic
(surface contamination), embedded in the surface (contamination from the pressing operation) or
within the surface (contamination in the glass powder).

Figure 3 Contamination on the holder ceramic

By taking samples of sintered preforms from earlier in the process, it was possible to confirm
that the contamination was present before the final assembly and thermal processing, implying
that it was most likely to be present in the original glass powder, either as a result of
contamination in the preform pressing process or from contamination in the incoming glass
powder.

Figure 4. Contamination inside the holder ceramic

The particle of contamination was analysed by EDX and compared to the composition of the
holder ceramic.

The particle contained a mixture of silicon, lead,potassium, aluminium, oxygen, sodium and
zinc,whereas the normal holder ceramic contained mainly zinc, silicon and oxygen.

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EDX (Energy Dispersive X-ray analysis)

Figure 5 EDX spectra of particle (red) and the

Characterisation of Smaller Drug Particles:

This application note details the laboratory’s capabilities to mimic optical microscopy methods
using SEM, and extend beyond the capability of optical techniques using manual or automated
image collection and analysis. The SEM can automatically perform analysis down to a particle
size of 2 .m, below this manual operation is required (ultimate resolution of SEM is 2 nm) with
the advantage of chemical characterisation using EDX. The field of view is determined by the
particle size range to be analysed.

Identification of glass flakes:

Another way to use SEM/EDX is to make quantitative chemical analysis of an unknown
material.We use that for example when we want to determine the origin of glass fragments,found
in different types of foodstuffs.

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EDX (Energy Dispersive X-ray analysis)
Application of Energy-Dispersive X-ray Fluorescence to
Trace Metal Analysis of Natural Waters:
Energy-dispersive X-ray fluorescence has much to offer in the field of trace metal monitoring of
ecological systems.Coupled with dithiocarbamate precipitation for conversion of water samples
to XRF targets, it is capable of rapid, multielement analysis at relatively low cost. It is also a
convenient technique for performing separate analyses on dissolved and particulate fractions. For
studies requiring analyses of only one or two metals, atomic absorption spectrophotometry or
colorimetric methods may be more appropriate.

References:
http://www.lpdlabservices.co.uk/analytical_techniques/sem/sem_instrument.php
http://www.lpdlabservices.co.uk/analytical_techniques/sem/index.php
http://www.siliconfareast.com/edxwdx2.htm
http://www.herguth.com/technical/sem.pdf
http://serc.carleton.edu/research_education/geochemsheets/eds.html
http://www.amazingrust.com/Experiments/background_knowledge/EDAX.html
http://www.edax.com/applications/xrf-index.cfm

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