INDIAN INSTITUTE OF TECHNOLOGY ROORKEE

MATERIAL CHARACTERIZATION AND TESTING

Chapter 01 : Introduction

Prof. Kaushik Pal

Professor
Department of Mechanical and Industrial Engineering
Indian Institute of Technology Roorkee
About Course

Subject Code: MIN:615 Course Title: Material Characterization and Testing

Contact Hours: L:3 T:1 P : 2/2

Examination Duration (Hrs.): Theory : 3 Practical : 0

Relative Weightage: CWS: 15-30 PRS: 20 MTE: 15-25 ETE:30-40

PRE: 0

Credits: 4 Semester: Autumn Subject Area: PCC

Pre-requisite: Nil

Objective: To give students a thorough and conceptual understanding of various material

characterization and testing techniques.

2
Course Content
Contact
S. No. Contents
Hours
1. Introduction: Engineering Materials, Properties of Materials; Crystal 03
Structure, Strengthening Mechanisms in Metals; Fundamentals of
Materials Characterization; Basic Sample Preparation and Interpretation of
Data.

2. Optical Microscopy: Fundamentals of Optics, Optical Microscope and 05

Image Formation, Depth of Field and Depth of Focus; Specimen
Preparation, Metallographic Principles, Applications.

3. Electron Microscopy: Scanning Electron Microscopy- Working Principle, 08

Electron Specimen Interaction, Instrumentation and Applications of SEM,
Chemical analysis in SEM (EDS & WDS), Electron Backscatter
Diffraction, Applications of EBSD; Transmission Electron Microscopy-
Instrument Details and Imaging Modes, Specimen Preparation Methods.

3
4. X-ray Diffraction: Properties of X-rays, Geometry of Crystals, 10
Bragg’s Law, Diffraction Methods, Intensity of Diffracted Beams,
Structure Factor Calculations, Diffractometer Measurement;
Applications of XRD- Phase Identification, Crystal Structure and
Phase Diagram Determination, Crystallite Size, and Lattice Parameter
Determination.

5. Thermal and Thermomechanical Methods: Thermal Gravimetric 09

Analysis (TGA), Differential Thermal Analysis (DTA), Differential
Scanning Calorimetry (DSC), and Dynamic Mechanical Analysis
(DMA), Thermomechanical Analysis (TMA).

6. Mechanical Testing: Uniaxial Tension Test, Compression Test, Three 07

and Four Point Bending Test, Hardness Tests, Impact Tests, Creep and
Stress Rupture Tests, Fatigue Test and Failure Analysis.

Total 42

4
List of Experiments:
1. Sample preparation for optical and SEM observations.
2. Grain size determination of given metallic sample using optical microscopy.
3. Microstructural study and chemical analysis using SEM.
4. To demonstrate the TEM sample preparation and TEM analysis.
5. Determination of phases in multiphase powder sample using XRD.
6. DSC/DTA analysis.
7. To study dynamic mechanical behavior of polymers.
8. To determine the tensile properties of given samples.
9. To determine the hardness of given metallic sample by Brinell, Vickers, and Rockwell
hardness tester.
10. To determine the impact strength of given metallic sample by Izod and Charpy methods.
11. To perform fatigue test on given sample.

5
Introduction

• What is materials science?

• Why should we know about it?

• Materials drive our society

– Stone Age
– Bronze Age
– Iron Age
– Now?
• Silicon Age?
• Polymer Age?

6
 Materials

• Over 70,000 different kinds and grades of engineering

materials

• This number grows daily

• 1,000 different materials make up an automobile

7
Historical Perspective
• Earliest humans had access to only a very limited number
of materials, those that occur naturally:
 Stone, wood, clay, skins, and so on.
• With time they discovered techniques for producing
materials that had properties superior to those of the
natural ones (pottery and various metals).
• Furthermore, it was discovered that the properties of a
material could be altered by heat treatments and by the
addition of other substances.

8
Primary Classes of Materials
• Metals:
– Strong, ductile
– High thermal & electrical conductivity
– Opaque, reflective
– e.g. aluminum, iron, and titanium
• Polymers/plastics: Covalent bonding  sharing of electrons
– Soft, ductile, low strength, low density
– Thermal & electrical insulators
– Optically translucent or transparent
– e.g. acrylic, polyethylene, and nylon

9
• Ceramics: ionic bonding (refractory) – compounds of metallic &
non-metallic elements (oxides, carbides, nitrides, sulfides)
– Brittle, glassy, elastic
– Non-conducting (insulators)
– e.g. Al2O3, Fe3C, and SiC

Other “classes”:
• Composites
• Semiconductors (e.g. silicon, germanium)
10
 Metals

• Cast Iron
• Steel
– Mild steel, medium carbon steel, high carbon steel
• Specialty steel
– Stainless (tin plated or galvanized)
• Alloys (two or more pure metals)
– Steel= iron & carbon
– Brass= copper & zinc
– Bronze= copper & tin

11
 Polymers

• Natural
– Protein
– Natural rubber
– Cellulose
– Wool, Silk

• Synthetic
– Thermoplastics
– Thermosets

12
 Ceramics

• Clay based
– Structural clay-tile, brick
– Porcelain
• Refractories
– Heat resistant (fire bricks)
• Glasses
• Inorganic cements

13
 Composite Materials
 Multiphase materials with measurable fraction of every phase
 Obtained by artificial combination of different materials, so as to
attain properties that the individual components by themselves
cannot attain.
 Composite materials are not the by-product of any chemical
reaction between two or more of its constituents.

 Two major components in a composite:

I. Reinforcement (Discontinuous/dispersed
phase): Material that provide strength to
the matrix.
II. Matrix (Continuous phase): Material that
holds the reinforcement in place.

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Classification of Composite Materials:

Metal Matrix Composites

Based on matrix material Polymer Matrix Composites

Ceramic Matrix Composites

Composite Material

Particulate Composites

Based on reinforcing material Fibrous Composites

structure

Laminate Composites

15
Examples:
 Naturally Occurring Composites:
 Bone: Collagen fibers embedded in
hydroxyapatite matrix.
 Wood: Cellulose fibers held together by
lignin matrix.
 Man-made Composites:
 Reinforced Concrete: Steel reinforcing
bars embedded in the concrete.
 Fibrous Composites: Variety of fibers
(glass, Kevlar, carbon, nylon, etc.) bound
together by a polymeric matrix.
 Cermets: Composite material composed of
ceramic and metal materials.

16
Engineering Materials

Engineering
Materials

Metals Polymers Ceramics Composites

Ferrous Thermosets

Non-ferrous Thermoplastics

17
Classification of Metal Alloys
Metal Alloys

Ferrous Nonferrous

Steels
Steels Cast
Cast Irons
Irons
<1.4wt%C 3-4.5 wt%C

T(ºC)
1600
δ
1400 L
γ+L microstructure: ferrite,
1200 γ 1148ºC L+ Fe3C
austenite Eutectic:
graphite/cementite
1000 4.30

γ + Fe3C
α 800 727ºC Fe 3 C
ferrite Eutectoid: cementite
600 0.76 α + Fe3C
400
0 1 2 3 4 5 6 6.7
(Fe)
Co , wt% C
18
 Nonferrous Alloys
• Cu Alloys • Al Alloys
Brass: Zn is subst. impurity -low ρ: 2.7 g/cm3
(costume jewelry, coins, -Cu, Mg, Si, Mn, Zn additions
corrosion resistant) -solid sol. or precip.
Bronze : Sn, Al, Si, Ni are strengthened (struct.
subst. impurities aircraft parts
(bushings, landing & packaging)
gear) NonFerrous • Mg Alloys
Cu-Be : -very low ρ: 1.7 g/cm3
precip. hardened Alloys -ignites easily
for strength -aircraft, missiles
• Ti Alloys
-relatively low ρ: 4.5 g/cm3 • Refractory metals
-high melting T’s
vs 7.9 for steel • Noble metals -Nb, Mo, W, Ta
-reactive at high T’s -Ag, Au, Pt
-space applic. -oxid./corr. resistant

19
 Ferrous Alloys
Iron-based alloys
• Steels
• Cast Irons

Types of Steels
• Steels- alloys of iron-carbon, may contain other alloying elements
• Several grades are available
• Low Alloy (<10 wt%)
– Low Carbon (<0.25 wt% C)
– Medium Carbon (0.25 to 0.60 wt% C)
– High carbon (0.60 to 1.4 wt% C)
• High Alloy
– Stainless Steel (>11 wt% Cr)
– Tool Steel
20
 Steels
Low Alloy High Alloy
low carbon Med carbon high carbon
<0.25 wt% C 0.25-0.6wt% C 0.6-1.4wt% C

heat
Name plain HSLA plain plain tool stainless
treatable
Cr,V Cr, Ni Cr, V,
Additions none none none Cr, Ni, Mo
Ni, Mo Mo Mo, W
Example 1010 4310 1040 43 40 1095 4190 304, 409
Hardenability 0 + + ++ ++ +++ varies
TS - 0 + ++ + ++ varies
EL + + 0 - - -- ++
Uses auto bridges crank pistons wear drills high T
struc. towers shafts gears applic. saws applic.
sheet press. bolts wear dies turbines
vessels hammers applic. furnaces
blades Very corros.
resistant
increasing strength, cost, decreasing ductility
21
Low and Medium Carbon Steel Nomenclature

• Four digit number

– First two give alloy
– Second two give wt%
carbon  100
– UNS number starts
with G
• Some alloy types
– 10XX, plain carbon
– 41XX, Cr + Mo
– 43XX, Ni + Cr + Mo

22
Tool and Stainless Steel Nomenclature

• Tool steels
– High carbon content (0.6-1.4 wt. %)
– AISI code denoted by letter+number
• e.g. M1, A2, etc.
– UNS number starts with T
• Stainless steels
– >11 wt. % Cr
– 3XX series, austenitic
– 4XX series, ferritic and martensitic
– XX-XPH, precipitation hardened
– UNS number starts with S

23
 Cast Irons
 Ferrous alloys with carbon content above 2.14 wt.%, and in addition other
alloying elements
 Low melting – relatively easy to cast
 Generally brittle

Types of Cast Iron

• Grey Cast Iron - Carbon as Graphite
• White Cast Iron - Carbides, Often Alloyed
• Ductile Cast Iron
o Nodular, Spheroidal Graphite
• Malleable Cast Iron
• Compacted Graphite Cast Iron
• CG Or Vermicular Iron
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Production of Cast Irons

25
What do these things do in steels?

Change C content

Mechanical work
Change “structure”
Heat treat

Alloying elements

Changing structure changes properties

26
Components of Materials Engineering

• Materials science is the study of the relationships

between the structures and properties of materials.

• Materials engineering is the design or engineering of

a material to produce the desired properties.

Components of materials engineering:

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 Fundamental Principle of Material Science

• Structure, processing, and properties are interrelated

Structure

Processing Properties

28
The Structure of Crystalline Solids

• How do atoms assemble into solid structures?

• How does the density of a material depend on

its structure?

• When do material properties vary with the

sample (i.e., part) orientation?

29
 Energy and Packing
• Non dense, random packing Energy

typical neighbor
bond length

typical neighbor r
bond energy

• Dense, ordered packing Energy

typical neighbor
bond length

typical neighbor r
bond energy

Dense, ordered packed structures tend to have lower energies.

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 Materials and Packing
Crystalline materials...
• atoms pack in periodic, 3D arrays
• typical of: -metals
-many ceramics
-some polymers crystalline SiO2

Si Oxygen
Noncrystalline materials...
• atoms have no periodic packing
• occurs for: -complex structures
-rapid cooling
"Amorphous" = Noncrystalline noncrystalline SiO2

31
 Metallic Crystal Structures
• How can we stack metal atoms to minimize empty
space?
2-dimensions

vs.

Now stack these 2-D layers to make 3-D structures

32
 Metallic Crystal Structures

• Tend to be densely packed.

• Reasons for dense packing:
- Typically, only one element is present, so all atomic
radii are the same.
- Metallic bonding is not directional.
- Nearest neighbor distances tend to be small in
order to lower bond energy.
- Electron cloud shields cores from each other
• Have the simplest crystal structures.

We will examine three such structures...

33
 Simple Cubic Structure (SC)
• Rare due to low packing density (only Po has this structure)
• Close-packed directions are cube edges.

• Coordination # = 6
(# nearest neighbors)

34
 Atomic Packing Factor (APF)

Volume of atoms in unit cell*

APF =
Volume of unit cell
*assume hard spheres
• APF for a simple cubic structure = 0.52
volume
atoms atom
4
a unit cell 1 p (0.5a) 3
3
R=0.5a APF =
a3 volume
close-packed directions
unit cell
contains 8 x 1/8 =
1 atom/unit cell
35
 Body Centered Cubic Structure (BCC)

• Atoms touch each other along cube diagonals.

--Note: All atoms are identical; the center atom is shaded
differently only for ease of viewing.

ex: Cr, W, Fe (), Tantalum, Molybdenum

• Coordination # = 8

Adapted from Fig. 3.2,

Callister & Rethwisch 8e.

2 atoms/unit cell: 1 center + 8 corners x 1/8

36
 Atomic Packing Factor: BCC
• APF for a body-centered cubic structure = 0.68
3a

2a

Close-packed directions:
R length = 4R = 3 a
a
atoms volume
4
unit cell 2 p ( 3a/4 ) 3
3 atom
APF =
volume
a3
unit cell
37
 Face Centered Cubic Structure (FCC)

• Atoms touch each other along face diagonals.

--Note: All atoms are identical; the face-centered atoms are shaded
differently only for ease of viewing.

ex: Al, Cu, Au, Pb, Ni, Pt, Ag

• Coordination # = 12

4 atoms/unit cell: 6 face x 1/2 + 8 corners x 1/8

38
 Atomic Packing Factor: FCC
• APF for a face-centered cubic structure = 0.74
maximum achievable APF
Close-packed directions:
length = 4R = 2 a
2a
Unit cell contains:
6 x 1/2 + 8 x 1/8
= 4 atoms/unit cell
a
atoms volume
4
unit cell 4 p ( 2a/4 ) 3
3 atom
APF =
volume
a3
unit cell
39
 FCC Stacking Sequence
• ABCABC... Stacking Sequence
• 2D Projection
B B
C
A
A sites B B B
C C
B sites B B
C sites

A
• FCC Unit Cell B
C

40
Hexagonal Close-Packed Structure (HCP)

• ABAB... Stacking Sequence

• 3D Projection • 2D Projection

A sites Top layer

c
B sites Middle layer

A sites Bottom layer

a

• Coordination # = 12 6 atoms/unit cell

• APF = 0.74 ex: Cd, Mg, Ti, Zn
• c/a = 1.633
41
 Theoretical Density

Mass of Atoms in Unit Cell

Density =  =
Total Volume of Unit Cell

nA
 =
VC NA

where n = number of atoms/unit cell

A = atomic weight
VC = Volume of unit cell = a3 for cubic
NA = Avogadro’s number
= 6.022 x 1023 atoms/mol

42
 Theoretical Density

• Ex: Cr (BCC)
A = 52.00 g/mol
R = 0.125 nm
n = 2 atoms/unit cell

R a = 4R/ 3 = 0.2887 nm
a
atoms
g
unit cell 2 52.00 theoretical = 7.18 g/cm3
mol
= actual = 7.19 g/cm3
a3 6.022 x 1023 atoms
volume
unit cell mol
43
 Densities of Material Classes
In general Graphite/
metals > ceramics > polymers
Metals/ Composites/
Ceramics/ Polymers
Alloys fibers
Semicond
30
Why? Platinum *GFRE, CFRE, & AFRE are Glass,
20 Gold, W
Metals have... Tantalum Carbon, & Aramid Fiber-Reinforced
Epoxy composites (values based on
• close-packing 60% volume fraction of aligned fibers
10 Silver, Mo in an epoxy matrix).
(metallic bonding) Cu,Ni
Steels
• often large atomic masses Tin, Zinc
Zirconia

 (g/cm 3)
5
Ceramics have... 4
Titanium
Al oxide
• less dense packing 3
Diamond
Si nitride
Aluminum
• often lighter elements Glass -soda
Concrete
Silicon PTFE
Glass fibers
GFRE*
2 Carbon fibers
Polymers have... Magnesium G raphite
Silicone CFRE *
Aramid fibers
PVC
• low packing density PET
PC
AFRE *
1 HDPE, PS
(often amorphous) PP, LDPE
• lighter elements (C,H,O)
0.5
Composites have... 0.4
Wood

• intermediate values 0.3

44
What are some general categories of properties
of engineering materials?

• Mechanical
• Electrical
• Thermal
• Magnetic
• Optical

45
 The Materials Selection Process

1. Pick Application Determine required Properties

Properties: mechanical, electrical, thermal,
magnetic, optical, deteriorative.

2. Properties Identify candidate Material(s)

Material: structure, composition.

3. Material Identify required Processing

Processing: changes structure and overall shape
ex: casting, sintering, vapor deposition, doping
forming, joining, annealing.

46
 Electrical Properties
• Electrical Resistivity of Copper:
6
5
Resistivity, ρ
(10-8 Ohm-m)

4
3
2
1
0
-200 -100 0 T (°C)
• Adding “impurity” atoms to Cu increases resistivity.
• Deforming Cu increases resistivity.
47
 Thermal Properties

• Space Shuttle Tiles: • Thermal Conductivity

-- Silica fiber insulation of Copper:
offers low heat conduction. -- It decreases when
you add zinc!

400

Thermal Conductivity
300

(W/m-K)
200

100
0
0 10 20 30 40
Composition (wt% Zinc)

48
 Magnetic Properties

• Magnetic Storage: • Magnetic Permeability

-- Recording medium vs. Composition:
is magnetized by -- Adding 3 atomic % Si
recording head. makes Fe a better
recording medium!

Fe+3%Si

Magnetization
Fe

Magnetic Field

49
 Optical Properties
• Transmittance:
o Aluminum oxide may be transparent, translucent, or opaque
depending on the material’s structure (i.e., single crystal vs.
polycrystal, and degree of porosity).
Polycrystal: Polycrystal:
Single Crystal No Porosity Some Porosity

50
Deformation & Strengthening Mechanisms
• Materials experience two kinds of deformation:
1. Elastic deformation
2. Plastic deformation
• Elastic deformation:
o involves temporary stretching or bending of the bonds between atoms, but
the atoms do not slip past each other.
• Plastic deformation:
o Permanent deformation; strength and hardness are measures of a
material’s resistance to this deformation.
o On a microscopic scale, plastic deformation corresponds to the net
movement of large numbers of atoms in response to an applied stress.
o During this process, interatomic bonds must be ruptured and then
reformed.
o In crystalline solids, plastic deformation most often involves the motion of
dislocations, linear crystalline defects

51
 Dislocation Motion in Materials

• Metals (Cu, Al):

+ + + + + + + +
Dislocation motion easiest + + + + + + + +
- non-directional bonding + + + + + + + +
- close-packed directions ion cores
electron cloud
for slip
• Covalent Ceramics (Si, diamond):
Motion difficult
- directional (angular) bonding

• Ionic Ceramics (NaCl):

+ - + - + - +
Motion difficult
- + - + - + -
- need to avoid nearest
neighbours of like sign (- and +) + - + - + - +

52
 Dislocation Motion & Plastic Deformation
• Metals – plastic deformation occurs by slip – an edge
dislocation (extra half-plane of atoms) slides over adjacent
plane half-planes of atoms.

• If dislocations can't move,

plastic deformation doesn't occur!
53
 Dislocation Motion
• A dislocation moves along a slip plane in a slip direction
perpendicular to the dislocation line
• The slip direction is the same as the Burgers vector direction

Edge dislocation

screw dislocation

54
Deformation Mechanisms
Slip System
– Slip Plane - plane on which easiest slippage occurs
• Highest planar densities (and large interplanar spacings)
– Slip Directions - directions of movement
• Highest linear densities

– FCC Slip occurs on {111} planes (close-packed) in <110>

directions (close-packed)
=> total of 12 slip systems in FCC
– For BCC & HCP there are other slip systems.
55
 Stress and Dislocation Motion
• Resolved shear stress, 𝜏𝑅
– results from applied tensile stresses
Applied tensile Resolved shear Relation between
stress: σ = F/A stress: τR = Fs /A s σ and τR
F slip plane τR = FS /AS
A τR
normal, ns
AS F cos λ A /cos ϕ
FS
F nS ϕ
λ
A
τR FS AS
F

 R   cos  cos 
56
 Critical Resolved Shear Stress
• Condition for dislocation motion:  R   CRSS
• Ease of dislocation motion depends typically
on crystallographic orientation
10-4 GPa to 10-2 GPa
 R   cos  cos 
σ σ σ

τR = 0 τR = σ /2 τR = 0
λ = 90° λ = 45° ϕ = 90°
ϕ = 45°

 maximum at  =  = 45º
57
Single Crystal Slip

58
 Example: Deformation of single crystal
a) Will the single crystal yield?
b) If not, what stress is needed?
 = 60°
τcrss = 20.7 MPa
 = 35°

  (45 MPa) (cos 35 )(cos 60 )

 (45 MPa) (0.41)
  18.4 MPa   crss  20.7 MPa
σ = 45 MPa
So the applied stress of 45 MPa will not cause the crystal to
yield.
59
 Example: Deformation of single crystal

What stress is necessary (i.e., what is the yield

stress, σy)?

 crss  20.7 MPa   y cos  cos    y (0.41)

 crss 20.7 MPa

 y    50.5 MPa
cos  cos  0.41

So for deformation to occur the applied stress must be

greater than or equal to the yield stress.

   y  50.5 MPa

60
 Four Strategies for Strengthening:
1: Reduce Grain Size

• Grain boundaries are barriers to slip.

• Barrier "strength“ increases with
increasing angle of misorientation.
• Smaller grain size: more barriers to
slip.

Hall-Petch Equation:  yield   0  k y d 1/ 2

61
Four Strategies for Strengthening:
2: Form Solid Solutions

• Impurity atoms distort the lattice & generate lattice strains.

• These strains can act as barriers to dislocation motion.
• Smaller substitutional • Larger substitutional
impurity impurity

A C

B D

Impurity generates local stress at A and Impurity generates local stress at C and
B that opposes dislocation motion to the D that opposes dislocation motion to the
right. right.

62
Lattice Strains Around Dislocations

63
 Example: Solid Solution Strengthening in Copper

• Tensile strength & yield strength increase with wt% Ni.

180
Tensile strength (MPa)

Yield strength (MPa)

400
120
300

200 60
0 10 20 30 40 50 0 10 20 30 40 50
wt.% Ni, (Concentration C) wt.%Ni, (Concentration C)

• Empirical relation:  y ~ C 1/ 2
• Alloying increases σy and TS.

64
Four Strategies for Strengthening:
3: Precipitation Strengthening

• Hard precipitates are difficult to shear.

Example: Ceramics in metals (SiC in Iron or Aluminium).
precipitate
Large shear stress needed
Side View to move dislocation toward
precipitate and shear it.

Unslipped part of slip plane Dislocation

Top View
“advances” but
precipitates act as
S “pinning” sites with
spacing S .
Slipped part of slip plane

1
• Result:  y~
S

65
Four Strategies for Strengthening:
4: Cold Work (Strain Hardening)

• Deformation at room temperature (for most metals).

• Common forming operations reduce the cross-sectional area:

-Forging force -Rolling

roll
die Ad
A o blank Ad Ao
roll

-Drawing force -Extrusion

Ao
die Ad container die holder
Ao tensile force
force ram billet extrusion Ad
die container die
Ao  Ad
%CW  x 100
Ao
66
Dislocation Structures Change During Cold Working

• Dislocation structure in Ti after cold working.

• Dislocations entangle
with one another
during cold work.
• Dislocation motion
becomes more difficult.

67
Fundamentals of Materials Characterization

• Definition of Material Characterization:

“Characterization describes those features of a composition
and structure (including defects) of a material that are
significant for a particular preparation, study of properties, or
use, and suffice for the reproduction of the material”
• Two main aspects of the material characterization:
 Accurately measuring the physical and chemical properties of materials.
 Accurately measuring (determining) the structure of a material (Atomic
level structure and microscopic level structure)
• Mechanical, electrical, magnetic and optical properties of a
material are strongly dependent on its structural characteristics.

68
Sample Preparation in Characterization

• Preliminary (and important) step in material characterization

• Before samples can be analysed using advanced scientific
equipment and instruments, they must be properly treated and
prepared.
• It is an important stage of the overall analysis process as it helps
to:
o prevent contamination
o improve accuracy
o minimize the risk of results distortion
• Almost always, sample preparation starts with extraction -
isolating a representative piece of material from a larger source.

69
Thank You!

70