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Lecture 12

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10 views9 pages

Lecture 12

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hamaidhqais
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14/04/2024

Lecture 12

Electron Microscopy

Dr. Enshirah Da'na 1

Electron Microscopy
• Microscope forms an enlarged image of the original object in order
to convey its internal or external structure.

Two main types of electron microscopes:


Ø Transmission electron microscopes (TEM)

Ø Scanning electron microscopes (SEM)

Dr. Enshirah Da'na 2

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Transmission Electron Microscopes (TEM)


• The optics of the TEM is similar to conventional transmission light
microscope.
• It is capable of displaying magnified image of thin specimen
with magnificaCon in range of 103 to 106 .

Information that can be obtained using TEM include :


Ø Topography : surface features , texture
Ø Morphology : shape and size of the parCcles
Ø Crystallographic arrangement of atoms
Ø ComposiCon : elements and the their relaCve amounts
Dr. Enshirah Da'na 3

Working Principle and InstrumentaCon


• An electron gun at the top of the microscope emits electrons that
travel through vacuum in the microscope column.
• Vacuum is essential to prevent strong scattering of electrons by gases.
• ElectromagneCc condenser lenses focus the electrons into a very thin beam.
• Electron beam then travels through the specimen
and then through the electromagnetic objective
lenses.
• UnscaOered electrons hit the fluorescent
screen giving image of specimen with its
different parts displayed in varied darkness,
according to their density.
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Sample preparation

• To make the material electronically transparent, material thickness


is limited.
• Specimens have to be prepared with thickness of ~ 100 nm.
• For higher atomic weight material, the specimen has to be thinner.

Scanning electron microscope (SEM)


• SEM is most widely used type of electron microscope for
study of microscopic structure.
• Image is formed by focused electron beam that scans over the surface
area of specimen.
Dr. Enshirah Da'na 5

• Selected area electron diffraction


(SAED)
• SAED photos show polycentric
rings, which confirm the
polycrystallinity of the
prepared materials.

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• The incident beam in SEM is also called electron probe.


• The incident beam is of typically 10 nm diameter in contrast to beam
of TEM which is about 1 nm.
• In SEM, image is not formed by instantaneous illuminaCon of the
whole field as for TEM.
• SEM is relatively easy to operate and maintain, compared to a TEM.

• In TEM, unless specimen is made very thin, electrons are strongly


scaOered within the specimen or even adsorbed rather than
transmiOed. SEM overcomes this limitaCon.

Dr. Enshirah Da'na 7

Working principle and instrumentaCon

• Electron probe or beam is scanned across the specimen and the


procedure is known as Raster scanning.

• Raster scanning causes the beam to sequentially cover a rectangular


area on the specimen.

• The signal electrons emiOed from the specimen


are collected by the detector, amplified and used
to reconstruct the image.

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Sample preparaCon
• Sample preparation for SEM is minimal.

• This has made SEM more widely used than TEM which requires a very
thin specimen and tedious sample preparation procedure.

• Sample preparaCon for SEM involves only sizing the specimens to fit


SEM specimen holder and removing surface contaminants.

• This also helps to preserve the surface characteristics for topographic


study.

Dr. Enshirah Da'na 9

• SEM images of ZnO under


the effect of Zn precursor
concentration, 0.1 A (a),
0.2 A (b), 0.3 A (c), 0.4 A
(d) and 0.5 A (e).

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• SEM images of
ZnO under the
effect of pH, 7 B
(a), 9 B (b), 11 B
(c) and 13 B (d).

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• SEM images of ZnO under


the effect of temperature,
50 C (a), 150 C (b) and 250
C (c) and under the effect
of time, 1.5D (d) and 2.5D
(e).

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Energy dispersive spectrometer (EDS)

• In this method, the X-ray generated from interacCon of electron


beam with sample, is used for chemical analysis of the sample.

• As high energy electrons strike the sample surface, along with


secondary and backscattered electrons, characteristic X-rays are
emitted whose wave length depends on nature of atoms in sample.

• These X-rays can be used to characterize all type of solid materials.

• The characterisCcs X-ray is generated when an inner shell electron is


knocked out of the atom and the vacant site is filled with electron
from outer shell.
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• The excess energy is released and the amount of released


energy, corresponding to X-ray range, is characterisCcs of the
parCcular atom.
• The energy and wavelength of X-rays are different for each atomic
species and by measuring them, the elements present in sample
can be detected and quantified.

• From X- ray spectrum following analysis can be done:


Ø Measurement of wavelength/energy of each characteristics X-ray
emitted. It can be used to determine the elements present in sample.
This is a qualitative analysis.

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Ø Measurement of X-ray of any type emiOed per unit Cme. This


corresponds to amount of the element present in sample. This
is quanCtaCve analysis.

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Book References
P.J. Goodhew, J. Humphreys ,R. Beanland, Electron microscopy and
analysis , 3rd ed.,Taylor & Francis, 2001
Y. Leng, Materials Characterization: Introduction to microscopic and
spectroscopic methods, John Wiley & Sons, 2008

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