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❖ Explain Scanning electron microscopy (SEM) in detail.

➢ The SEM was developed by Dr. Charles Oatlev and others in 1950s, which is one of the three types
of electron microscopes (EM).
➢ Every electron microscope works by accelerating a focused stream of electrons in a vacuum towards
a sample. Interactions between the electron beam and the sample create an image, similar to how
optical microscopes use light to capture images. The image created reveals details of a sample’s
surface or internal composition, depending on the type of electron microscope that is used.
➢ A scanning electron microscope (SEM) is a type of electron microscope that produces images of a
sample by scanning the surface with a focused beam of electrons.
➢ The electrons interact with atoms in the sample, producing various signals that contain information
about the surface topography and composition of the sample. The electron beam is scanned in a
raster scan pattern (A raster scan, or raster scanning, is the rectangular pattern of image capture and
reconstruction in television.), and the position of the beam is combined with the intensity of the
detected signal to produce an image.
➢ In the most common SEM mode, secondary electrons emitted by atoms excited by the electron beam
are detected using a secondary electron detector. Some SEMs can achieve resolutions better than 1
nanometer.
➢ Principle:
➢ In SEM, the specimen (sample) is exposed to a narrow electron beam, which rapidly moves over or
scans the surface of the specimen. This causes the releasee of a shower of secondary electrons,
backscattered electrons (BSE), diffracted backscattered electrons and other types of radiations from
sample surface.
➢ The intensity of these secondary electrons depends upon the shape and the chemical composition of
the irradiated object (sample). These electrons are collected by a detector, which generates electronic
signals. These signals are scanned in the manner of a television system (raster scan) to produce an
image on a cathode ray tube (CRT).
➢ Instrumentation:
➢ SEM consists of following components,
1. Electron gun: It generates a beam of energetic electrons. The most common from of an
electron gun is a thermionic emitter.
2. Electromagnetic and Electrostatic lenses: The electron beam generated by electron gun is
focused to a very small sized using electromagnetic and/or Electrostatic lenses.
3. Scan coils: The next part of the SEM consists of the scan coils. In SEM, the scanned image is
formed point by point and the scan is achieved by the scan coils. There are two pairs of coils,
one each for the X and Y axes.
4. Vacuum chamber: To avoid the oxidation of electron generator and contamination, vacuum
chamber is there. Usually vacuum about 10-5 torr or better is necessary for a normal operation
in SEM.
5. Sample chamber: Sample is placed in this chamber in form of solid coated with metal film.
6. Detectors (one or more): There are two kinds of electrons, with high energies and the
secondary electrons which have energies of a few eV. These electrons are collected on
backscattered detector and secondary electron detector (SED).
➢ SEM produces black and white, three-dimensional images. In the most common or standard detection
mode, secondary electron imaging or SEI, the secondary electrons are emitted from very close to the

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sample surface. Due to that SEM can produces very high-resolution image of a sample surface,
revealing details less than 1 nm in size. Back-scattered electrons (BSE) are beam electrons emerge from
deeper locations within the specimen and consequently the resolution of BSE images is generally poorer
than secondary electron (SE) images.

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❖ Enlist advantages and disadvantages of SEM along with applications.

⚫ Advantages of Scanning electron microscope includes,
➢ Wide-array of application increases selectivity
➢ Detailed three-dimensional and topographical imaging with high resolution up to 1 nm
➢ Easy to operate with training
➢ Works fast as compared to conventional EM
➢ Most SEM samples requires minimal preparation actions
⚫ Disadvantages of Scanning electron microscope includes,
➢ Expensive and Larger in size creating limitation of capital cost and area requirement
➢ Special training required before operation to minimize chances of sample contamination
➢ Limited to solids, inorganic materials which are small enough to fit inside the vacuum
chamber
➢ Carries a small risk of radiation exposure associated with the electrons that scatter from
beneath the sample surface.
⚫ Applications:
➢ SEM responsible for some of the most detailed Nano and microscopic images ever produced.
➢ SEM is a robust analytical tool that has a wide scope of practical applications in the
analytical, commercial, and industrial spaces. It is widely utilized for quality control (QC)
and good-bad testing of pharmaceutical products, and it has proven useful for detecting and
identifying unknown contaminants in manufactured goods.
➢ SEM applications specific for Nanotechnology:
1. Surface structure morphology of polymer nano composites, fracture surfaces, nano fibers, nano coating
can be done effectively using SEM characterization.
2. SEM can also be employed for viewing the dispersion of nanoparticles such as carbon nanotubes,
nanoclay, and hybrid nanofillers in bulk and on nano composite fibers.
3. Heavy metal traces can be determined by EDX technique which requires SEM as an integral part of
technique.
4. Nanowires for gas sensing
➢ Examination of paint particles and fibers
➢ Investigation of gemstones and jewellery
➢ Semiconductor inspections
➢ Archaeological surveys
➢ Biological sciences
➢ Solid and rock sampling
➢ Forensic investigations

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❖ Explain Transmission electron microscopy (TEM) in detail.

➢ The first TEM was demonstrated by Max Knoll and Ernst Ruska in 1931, with this group developing
the first TEM with resolution greater than that of light in 1933 and the first commercial TEM in 1939.
In 1986, Ruska was awarded the Nobel Prize in physics for the development of transmission electron
microscopy.
➢ Principle:
➢ The working principle of the Transmission Electron Microscope (TEM) is similar to the light
microscope. The major difference is that light microscopes use light rays to focus and produce an image
while the TEM uses a beam of high energy electrons to transmit through the sample to produce an
image. Here, only certain part of the beam can pass through sample. Thus, transmitted beam replicates
the structural patterns of the sample. These transmitted electrons are used to create an image of the
sample.
➢ The specimen (sample) is most often an ultra-thin section less than 100 nm thick or a suspension in grid.
An image is formed from the interaction of the electrons with the sample as the beam is transmitted
through the specimen. The image is then magnified and focused onto an imaging device, such as a
fluorescent screen, a layer of photographic film, or a sensor.
➢ Transmission electron microscopy is a major analytical method in the physical, chemical and biological
sciences. TEMs find application in cancer research, virology, and materials science as well as pollution,
nanotechnology and semiconductor research, but also in other fields such as paleontology.
➢ Instrumentation:
➢ An electron source/Thermionic gun: To produce high energy electrons
➢ Electromagnetic lenses: Some additional lenses are used to improve the image quality and resolution of
the image.
➢ Vacuum chamber: Ensures prevention of contamination
➢ 2 Condenser lenses: To control the penetration of electrons
➢ Fluorescent screen: Used as imaging device on which transmitted electrons will focus and give higher
resolution of image.
➢ Working Mechanism of TEM:
➢ A heated tungsten filament in the electron gun produces electrons that get focus on the specimen by the
condenser lenses.
➢ Magnetic lenses are used to focus the beam of electrons of the specimen. By the assistance offered by
the column tube of the condenser lens into the vacuum creating a clear image, the vacuum allows
electrons to produce a clear image without collision with any air molecules which may deflect them.
➢ On reaching the specimen, the specimen scatters the electrons focusing them on the magnetic lenses
forming a large clear image, and if it passes through a fluorescent screen it forms a polychromatic
image.
➢ The denser the specimen, the more the electrons are scattered forming a darker image because fewer
electron reaches the screen for visualization while thinner, more transparent specimens appear brighter.

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❖ Enlist advantages and disadvantages of SEM along with applications.

⚫ Advantages of Transmission electron microscope includes,
➢ TEMs offer the most powerful magnification as compared to conventional optical microscope
(very powerful magnification of about 2 million times that of the optical microscope)
➢ TEMs have a wide range of applications and can be utilized in a variety of different
scientific, educational and industrial field
➢ Images are high quality and detailed
➢ TEM can be used to acquire vast information on compounds and their structures.
➢ TEMs are able to yield information of surface features, shape, size and structure along with
its composition
➢ TEM can produce permanent images.
➢ Easy to operate with proper training
⚫ Disadvantages of Transmission electron microscope includes,
➢ Expensive and Larger in size creating limitation of capital cost and area requirement
➢ Special training required before operation to minimize chances of sample contamination
➢ Samples are limited to those that are electron transparent, able to tolerate the vacuum camber
and small enough to fit in the chamber
➢ TEM requires special housing and maintenance, they are extremely sensitive to vibrations
and electro-magnetic movements hence they are used in isolated areas, where they are not
exposed.
➢ Carries a small risk of radiation exposure
⚫ Applications:
➢ To visualize and study cell structures of bacteria, viruses, and fungi etc.
➢ To view the shapes and sizes of microbial cell
➢ To study and differentiate between plant and animal cells.
➢ Its also used in nanotechnology to study nanoparticles such as ZnO nanoparticles
➢ It is used to detect and identify fractures, damaged micro-particles which further enable repair
mechanisms of the particles.
➢ To obtained detailed crystalline structure of sample
➢ To measure mechanical and electrical properties of individual nanowires and nanotubes,
TEM can help to understand relationship between structure and properties

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❖ Enlist difference between TEM and SEM characterization methods.

SEM TEM

➢ Used to produce excellent images of the surfaces ➢ Used to study the ultra-structure of the cell and
of cells and small crystalline structures. its components. It can see objects small as a
Excellent for studying surface morphology of molecular level or even at Nano level. Provides
the Nano-materials or suitable material. detailed information regarding suitable materials
as compared to SEM.

➢ Electron beam scans over the surface of the ➢ Electron beam pass through the sample
sample causing scattering of electrons. (transmitted through thin-film sample)

➢ Based on scattered electrons or produces images ➢ Based on transmitted electrons or produces

by detecting secondary electrons which are images by detecting primary electrons
emitted from the surface due to excitation by the transmitted from the sample.
primary electron beam.

➢ Comparatively low resolution than TEM; ➢ High resolution; Resolution- 10 nm (Average),

Resolution 2 nm (Average), 0.2 nm (Special) 0.5 nm (Special)

➢ Depth of field: High ➢ Depth of field: Moderate

➢ Specimen contrast: By electron scattering ➢ Specimen contrast: By electron transmission

➢ Produces 3-D black and white images ➢ Produces 2-D black and white images

➢ Magnifying power: 100000 X ➢ Magnifying power: 500000 X

➢ Preparation technique: Easy ➢ Preparation technique: Skilled person required

➢ Preparation thickness: Variable ➢ Preparation thickness: Very thin

➢ Specimen mounting: Aluminum stubs ➢ Specimen mounting: Thin films on copper grids

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❖ Explain X-ray diffraction (XRD) in detail.

➢ This method is used to get the knowledge of arrangements of atoms, particle shape and morphology of
nanomaterials.
➢ Principle:
➢ X-ray diffraction is based on constructive interference of monochromatic x-rays and a crystalline
sample. Monochromatic X-rays are directed toward the sample.
➢ The interaction of the incident rays with the sample produces constructive interference (and a diffracted
ray) when conditions satisfy bragg’s law. This law relates the wavelength of electromagnetic radiation
to the diffraction angle and the lattice spacing in a crystalline sample. Diffracted X-rays are then
detected, processed and counted.
➢ Instrumentation:
➢ X-ray diffractometer consists of three basic elements:
1. X-ray source tube (Cathode ray tube)
2. Sample holder
3. X-ray detector
➢ X-rays are generated in a cathode ray tube by heating a filament to produce electrons, accelerating the
electrons toward a target by applying a voltage, and bombarding the target material with electrons.
When electrons have sufficient energy to dislodge inner shell electrons of the target material,
characteristic X-ray spectra are produced.
➢ The resolution of an X-ray diffraction detector is also determined by the bragg’s equation.
𝟏 𝜶
d= ( )
𝟐 𝒔𝒊𝒏 𝜽
➢ Where, d is the resolution detector, α is the incident X-ray wavelength and θ is the angle of diffraction.

⚫ Advantages of XRD:
➢ Powerful and Rapid technique≤ 20 min.
➢ Non-destructive method and minimum quantity of sample required
➢ XRD units are extensively available
➢ Data interpretation is relatively easier

⚫ Disadvantages of XRD:
➢ Homogeneous and single-phase material is best for identification of an unknown contents
➢ Peak overlay may occur and worsen for high angle ‘reflections’

⚫ Applications of XRD:
➢ As a primary characterization tool for obtaining critical features such as crystal structures, crystalline
size, and strain, x-ray diffraction patterns have been widely used in nanoparticle research. The randomly
oriented crystals in nanocrystalline materials cause broadening of x-ray diffraction peaks.

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❖ Explain Atomic force microscopy (AFM) in detail.

➢ The atomic force microscope (AFM) is a type of scanning probe microscope whose primary roles
include measuring properties such as magnetism, height, friction.
➢ The resolution is measured in a nanometer, which is much more accurate and effective than the optical
diffraction limit. It uses a probe for measuring and collection of data involves touching the surface that
has the probe. An image is formed when the scanning probe microscope raster-scans the probe over a
section of the sample, measuring its local properties concurrently.
➢ They also have piezoelectric elements, which are electric charges that accumulate in selected solid
materials to enable tiny accurate and precise movement during scanning upon an electric command.
➢ Working principle of the AFM:
➢ The Atomic Force Microscope works on the principle measuring intermolecular forces and sees atoms
by using probed surfaces of the specimen in nanoscale. Its functioning is enabled by three of its major
working principles that include Surface sensing, Detection, and Imaging.
1. The Atomic Force Microscope (AFM) performs surface sensing by using a cantilever. The cantilever
has a sharp tip which scans over the sample surface, by forming an attractive force between the surface
and the tip when it draws closer to the sample surface. When it draws very close making contact with
the surface of the sample, a repulsive force gradually takes control making the cantilever avert from the
surface.
2. During the deflection of the cantilever away from the sample surface, there is a change in direction of
reflection of the beam and a laser beam detects the aversion, by reflecting off a beam from the flat
surface of the cantilever. , it tracks these changes of deflection and change in direction of the reflected
beam and records them.
3. The Atomic Force Microscope (AFM) takes the image of the surface topography of the sample by force
by scanning the cantilever over a section of interest. Depending on how raised or how low the surface of
the sample is, it determines the deflection of the beam, which is monitored by the Positive-sensitive
photo-diode (PSDP). The microscope has a feedback loop that controls the length of the cantilever tip
just above the sample surface, therefore, it will maintain the laser position thus generating an accurate
imaging map of the surface of the image.

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❖ Enlist advantages and disadvantages of AFM along with applications.

⚫ Advantages of Atomic force microscope includes,
➢ Easy to prepare samples for observation
➢ It can be used in vacuums, air, and liquids.
➢ Measurement of sample sizes is accurate
➢ It has a 3D imaging
➢ It can be used to study living and nonliving elements
➢ It can be used to quantify the roughness of surfaces
➢ It is used in dynamic environments.
⚫ Disadvantages of Atomic force microscope includes,
➢ It can only scan a single nanosized image at a time of about 150x150nm.
➢ They have a low scanning time which might cause thermal drift on the sample.
➢ The tip and the sample can be damaged during detection.
➢ It has a limited magnification and vertical range.
⚫ Applications of AFM:
➢ This type of microscopy has been used in various disciplines in natural science such as solid-
state physics, semiconductor studies, molecular engineering, polymer chemistry, surface
chemistry, molecular biology, cell biology, medicine, and physics.
➢ Some of these applications include:
➢ Identifying atoms from samples
➢ Evaluating force interactions between atoms
➢ Studying the physical changing properties of atoms
➢ Studying the structural and mechanical properties of protein complexes and assembly, such
as micro-tubules.
➢ used to differentiate cancer cells and normal cells.
➢ Evaluating and differentiating neighboring cells and their shape and cell wall rigidity.

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❖ Explain Fourier transform infrared spectroscopy in detail.

➢ IR spectroscopy is a useful tool for characterization of a compound based on the presence of functional
groups in the molecule. Such functional groups have characteristic absorption wavelengths in the IR
region and the presence of such groups is easily identified by such characteristic absorptions.
➢ FTIR Analysis measures the infrared region of the electromagnetic radiation spectrum, which has a
longer wavelength and a lower frequency than visible light, and is measurable in a sample when
submitted to infrared radiation (IR). The basic theory at work is that the bonds between different
elements absorb light at different frequencies.
• Working mechanism:
➢ FTIR analysis measures the range of wavelengths in the infrared region that are absorbed by a
material. This is accomplished through the application of infrared radiation (IR) to samples of a
material. The sample’s absorbance of the infrared light’s energy at various wavelengths is measured to
determine the material’s molecular composition and structure.
➢ Unknown materials are identified by searching the spectrum against a database of reference spectra.
Materials can be quantified using the FTIR materials characterization technique as long as a standard
curve of known concentrations of the component of interest can be created.
➢ FTIR Analysis can be used to identify unknown materials, additives within polymers, surface
contamination on a material, and more. The results of the tests can pinpoint a sample’s molecular
composition and structure.
➢ A simple device called an interferometer is used to identify samples by producing an optical signal
with all the IR frequencies encoded into it. The signal can be measured quickly.
➢ Then, the signal is decoded by applying a mathematical technique known as Fourier transformation.
This computer-generated process then produces a mapping of the spectral information. The resulting
graph is the spectrum which is then searched against reference libraries for identification.
➢ With the microscope attachment, samples as small as 20 microns can be analyzed. This allows quick
and cost-effective identification of unknown particles, residues, films or fibers. FTIR testing can also
measure levels of oxidation in some polymers or degrees of cure in other polymers as well as
quantifying contaminants or additives in materials.
• Testing process:
➢ Place sample in FTIR spectrometer. The spectrometer directs beams of IR at the sample and measures
how much of the beam and at which frequencies the sample absorbs the infrared light. The sample
needs to be thin enough for the infrared light to transmit through, or a thin slice of the material must be
removed. Reflectance techniques can be used on some samples and no damage is done to the sample.
➢ Infrared radiation is typically generated by passing electricity through a conducting ceramic bar (glow
bar). First the radiation reaches a “beam splitter”. The beam splitter is a partially coated mirror that
reflects half of the infrared radiation and passes the remaining half. The radiation follows either path 1
or path 2 to mirrors that return it to the beam splitter where the beams recombine and they are reflected
in to an sample infrared detector.
➢ The reference database houses thousands of spectra, so samples can be identified. The molecular
identities can be determined through this process.

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❖ Enlist advantages and disadvantages of FTIR along with applications.

⚫ Advantages of FTIR includes,
➢ FT-IR offers significant advantages in terms of speed and sensitivity which has resulted in
dispersive instruments becoming obsolete.
➢ High sample throughput – the biggest advantage is high sample throughput. In comparison
to the time taken by dispersive instruments the complete spectrum is scanned and displayed
in a matter of seconds.
➢ Improvement in sensitivity – multiple spectra can be collected and co-added in given time,
say 1 min.
➢ Low maintenance – the system consists of: one moving part only, that is, the moving mirror.
On the other hand, there are several moving parts in dispersive systems. This results in
greater system reliability and less of maintenance due to reduced wear and tear
➢ Majority of universal molecules are absorbing mid-infrared light, making it highly useful
tool.
➢ Constant resolution – resolution is uniform at all the wavelengths.
➢ Simpler mechanical design
➢ Powerful data stations
➢ Elimination of secondary light
⚫ Disadvantages of FTIR includes,
➢ It can only scan a single nanosized image at a time of about 150x150nm
➢ Inaccurate data may provide If not functionalized properly
➢ Skilled person needed
➢ Requires routine checkup with reference sample
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⚫ Applications of FTIR:
➢ Numerous components on automobiles are ideal for FTIR analysis: epoxies, oil coatings on
parts, fuel, rubber seals and O-rings, tires, paints, fabrics (flame retardants) and exhaust
emissions
➢ Quality verification of incoming/outgoing materials
➢ DE-formulation of polymers, rubbers, and other materials through thermogravimetric infra-
red (TGA-IR) or gas chromatography infra-red (GC-IR) analysis
➢ Microanalysis of small sections of materials to identify contaminants
➢ Analysis of thin films and coatings
➢ Monitoring of automotive or smokestack emissions
➢ Failure analysis
➢ FTIR is a valuable technique for monitoring air quality, testing water quality, and analyzing
soil to address environmental and health concerns caused by increasing pollution levels. The
technique offers a “green” method of testing and fast, accurate results with the added benefit
of saving money on the cost of consumables.

❖ Explain UV visible spectroscopy in detail.

➢ Ultraviolet-visible (UV-vis) spectroscopy is used to obtain the absorbance spectra of a compound in
solution or as a solid. What is actually being observed spectroscopically is the absorbance of light energy
or electromagnetic radiation, which excites electrons from the ground state to the first singlet excited
state of the compound or material.
➢ The UV-vis region of energy for the electromagnetic spectrum covers 1.5 - 6.2 eV which relates to a
wavelength range of 800 - 200 nm.
➢ Ultraviolet-visible (UV-Vis) spectroscopy is a widely used technique in many areas of science ranging
from bacterial culturing, drug identification and nucleic acid purity checks and quantitation, to quality
control in the beverage industry and chemical research.
➢ All of these instruments have a light source (usually a deuterium or tungsten lamp), a sample holder and
a detector, but some have a filter for selecting one wavelength at a time. The has a filter or a
monochromator between the source and the sample to analyze one wavelength at a time.
➢ The double beam instrument has a single source and a monochromator and then there is a splitter and a
series of mirrors to get the beam to a reference sample and the sample to be analyzed, this allows for
more accurate readings.
➢ the simultaneous instrument does not have a monochromator between the sample and the source;
instead, it has a diode array detector that allows the instrument to simultaneously detect the absorbance
at all wavelengths. The simultaneous instrument is usually much faster and more efficient, but all of
these types of spectrometers work well.
➢ UV-vis spectroscopic data can give qualitative and quantitative information of a given compound or
molecule. Irrespective of whether quantitative or qualitative information is required it is important to use
a reference cell to zero the instrument for the solvent the compound is in.
➢ For quantitative information on the compound, calibrating the instrument using known concentrations of
the compound in question in a solution with the same solvent as the unknown sample would be required.
If the information needed is just proof that a compound is in the sample being analyzed, a calibration

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curve will not be necessary; however, if a degradation study or reaction is being performed, and
concentration of the compound in solution is required, thus a calibration curve is needed.

Single beam instrument

Double beam instrument

Simultaneous instrument
instrument

➢ The advantage of an Ultraviolet - Visible Light Spectrophotometer (UV-Vis spectrophotometer) is its

quick analysis ability and easy to use. In astronomy research, an UV / Vis spectrophotometer helps the
scientists to analyze the galaxies, neutron stars, and other celestial objects. In other industries, UV / Vis
spectrophotometer also brought the high-tech spectral analysis possibilities.
➢ In the food industry, the quality and safety of foods are two most important factor for consumers. Thus,
in addition to the general sense of food quality factors, such as color, appearance, smell, taste, an UV /
Vis spectrophotometer can further assist the food supplier an instrumentation way of analysis by
chemistry, biology and by the high standards of quality control and production processes to improve the
shelf life of the foods as well as maintaining the safety.
➢ The stray light of UV-Vis spectrophotometer that caused by the faulty equipment design and other
factors could influence spectra measurement accuracy of the absorption in substance, because the stray
light will decrease linearity range and reduce the absorbency of substance it measures.

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❖ Explain dynamic light scattering in detail.

➢ Dynamic Light Scattering (DLS, also known as Photon Correlation Spectroscopy or Quasi-Elastic Light
Scattering) is one of the most popular light scattering techniques because it allows particle sizing down
to 1 nm diameter.
➢ Typical applications are emulsions, micelles, polymers, proteins, nanoparticles, or colloids. The basic
principle is simple: The sample is illuminated by a laser beam and the fluctuations of the scattered light
are detected at a known scattering angle θ by a fast photon detector.
➢ Simple DLS instruments that measure at a fixed angle can determine the mean particle size in a limited
size range. More elaborated multi-angle instruments can determine the full particle size distribution.
➢ From a microscopic point of view, the particles scatter the light and thereby imprint information about
their motion. Analysis of the fluctuation of the scattered light thus yields information about the particles.
Experimentally one characterizes intensity fluctuations by computing the intensity correlation function,
whose analysis provides the diffusion coefficient of the particles (also known as diffusion constant).
➢ The quality of a DLS measurement depends on several factors. Some obvious, such as the quality of the
components (the laser, the detector, the correlator...), other factors are not as straightforward but may
influence the measurement significantly.

➢ Advantages of DLS is wide time range, cheaper, and consists of simple experimental setup.
➢ Disadvantages of DLS is Time consuming, especially for slow dynamics, Only transparent sample,
Sensitive for mechanical, Disturbances, Lack of selectivity and relatively low signal strength.
➢ DLS is most commonly used to analyze nanoparticles. Examples include determining nanogold size,
protein size, latex size, and colloid size. In general, the technique is best used for submicron particles
and can be used to measure particle with sizes less than a nanometer.
➢ Dynamic light scattering can also be used as a probe of complex fluids such as concentrated solutions.
However, this application is much less common than particle sizing.

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❖ Explain Energy dispersive spectroscopy in detail.

➢ Energy-dispersive X-ray spectroscopy (EDS, EDX, or XEDS) is an analytical technique used for the
elemental analysis or chemical characterization of a sample. Energy Dispersive X-ray Spectroscopy
(EDX) is used to determine the composition of a sample such as thin films. Not only can relative
amounts of each atom be measured, but the distribution of the atoms in our samples can be mapped.
➢ It relies on the investigation of the 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 sets 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 (or unexcited) electrons in discrete energy
levels or electron shells bound to the nucleus. The incident 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) is also used in combination with SEM and enables the analysis of near-surface elements and
their amount at different positions providing a map of the sample. The X-rays are produced in a region
about 2 microns deep, making EDX not a true surface science technique.
➢ Electron beam is moved across the material and an image of the elements in the specimen can be
formed; however, due to low X-ray intensity, image generation usually takes a couple of hours.
➢ If the nanoparticles near or at the surface of a specimen are heavy metal ions, such as Au, Pd and Ag
nanoparticles, the composition and the amount can be estimated with EDX; however, elements with low
atomic numbers are difficult to detect. (below 11-Na)
➢ Advantages of EDX; low sensitive with molecules causing least change in composition, can analyze for
all materials at once, precision and accuracy are good with simple spectra, and surface sensitive.
(penetration up to 100 μm)
➢ Disadvantages are; surface sensitive (not used for bulky materials) and modest limit of detection
conventional techniques.
➢ Energy dispersive X-ray spectroscopy (EDS) in electron microscopy has been widely used in many
research areas since it provides precise information on the chemical composition of subcellular
structures that may be correlated with their high-resolution images.

Prepared by: Mr. Akash K. Dave Assistant Professor, LJIET

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 NANOSCIENCE AND TECHNOLOGY [3170509]
Chapter 4: Nanomaterials Characterization

Prepared by: Mr. Akash K. Dave Assistant Professor, LJIET

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