 Material Characterization techniques

 Classroom= Sect.1:Room 204,Teusday

Sect.2: Room 212,monday

Local time: 9:0-11:50

 Targeted group= 4th year students

 Instructor name= Dr. Gebisa Bekele

 Office hour = Friday 8 - 11 pm(local time)

 Material Characterization techniques

 MATERIAL SCIENCE TETRAHEDRON

 Material science tetrahedron shows the role of material characterization in

relationship with material processing, performance, properties and structure

 Material Characterization techniques

 What is material characterization techniques?

 Its is a process by which the material structure and properties are

probed or measured

 In characterization, two basic components are :

 What to be characterized: Material properties

 How could be characterized: characterization techniques

 Therefore, Characterization is an inevitable part of materials scientists

• Without characterization, no scientific understanding of material engineering

could be ascertained
 Material Characterization techniques

COURSE OVERVIEW
 The main emphasis of this course have two folds:
1. Describe the fundamental interaction that are used in modern material analysis

Probe beam
Detected beam
into the sample out of the sample

• Visible light • Visible light

• X-ray radiation, • X-ray radiation, Energy: Identification of atoms
• High energy • High energy
electrons beam electrons beam Intensity: Amount of atoms

 Reaction between the beam

and sample
• Nature of interaction

• Probability of interaction

• Interaction volume

• Resolution and sensitivity

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 Material Characterization techniques

COURSE OVERVIEW
 The main emphasis of this course have two folds:
2. Illustrate the use of this understanding in practical material analysis

Analysis chamber

Source Detector

Sample

 Characterization techniques divided into three:

• Microscopic, Diffraction, Spectroscopic

 Thermal and mechanical analysis methods are also considered as material characteriza-
6
tion or testing methods
 Material Characterization techniques


 Introduction Evaluation
• Continuous assessments(25%)
 Microscope • Midterm exam (15%)
• Lab report(30%)
 Diffraction, XRD • Final project presentation (10%)
• Final exam (15%)
 Spectroscopy

 Fourier infrared spectroscopy

 Thermal analysis methods

 Mechanical properties analysis methods

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 Material Characterization techniques

 REFERENCE
Microstructural Characterization of Materials,” David Brandon and Wayne D. Kaplan.

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 Material Characterization techniques

 Concept of microstructure
 Proper caring and tuning of parameters are very important to get high quality
materials that possess strong potential for diverse applications

Processing Structure Properties Performance

 The characteristics and performance of a material depends on the method of

preparation and pretreatment conditions

 We can tune the mechanical, thermal, chemical and electrical properties of

the material for specific applications

 In order to make a correlation between properties of the materials and its

application, suitable characterization techniques are essential

 Material Characterization techniques

 Concept of microstructure
 What is microstructure?
 Microstructure is used to describe the
Chemical composition
( Crystal structure ) appearance of material on nm-cm length scale.
 The arrangement of phases and defects

Ceramic Intrinsic material within a materials

fabrication selection

Microstructure
Properties
(Characterization)

 The properties of the materials are

Two phases intergrowth in
solely determined by size of Dislocation network
etched ilmenite-hematite
microstructure and intrinsic
materials composition
 Crystal structure: describe the average position of atoms within a unit cells

 the appearance of material on an atomic length scale

 Material Characterization techniques

 Concept of Microstructure
 Microstructural Features
 Structure – properties relationship

 Structural sensitive  Structural insensitive

Directly and sensitively related to  Invariable with the microstructure of
microstructure of materials the materials

• Yield strength, dislocation • Elastic constants

density, thermal conductivity Example, All steels have the same

and electrical resistivity young’s modulus

• Fracture toughness of an • Thermal expansion coefficient

engineering material • Specific density of the materials

Petch equation: related the yield strength to

D
Note: D is grain size
−𝟏/𝟐
microstructure feature. 𝝈𝒚 = 𝝈𝟎 + 𝒌𝒚 𝑫
 Material Characterization techniques

 Concept of Microstructure
 Microstructural Scale and Characterization techniques
XRD TEM,STM SEM OM

 Microstructure ranging from crystal structure to Engine components

 Material Characterization techniques

 Level of Characterization
 Material Characterization techniques

 Concept of Microstructure
 Microstructural parameters:
• Petch equation: 𝝈𝒚 = 𝝈𝟎 + 𝒌𝒚 𝑫−𝟏/𝟐

 Grain size: the average separation of two

parallel tangent planes that touch the surfaces
of any randomly oriented grain

 Dislocation and dislocation density

 Material Characterization techniques

 Crystallography and Crystal structure

 Crystallography:
 gives a concise representation of a large assemblage of species by

describing or characterizing the structure of the crystals.

 It gives the first view towards understanding of the properties of the

crystals

 Crystal: 3D translationally periodic arrangement of atoms in space

 Lattice: 3D translationally periodic arrangement of the points in the space

 Basis : an atoms or group of atoms associated with each lattice point

 Space Lattice: A 3D network of imaginary lines connecting the atoms

 Material Characterization techniques

 Crystallography and Crystal structure

 Unit cell: Smallest unit having the full symmetry of the crystal

The smallest portion of the lattice that can

be repeated by translation to cover the entire

3-D space.

 The specific unit for each metal defined by:

• Edge of the unit cell including a ,b and c

• Angles α,β,γ

 There are 14 possible types of the space lattice (Bravias lattice) and they

fall into 7 crystal systems.

 Material Characterization techniques

 Crystallography and Crystal structure

Bravias Lattice
Number Crystal system Lattice parameter P I F C

1 Cubic a=b=c, 𝛼 = 𝛽 = 𝛾 = 900 √ √ √

2 Tetragonal a=b≠c, 𝛼 = 𝛽 = 𝛾 = 900 √ √ P=primitive

I=Body centered
3 Orthorhombic a≠b≠c, 𝛼 = 𝛽 = 𝛾 = 900 √ √ √ √
F=face centered
4 Hexagonal a=b≠c, 𝛼 = 𝛽 = 900 , 𝛾 = 1200 √
A/B/C-centered

5 Trigonal a=b=c, 𝛼 = 𝛽 = 𝛾 ≠ 900 √

6 Monoclinic a≠b≠c, 𝛼 = 𝛾 = 900 ≠ 𝛽 √ √

7 Triclinic a≠b≠c, 𝛼 ≠ 𝛽 ≠ 𝛾 √
 Material Characterization techniques

 Crystallography and Crystal structure

 Crystallographic direction : line between two points or vector

 The three directional indices are determined

by :
1. The vector of convenient length is positioned such
that it passes through the origin of the coordinate
2. If parallelism is maintained, any vector may be
translated throughout the crystal lattice without
alteration.
3. The length of the vector projection on each of the
three axes is determined, these are measured in

 The direction of vector r is [uvw] terms of unit cell dimensions, a, b and c.

4. These 3 numbers are divided or multiply by a
common factor to reduce them to the smallest integer
values
5. The 3 indices are enclosed in square [uvw]
 Material Characterization techniques

 Crystallography and Crystal structure

 Family of direction
 A set of direction related by symmetry operation of the lattice or
crystal
 It is represented by Miller index notation:<uvw>

Index Members in family for cubic lattice

<100> [100],[100], 010 , 010 , 001 , [001]
<110> 12

[ ]  Particular direction

 < > or [[]]  family of directions

 Material Characterization techniques

 Crystallography and Crystal structure

 Crystallographic planes

In all but hexagonal crystal systems are specified by 3 Miller indices (hkl)
Any two planes parallel to each other are equivalent and have identical indices

 Steps to determine the Miller indices:

1. If the plane passes through the selected origin, either another parallel plane must be constructed within the
unit cell by appropriate translation, or a new origin must be established at the corner of another unit cell

2. The crystallographic plane either intersect or parallel to each of the 3 axes, the length of the planer intercept
each for each axis is determined in term of the lattice constant a, b and c.

3. The reciprocal of these numbers are taken. A plane that parallels an axis may be considered to have infinite
intercept, & therefore, zero index.

4. These three numbers are changed to the set of smallest integers by multiplication or division by common
factor.

5. Finally the integer indices are enclosed in parentheses: (hkl)

 Material Characterization techniques

 Crystallography and Crystal structure

 Crystallographic planes

1. Intercept: x=1, y=∞, and z= ∞

1) 2) 3)  (hkl) =(100)
2. Intercept: x=1, y=1,z= ∞
(hkl)=(110)
3. Intercept: x=1,y=1,z=1
(hkl)=(111)

 Interplanar spacing(𝒅𝒉𝒌𝒍 )
in cubic lattice:
𝒂
4) 5) 𝒅𝒉𝒌𝒍 =
𝒉𝟐 +𝒌𝟐 +𝒍𝟐
 Material Characterization techniques

 Crystallography and Crystal structure

 Family of planes: set of planes related by symmetry operations on the

lattice or the crystal
 Family of planes is represented by {hkl}

 Plane  (100)  Plane  (111)  Plane  (110)

 Family of planes  {100}  6  Family of planes  {111}  8  Family of planes  {110}  6
 Material Characterization techniques

 Crystallography and Crystal structure

 Hexagonal lattices:
Direction and planes in hexagonal lattices and crystal are designated by the
4-index Miller- Bravias notations
In the four index notation: (hkil)
 The first three indices are a symmetrically related
set on the basal planes

Related to ‘l’  The third index is a redundant one and introduced to

make sure that a member of a family directions or
planes have a set of members which are identical.
 The fourth index is the ‘c’ axis, which is
Related to ‘k’
Related to ‘k’ perpendicular to the basal plane.
Related to ‘h’
 Material Characterization techniques

 Crystallography and Crystal structure

𝑎3
 Hexagonal Lattice o (hkil)
i=-(h+k)

𝑎2

𝑎1

 Intercept: ∞, 1,-1, ∞
 Intercept: 1,-1, ∞, ∞
 Miller indices: (01-1)
 Miller indices: (1-10)
 Miller- Bravias:(01-10)
 Miller- Bravias:(1-100)
 Material Characterization techniques

 Crystalline and non-crystalline Materials

 Isotropic materials

 If the properties of the material is independent of the direction in which they

are measured.

 Anisotropic materials

 If the properties of the material is dependent of the direction in which they are

measured.

Example: Periodicity of the atoms in the crystal structure, density of

crystalline solid, carrier velocity, phonon velocity.

 Allotropy: elements that can exhibit more than one crystal structure

 Polymorphism: Compounds behaves in the same manner

 Material Characterization techniques

 Crystalline and non-crystalline Materials

 Single crystal: A continuous periodic crystal structure only interpreted by the
boundaries of the solid

 Amorphous: A though short range periodicity may be presented, long range of

periodicity is absent.

 Polycrystalline: A materials composed of from two to many single crystal grains.

 Why do we need to discuss about the fundamental

properties of the materials ?
 to know what to be characterized
 Material Characterization techniques

 What to be characterized
 Structure
 Composition
 Elemental: Major, minor, impurity, dopant
 Elemental distribution
 Valency: atomic bonding state
 Structure
 Microstructure
 Grain shape and size, distribution
 Crystal structure
 Space group, lattice parameters
 Electronic structures: Fermi level, and density of state
 Defects and their concentration:
 Point, line and planer
 Material Characterization techniques

 What to be characterized
 Surface of the materials
 Morphology

 Porosity ( size and concentration), Surface area

Composition and Bonding state
 Chemi-sorption and Physi-sorption
 Structure
 Ad- atom arrangement (1x1,2x2,..)
 Reconstruction/ relaxation, defects
 Surface electron density
 Volume, thermal stability
 Internal stress, Nature of stress and distribution
 Phase stability
 Material Characterization techniques

 Material characterization techniques tools

 Properties and nature of the materials under investigation can be identified
perfectly with the help of suitable characterization tools.

 Characterization techniques: Qualitatively provide the surface images and

quantatively give deep insight into the relative concentration of the atoms

 Suitable characterization technique is very necessary to understand the

whole picture of the material that in turn helps the researcher to find out

the exact field of its application!