XRD

X-ray diffractor is a device that uses X-rays to measure the structure and properties of materials. It
works by shining a beam of X-rays on a sample and detecting the scattered X-rays that form a
diffraction pattern. The diffraction pattern can reveal information such as the crystal structure,
phase, preferred orientation, strain, and grain size of the material.

The main components of an X-ray diffractor are an X-ray source, a sample holder, and a detector.
The X-ray source generates X-rays by bombarding a metal target with high-energy electrons. The X-
rays are then filtered and collimated to produce a monochromatic and parallel beam. The sample
holder rotates the sample at different angles to expose it to the X-ray beam. The detector records
the angles and intensities of the diffracted X-rays that reach it. The data collected by the detector
can be analyzed using software to determine the structure and composition of the material.

SEM

A scanning electron microscope (SEM) is a device that uses a beam of electrons to scan the
surface of a sample and produce a magnified image of its features. The basic construction and
working of an SEM are as follows:

- The SEM has an electron gun** that generates a stream of electrons and accelerates them
towards the sample. The electron gun can be a thermionic emitter, a field emitter, or a laser-driven
emitter¹.
- The electron beam is focused and shaped by a series of **condenser lenses** that use magnetic
fields to control the beam diameter and convergence angle¹.
- The beam is scanned over the sample surface by a pair of scanning coils** that deflect the beam
in horizontal and vertical directions. The scanning coils are synchronized with the display device to
produce a raster image¹.
- The sample is mounted on a *sample stage* that can be moved in x, y, and z directions to adjust
the position and focus of the sample. The sample stage is usually inside a vacuum chamber to
prevent air molecules from scattering the electrons.
- When the electron beam hits the sample, it interacts with the atoms and generates various
signals, such as *secondary electrons*, *backscattered electrons*, *characteristic X-rays*, and
*cathodoluminescence*. These signals contain information about the surface morphology,
composition, and properties of the sample.
- The signals are detected by different types of *detectors* that convert them into electrical signals.
The most common detectors are the *secondary electron detector*(SED) and the *backscattered
electron detector* (BSED). The SED collects the low-energy secondary electrons that are emitted
from the surface of the sample. The BSED collects the high-energy backscattered electrons that
are reflected from deeper layers of the sample.
- The electrical signals are amplified and processed by an *analogue or digital system* that
converts them into brightness values for each pixel of the image. The image is then displayed on a
*
*monitor or screen* that shows the magnified view of the sample surface.

The SEM can produce high-resolution images of up to 10 nanometers and magnify objects up to
300,000 times. It can also perform elemental analysis and phase identification using EDS (energy-
dispersive X-ray spectroscopy) and CL (cathodoluminescence) techniques. The SEM is widely used
in various fields of science, engineering, medicine, and industry for studying the structure and
composition of materials.
AFM

The Atomic Force Microscope (AFM) is a type of scanning probe microscope that can measure the
properties and structure of a sample at the nanoscale level. The basic principle, construction and
working of AFM are as follows:

- **Principle**: The AFM works on the principle of measuring the intermolecular forces between a
sharp tip attached to a flexible cantilever and the sample surface. The tip scans the surface in a
raster pattern and the cantilever deflects according to the variations in the surface topography and
the force interactions. The deflection of the cantilever is detected by a laser beam that reflects off
the cantilever and hits a position-sensitive photodiode (PSPD). The PSPD converts the changes in
the laser beam position into electrical signals that are used to generate an image of the surface¹².

Construction: The AFM consists of the following main components¹²:

- A **cantilever** with a **sharp tip** at its end. The cantilever is usually made of silicon or silicon
nitride and has a tip radius of curvature of a few nanometers. The tip is the part that interacts with
the sample surface and senses the forces.
- A **laser** that emits a beam of light that reflects off the back of the cantilever. The laser beam
is used to monitor the deflection of the cantilever as it scans the surface.
- A **position-sensitive photodiode (PSPD)** that receives the reflected laser beam and measures
its position. The PSPD consists of four quadrants that generate different currents depending on
where the laser beam hits them. The difference between these currents is proportional to the
deflection of the cantilever.
- A **piezoelectric scanner** that moves the sample or the cantilever in three dimensions (x, y, z)
with high precision and accuracy. The piezoelectric scanner is controlled by a feedback circuit that
adjusts the z-position of the scanner to maintain a constant force or distance between the tip and
the sample.
- A **detector and feedback circuit** that processes the signals from the PSPD and controls the
piezoelectric scanner. The detector and feedback circuit also generate

TEM

The Transmission Electron Microscope (TEM) is a type of electron microscope that uses high
energy electrons to image the internal structure of materials. Its construction involves several
components:

1. Electron Source: A thermionic electron source is used to generate a beam of high energy
electrons. This source is typically made of a tungsten filament.

2. Electron Accelerator: An electron accelerator is used to accelerate the electrons generated by

the electron source. This is usually a series of electrostatic lenses that generate a high voltage.

3. Sample Holder: The sample holder is a stage that holds the sample to be imaged. It allows for
the precise placement and orientation of the sample to be examined.

4. Electron Optics Column: The electron optics column houses the series of electrostatic lenses
used to focus and direct the electron beam.

5. Detector: The detector is placed at the end of the column and captures the electron beam as it
passes through the sample.
The working of the TEM involves the following steps:

1. High energy electrons are generated by the electron source.

2. These electrons are accelerated by the electron accelerator, gaining high velocities.
3. The electrons pass through the sample on the sample holder.
4. As the electrons pass through the sample, they interact with the material, causing scattering and
diffraction of the electron beam.
5. The detector at the end of the column captures the scattered electrons and converts them into a
visual image that can be analyzed.

The principle behind the operation of a TEM is based on the wave nature of electrons. When high
energy electrons are focused on a thin sample, some of the electrons are transmitted through the
sample while others are scattered. By analyzing the scattering pattern of the electrons, the internal
structure of the material can be visualized in high resolution.