Energy-dispersive X-

ray spectroscopy
JAMUNA SETHI
ROLL-NO-25607
REGD-NO-0601105044
 Content
 INTRODUCTION
 PRINCIPLE OF OPERATION
 INSTRUMENT
 ADVANTAGE
 DISADVANTAGE
 GENERAL USE
 APPLICATION
 CONCLUSION
 Introduction
 Energy dispersive X-ray spectroscopy (EDS) is an analytical
technique used for the elemental analysis of a sample. As a type
of spectroscopy, it relies on the investigation of a sample through
interactions between electromagnetic radiation and matter,
analysing x-rays emitted by the matter in response to being hit
with charged particles. Its characterization capabilities are due in
large part to the fundamental principle that each element has a
unique atomic structure .
 Many laboratories have already shown interest in energy
dispersive x-ray spectroscopy. The reasons for this are:
 Different sample types (solid materials, liquids, powders, metals,
minerals, etc.) can be analyzed with simple sample preparation.
 Analysis over a wide range of concentrations (from traces to main
components) is possible without dilution.
 A wide range of elements can be analyzed simultaneously.
 PRINCIPLE OF OPERATION
 When the electron beam of the scanning electron microscopy is
scanned across the sample .
 It generate x-ray from the atoms in top two microns. The energy of x-
ray is characteristic of atom from which is escaped .
 The EDS system collect the x-ray ,sorts them by energy and displays
the number of x-ray verse their energy can be plotted or photograph
 The data can then further analysed to produced an area elemental
analysis (displayed as dot map) or as linear elemental analysis (display
as line scan) showing of the distribution particular element within top
two microns of the surface of sample .
 The EDS data can be compared to either known as standard material
or computer generated theoretical standard and produced either full
qualitative or semi quantitative
 DATA OUT PUT
 EDS dot maps and line scans may be smoothed
background corrected and ever load to show to
distribution of several element together .
 EDS system also produced color dot map which
show each elements distribution in different color .
 Qualitative EDS data is typical present as color
photograph or as full page spectral plane while
quantitative data is typical as table.
 SAMPLE CONSTRAINTS.

The sample can be up to 15cm* 15cm* 75cm size.

 INSTRUMENT with SEM
 There are four primary components of the EDS setup: the beam
source; the X-ray detector; the pulse processor; and the analyzer.
 EDS systems are most commonly found on
scanning electron microscopes (SEM-EDS)
 Scanning electron microscopes are equipped with a cathode and
magnetic lenses to create and focus a beam of electrons, and since the
1960s they have been equipped with elemental analysis capabilities.
 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 analyszer for data display and analysis
 WORKING of EDX
 The excess energy of the electron that migrates to an
inner shell to fill the newly- created hole can do
more than emit an X-ray.
 Often, instead of X-ray emission, the excess energy is
transferred to a third electron from a further outer
shell, prompting its ejection. This ejected species is
called an Auger electron,
 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-specific and allows chemical characterization
of a sample
 Emerging Technology
 There is a trend towards a newer EDS detector, called the
Silicon Drift Detector (SDD). The SDD consists of a high-
resistivity silicon chip where electrons are driven to a small
collecting anode. The advantage lies in the extremely low
capacitance of this anode, thereby utilizing shorter
processing times and allowing very high throughput.
Benefits of the SDD include 1) High count rates and
processing 2) Better resolution than traditional SiLi
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 and 5) Ability to be stored and operated at
relatively high temperatures, eliminating the need for liquid
nitrogen cooling
 DETECTOR
• The solid-state, lithium-drifted silicon
detector [Si (Li)] was developed and
applied to x-ray detection in the 1960s .
• The Si (Li) detector provides excellent
resolution. It can be considered as a
layered structure in which a lithium-
diffused active region separates a p-
type entry side from an n-type side.
• When an x-ray photon enters the active
region of the detector, photo ionization
occurs with an electron-hole pair
created for each 3.8 eV of photon
energy.
• Ideally, the detector should completely
collect the charge created by each
photon entry and result in a response
for only that energy.
PULSE PROCESSOR
 In EDS:
1. An electron is fired at an atom
2. The incident electron collides with the atom and an inner
electron is ejected
3. The atom wants to return to its equilibrium state and an
electron from a higher orbital level “falls” to the vacant
orbital level
4. This involves a change in energy E = E(Final Orbital )- E(Initial
Orbital ) .which is released in the form of a photon (hν = ΔE)
ΔE increases with Z (0.1 keV < ΔE < 10 keV)
5. The energy of the emitted x-ray is measured by an energy
dispersive spectrometer
 Energy Dispersive
Spectrometer
 First Semiconductor ED spectrometer: 1968, Si(Li)
 Once the x-ray is emitted from the atom its energy
must be precisely measured (~0.1 keV resolution)
 Semiconductor Energy Dispersive Spectrometers
permitted EDS to become practical
 Provides qualitative and quantitative data.
 Also performs Wavelength Dispersive Spectrometry
(WDS)
 (wavelength of x-rays instead of energy, more precise
 Detectors for
Energy Dispersion Spectrometers
 The detector consists of a semiconductor
diode.
 Generally a few mm thick
 A reverse bias is applied i.e. there is no
current flowing
 When the x-ray enters it creates charge
carriers
 These carriers flow through the circuit and
are collected
 Energy Dispersion
 X-ray enters and ejects a
K electron.
K e- scatters andcreates
e- - h pairs. An L e- falls to
the K orbital and either
emits a photon or an Auger e-
is released.
 Each process scatters and
creates
 e- - h pairs Ideal number of
electrons collected: n =
hν/3.8eV
 5 keV x-ray => 2 × 10-16 C.
 Qualitative Analysis
Spectrum measured by EDS

 The peaks have a width because the

energy dispersion is a statistical event, i.e.
not every photon produces the same
number of electron hole pairs and there is
thermal noise caused by the amplification
process
 FWHM α (C2E + N2)1/2
 C = uncertainty of carrierformation
 E = x-ray Energy
 N = Noise
 Peaks can overlap because of width.
Continue……
 Quantitative
Analysis
Quantitative analysis requires much more effort and care, but with
proper settings one can obtain an accuracy of ± 1 - 2% of the wt%.
Samples must be flat-polished (scratches < 0.1 μm) and conductive
or grounded to prevent charging. A qualitative analysis must be
performed as well to identify present elements.
Standards must be measured. Standards are materials of known
compositions and homogeneous at the microscopic level.
The electron beam energy must selected, usually 2 or 3 times the
measured x-ray energy.
This will influence the depth of probing Once the spectrum is
collected the background must be removed, usually performed by a
digital filtering algorithm
How EDS Different WDS

 WDS differs from EDS in that it uses the diffraction patterns

created by light-matter interaction as its raw data. WDS has a
much finer spectral resolution than EDS. WDS also avoids the
problems associated with artifacts in EDS. In WDS only one
element can be analyzed at a time, while EDS gathers a spectrum
of all elements, within limits, of a sample.
 WDX analysis over EDX analysis:
• much better energy resolution, preventing many peak overlap
errors frequently encountered in EDX analysis;
• lower background noise allowing a more accurate quantitative
analysis
 ADVANTAGE
 Applicable to various samples, including solids
 Relatively rapid and easy to learn
 Semi quantitative results can be obtained from many samples without use
of standards; most standards may be kept for long periods of time,
because most applications are for solids
 Instrumentation is relatively inexpensive

DISADVANTAGE
 Detection limits for bulk determinations are normally a few ppm to a few
tens of ppm, depending on the x-ray energy used and the sample matrix
composition.
 For thin-film samples, detection limits are approximately 100 ng/cm2
 Not suitable for elements of atomic number less than 11 unless special
equipment is available.
 General Uses
 Nondestructive multielemental analysis of thin
samples, sodium through uranium, to approximately
1ppm or 10-9 g/cm2
 Nondestructive multielemental analysis of thick
samples for medium and heavy elements
 Semiquantitative analysis of elements versus depth
 Elemental analyses of large and/or fragile objects
through external beam proton milliprobe
 Elemental analyses using proton microprobes,
spatial resolution to a few microns, and mass
detection limits below 10-16 g
 Applications
 Analysis of atmospheric aerosols by particle size for source transport,
removal, and effect studies
 Analysis of powdered plant materials and geological powders for broad
elemental content
 Analysis of air filters for a wide range of elements
 Analysis of elemental content of waters, solute, and particulate phases,
including suspended particles
 Analysis of materials for the semiconductor industry and for coating
technology
 Forensic studie
 Cement can be analyzed using EDS, after being dried and ground to a fine
particle size and prepared as pressed pellet specimens
 Energy-dispersive x-ray spectrometry, with its multielement capabilities, is
ideally suited for many analyses of petroleum products
 C0NCLUSION

• The development of compact ED

spectrometers has permitted EDS to
become practical and to be added to SEM
columns.
• High accuracy method to identify elemental
compositions
• Quick, versatile and non intrusive
 REFERENCE
 E. P. Bertin, Principles and Practice of X-Ray
Spectrometric Analysis
 R. Jenkins, R. W. Gould, and D. Gedcke, Quantitative
X-Ray Spectrometry Marcel Dekker
 R. Tertian and F. Claisse, Principles of Quantitative
X-Ray Fluorescence Analysis
 R. Woldseth, All You Ever Wanted to Know About
XES
 G. F. Knoll, Radiation Detection and Measurement
 ASM Metal Handbook, volume-10