EDX (Energy Dispersive X-ray)

Group Members:
Abdul-Karim Mahaar
Saim Rafique
Talal Hassan Bajwa
Submitted to:
Sir Shaukat Hayat
SAP ID:
70147705
70146716
70152003
Subject: Applied Physics
Department Name:
Computer Science (1st semester)
UNIVERSITY OF LAHORE
Abstract:
Energy dispersive X-ray spectroscopy is a powerful elemental mapping tool
capable of analyzing the elemental composition of any substance. In this technique,
the characteristic X-ray signals emitted by the elements are detected. Through this,
it is also possible to perform quantitative analysis of the elements as well. Over the
years, this has been used commonly in conjunction with electron
microscopy techniques such as scanning electron microscopy (SEM)
and transmission electron microscopy (TEM). The sources used in these
microscopic techniques are also used for excitation of the sample so that they can
emit the characteristic X-rays. Over the years, SEM-EDX and TEM-EDX have
been used for myriad applications such as in the detection of metals, particle
contamination, and product failures. However, in forensic science, SEM-EDX has
found increased usage, especially when compared to TEM. In this field, samples
such as biological samples, explosives, glass, gunshot residue (GSR), paint, soil,
and toxins have been widely analyzed using these techniques. In this chapter, a
brief overview of the principle and theory of EDX and its instrumentation along
with its application in forensic science for the analysis of various evidence is
given.
Introduction:
The Energy Dispersive X-ray (EDX) microanalysis is involved in different
biomedical fields of study due to its high sensitivity in detecting the different
elements in tissues. In fact, EDX technique is made particularly useful in the study
of drugs delivery in which the EDX is an important tool to detect nanoparticles
(generally, used to improve the therapeutic performance of some chemotherapeutic
agents). EDX technique is also used in the study of environmental pollution. In
particular, EDX microanalysis can carry a huge vantage in the detection of heavy
metals pollutions as it has been demonstrated by Scimeca et al.1 In another study,
authors investigated whether the impact of heavy metals accumulation in bone
tissues could be related to the altered bone metabolism and architecture of
osteoporotic patients.2 Otherwise, EDX was used by Barba et al. to study how
infection associated to prosthesis could be linked to metallosis3 or in the case
report of Khan et al. where they show a metallosis following a shoulder hemi -
arthroplasty with a humeral component resurfacing shoulder replacement.4
Moreover, the EDX microanalysis on the pathological deposition of calcium has
been useful to characterize the differences in the elemental composition of breast
calcifications, in particular the composition of benign and malignant lesions5 or
the tight association of asbestos nano-fibers and lung cancer cells.6 In fact, EDX
microanalysis has greatly improved the characterization of the asbestos isotype and
shed new light in the study of the possible bioaccumulation of polluting agents in
different human organs and systems.
Basic Principal:
EDX spectroscopy is involved in the detection of elemental composition of
substances by using scanning electron microscope. EDX is able to detect elements
that possess the atomic number higher than boron and these elements can be
detected at concentration of least 0.1%. The application of EDX includes material
evaluation and identification, contamination identification, spot detection analysis
of regions up to 10 cm in diameter, quality control screening, and others.

Upon collision with the electron beam in typical SEM, the samples interact with
the beam and produce characteristic X-rays. Due to the principle that none of the
elements have the same X-ray emission spectrum, they can be differentiated and
measured for its concentration in the sample. The X-ray is the result of the primary
beam of electron interaction with the nucleus of the sample atom. Primary electron
beam will excite the electron in the nucleus of an atom, ejecting it from the nucleus
and creating an electron hole. An electron from the outer shell (higher energy) of
the atom will replace the missing ejected electron and release the superfluous X-
ray. The emitted X-ray consists of X-ray continuum (generated by the deceleration
of electron) and characteristic X-ray (generated as result of higher shell electron
filling the electron hole in the nucleus shell). as shown in Fig.
X-ray continuum is not paramount for the identification of elements in the sample
and needs to be identified to differentiate them. The intensity of the X-ray
continuum is contributed by factors such as probe current, accelerating voltage
supplied, and the atomic number of the sample. On the other hand, the
characteristic X-ray will be recorded by the energy dispersive spectrometer for the
measurement of the elemental composition in the specimen.
Method of Operation (Working):
Energy-dispersive X-ray spectroscopy (EDS, EDX, or XEDS) is an analytical
technique used for the elemental analysis or chemical characterization of a sample.
It relies on the investigation of an interaction of some source of X-ray excitation
and a sample. Its characterization capabilities are due in large part to the
fundamental principle that each element has a unique atomic structure allowing
unique set of peaks on its X-ray spectrum. To stimulate the emission of
characteristic X-rays from a specimen, a high-energy beam of charged particles
such as electrons or protons, or a beam of X-rays, is focused into the sample being
studied. At rest, an atom within the sample contains ground state (unexcited)
electrons in discrete energy levels or electron shells bound to the nucleus. The
incident electron beam may excite an electron in an inner shell, ejecting it from the
shell while creating an electron hole where the electron was. An electron from an
outer, higher-energy shell then fills the hole, and the difference 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 from a specimen can be
measured by an energy-dispersive spectrometer. As the energy of the X-rays is
characteristic of the difference in energy between the two shells, and of the atomic
structure of the element from which they were emitted, this allows the elemental
composition of the specimen to be measured.
EDX can be used for elemental analysis of the surface of the coupons while
obtaining SEM or ESEM images.
Overall Discussion:
Energy-dispersive X-ray analysis (EDX) is applied along with SEM to analyze the
types and the quantity of elements at the nanomaterial surface or in the vicinity of
surface to provide specimen map. Since X-rays are formed in 2-µm deep area,
EDX is not an accurate technique for surface characterization. During EDX
analysis, the electron beam is transported across the sample to form the image of
the elements in the samples. This process generally takes several hours. In the
EDX, the composition and the quantity of the heavy metal ions of the
nanoparticles, which are placed near or at the surface of a sample, can be
measured, while elements with atomic number below 11 are hard to be detected by
EDX. Recently, several X-ray characterization techniques, including small-angle
X-ray scattering, X-ray absorption fine structure (XAFS), X-ray diffraction, and X-
ray photoelectron spectroscopy (XPS) have been applied for characterizing
nanomaterials. The chemical composition of materials can be analyzed by X-ray
characterization techniques, such as X-ray absorption near-edge structure, XPS, X-
ray fluorescence spectroscopy, EDX and X-ray absorption fine structure.
Applications / Uses of Energy Dispersive X-ray (EDX):
Energy Dispersive X-ray (EDX) spectroscopy is a versatile analytical technique
with applications across various scientific disciplines. Integrated with electron
microscopes, EDX provides valuable insights into the elemental composition of
materials at the micro- and nanoscale. Here are some notable uses of EDX:
1. Materials Science:

Composition Analysis: EDX is widely used in materials science for qualitative

and quantitative analysis of metallic alloys, ceramics, polymers, and composite
materials.
Microstructure Characterization: Researchers utilize EDX to investigate the
microstructure of materials, studying the distribution of elements within a sample.
2. Geology and Earth Sciences:

Mineral Analysis: Geologists employ EDX for the analysis of minerals and rocks,
helping identify and quantify elements in geological samples.
Environmental Geochemistry: EDX is used in environmental science to study
soil and sediment samples, aiding in the identification of pollutants and
understanding geochemical processes.
3. Biology and Life Sciences:

Biological Sample Analysis: In life sciences, EDX is used to study biological

specimens, providing information on the elemental composition of tissues and
cells.
Biomineralization Studies: EDX aids in understanding biomineralization
processes in biological structures, such as bones and shells.
4. Chemistry and Nanotechnology:

Nanomaterial Characterization: EDX is crucial for characterizing nanomaterials,

nanoparticles, and nanocomposites, providing insights into their elemental makeup.
Chemical Analysis: Chemists use EDX to analyze the composition of organic and
inorganic compounds, contributing to the understanding of chemical structures.
5. Forensics:
Trace Element Analysis: In forensic science, EDX assists in trace element
analysis of evidence, aiding in crime scene investigations and providing valuable
information for forensic experts.
6. Archaeology and Cultural Heritage:

Art and Artifact Analysis: EDX is employed to analyze pigments, metals, and
other materials in artworks and archaeological artifacts, helping conservators and
researchers understand their composition and degradation.
7. Environmental Science:

Pollution Monitoring: EDX plays a role in environmental science by analyzing

samples from air, water, and soil, aiding in the identification and quantification of
pollutants.
Ecotoxicology Studies: Researchers use EDX to study the impact of pollutants on
organisms by analyzing the elemental composition of biological samples.
8. Semiconductor Industry:

Quality Control: In the semiconductor industry, EDX is used for quality control
and process monitoring to ensure the desired elemental composition in
semiconductor materials.
9. Metallurgy:

Metal Alloy Analysis: EDX is extensively used in metallurgy for the analysis of
metal alloys, ensuring the desired composition and properties of materials used in
various industries.
10. Educational and Research Purposes:

Teaching and Training: EDX is used as an educational tool for teaching and
training in various scientific disciplines.
Research Exploration: Researchers leverage EDX for exploratory studies,
investigating unknown materials and expanding our understanding of elemental
composition.
Advantages and Disadvantages:

*Advantages of Energy Dispersive X-ray (EDX):

The advantages of Energy Dispersive X-ray are:
Elemental Analysis: EDX provides detailed information about the elemental
composition of a sample. It can identify and quantify elements present in a
material, aiding in materials characterization.
High Spatial Resolution: When integrated with electron microscopes, EDX offers
excellent spatial resolution. This allows researchers to analyze specific regions or
individual particles within a sample.
Versatility: EDX is versatile and applicable to a wide range of materials, including
metals, minerals, polymers, biological specimens, and more.
Qualitative and Quantitative Analysis: EDX can perform both qualitative and
quantitative elemental analysis. It not only identifies elements but also provides
information about their relative concentrations.
Real-time Analysis: EDX allows for real-time analysis, providing immediate
feedback on the elemental composition of a sample.
Non-destructive: In many cases, EDX analysis is non-destructive, allowing for the
examination of samples without altering their integrity.
Sensitivity to Trace Elements: EDX is sensitive to trace elements, making it
valuable in detecting and analyzing elements present in small concentrations.
Ease of Use: Compared to other analytical techniques, EDX is relatively easy to
use, making it accessible for a wide range of researchers and technicians.

*Disadvantages of Energy Dispersive X-ray (EDX):

The dis-advantages of Energy Dispersive X-ray are:
Limited Light Element Detection: EDX has limitations in detecting light
elements (elements with low atomic numbers). This can make it challenging to
analyze materials composed primarily of lighter elements.
Sample Preparation: Achieving accurate and reliable results often requires
meticulous sample preparation. Inhomogeneous samples or those with surface
contamination may lead to misleading outcomes.
Resolution Limits: While EDX provides excellent spatial resolution, it may not
achieve the same level of resolution as other analytical techniques, such as
Wavelength Dispersive X-ray Spectroscopy (WDS).
Interference from Matrix Elements: The presence of matrix elements in a
sample can interfere with the detection of specific elements, affecting the accuracy
of the analysis.
Detection Limits: The sensitivity of EDX may be limited when analyzing samples
with very low concentrations of certain elements. Achieving lower detection limits
may require more sophisticated and expensive equipment.
Peak Overlaps: Overlapping X-ray peaks can occur, particularly when elements
have similar characteristic X-ray energies. This can complicate the analysis and
interpretation of results.
Complex Spectra: The interpretation of complex spectra can be challenging,
especially in samples with multiple elements or when dealing with overlapping
peaks.
Instrument Cost: While EDX can be more accessible than some other analytical
techniques, high-end instruments with advanced features can be expensive.

Conclusion and References:

Conclusion:
Energy Dispersive X-ray (EDX) spectroscopy is a powerful analytical technique
that provides crucial insights into the elemental composition of materials. Its
advantages, including high spatial resolution, versatility, and real-time analysis,
make it an invaluable tool in various scientific disciplines. The integration of EDX
with electron microscopes enhances its capabilities, allowing for detailed
investigations at the micro- and nanoscale. While EDX offers numerous benefits,
researchers must be mindful of its limitations, such as challenges in detecting light
elements and potential interference from matrix elements. Careful experimental
design and data interpretation are essential to harness the full potential of EDX.
Overall, EDX contributes significantly to materials science, geology, biology, and
other fields, enabling researchers to explore the intricacies of elemental distribution
and composition. As technology advances, EDX continues to evolve, ensuring its
continued relevance and impact in the ever-changing landscape of analytical
techniques.
References:
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