Department of Physics & Astrophysics

NANOMATERIALS LAB

SEM Analysis of ZnO Nanoparticles

Submitted to: Submitted by:

1. Dr. Shyama Rath Anchal,22056762026
2. Dr. Ayushi Paliwal Gunjan, 22222762083
3. Dr. Yana Bagbi Jeptha, 22222762090
Samarth
 Experiment-3
Aim
To study the morphological characterization of synthesized ZnO nanoparticles
using SEM (Scanning Electron Microscopy).

Chemicals Used
ZnO nanoparticles in powder form, synthesized by Sol-Gel method.

Apparatus
 Scanning Electron Microscope (JEOL - JSM-6610LV)
 Computer for data analysis

Specifications of the microscope used

The JEOL JSM-6610 SEM is an analytical Scanning Electron Microscope capable
of achieving 3nm point-to-point resolution at an accelerating voltage of 30kV. It is
equipped with a tungsten filament, and a large imaging chamber for observation of
specimens ranging from small pieces up to 200mm in diameter.
With Nanometer Pattern Generation System (NPGS) software, the system is
capable of Electron Beam Lithography.
Key Specifications:
 Model: JEOL JSM-6610 SEM
 Large sample size: up to 200mm diameter and 80mm height
 Resolution: 3.0 nm（30 kV）、15 nm（1 kV)
 Magnification: × 5 to × 300,000
 Accelerating voltage: 1 kV to 30 kV
 Filament: Tungsten hairpin
 Equipped with Nanometer Pattern Generation System (NPGS) for
Electron Beam Lithography

Theory
Introduction
Scanning Electron Microscopy (SEM) is a sophisticated imaging technique that
utilizes a focused beam of electrons to examine the surface of a specimen in great
detail. Unlike conventional optical microscopes that use visible light, SEM
employs electrons, enabling much higher magnification and resolution.
Scanning Electron Microscopy (SEM) revolutionizes our ability to explore the
microscopic world with unprecedented precision. Unlike traditional optical
microscopes, SEM employs a focused beam of electrons to scrutinize the surface
of specimens. This electron beam, meticulously scanned across the specimen,
induces interactions that generate signals, such as secondary electrons and
backscattered electrons. By harnessing these signals and employing specialized
detectors, SEM produces intricate, high-resolution images of the specimen's
surface. This technique is instrumental in diverse scientific domains, from
materials science to biology, offering invaluable insights into the topography and
composition of materials at a nanoscale level. SEM's capability to achieve
magnifications ranging from 10x to over 100,000x makes it an indispensable tool
for unraveling the hidden details of microstructures, contributing to advancements
in research and technology.

Principle
The principle of SEM involves the use of electrons instead of light for imaging. A
focused electron beam scans the specimen, causing various interactions that
produce signals. These signals, such as secondary electrons, backscattered
electrons, and X-rays, are detected and used to generate detailed images.
When the electron beam interacts with the specimen, it may result in the emission
of secondary electrons, which are sensitive to surface topography. Backscattered
electrons, on the other hand, provide information about the atomic composition of
the material. The signals are then collected and processed to create a high-
resolution, three-dimensional image of the specimen's surface.
SEM offers advantages such as high depth of field, allowing for clear imaging of
three-dimensional structures. The technique is widely used in various scientific
disciplines, including materials science, biology, and geology, providing valuable
insights into the microstructure and composition of diverse samples.

Scanning Electron Microscope

A scanning electron microscope (SEM) projects and scans a focused stream of
electrons over the surface of a sample and collects the different signals produced
using specialized detectors. The electrons in the beam interact with the atoms
within the sample, thereby producing various signals that can be used to obtain
information about the surface’s topography and composition. Images are viewed in
real-time on an external monitor using software that correlates the beam’s position
with the intensity of electrons acquired by the detector(s). A secondary electron
detector (SED) and a backscattered electron detector (BSD) are the two most
common types of detectors used for high-resolution imaging in an SEM.
Microanalysis of the surface composition can be accessed using energy dispersive
X-ray spectroscopy (EDS) detectors. The unique configuration of the SEM will
ultimately determine its resolution and available imaging modes.

Working of a Scanning Electron Microscope

The Scanning Electron Microscope (SEM) is a complex instrument with several
key components that work together to enable high-resolution imaging at the
nanoscale. Here's an overview of the instrumentation involved in SEM:
1. Electron Source: SEMs use an electron source to generate a focused beam
of electrons. Common sources include tungsten filaments or field emission
guns (FEG) for advanced SEMs.
2. Electron Lenses: Electromagnetic lenses focus and control the electron
beam's path, allowing for precise imaging. These lenses include condenser
lenses to shape the beam and objective lenses for focusing.
3. Specimen Stage: The specimen stage holds and positions the sample. It is
adjustable for tilt, rotation, and X-Y movement, providing flexibility for
imaging different regions of the specimen.
4. Vacuum System: SEMs operate in a high vacuum to prevent electron
scattering and maintain a stable electron beam. The vacuum system includes
pumps to create and maintain the vacuum environment.
5. Detectors: SEMs are equipped with detectors to capture various signals
emitted from the specimen.
● Secondary Electron Detector (SED): Captures secondary electrons
emitted from the specimen's surface, providing topographical
information.
● Backscattered Electron Detector (BSD): Detects electrons that are
backscattered from the specimen, providing compositional
information.
 6. Scanning System: A scanning system controls the movement of the electron
beam across the specimen's surface in a raster pattern. This scanning process
generates signals that are used to create images.
7. Control and Imaging Software: Advanced software controls the SEM's
operation. It allows users to adjust imaging parameters, such as
magnification and focus, and provides tools for image acquisition and
analysis.
8. Coating System: Some SEMs have coating systems that apply a thin
conductive layer to non-conductive specimens. This coating helps prevent
charging effects during imaging.
9. Chamber: The chamber encloses the entire system and maintains the
vacuum. It is designed to accommodate various sample sizes and shapes.
10.Display and Imaging System: SEMs are equipped with display systems to
visualize the acquired images. High-resolution monitors or digital imaging
systems are used for real-time observation and analysis.
11.Cooling Systems: Cooling systems are often integrated to maintain stable
operating temperatures for sensitive components, ensuring optimal
performance.
In summary, the instrumentation of SEM involves a combination of electron
optics, detectors, control systems, and imaging software working cohesively to
provide detailed and high-resolution images of specimens at the nanoscale. These
components collectively contribute to the versatility and power of SEM in
scientific research and materials characterization.
Instrumentation:
The main SEM components include:
 Electron source (gun)
 Condenser lenses
 Objective lens
 X-Y scan coils & scan generator
 Detectors
 Sample stage
 Computer and display to view the images
1. Electron Source (Gun):
The electron source is a fundamental component of the SEM, responsible for
generating a focused beam of electrons essential for imaging. In tungsten filament
sources, electron emission occurs through thermionic emission when the filament
is heated. In field emission guns (FEG), a strong electric field is applied to extract
electrons from a small pointed cathode. The choice between these sources
influences the coherence and brightness of the electron beam, affecting imaging
resolution and quality. Efficient operation of the electron source is critical for the
overall performance of the SEM, influencing the clarity and detail of the resulting
images.

2. Condenser Lenses:
Condenser lenses in the SEM play a pivotal role in focusing and shaping the
primary electron beam before it reaches the specimen. These electromagnetic
lenses apply magnetic fields to converge the electron beam, ensuring it is well-
defined and directed toward the specimen. The precision of condenser lenses
directly impacts the resolution of the SEM, influencing the clarity of the final
images. By manipulating the magnetic fields, these lenses contribute to controlling
the beam's intensity and size, optimizing the imaging conditions for a
comprehensive examination of the specimen's surface morphology and
composition.

3. Objective Lens:
The objective lens in the SEM serves as a critical element in the focusing system,
directing the electron beam precisely onto the specimen for high-resolution
imaging. By manipulating the magnetic field within the lens, it controls the
trajectory and convergence of electrons, influencing the resolution of the SEM.
The objective lens's ability to focus the electron beam plays a crucial role in
determining the level of detail and clarity achievable in the final images. This
component's precision is vital for achieving the nanoscale resolution required for
in-depth exploration of specimen surfaces in diverse scientific disciplines,
including materials science, biology, and nanotechnology.

4. X-Y Scan Coils & Scan Generator:

X-Y scan coils and the scan generator are integral components of the SEM
responsible for controlling the movement of the electron beam across the
specimen's surface. The X-Y scan coils, under the influence of the scan generator,
orchestrate a systematic scanning process in a raster pattern. This controlled
movement ensures thorough coverage of the specimen, allowing for a detailed
examination of its surface features. The scan generator provides the necessary
signals to the X-Y scan coils, dictating the path and speed of the scanning process.
The collaboration between these components enables researchers to acquire
comprehensive images, contributing to a more profound understanding of the
specimen's topography and composition at the nanoscale.

5. Detectors:
Detectors in the SEM play a pivotal role in capturing signals emitted from the
specimen during electron interactions, providing essential information for image
formation. Two primary types of detectors are employed: Secondary Electron
Detectors (SED) and Backscattered Electron Detectors (BSD). SEDs capture low-
energy secondary electrons, offering topographical details and contributing to
surface imaging. On the other hand, BSDs detect higher-energy backscattered
electrons, providing valuable insights into the specimen's composition. The
collaboration between these detectors enables SEM users to obtain a
comprehensive understanding of both surface morphology and material
composition, enhancing the analytical capabilities of the microscope in various
scientific fields.

6. Sample Stage:
The sample stage in the SEM serves as a crucial platform for holding and
positioning the specimen within the microscope's chamber. Its primary function is
to provide stability to the specimen while allowing precise control over its
orientation and position. The adjustability of the sample stage is a key feature,
enabling researchers to tilt, rotate, and move the specimen in X, Y, and Z
directions. This flexibility is essential for acquiring images from different
perspectives and exploring various regions of interest on the specimen's surface.
The precision and versatility of the sample stage contribute significantly to the
overall functionality of the SEM, facilitating detailed examinations and analyses of
diverse samples in fields such as materials science, biology, and geology.

7. Computer and Display:

The computer and display system in the SEM constitute the interface through
which researchers interact with the microscope, control its parameters, and analyze
acquired images. The computer serves as the central control unit, managing SEM
settings such as scanning parameters, detector configurations, and other operational
aspects. Researchers use the computer interface to optimize imaging conditions,
ensuring the acquisition of high-quality data. The display system provides real-
time visualization of SEM images, allowing researchers to observe and analyze the
specimen's surface with exceptional detail. This combination of computer control
and display capabilities enhances the efficiency and usability of the SEM, making
it a powerful tool for scientific research and materials characterization in various
disciplines.

SEM Analysis
The most widely known form of analysis performed by an SEM is morphological
and topographical analysis of a sample. In layman's terms, this means studying a
sample's structure and physical features under extreme magnification. This
information is gathered by the SEM using the secondary and backscattered electron
signals; however, it is the secondary electrons that give the most detailed view of
the sample. The uses for high resolution magnification are extremely vast, and
span many different scientific disciplines. This can include anything from
assessing the length of nanowires, viewing cellular structure, analyzing minute
surface fractures in substances, and much more.

ADVANTAGES OF SEM
Scanning Electron Microscopy (SEM) stands as a powerful and versatile tool in the
realm of scientific research, offering numerous advantages that contribute to its
widespread use across various disciplines.
1. High Resolution:
- One of SEM's primary advantages is its exceptional resolution, allowing
researchers to visualize specimens at the nanoscale. This capability provides
intricate details of surface structures that are beyond the reach of optical
microscopes.
2. 3D Imaging:
- SEM facilitates three-dimensional imaging, providing depth information about
the specimen's topography. This feature is crucial for understanding the spatial
arrangement of microstructures and enhancing the overall comprehension of the
sample.
3. Magnification Range:
- SEMs offer a broad magnification range, covering a spectrum from low to
extremely high magnifications. This flexibility allows scientists to investigate a
wide variety of samples with different size scales and complexities.
4. Versatility:
- SEM is versatile and applicable to a diverse range of materials and samples,
including biological specimens, metals, minerals, polymers, and composites. Its
adaptability makes it an indispensable tool in fields like materials science, biology,
geology, and nanotechnology.
5. Elemental Analysis:
- SEM can be coupled with energy-dispersive X-ray spectroscopy (EDS) for
elemental analysis. This capability enables researchers to determine the chemical
composition of the sample, providing valuable insights into material properties.
6. Surface Sensitivity:
- SEM is highly sensitive to surface features. Secondary electrons, one of the
signals detected, are emitted from the specimen's surface, making SEM particularly
effective in studying surface morphology and textures.

7. Real-Time Observation:
- Researchers can observe specimens in real-time during the imaging process.
This capability allows for immediate adjustments and ensures that data is collected
efficiently.
8. Non-Destructive Imaging:
- SEM allows for non-destructive imaging, preserving the integrity of the
specimen. This is especially beneficial when studying delicate biological samples
or rare materials that cannot be easily replaced.
9. High Depth of Field:
 - SEM provides a high depth of field, allowing clear imaging of three-
dimensional structures. This feature is advantageous when studying complex
surface topographies.
10. Rapid Imaging:
- SEM can rapidly generate high-quality images, making it a time-efficient tool
for researchers. This speed is crucial for analyzing large datasets and conducting
comprehensive studies.

DISADVANTAGES OF SEM
While Scanning Electron Microscopy (SEM) offers unparalleled advantages, it
also comes with certain limitations and challenges that researchers need to
consider.
1. High Cost:
- The initial cost of acquiring and maintaining SEM equipment is significant.
Additionally, operating and maintaining the high vacuum conditions required by
SEM can contribute to ongoing expenses.
2. Complex Sample Preparation:
- Preparing samples for SEM can be intricate and time-consuming. Non-
conductive specimens may need to be coated with a thin layer of conductive
material to prevent charging effects, and biological samples often require
dehydration and coating.

3. Limited Sample Size:

- The size of the sample that can be accommodated in the SEM chamber is
limited. Larger samples may need to be sectioned or trimmed, potentially altering
their original state.
4. Specimen Conductivity:
- Non-conductive specimens can accumulate a charge under the electron beam,
leading to image distortions or artifacts. Conductive coatings may be required,
introducing potential alterations to the specimen.
5. Limited Depth Penetration:
- SEM primarily provides surface information. It has limited depth penetration,
making it less suitable for studying internal structures. For detailed internal
imaging, other techniques like transmission electron microscopy (TEM) may be
more appropriate.
6. Vacuum Requirement:
- SEM operates in a high vacuum environment, restricting the analysis of volatile
or wet samples. This limitation can impact the study of certain biological
specimens or materials sensitive to vacuum conditions.
7. Beam Damage:
- The high-energy electron beam in SEM can cause radiation damage to some
specimens. This effect may alter the surface characteristics and complicate the
interpretation of results.
8. Lack of Color Information:
- SEM images are typically grayscale, lacking color information. While
elemental analysis can provide information about the chemical composition, the
grayscale nature of SEM images may limit the visual interpretation.
9. Instrument Sensitivity:
- SEM instruments can be sensitive to environmental conditions, and variations
in temperature or humidity may affect performance. This sensitivity necessitates
careful control of the laboratory environment.

10. Steeper Learning Curve:

- Operating and interpreting SEM results require specialized knowledge and
training. The complexity of the instrument and the need for understanding electron
optics and sample interactions contribute to a steeper learning curve compared to
simpler microscopy techniques.
In conclusion, while Scanning Electron Microscopy offers remarkable advantages
in terms of resolution, versatility, and real-time observation, researchers must
navigate its challenges, such as high cost, sample preparation complexities, and
limited depth penetration. Careful consideration of these factors ensures that SEM
is employed effectively for diverse scientific investigations.

RESULT (Surface morphology characterization using SEM technique)

1. Sample 1 (calcined at 500 °C)

Fig.1: x10,000 Fig. 2: x20,000

Fig.3: x5000
2. Sample 2 (calcined at 600oC)

Fig. : x20,000 Fig. : x10,000

Fig. : X5,000

DISCUSSION:
We have a microscopic image of the obtained ZnO nano particles shown at
different magnifications.
 The studies of the nanomaterial show different sizes of the particles
comprised in a range of 40 <d<60 nm.
  The microstructure of nano crystalline ZnO has irregular rod-shaped
structures resulting from the process of coagulation.
 The nano particles formed as a result of the decomposition have the shape of
faceted crystals. This material is characterized by high porosity

PRECAUTIONS
1. Sample Preparation:
- Avoid contamination during sample handling and use clean tools and surfaces
for preparation.
2. Sample Coating:
- Apply a thin conductive coating to non-conductive samples to mitigate
charging effects.

3. Vacuum Conditions:
- Ensure proper maintenance of the high vacuum environment to prevent electron
scattering.

4. Electron Beam Parameters:

- Optimize electron beam parameters (voltage, current) based on the sample to
enhance imaging quality.

5. Instrument Calibration:
- Regularly calibrate the SEM instrument to maintain accuracy in measurements
and imaging.