JIMMA UNIVERSITY INSTITUTE OF

TECHNOLOGY
SCHOOL OF CHEMICAL ENGINEERING

course:- Material Science And Engineering

 Part I

Title:- Characterization of materials

using XRD
Introduction

X-ray diffraction XRD?

 is a powerful technique used for the characterization of
materials, especially crystalline substances
 provides information about the
 crystal structure
 crystallographic phases,
 lattice parameters and
 orientation of crystalline grains in a material
working principle

 based on the interaction of X-rays with the crystal lattice of a

material.
 When X-rays strike a crystalline sample, they undergo
constructive interference due to the regular arrangement of atoms
in the crystal lattice.
 This constructive interference results in a diffraction pattern,
which can be analyzed to obtain information about the crystal
structure of the material.
The key steps in the working principle of
XRD are as follows:
1 X-ray Source:
 X-ray diffraction experiments typically use a laboratory X-ray
tube as the source of X-rays.
 The X-ray tube generates X-rays with a specific wavelength,
often in the range of 0.1 to 2.5 angstroms.
2 Incident X-rays:
• The generated X-rays are directed toward a crystalline sample.
The incident X-rays have a high energy and short wavelength,
allowing them to penetrate the sample.
3 Scattering by Crystal Lattice:
 When the X-rays interact with the atoms in the crystal lattice, they are
scattered in various directions.
 However, the scattering is most intense in specific directions determined by
the arrangement of atoms in the crystal.
4 Bragg's Law:
 The scattered X-rays undergo constructive interference when the conditions
described by Bragg's law are met.
 Bragg's law relates the angle of incidence (θ), the wavelength of the X-rays
(λ), and the interplanar spacing (d) of the crystal lattice:
2dsin (θ)= nλ
where n is an integer representing the order of the diffraction peak
5 Diffraction Pattern:
 The diffracted X-rays form a pattern of bright spots on a
detector, known as the diffraction pattern.
 Each bright spot corresponds to a specific set of crystallographic
planes within the material.
6 Data Collection and Analysis:
 The diffraction pattern is recorded by a detector, and the data are
analyzed to determine the angles and intensities of the
diffraction peaks.
 The positions and intensities of these peaks provide information
about the crystal structure, including lattice parameters, crystal
symmetry, and the presence of different crystalline phases.
Sample preparation
Importance of sample preparation
 Sample preparation is crucial for X-ray diffraction (XRD) because it directly
impacts the accuracy and reliability of the results.
How is a sample prepared for XRD analysis

1.Crushing and Grinding:

 to reduce particle size.
 ensures a fine, homogeneous powder, aiding in uniform X-ray penetration
2.Homogenization:
 To have consistent and representative sample.
 involves thorough mixing to eliminate potential variations within the material.
3.Mounting:
 The powdered sample is often placed on a sample holder or mount.
 to ensure an even layer for accurate diffraction measurements.
4.Compaction:
 for amorphous materials
 to obtain a more uniform structure.
5.Surface Preparation:
 To obtain smooth and flat surface to avoid irregular scattering.
 involve polishing or other surface treatments.
6.Orientation Control:
 is important to avoid preferential orientation effects. This is
 particularly relevant for textured or anisotropic materials.
7.Moisture Control:
 Moisture can affect certain materials.
 to prevent changes in crystal structure due to hydration or dehydration.
Crystallinity

 refers to the degree to which a material exhibits a crystalline

structure.
 In a crystalline material, the atoms, ions, or molecules are
arranged in a highly ordered, repeating pattern called a crystal
lattice.
 This regular arrangement extends throughout the material,
resulting in well-defined planes of atoms and a three-dimensional
structure with long-range order.
crystallinity index

 The term "crystallinity index" typically refers to a quantitative

measure of the degree of crystallinity in a material, especially in
the context of polymers.
 provides information about the proportion of a material that exists
in a crystalline state compared to the overall material.
 It is commonly expressed as a percentage.
how to calculate crystallinity index using
XRD results.
 Calculating the crystallinity index from XRD results involves
determining the proportion of crystalline material in the sample
based on the intensities of crystalline and amorphous peaks in the
XRD pattern.
 Here is a step-by-step guide on how to calculate the crystallinity
index:
1. Collect XRD Data:
• Perform X-ray diffraction analysis on your sample using a calibrated XRD instrument.
2. Identify Crystalline Peaks:
• Identify the diffraction peaks in the XRD pattern that correspond
to the crystalline phase of your material.
• These peaks should be sharp and well-defined.
3. Identify Amorphous Baseline:
• Identify the baseline of the XRD pattern corresponding to the
amorphous background.
• This baseline separates the diffraction peaks from the amorphous
contribution.
4. Integrate Peak Areas:
• Integrate the areas under the crystalline peaks.
• This involves summing the intensity values within a specified range
around each peak. Many XRD analysis software tools have
automated peak integration features.
5. Total Integrated Intensity:
• Calculate the total integrated intensity of the entire XRD pattern,
including both crystalline and amorphous contributions.
• This value represents the total X-ray scattering intensity from the
sample
 6. Crystallinity Index Calculation:
• Use the integrated peak areas to calculate the crystallinity index
using the formula:
=
Part II

Title: Characterization of materials

using FTIR
Introduction

What is FTIR?
 FTIR stands for Fourier Transform Infrared Spectroscopy.
 It is a technique used to analyze the molecular structure and chemical
composition of a sample.
 Infrared radiation is passed through the sample, and the resulting spectrum is
analyzed to identify the types of chemical bonds present in the sample.
 FTIR is commonly used in the fields of chemistry, materials science, and
biology to identify and characterize a wide range of organic and inorganic
compounds.
Working principle of FTIR
 measures the absorption of infrared light by a sample.
 The key to its working principle lies in the interference of infrared
light and the mathematical technique of Fourier transformation.
 Here's a step-by-step explanation of the working principle of FTIR
1. Generation of Infrared Light:
• The FTIR spectrometer generates a broadband infrared light source.
• This light source typically covers a range of wavelengths that
correspond to the infrared region of the electromagnetic spectrum.
 2. Interaction with the Sample:
• The infrared light is directed through the sample.
• When the infrared light interacts with the sample, certain
wavelengths are selectively absorbed by the sample's molecular
vibrations.
3 Vibrational Modes:
• Molecules have specific vibrational modes associated with the
movement of atoms within the molecule.
• These vibrational modes are characteristic of different functional
groups in the molecules.
4. Absorption of Infrared Light:
• At specific wavelengths, the infrared light is absorbed by the sample,
causing the vibrational transitions of chemical bonds.
• The absorption of infrared light results in the excitation of molecular
vibrations
5. Interferometer:
• In FTIR, an interferometer is employed to modulate the infrared light.
The interferometer consists of a moving mirror and a fixed mirror. The
moving mirror introduces a path difference between the two beams of
infrared light.
6. Interference Pattern:
• The interference pattern is created as the two beams with a varying path
difference recombine. This interference pattern is recorded as an
interferogram.
 7. Fourier Transformation:
• The interferogram is subjected to Fourier transformation, a
mathematical process that converts the time-domain data
(interferogram) into the frequency-domain data (spectrum).
 8. Obtaining the Spectrum:
• The Fourier-transformed data provides the infrared spectrum of
the sample.
• The spectrum displays peaks at specific wavenumbers,
corresponding to the frequencies of absorbed infrared light.
 9. Data Analysis:
• The resulting spectrum is analyzed to identify peaks and patterns.
Each peak corresponds to a specific vibrational mode associated
with the molecular structure of the sample.
 10. Quantitative Analysis:
• FTIR can be used for quantitative analysis by measuring the
intensity of specific peaks and relating them to the concentration
of components in the sample.
sample preparation for FTIR analysis
 crucial to obtain reliable and accurate results
 The goal is to prepare a representative sample that interacts with
infrared radiation effectively.
 Here are the general steps for sample preparation for FTIR
analysis:
1. Selection of Sample Form:
 Determine the appropriate form for your sample.
 FTIR can analyze solids, liquids, gases, and films.
 The sample form depends on the nature of the material.
2. Solids:
a. KBr Pellet Method: - For solid samples
 grinding a small amount of the sample with dry potassium bromide (KBr) to form a pellet.
 The mixture is pressed into a transparent disc for analysis.
b. Attenuated Total Reflectance (ATR): -
 for solid samples that can be placed directly onto the ATR crystal.
 This method requires minimal sample preparation
 is commonly used for quick analysis.
c. Thin Films or Powders: -
 Solid films or powders can be spread evenly over a suitable substrate for analysis.
3. Liquids:
a. Liquid Cell Method: -
 Place a small amount of the liquid sample between two transparent windows,
forming a liquid cell.
 The liquid cell is then analyzed in the FTIR spectrometer.
b. Solvent Evaporation: - For volatile liquids
 the sample can be dissolved in a volatile solvent, and a drop of the solution is
deposited onto a suitable substrate.
 The solvent is allowed to evaporate before analysis.
4. Gases:
• Gaseous samples can be analyzed directly by passing them through a gas cell.
• This requires specialized sample handling equipment.

5. Film Analysis:
• For thin films, the film can be directly placed on an ATR crystal or sandwiched
between KBr pellets.
• Film thickness can affect the intensity of absorption bands.

6. Homogeneity:
• Ensure the homogeneity of the sample.
• Irregularities in sample distribution can lead to variations in the FTIR spectrum.
7. Background Correction:
• Record a background spectrum by analyzing a blank sample or the background material
used in the sample preparation.
• This is crucial for proper baseline correction.

8. Avoid Contaminants:
• Minimize contamination by handling samples with clean tools and wearing gloves to
avoid introducing foreign substances
 9. Temperature and Humidity Control:
 Some materials may be sensitive to temperature and humidity. Control these
parameters to avoid interference with the analysis.
 10. Record Sample Information:
 Record detailed information about the sample, including its origin, any
treatments or modifications, and any relevant contextual information.
Uses Of FTIR

 widespread applications in various fields due to its ability to provide detailed

information about the molecular composition of a sample.
Chemical Analysis:
• FTIR is extensively used for qualitative and quantitative analysis of chemical
composition.
• It can identify functional groups, chemical bonds, and molecular structures in a wide
range of materials.
Polymer Analysis:
• FTIR is crucial for the analysis of polymers.
• It helps in characterizing polymer structures, determining the degree of polymerization,
and identifying additives or impurities in polymer samples.
Pharmaceuticals:
• FTIR is used in the pharmaceutical industry for the analysis of drug formulations,
identifying active pharmaceutical ingredients (APIs), monitoring manufacturing
processes, and detecting impurities.
Environmental Monitoring:
• FTIR is employed for environmental analysis, including the identification of pollutants,
monitoring air quality, and analyzing soil and water samples.
Food and Beverage Industry:
• FTIR is used for quality control and analysis in the food and beverage industry. It helps
identify components such as fats, proteins, sugars, and additives in food products.
Forensic Science:
• FTIR is utilized in forensic analysis for the identification of substances, including
drugs, explosives, and trace evidence.
 Material Science:
• FTIR is widely used in material science to analyze and characterize a variety of
materials, including metals, ceramics, composites, and coatings.
 Biomedical Research:
• In biomedical research, FTIR is employed for the analysis of biological samples, such
as tissues, cells, proteins, and other biomolecules. It is used in disease diagnostics and
drug development.
Process Control:
• FTIR is employed for real-time process monitoring and control in industries such as
pharmaceuticals, petrochemicals, and food processing.
Petroleum and Petrochemical Industry:
• FTIR is used for the analysis of petroleum products, including crude oil, lubricants, and
refined fuels, to determine composition and monitor refining processes.