Material science

Assignment
 JIMMA UNIVERSITY
JIMMA INSTITUTE OF TECHNOLOGY
SCHOOL OF CHEMICALENGINEERING
Material science Assignment
 Student Name Id

Yonas Tarekegn Ru1540/12

Yonas Getachew Ru1540/12
Yosef Alemayehu Ru1540/12
Yosef Sisay Ru1540/12
 Contents
Characterization of Materials
X-ray Diffraction (XRD) and (FTIR)
Applications of XRD and FTIR in material characterization
Working Principle of X-ray Diffraction (XRD)
Sample Preparations in both FTIR and XRD
 Characterization of Materials

Materials characterization is the process of studying and understanding the physical,

chemical, and structural properties of materials. It is a crucial process in various
fields, including:
 Materials science and engineering: To develop new materials with specific
properties for applications in various industries.
 Manufacturing: To ensure the quality and consistency of materials used in
production.
 Product development: To optimize the performance and lifespan of products.
Cont.…
Materials characterization involves a variety of techniques, depending on the specific properties of
interest. These techniques can be broadly categorized into:
1. Chemical characterization
 Spectroscopy: Techniques like X-ray photoelectron spectroscopy (XPS) and Fourier-transform
infrared
 spectroscopy (FTIR) can identify the functional groups and chemical bonds present in a material.
2. Microstructural characterization
3. Physical property characterization
4. Surface characterization
 X-ray Diffraction (XRD)

The model which is available in jimma university is Drawell XRD 7000 which has
Scanning range : 5°-80°
Scanning Rate : 0.0012°-70 °min
X-Ray Source : Cu-Ka (3kw)
X-ray diffraction (XRD) is a powerful analytical technique used to determine the phas,
composition and crystal structure of a material.
It is based on the principle that X-rays are scattered by the electrons in a material,
and this scattering can be constructive or destructive depending on the angle of
incidence of the X-rays and the spacing between the atoms in the material.
Applications of XRD in material characterization:
Identification of unknown materials: XRD can be used to identify unknown materials
by comparing their diffraction patterns to known patterns in a database.
 Study of phase transformations: XRD can be used to study how materials change their phase as a
function of temperature, pressure, or other conditions.
 Analysis of thin films: XRD can be used to determine the thickness, crystallinity, and composition of
thin films.
 Study of defects in materials: XRD can be used to study the presence and type of defects in materials,
such as dislocations, vacancies, and grain boundaries.
 Development of new materials: XRD can be used to develop new materials with specific properties by
tailoring their crystal structure.
Working Principle of X-ray Diffraction (XRD)
 X-ray diffraction (XRD) is a powerful technique used to determine the crystal
structure of materials.
 It works by directing a beam of X-rays at a sample and measuring the angles
and intensities of the diffracted X-rays. By analyzing the diffraction pattern,
scientists can determine the arrangement of atoms in the crystal lattice.
It has the following parts
a) X-ray Generation:
b) Diffraction
c) Detection
d) Analysis
Cont.…
1. X-ray Generation:
X-rays are generated in a cathode ray tube. Electrons are emitted from a heated filament and
accelerated towards a metal (Cu) target. When the electrons collide with the target, X-rays are
emitted
2. Diffraction
The X-ray beam is directed at the sample. The X-rays interact with the atoms in the sample,
causing them to scatter in all directions. When the X-rays scatter from the atoms in a crystal, they
interfere with each other. Constructive interference occurs only when the scattered X-rays are in
phase with each other. This constructive interference results in diffracted beams that emerge from
the sample at specific angles
Cont.…
3. Detection:
The diffracted X-rays are detected by a detector. The detector measures the intensity
and angle of each diffracted beam. The intensity of the diffracted X-ray is related to
the number of atoms that are scattering in a particular direction. The angle of the
diffracted X-ray is related to the spacing between the atoms in the crystal lattice.
4. Analysis:
The diffraction pattern is analyzed using a computer program. The computer
program calculates the crystal structure of the sample based on the intensity and
angle of the diffracted X-rays
Sample Preparations
1. Grinding:
Most solid samples need to be ground to a fine powder. This increases the surface area
available for X-ray interaction and reduces preferred orientation effects. Grinding can be
done manually using a mortar and pestle or mechanically using a ball mill. The grinding
time and media should be chosen carefully to avoid introducing contamination or altering
the crystal structure of the sample.
2. Drying:
Some samples may need to be dried to remove moisture. This is important for accurate
quantitative analysis and to prevent sample decomposition during analysis. Drying can be
done in a vacuum oven or by freeze-drying.
Cont...
3. Mounting:
The prepared sample powder is mounted on a sample holder in a specific way to
ensure proper alignment with the X-ray beam. Different mounting techniques are
used for different types of samples. Some common mounting methods include back-
packing, front-loading, and spinning.
4. Special considerations:
Air-sensitive samples may need to be mounted in an inert atmosphere to prevent
oxidation or other reactions. Samples that are prone to preferred orientation may
need to be treated with a dispersing agent or textured in a specific way.
 Crystallinity
Crystallinity is the percentage of a material that exists in a
crystalline state.
It is an important parameter that influences the physical and
chemical properties of a material.
XRD can be used to determine the crystallinity of materials.
Determination of crystallinity using XRD
Crystalline vs. amorphous: Crystalline materials have a well-defined, ordered arrangement
of atoms, while amorphous materials lack this long-range order. This difference in structure
affects how X-rays interact with the material.
Diffraction pattern: When X-rays are directed at a crystalline material, they diffract at
specific angles according to Bragg's law. This results in a characteristic diffraction pattern
with sharp peaks.
Amorphous scattering: Amorphous materials, on the other hand, scatter X-rays in all
directions, resulting in a diffuse background signal in the diffraction pattern.
Crystallinity calculation: The crystallinity can be calculated from the diffracted intensities
of the crystalline peaks and the background intensity.
Cont…
There are two main methods for calculating crystallinity from XRD data:
1. Area integration method: This method involves measuring the total areas
under the crystalline peaks and the background. The crystallinity is then
calculated as the ratio of the area under the crystalline peaks to the total area.
2. Peak intensity method: This method involves comparing the intensity of the
strongest crystalline peak to the background intensity. The crystallinity is then
calculated using a calibration curve or a theoretical equation.
Crystallinity Index (CI)
The crystallinity index (CI) is a quantitative measure of the
degree of crystallinity in a material.
It represents the relative proportion of crystalline and
amorphous regions within the material.
The higher the CI value, the greater the proportion of
crystalline material.
 Cont…
General principles are as follows
A) Identify the crystalline and amorphous regions in the analysis data: This can be done using various
techniques, such as X-ray diffraction (XRD), infrared spectroscopy (IR), or differential scanning calorimetry
(DSC).
B) Measure the intensity or area associated with the crystalline and amorphous regions: This involves
integrating the intensity or area under specific peaks or bands in the data.
C) Calculate the CI using the following formula:

Where :
IC is the intensity or area associated with the crystalline region
I total is the total intensity or area of the data
CI is a dimensionless number between 0 and 100%.
 Fourier Transform Infra Red Spectroscopy
(FTIR)
Fourier Transform Infrared (FTIR) spectroscopy is a powerful
analytical technique used to identify and characterize materials
based on their molecular structure.
 It provides information about the functional groups present in
the sample and their relative abundance.
The model available in jimma university is: parkinelmer
spectrum two, which has wavenumber range : 8300-350
cm-
.
 Applications of FTIR
The PerkinElmer Spectrum Two is a versatile FTIR spectrometer that can be used for
a wide range of applications, including:
1. Identification of Functional Groups: FTIR provides rapid and non-destructive
identification of functional groups present in a sample. This information is crucial for
understanding the properties and reactivity of the molecule.
2. Identification of Polymers: can quickly and accurately identify unknown
polymers by comparing their spectra to a library of known polymers. This is
invaluable for quality control and product development.
CONT…
3. Determination of Degree of Polymerization: FTIR can be used to
determine the average number of repeating units in a polymer chain
(degree of polymerization). This information is crucial for understanding
the physical properties of the polymer.
4. Quality Control in Pharmaceutical and Chemical Industries:: FTIR
can be used to ensure the purity and identity of raw materials,
intermediates, and final products. This is essential for ensuring the safety
and efficacy of pharmaceuticals and other chemical products.
CONT…
Material characterization using FTIR typically involves the following steps
Sample preparation: The sample must be prepared in a way that is compatible with the FTIR
spectrometer. This may involve grinding the sample into a powder, dissolving it in a suitable solvent, or
making a thin film.
Data acquisition: The FTIR spectrum of the sample is collected over a range of wavenumbers.
Data analysis: The spectrum is analyzed to identify the functional groups present in the sample and to
determine their relative abundance. This can be done by comparing the spectrum to known reference
spectra or by using software to analyze the data.
Interpretation of results: The results of the FTIR analysis are then interpreted to provide information
about the chemical composition and structure of the material
Working Principles of Spectrometer
The PerkinElmer Spectrum Two FTIR spectrometer utilizes the principles of Fourier
Transform Infrared Spectroscopy (FTIR) to analyze the chemical composition of a
sample. 1. Radiation Source:
A broad-spectrum infrared (IR) light source emits IR radiation covering the desired
spectral range (typically 4000-400 cm-1).
2. Interferometer:
The heart of the instrument, the interferometer splits the IR beam into two paths and
introduces a controlled path difference between them. This path difference is constantly
varied, resulting in an interferogram - a signal containing information about all the IR
frequencies present in the original beam.
CONT…
3. Sample Interaction:
The IR beam passes through the sample, where some frequencies are absorbed
by the molecule's functional groups, while others are transmitted. The specific
absorption pattern depends on the molecule's structure and composition.
4. Detector:
The transmitted IR radiation is detected by a sensitive LiTaO3 (lithium tantalate)
or DTGS (deuterated triglycine sulfate) detector, which converts the IR signal into
an electrical signal.
CONT….
5. Fourier Transform:
The interferogram signal is mathematically transformed using a Fourier
Transform algorithm. This process converts the time-domain data
(interferogram) into the frequency domain data (spectrum).
6. Spectrum Analysis:
The resulting spectrum is a plot of the intensity of transmitted IR radiation
versus the wavenumber. This spectrum is unique to the sample and provides
information about the functional groups present and their concentration.
Sample Preparation for FTIR Analysis
Sample preparation is a crucial step in FTIR analysis, as it directly affects the quality and
accuracy of the acquired spectrum.
The preparation method depends on the type of sample and the desired information to be
obtained. Here's a breakdown of various sample preparation techniques commonly used in
FTIR:
Solids ex.Thin film: The sample is dissolved in a suitable solvent and cast onto a
transparent window. This method is useful for analyzing thin films and coatings.
Liquids ex Solution: The sample is dissolved in a suitable solvent and placed in a liquid
cell. This method is useful for diluting concentrated samples and reducing solvent
interference
Thank
You!!!