EXPERIMENTAL RESEARCH TECHNIQUES

PROCEDURE:
The experimental research has basically three main tasks:
1. Choice of material
2. Decision about desired property to be studied
3. Techniques required
We should have a sound knowledge of the techniques that will be used.

SYNTHESIS/GROWTH TECHNIQUES:
The first step after the selection of the material is to synthesize or grow the material. there
are different techniques such as:
 Solid state reaction
 Sol -Gel method
 Zone melting technique
 Czochralski method
 Molecular beam epitaxy [MBE]
 Sputtering
 Pulsed Laser Deposition [PLD]
 Physical Vapor Deposition [PVD]
 Spin Coating Technique
 Dip Coating
 Chemical Bath Deposition [CBD]

MATERIAL CHARACTERIZATION TECHNIQUES:

Materials Characterization is an important process in which a material's chemical,
microstructure and physical properties are probed, measured and determined using a
variety of analytical methods, techniques and tools. Following properties can be studied
using characterization:
 Structural properties
 Surface or morphological properties
 Electrical or dielectric properties
 Magnetic properties
 Mechanical properties
 Optical properties
 Thermoelectric properties
Following techniques are used for characterization:
o X ray diffraction [XRD]
o Hall effect measurement
o Band gap measurement using IR or UV Vis spectroscopy
o Vibrating sample magnetometer [VSM]
o Fourier transform infrared spectroscopy [FTIR]
o X ray Photoelectron Spectroscopy [XPS]
o Scanning electron microscopy [SEM]
o Transmission Electron Microscopy [TEM]
 o Atomic Force Microscopy [AFM]
o Magnetic Force Microscopy [MFM]
o Scanning Tunneling microscopy [STM]
o SQUID magnetometry
o Brunauer-Emmett-Teller (BET) analysis

PROPERTIES CHANGES AT NANOSCALE:

The material shows different optical, electric, magnetic, mechanical and structural
properties at Nano scale. Some examples are:
Material Macroscale Microscale
Copper Opaque Transparent
Platinum Inert Catalytic
Aluminum Stable Combustible
Gold Solid at room T Liquid at room T
Silicon Insulator Conductor

HOW TO PRODUCE NANOPARTICLES?

There are two approaches:
1. Top-down approach:
 Physical process
 Large scale objects are progressively reduced in dimensions
 Time consuming and costly
2. Bottom-up approach:
 Chemical process
 Different material and devices are constructed from molecular components which do
not require any external agent to assemble them. They chemically assemble each other
by recognizing molecules of their own type.
 It starts by collection of atoms and molecules to build complex structures.

Ball milling method:

 Top-down approach
 Mechanical energy is used
 It consists of a stain less steel container, hardened steel silicon carbide or tungsten
carbide balls.
 The mill rotates and grinds the material into fine powder.
 It requires almost 100 t0 150 hrs. to get uniform fine powder.
Advantages:
 Nanoparticles of size 2 to 20 nm can be produced (size of particles also depend upon
the speed of rotation of balls)
 Inexpensive and easy process
Disadvantages:
 As the process is not sophisticated, the shape of particles is irregular.
 There may be contaminants inserted from ball and milling additives, this produces
crystal defects.
Solid state reaction:
Solid-state reactions are the reactions that are performed in the absence of solvents. The
reaction is mechanochemical.
Procedure:
In this reaction, the starting material is either ground or melted or simply heat is applied to
a mixture of starting material. The traditional solid-state reaction route for the synthesis of
multiferroics consists of mixing by milling the appropriate metal oxides or carbonates and
then calcinating at high temperature to allow interdiffusion of the cations. The chemical
reaction occurs by solid-state diffusion of the ions, which is characterized by a slow kinetic
rate.
Advantages:
It is relatively inexpensive, simple, and it leads to acceptable results
Disadvantages:
Poor sintering (the process of compacting and forming a solid mass of
material by pressure or heat without melting it to the point of liquefaction)
behavior, non-uniformity of particle size and shape, lack of reproducibility, multiphase
character, and loss of stoichiometry (Stoichiometry is the relationship between
the weights of reactants and products before, during, and following
chemical reactions).

Zone melting technique:

The floating zone (FZ) technique is a crucible-free crystal growth method. In FZ growth, the
molten zone is kept between two vertical solid rods by its own surface tension. A single
crystal is grown by dipping a seed crystal into one end of the zone and translating the
molten zone toward the feed stock.
The main advantage of the float-zone technique is the very low impurity concentration in
the silicon crystal. The oxygen and carbon concentration are much lower as compared to CZ
silicon, since the melt does not come into contact with a quartz crucible, and no hot
graphite container is used.

Czochralski method:
  The Czochralski (CZ) method is a crystal growth technology that starts with insertion
of a small seed crystal into a melt in a crucible, pulling the seed upwards to obtain a
single crystal.
 The method is named after the Polish scientist Jan Czochralski, who developed it in
1916.
 Seed crystal is connected with any pulling mechanism and rotating chunk. When we
pull seed crystal liquid EGS is solidified into crystal.
 Pulling velocity of seed crystal is inversely proportional to radius of crystal.

Physical vapor deposition:

 Bottom-up approach
 Material is evaporated in vacuum
 Vapor particles travel towards cold target(substrate), deposited and condensed back
to solid states
 The evaporation can be done through two methods:
a. Resistive method; heat is generated to evaporate material by passing current
through high resistance coil.
b. Sputtering method; atoms are ejected from solid target due to bombardment of
target by energetic electrons.
Sol Gel process:
 Bottom-up approach
 Chemical process
 A sol is a colloidal (the dispersed phase in which size of the particle is so small that
gravitational forces do not exist, only van der fall forces and surface charges are
present)
 A gel is semi rigid mass that forms when solvent from sol begins to evaporate and
particles or ions left behind begin to join together in a continuous network.
Advantages
 Cheap and low T technique that allows fine control of product’s chemical
composition.
 Rate of reaction can be easily controlled by maintaining T
 Even small quantities of dopant can be introduced in sol and ends up uniformly
dispersed in final product.

Molecular beam epitaxy:

Epitaxy; method of depositing a mono crystalline film. Greek root, Epi means above and
Taxis means ordered.
Molecular Beam Epitaxy, otherwise known as MBE, is a material deposition technology in
which molecules are evaporated onto a wafer surface, stacking layer by layer to form high
quality crystal films. This process requires low pressure, low contamination and takes place
in an ultrahigh vacuum (UHV) chamber.
Working principle:
 The term beam means the evaporated atoms do not interact with each other not
with the vacuum chamber gases until they reach the wafer.
 Ultra-pure elements are heated in effusion cells until they began to slowly sublimate.
 Epitaxial growth takes place due to interaction of molecular or atomic beam on a
surface of heated crystalline substrate:
 They provide an angular distribution of atoms or molecules in a beam
 The substrate is heated to necessary temperature.
 Atoms on a clean surface are free to move until found correct position in the crystal
lattice to bond.
RHEED:

The MBE technique also allows us to characterize the material. RHEED stands for
“Reflection High Energy Electron Diffraction”. It is used to measure the growth of crystal
layer. RHEED is a valuable in-situ technique in Molecular Beam Epitaxy that provides
real-time information about the growth and quality of thin films. It aids in the precise
control of film thickness, crystal structure, and surface morphology, making it an
indispensable tool for researchers and engineers working with MBE processes.

Advantages:
This technique produces oxide layer free crystals, less crystal defects, good control of layer
thickness and deposition.

Pulsed laser deposition:

PLD is a thin-film deposition technique using high-energy laser pulses to vaporize the surface
of a solid target inside a vacuum chamber and condensing the vapor on a substrate to form
a thin film up to a few micrometres in thickness.
Working principle:
The process is divided into three groups:
(1) laser ablation;
(2) plasma formation and the expansion of target material;
(3) subsequent nucleation and growth of the target material on the substrate.
Advantages:
 Adhesion between the coating and substrate is excellent.
 Materials can be deposited at low temperatures close to room temperature.
 The coating can be applied on sensitive substrates such as thin polymer membranes

Spin coating technique:

Spin coating is a laboratory method to generate thin and homogeneous organic films out
of solutions. An excess amount of solution is placed on an ultra porous substrate that is
then rotated at high speed. The liquid spreads due to centrifugal forces and a uniform
liquid layer forms on the substrate.
Working principle:
Spin coating is performed in four steps, deposition, spin up, spin off, and evaporation,
Advantages:
This has become such a common form of coating such a wide variety of materials is
the simplicity and ease of use that it offers. High-speed spinning meaning a much
quicker drying time, further enhanced by the ability for higher air flow.
Dip coating:
Dip coating is a simple, low-cost, reliable and reproducible method which involves the
deposition of a wet liquid film by immersion of the substrate into a solution containing
hydrolysable metal compounds (or readily formed particles) and its withdrawal at constant
speed into an atmosphere containing water vapor.

Chemical bath deposition:

Chemical bath deposition (CBD) method is most commonly used because it is a very simple,
cost effective and economically reproducible technique that can be applied in large area
deposition at low temperature. Chemical bath deposition is used to deposit thin films of a
wide-range of materials.
Process:
Chemical Bath Deposition relies on creating a solution such that deposition (changing from
an aqueous to a solid substance) will only occur on the substrate, using the method below:

 Metal salts and (usually) chalcogenide precursors are added to water to form an
aqueous solution containing the metal ions and chalcogenide ions which will form the
compound to be deposited.
 Temperature, pH, and concentration of salts are adjusted until the solution is in
metastable supersaturation, that is until the ions are ready to deposit but can’t
 overcome the thermodynamic barrier to nucleation (forming solid crystals and
precipitating out of the solution).
 A substrate is introduced, which acts as a catalyst to nucleation, and the precursor ions
adhere to onto the substrate forming a thin crystalline film by one of the two methods
described below.

X ray diffraction technique:

 It used to determine structure of any crystal.
 It is a non-destructive technique (sample can be reused)
Principle:
It basically follows the brags law of diffraction
Construction:

X ray source Photographic plate

Goniometer (film, strip chart,
(monochromatic magnetic\storage
(crystal rotating)
x ray beam) medium

Working:

X-Ray Diffraction (XRD) allows one to ascertain the molecular structure of a crystalline
material by diffracting x-rays through the sample. An XRD analyser obtains interference
patterns reflecting lattice structures by varying the angle of incidence of the X-Ray beam.
A diffraction pattern is obtained which is a 2D image from which electron density map is
created and atomic model is generated using software.
Application:

X-ray diffraction can help scientists understand the value of their mineralogical samples by
determining their mineralogy and phase composition. XRD can also help to identify and
quantify toxic or undesirable elements or compounds that can adversely affect the final
product or the environment.

X ray photoelectron spectroscopy:

 XPS is also known as Electron Spectroscopy for Chemical Analysis ESCA is a widely use
technique to detect and quantify elements, and provide chemical state information,
making it a powerful survey analysis technique.
 Surface sensitive technique which typically analyzes sample to the depth of 5mm.
 Standard tool for surface material characterization.
 We get information from the ejection of core electrons. Core electrons are tightly
bound to the nucleus and have binding energy characteristics of the element.
Principle:
XPS is based on the photoelectric effect which was developed in the mid 1960 by Kei
Siegbahn and his research group.
Instrument:
A modern instrument for electron spectroscopy contains XPS and AES in a single chamber
coupled with a SEM as a multifunctional surface analysis system consisting of:
 An electron guns
 An X ray gun
 A shared analyzer of electron energy
 Detector system
1. Ultrahigh Vacuum system (UHV):
  Instruments for electron spectrometry require ultrahigh vacuum environment,10-
8_
10-10 mbar.
Reasons for such high vacuum are:
i. To reduce the chance of low energy electrons being scattered by the air
molecules on their way to reach the detector
ii. To keep the sample, clean from gas molecule contamination.
 Low energy photoelectrons or auger electrons are easily scattered by gas
molecules. Scattering can reduce signal intensity and increase background noise
in spectra.
 While collecting spectra from sample, its surface can adsorb a monolayer of gas
molecules in one second in a vacuum environment of 10-6mbar causing
contamination of surface. Contaminants will produce an x ray signal and can lead
to incorrect analysis of the sample.
 The ultrahigh vacuum is maintained by ion pumps or turbomolecular pumps.
 To achieve ultrahigh vacuum condition, the vacuum chamber must be baked at
an elevated temperature (250 – 350 C) and pumped. This baking process allows
the gas molecules adsorbed onto the chamber wall to be pumped out.
2. XPS/AES chamber material:
 the trajectory of the single electr6on is strongly affected by any magnetic field
even the earth’s magnetic field
 the UHV vessel is composed of Mu metal (ni iron alloy) or SS.
3. X ray source:
The x rays with energies as follows are used to generate the photoelectrons:
 Mg kα photon energy of 1253.6 Ev.
 Al kα photon energy of 1486.6 Ev.
XPS spectrum:
 It is basically a plot of no, of electrons detected at specific binding energy.
 The kinetic energy and intensities of photoelectron peaks make it able to identify
and quantify all surfaces (except hydrogen):
 No. of electrons present in sample
 Concentrations
 Empirical formula
 Oxidation states
 Chemical state and electronic state
 Surface chemical composition
o No. of electrons in each peak is directly related to amount of element exist within
XPS sampling volume.
Scanning electron microscope (SEM):
The scanning electron microscope is a tool used for material characterization with an aim to
obtain information about the structure, composition and defects in materials. The images
are obtained by scanning an electron beam of high energy on the sample surface, thus
named scanning electron microscope.
Following information is gained through SEM:
 Surface topography, grain shape/size/structure (secondary electron imaging)
 Atomic number contrast, grain boundaries, domains in magnetic materials
(backscattered electron imaging)
 Chemistry, elemental identification and quantification, line scans, x ray maps (energy
dispersive x ray spectroscopy)
 Pore size/shape/distribution in rock minerals, organic samples. (cryogenic
applications)
 Image non-conductive charging samples such as polymers rocks etc. without coating
(low vacuum mode)
 Details of surface structure (imaging at low kV)
 Printing of circuit boards in electronic circuits (Electron beam lithography)
Components
 Electron column
 Specimen chamber
 Computer control system

Image formation:
An electron beam is raster scanned (operated by a beam deflection system incorporated
within the objective lens) across the specimen surface resulting in the generation of:
  Secondary and backscattered electrons which are used to form images.
 X rays used to determine elemental constitution of the specimen material.
The beam is positioned in a particular location remains there for a fixed time, called dwell
time, and then it is moved to the next point.
The signal electrons emitted from the specimen are collected by a detector, amplified and
used to reconstruct an image, according to one to one correlation between scanning points
on the specimen and picture points on a screen of a cathode ray tube or liquid crystal
display
The SEM image is a 2D intensity map in the analog or digital domain. The image is generated
and displayed electronically.
 Magnification of up to 1 million times can be produced
 Resolution of 0.4nm at 30KV and 0.9nm at 1KV has been achieved.

Transmission Electron microscopy TEM:

It is used to reveal the internal structure of a material.
Construction:
 Electron gun
 Set of Condenser lenses
 Objective lens
 Magnifying lenses
Working:
The electron beam is directed through the sample. As electrons pass through the
specimen, they interact with the sample's atoms, leading to several phenomena:
 Elastic Scattering: Electrons can scatter elastically, providing information
about the atomic arrangement and crystal structure.
 Inelastic Scattering: Some electrons lose energy through inelastic scattering,
contributing to contrast in the resulting images.
 Diffraction: When electrons interact with the periodic lattice of crystalline
materials, they produce diffraction patterns, revealing information about the
crystallography of the sample.
Image Formation: The transmitted electrons or other signals generated during the
interaction are collected by detectors. These signals are used to create high-resolution
images and diffraction patterns. Researchers analyse the TEM images and diffraction
patterns to study various aspects of the sample, including its atomic structure,
crystallography, defects, and composition.
  TEMs can magnify objects up to 2 million times and have spatial resolutions of
slightly more than 0.2 nm.

Atomic force microscope:

 High resolution scanning probe tip microscope.
 It can examine all type of material surfaces including ceramics, polymers
 The van der wall forces, magnetic forces and other forces which arise due to physical
interaction b\w surface atoms cause cantilever tip to deflect.

Application:

It offers both qualitative and quantitative information on many physical properties

including size, morphology, surface texture and roughness. Statistical information, including
size, surface area and volume distributions, can be determined as well.

Magnetic Force Microscopy MFM:

Magnetic Force Microscopy (MFM) is an advanced microscopy technique that is used to
visualize and map the magnetic properties of materials at the nanoscale. MFM is a
specialized branch of Atomic Force Microscopy (AFM) that utilizes a magnetic tip to measure
magnetic forces between the tip and the sample surface.
Working:
The MFM tip is brought into close proximity to the sample surface without making direct
contact. When the tip is sufficiently close, it experiences magnetic forces arising from the
sample's magnetic properties. As the tip scans over the sample, the cantilever to which it is
attached experiences deflection due to the magnetic forces acting on the magnetic tip. This
deflection is detected and measured by a laser or other detection method, which is part of
the AFM setup.
Applications:
It is particularly useful for investigating magnetic domains, domain walls, and magnetic
defects in a wide range of materials, including ferromagnetic, antiferromagnetic, and
magnetic nanostructures.

Hall Effect measurement:

Hall effect measurements are used to determine a material’s conducting properties. From
the Hall resistivity, the carrier type and carrier concentration n are determined. Longitudinal
resistivity measurements are used in order to determine the conductivity and carrier
mobility.

Two probe method:

In a two-probe Hall Effect measurement, we use a simple setup to determine these
properties.
Probes: Only two probes are used. One probe is connected at one end of the sample, and
the other probe at the opposite end.
Current Path: The current flows from one probe to the other through the sample.
Voltage Measurement: A voltage measurement is made across the entire width of the
sample, perpendicular to the current direction. This voltage is called the Hall voltage.
Analysis: The Hall coefficient is calculated from Vh, and it provides information about the
charge carriers' type (electrons or holes) and mobility.

Four probe method:

Probes: Four probes are used, creating a square or rectangular pattern on the sample
surface.
Current Path: Two probes are used to apply the current, and the other two are used to
measure voltage.
Current Flow: The current flows from one pair of probes to the other pair, making it possible
to precisely measure the voltage drop exclusively across the material between the voltage
probes.
Voltage Measurement: Two types of voltage measurements are made:
Hall Voltage (Vh): Measured between the voltage probes perpendicular to both the current
and magnetic field directions.
Longitudinal Voltage (Vx): Measured between the voltage probes along the direction of the
current flow.
Analysis: The Hall coefficient is still calculated from Vh, providing information about charge
carriers. In addition, the resistivity (ρ) of the material can be calculated using Vx, which
measures the voltage drop along the current path.
Advantage of four probe method over two probe method:
Four-point probe is preferred than two-point probe as the contact and spreading
resistances in two-point probe are large and the true resistivity cannot be actually separated
from measured resistivity. In the four-probe method, contact and spreading resistances are
very low with voltage probes and hence accuracy in measurement is usually very high. To
measure very low resistance values, four probe method is used. The resistance of probe will
be not be added to that of sample being tested. It uses two wires to inject current in the
resistance and another two wires to measure the drop against the resistance.

Band gap measurement:

The band gap is measured using spectroscopy. The band gap is the energy difference
between the highest energy valence band and the lowest energy conduction band in a solid-
state material.

UV-Visible Absorption Spectroscopy:

It is commonly used to determine the band gap of materials, especially semiconductors and
insulators.
Principle:
The basic principle is that electrons in a material can absorb photons (light) when their
energy matches the energy difference between the valence band and the conduction band
(i.e., the band gap).
Working:
The sample is exposed to a range of wavelengths of light, typically in the UV and visible
regions. The spectrophotometer measures the intensity of transmitted light as a function of
wavelength. The absorption spectrum is plotted, showing how the material absorbs light at
different wavelengths. The band gap energy can be determined by locating the onset of
absorption, where there is a sharp increase in absorption. This corresponds to the energy
required to excite electrons from the valence band to the conduction band.

Photoluminescence Spectroscopy:
Photoluminescence spectroscopy measures the emission of light (photons) from a material
when it is excited by incident photons or other forms of energy (e.g., lasers or electron
beams). This technique is particularly useful for studying the optical properties and band
gap of semiconductors, quantum dots, and nanomaterials.
Working:
The material is excited by an external source, often a laser or intense light source. This
energy excites electrons from the valence band to the conduction band, creating electron-
hole pairs. After excitation, the material emits light as electrons recombine with holes and
return to lower energy states. This emitted light is detected and analysed using a
photoluminescence spectrometer. The emission spectrum shows the energy (or
wavelength) of the emitted light. The peak of the emission spectrum corresponds to the
band gap energy of the material. The band gap energy is determined from the peak
emission wavelength using the same energy-wavelength relationship as in UV-Visible
absorption spectroscopy.

Infrared (IR) spectroscopy:

IR radiation is part of the electromagnetic spectrum with wavelengths ranging from about
0.7 micrometres (microns) to 1000 microns. This region corresponds to the energy levels
associated with molecular vibrations and rotations. Infrared (IR) spectroscopy is a powerful
analytical technique used in chemistry, materials science, and various other fields to study
the vibrational and rotational modes of molecules and identify chemical compounds.
Principle:
It is based on the interaction of molecules with infrared radiation, specifically the
absorption, emission, or scattering of infrared light.
Working:
When IR radiation passes through the sample, it interacts with the molecules. The energy of
the IR photons is absorbed by the molecules, causing changes in their vibrational and
rotational states. The IR spectrometer measures the intensity of the transmitted or reflected
light as a function of wavelength. The result is an absorption spectrum, which shows the
specific wavelengths at which the sample absorbed IR radiation.

Fourier Transform Infrared Spectroscopy (FTIR):

FTIR is an analytical technical that is used to identify organic compounds.
Working principle:
 It is based on the interferometer.
 Sample is exposed to infrared light.
 The infrared light is absorbed by the sample which causes the molecules to vibrate.
 The detector measures the light that reaches the sensor, which provides raw
information on what was absorbed by the sample.
 The results are presented as light absorption versus wavenumber. The shape,
intensity and position of peaks are utilized for interpretation.
 The functional group of the material dictate the pattern of absorption bands.
Applications:
It can be used for material identification, material contamination, polymer modification
from field and monitoring of reaction rates and progress.
Limitations:
 Materials with similar structures are hard to identify.
 Complex mixtures can be difficult to analyze.
 Quantitative analysis of components or contaminants in a material is difficult.

Vibrating Sample Magnetometer VSM:

 It is a scientific instrument used to measure magnetic field.
 Sample to be studied can be in powdered, bulk or crystalline.
Principle:
It is based on faradays law of induction which tells us that changing magnetic field
produces electric field.
Working:
The sample holder, along with the attached sample, is set into controlled mechanical
vibrations. This vibration helps reduce friction between the sample and the sample
holder, allowing for precise measurements of small changes in the sample's magnetic
properties. An external magnetic field is applied to the sample using an electromagnet
or a permanent magnet. This magnetic field is typically adjustable in both strength and
direction. The sample is exposed to this magnetic field, causing the magnetic moments
within the sample to align with the applied field. As the sample vibrates within the
magnetic field, the changing magnetic field induces a voltage in a pickup coil or a Hall
sensor that surrounds the sample. This induced voltage is directly proportional to the
magnetic moment of the sample, which is the measure of its magnetization.
The data collected during the measurement is analysed to determine various magnetic
properties of the sample, including:
 Magnetic Susceptibility: A measure of how easily a material can be magnetized.
 Coercivity: The strength of the magnetic field required to demagnetize the sample.
 Magnetic Hysteresis Curve: A plot of magnetization versus applied magnetic field,
which provides insight into the material's magnetic behaviour.

Scanning Tunneling Microscopy:

Scanning Tunnelling Microscopy (STM) is a high-resolution imaging technique that allows
scientists to visualize and study the topography of surfaces at the atomic and molecular
scale.
Principle:
 STM operates on the principles of quantum tunnelling and is a fundamental tool in
nanoscience and surface science.
Working:
1. Initial Positioning: The STM tip is positioned at a relatively large distance (several
nanometres) above the sample surface.
2. Approach: The tip is brought closer to the sample by using the piezoelectric scanner.
When the tip is sufficiently close to the surface (typically within 1-2 nanometres),
quantum tunnelling of electrons can occur.
3. Tunnelling Current: Electrons can "tunnel" through the small gap between the tip
and the sample due to quantum mechanical effects. The tunnelling current depends
exponentially on the tip-sample distance and is highly sensitive to changes in this
distance.
4. Feedback Loop: The feedback control system continuously adjusts the tip's height to
maintain a constant tunnelling current. As the tip scans the surface, it moves up and
down to follow variations in the sample's topography.
5. Image Formation: The movement of the tip in the x and y directions, along with the
corresponding adjustments in the z direction to maintain a constant current, is
recorded. This information is used to create a high-resolution topographic image of
the sample's surface. The image is typically displayed as a series of height contours.

SQUID magnetometry:
The Superconducting Quantum Interference Device (SQUID) is a highly sensitive instrument
used for the characterization of various material properties, particularly those related to
magnetism and superconductivity.
Principle:
When the sample is moved up and down it produces an alternating magnetic flux in the
pick-up coil.
Working:
The SQUID magnetometer is capable of measuring extremely small changes in magnetic
flux. As the applied magnetic field is varied, the SQUID detects the magnetization response
of the sample, which is a result of the alignment of magnetic moments within the
materialal. The recorded data is analysed to determine various magnetic properties, such as
the magnetic susceptibility, magnetic moment, and critical temperatures associated with
magnetic phase transitions.
Applications:
Researchers use them to study a wide range of materials, including superconductors,
ferromagnetic and antiferromagnetic materials, magnetic nanoparticles, and more.

BET Analysis:
The Brunauer-Emmett-Teller (BET) technique is a widely used method for characterizing the surface
area of solid materials, particularly porous materials like catalysts, adsorbents, and nanomaterials. It
provides a quantitative measurement of the specific surface area, which is crucial for understanding
and optimizing the performance of these materials.

Principle:
The BET technique is based on the adsorption of gas molecules onto the surface of a solid
material. The fundamental premise is that when a gas (commonly nitrogen) is brought into
contact with a solid, it forms a monolayer of gas molecules on the surface. The BET theory
assumes that gas molecules adsorb in discrete layers, starting with a monolayer, followed by
the formation of additional layers, each less densely packed than the previous one.
BET Plot:
The data obtained from the adsorption isotherm is used to create a BET plot, which is a
graphical representation of the BET equation. From the slope and intercept of the straight
line in the BET plot, the specific surface area of the material can be calculated.
Bet equation: