MSE-303L_Lab-III________________________________________________________________________________

Demonstration of Scanning Electron Microscope

(SEM)

EXPERIMENT # 3

SUBMITTED BY

Arooj Fatima 393776

Usman Yaqoob 378256
Hamza Hassan 366272

Materials:
Sample to be analyzed

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Equipment:
Scanning Electron Microscope

Standard/Software:
Image J

Procedure :
1. Sample Preparation:

 Begin by preparing your sample. The sample should be small

enough to fit into the SEM chamber and must be electrically
conductive or coated with a conductive layer if it's an insulator.

 If your sample is biological, it may require fixation, dehydration,

and coating with a conductive material like gold or platinum.

2. Instrument Startup:

 Turn on the SEM and let it warm up to operating conditions. This

can take some time depending on the instrument.

3. Sample Loading:

 Carefully load your prepared sample into the SEM chamber. Make
sure it's securely positioned and at the right working distance from
the electron source.

4. Vacuum Pumping:

 SEM operates in a high vacuum to avoid electron scattering. Allow

the instrument to reach the desired vacuum level.

5. Electron Gun Setup:

 Configure the electron gun settings, including beam energy and

current. These settings may vary depending on your sample and the
type of information you want to obtain.

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6. Beam Alignment:

 Align the electron beam to the center of the sample. This ensures
that you're scanning the area of interest.

7. Image Acquisition:

 Choose the imaging mode you want to use. The two primary
modes are secondary electron imaging (SEI) and backscattered
electron imaging (BEI).

 Select appropriate imaging parameters such as dwell time, scan

speed, and image resolution.

 Start the scanning process. The electron beam scans the sample
surface, and signals from secondary electrons or backscattered
electrons are collected and converted into an image.

8. Image Analysis:

 After acquiring the images, you can perform image analysis using
specialized software. You can measure dimensions, analyze
particle distributions, and more.

9. Other Imaging Modes:

 SEMs often have additional capabilities, such as energy-dispersive

X-ray spectroscopy (EDS) or electron backscatter diffraction
(EBSD), which can provide information about elemental
composition and crystallography. If needed, configure and perform
these analyses.

10.Data Interpretation:

 Interpret the images and data obtained from the SEM to draw
conclusions about the sample's structure, composition, or other
properties.

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11.Sample Removal:

 Carefully remove your sample from the SEM chamber, ensuring

it's not contaminated or damaged.

12.Shutdown:

 Turn off the SEM and pump down the chamber to prevent
contamination.

13.Data Storage and Reporting:

 Store your data appropriately and document your findings. This

information can be used for research, quality control, or other
purposes.

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Q1. What is the main difference between an optical and scanning electron
microscope?

Ans. The main difference between an optical microscope and a scanning

electron microscope (SEM) is the beam applied to the sample . An optical
microscope uses a beam of light, ranging from 400nm to 650nm in wavelength,
allowing the observer to analyze the effect of light as it is applied to a specimen.
Optical microscopy is an ideal method for general inspection purposes,
illuminating and producing a magnified image of a specimen.

On the other hand, SEMs scan a focused beam of electrons across the surface of
a sample, where electromagnets are used to focus the negatively charged
electrons. The interaction of the electron beam with the surface of the sample
affects the images received. The electrons coming out of the sample are used to
create a detailed image and reveal information including the texture
(morphology), chemical composition, crystalline structure, and material
orientation.

Q2. How SEM can be useful in materials science and engineering?

Ans. SEM can determine the microstructure, morphology, and elemental

composition of electrically conductive samples 1. SEMs can have a resolution
as low as 1 nm (over 100,000x magnification). The Scanning Electron
Microscope (SEM) is one of the most versatile characterization techniques for
materials. It allows scientists to observe materials at length scales that are too
small for visible light 1. The SEM can be used to study the surface morphology
of materials, including the topography and texture of surfaces, as well as the
size and shape of particles. It can also be used to determine elemental
composition of electrically conductive materials.

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Q3. What kind of electron emission occurs by interaction of electron beam
with the specimen surface?

Ans. When a focused electron beam interacts with a specimen surface, a large
number of interactions occur, and among the signals produced are secondary
electrons, backscattered electrons, characteristic and continuum x-rays, Auger
electrons, and photons of various energies . The most widely used signal
produced by the interaction of the primary electron beam with the specimen is
the secondary electron emission signal. When the primary beam strikes the
sample, loosely bound electrons may be emitted and these are referred to as
Secondary Electrons (SE).

Q4. Why does the SEM work under vacuum and what is the working
pressure?

Ans. The Scanning Electron Microscope (SEM) works under vacuum to prevent
the electrons from colliding with gas molecules and losing energy before they
reach the sample 1. If the column were full of air, the electrons would collide
with the gas molecules and never reach the sample. If gas molecules react with
the sample, different compounds could form and condense on the sample, which
can lower the quality of the image 1. The vacuum environment is also necessary
in part of the sample preparation.

The working pressure of an SEM depends on the type of SEM and its
application. The pressure range for SEMs can vary from 10^-7 to 10^-9 torr.

Q5. What are the factors effecting the secondary electron emission?

Ans. Several factors can affect secondary electron emission in an SEM:

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Primary Electron Energy: The energy of the primary electron beam plays a
significant role in SEE. Higher-energy primary electrons can cause more
secondary electron emission events. However, excessive beam energy can also
lead to surface damage or charging effects.

Operating Conditions: SEM operating conditions, such as vacuum level and

accelerating voltage, can affect SEE. Operating at higher vacuum levels (closer
to high vacuum) is generally preferred for maximizing SEE efficiency.

Conclusions:

Scanning Electron Microscopy (SEM) is a powerful tool for materials science

and engineering that can be used to determine microstructure, morphology, and
elemental composition of electrically conductive samples. It is also versatile in
its ability to study surface morphology and chemical composition using EDS.
When a focused electron beam interacts with a specimen surface, a large
number of interactions occur, and among the signals produced are secondary
electrons, backscattered electrons, characteristic and continuum x-rays, Auger
electrons, and photons of various energies. The most widely used signal
produced by the interaction of the primary electron beam with the specimen is
the secondary electron emission signal. When the primary beam strikes the
sample, loosely bound electrons may be emitted and these are referred to as
Secondary Electrons (SE). The secondary electron emission in SEM is
influenced by several factors such as the material matter which is prone to
secondary emission, the momentum possessed by the bombarding beam strikes
the surface, and the number of primary electrons that bombard the surface.