SCANNING ELECTRON MICROSCOPY
Aim
To study the surface morphology and microstructural features of a given sample using Scanning
Electron Microscopy (SEM).
Introduction
The precise characterization of material morphology, especially particle size and distribution, is
paramount in material science, particularly in electronics where microstructure dictates
functional properties. Smaller and more uniform particles generally lead to improved material
performance, such as better packing density, enhanced surface area for reactions, or more
consistent electrical conductivity.
This practical aimed to quantitatively determine the particle size and morphological parameters
of a sample material using Scanning Electron Microscopy (SEM). SEM provides high-resolution
imaging by scanning the sample surface with a focused beam of electrons, which yields detailed
topographical information. The subsequent image analysis, facilitated by software (such as
ImageJ/Fiji, which typically generates the provided data), allows for the statistical quantification
of physical attributes from the two-dimensional projections of the particles. Specifically, this
report utilizes measurements such as the Feret diameter to characterize the particle size and a
histogram to visualize the distribution of these sizes, thereby providing critical insight into the
quality and uniformity of the prepared material.
Principle
Scanning Electron Microscopy (SEM) is an advanced imaging technique that uses a focused
beam of high-energy electrons to generate signals from the surface of a specimen. These signals
provide detailed information about the sample’s surface topography, composition, and
crystallographic structure.
When the electron beam interacts with the atoms of the sample, various signals such
as secondary electrons, backscattered electrons, and X-rays are emitted.
• Secondary electrons give information about surface morphology.
• Backscattered electrons provide contrast based on atomic number differences.
• Characteristic X-rays are used for elemental analysis through Energy Dispersive X-ray
Spectroscopy (EDS).
Procedure:
1. Sample Preparation
o The sample should be clean, dry, and small enough to fit inside the specimen chamber.
o Non-conductive samples are coated with a thin layer of gold, platinum, or carbon using a
sputter coater to prevent charging under the electron beam.
2. Mounting the Sample
o The prepared sample is mounted on a metallic stub using carbon tape or adhesive.
3. Loading the Sample into SEM Chamber
o The sample stub is placed inside the specimen chamber, and the chamber is evacuated
to a high vacuum.
4. Setting Parameters
o Adjust the accelerating voltage (commonly between 5–30 kV), spot size, and working
distance as per the sample type.
5. Focusing and Imaging
o Focus the electron beam on the sample surface using the electron gun.
o Adjust magnification and contrast to obtain a clear image.
o Capture images at different magnifications for detailed surface study.
6. Data Analysis
o Analyze the surface morphology, particle size, and microstructural features.
o If connected to an EDS detector, perform elemental analysis for composition study.
Results and Discussion:
Average Particle Size Calculation
Result (units from your
Column Calculation
data)
Sum of Feret values / Count of
Feret (Diameter) 48.337
particles
MinFeret (Minimum Sum of MinFeret values / Count of
41.777
Diameter) particles
Sum of Area values / Count of
Area 1723.167
particles
Quantitative Analysis
The statistical analysis of the measured data (summarized in the table above) provides the
following key findings:
1. Average Feret Diameter: The average particle size, based on the maximum dimension
(Feret), was calculated to be 48.34 units. This value serves as the primary metric for the
representative size of the particles in the sample.
2. Average Minimum Feret Diameter: The average MinFeret was found to be 41.78 units.
The difference between the average Feret and MinFeret values (~6.56 units) is an
indicator of the particles' non-spherical or elongated nature. If the particles were
perfectly spherical, these two values would be nearly identical.
Particle Size Distribution (PSD)
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The bar histogram provided clearly visualizes the Particle Size Distribution (PSD), plotting
the Number of Particles against their respective Size of Particles. The distribution exhibits the
following characteristics:
• Peak Position: The histogram appears to peak in the size range approximately
between 45 and 55 units (based on a visual estimation of the most populated bins),
which is consistent with the calculated average Feret diameter of 48.34 units.
• Distribution Shape: The distribution is generally unimodal (having a single peak),
suggesting a relatively uniform synthesis or processing route. However, the distribution
shows a moderate spread (variance), indicating that while a majority of particles fall
near the average, there is a noticeable presence of both significantly smaller and larger
particles (as shown by the tails extending from ~30 units up to ~70 units).
Conclusion
The Scanning Electron Microscopy and subsequent image analysis successfully characterized the
particle morphology of the sample material. The analysis of 85 individual particles revealed an
average particle size (Feret diameter) of 48.34 units. The Particle Size Distribution, as depicted
by the histogram, confirms a single primary particle population centered near the mean, but
with a degree of size variance and non-spherical shape. This combination of size and
morphology data is crucial for assessing the material's suitability for specific applications within
the field of electronics, and highlights the need for precise control over synthesis and processing
to optimize particle uniformity.