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An understanding of

Microstructures

Dr. Y. Ravi Kumar


Metallurgy & Failure Analysis
Laboratory

NTPC Energy Technology Research Alliance


(NETRA), NTPC Limited
Greater Noida
Contents
1. Brief History of Metals
2. Metallurgy of Iron & Steel
3. Phase diagram of Iron – Carbon
4. Classification of Steels & Alloys
5. Metallurgical Laboratory Equipment
6. Microstructure of Steels
Micro constituents of microstructure
Effect of alloying elements
Microstructural degradation
8. RLA & Replicas
9. Failure Analysis Case Studies
Conventional Boiler Materials
Area of Material type Typical spec. Upper limit Guiding
Application for Plates, Temp. deg Reason for
Tubes, Pipes C(Heat Upper Limit
Absorbing
Surface)
Drum C Steel/ Low SA299 425
Alloy Steel
Water walls, C Steel SA192, SA210, 425 Graphitisation
Economiser SA106
Superheater and C ½ Mo steel A209 T1 465 Graphitisation
Reheater
1Cr ½ Mo SA213T11, 565 Oxidation/
SA335P11 corrosion, Flue
gas
2 ¼ Cr 1Mo SA213T22, 580 Oxidation/
SA335P22 corrosion, Flue
gas
18 Cr 8 Ni SA213 TP304 H 704

18 Cr 10 Ni Cb SA213 TP347 H 704

Modified 9Cr SA213T91, 650 ASME code


SA335P91
12%Cr X20CrMoV12 1 700 German Code
Evolution of Four Generations of Ferritic Steels
A Brief History of Metals
METALS
• No substance has been as important
as metal in the development of
human civilization.

• All the great civilizations like


Mesopotamians, Egyptians, Greeks,
Harappans and the Romans have
known metals and have extensively
used them.
FIRST METALS
• Gold, silver, copper,
Sl ELEMENT YEAR iron (from meteors)
No and mercury were
available in their
1 GOLD 6000 BC native states.
2 COPPER 4200 BC • However, the
occurrence of these
3 SILVER 4000 BC metals was not
4 LEAD 3500 BC abundant
5 TIN 1750 BC • Gold and copper
were the first two
6 IRON 1500 BC metals to be used
7 MERCURY 750 BC widely.
Periodic Table
India
• Dates back to ~ 250 BC
• The iron pillar of Delhi, located
in the Qutb complex, is an
important testimony of the
history of metallurgy in the
Indian subcontinent, and of the
history of ferrous metallurgy in
general.
• The pillar is made up of 98%
wrought iron of pure quality, and
is a testament to the high level
of skill achieved by ancient
Indian iron smiths in the
extraction and processing of
iron.
• Seven meters or 22 feet high
and weighing more than six tons
• The pillar was manufactured by
forge welding. The temperatures
required to form such a pillar by
forge welding can only be
achieved by the combustion of
coal.
WOOTZ – Indian Steel
Around 300 BC, under Mauryan rule, Indian
scientists were the first in the world to be smelting
iron with carbon to
make steel, called
Wootz

Wootz steel is characterized by a pattern of bands


or sheets of micro carbides within a tempered
martensite or pearlite matrix. The word wootz may
have been a mis-transcription of wook, an
anglicised version of ukku, the word for steel in
Kannada, Telugu and many other southern Indian
languages
• Something has been said about the chemical excellence
of cast iron in ancient India, and about the high industrial
development of the Gupta times, when India was looked
to, even by Imperial Rome, as the most skilled of the
nations in such chemical industries as dyeing, tanning,
soap-making, glass and cement...
• By the sixth century the Hindus were far ahead of
Europe in industrial chemistry; they were masters of
calcinations, distillation, sublimation, steaming, fixation,
the production of light without heat, the mixing of
anesthetic and soporific powders, and the preparation of
metallic salts, compounds and alloys. The tempering of
steel was brought in ancient India to a perfection
unknown in Europe till our own times; …
• The Moslems took much of this Hindu chemical science
and industry to the Near East and Europe; the secret of
manufacturing "Damascus" blades, for example, was
taken by the Arabs from the Persians, and by the
Persians from India.“
The Story of Civilization I: Our Oriental Heritage by Will Durant
Metallurgy of Iron and Steel
IRON
• Iron is rarely found in its native state
• Archaeological sites in India : -
Malhar, Dadupur, Raja Nala Ka Tila and
Lahuradewa in Uttar Pradesh
• In the early days iron was 5 times more
expensive then gold
• Hematite is the principle ore of iron.

• Symbol for Iron is “Fe” derived


from the latin word “ferrum”. Its
atomic number is 26
Metallurgy of Iron and Steel.
• Steel is the common name for a large
family of iron alloys which are easily
malleable after the molten stage.
• Steels are commonly made from iron
ore, coal, and limestone. When these
raw materials are put into the blast
furnace, the result is a "pig iron"
• Pig iron has a composition of iron,
carbon, manganese, sulfur,
phosphorus, and silicon.
Metallurgy of Iron and Steel.
Fe2O3(s) + 3 CO(g) → 2 Fe(l) + 3 CO2(g)
Metallurgy of Iron and Steel.
• Pig iron is hard and brittle
• It is refined and other elements are added
to strengthen the material
• The steel is next deoxidized by a carbon
and oxygen reaction.
• A strongly deoxidized steel is called
"killed", and a lesser degrees of de-
oxodized steels are called "semi killed",
"capped", and "rimmed".
Steel Making
• Three fundamental changes from pig iron.
– Reduction of the C content.
• 3-4% in pig iron to 0.005-1.5% in steel.
– Removal, through slag formation, of:
• Si, Mn, P (about 1% in pig iron)
• Other minor impurities.
– Addition of alloying elements.
• Cr, Ni, Mn, V, Mo, and W - give the
steel its desired properties.
Iron Carbon
Phase Diagram
IRON-CARBON (Fe-C) PHASE DIAGRAM
• 2 important T(°C)
1600
points 
-Eutectic (A): 1400 L
L    Fe3C +L
1200

1148°C
A L+Fe3C

Fe3C (cementite)
-Eutectoid (B): austenite) R S
    Fe3C 1000  
+
  +Fe3C
800
 B 727°C = Teutectoid

R S
600
+Fe3C
400
0 1 2 3 4 5 6 6.7
(Fe) 0.77 4.30 Co, wt% C
120m
Ceutectoid

Result: Pearlite = Fe3C (cementite-hard)


alternating layers of
 and Fe3C phases. (ferrite-soft)
21
Iron-Carbon Phase
1. Pure iron melts at 1539°C during the rise in
temperature from ambient, it undergoes
several solid phase transformations
a. Starting at room temperature the phase is alpha
iron or ferrite. With less than 0.025% carbon at
temperatures below 894 deg C
b. At 912 degrees C, ferrite transforms to gamma
iron, called austenite. With less than 2% carbon
c. At 1394 degrees C, austenite transforms to delta
iron, which remains until melting occurs at 1539°C
Iron-Carbon Phase
2. Solubility limits of carbon in iron are low in the ferrite
phase – only about 0.022% at 723 deg C. Austenite
can dissolve up to about 2.1 % carbon at 1130 deg
C. The difference in solubility between alpha and
gamma leads to opportunities for strengthening by
heat treatment
3. The eutectoid point is the lowest temperature at
which austenite can exist (722 deg C).
a. Eutectoid – the temperature and composition (0.77 -
0.81% Carbon) at which a single-phase solid goes
directly, on cooling, to a two-phase solid. Steels below
0.77% Carbon are considered hypoeutectoid steels
those above up to 2.1% are considered hypereutectoid
steels.
b. The eutectoid composition of the Iron-Carbon system is
called pearlite.
Iron-Carbon Phase
4. Even without head treatment, the strength of
iron increases dramatically as carbon
content increases, and we enter the region
in which the metal is called steel.
 More precisely, steel is defined as an iron-
carbon alloy containing from 0.02% to 2.1 %
carbon.
5. Another prominent phase in the iron-alloy
system is Fe3C also known as cementite. It
is a metallic compound of iron and carbon
that is hard and brittle Carbon content of
about 6.7%.
Iron-Carbon Phase
6. Above a carbon content of 2.1% up to
about 4% or 5% is defined as cast iron
7. If sufficient time is allowed for cooling of
the austenite
 it will revert completely to pearlite
 however, if the steel is cooled quickly from
the austenite, martensite is formed
 Martensitic steel has Rockwell C hardness of
about 66 and pearlite is very soft in
comparison.
Classification of Steels & Alloys
-Numbering Systems
Some Specifications applicable to Steel
Products and other Metals
Specifications

SAE-AISI Society of Automotive Engineers – American Iron


and Steel Institute
ASTM American Society for Testing and Materials
(UNS) (www.astm.org)
ASME American Society of Mechanical Engineers
MIL U.S. Department of Defense
AMS Aerospace Materials Specification
BS British Standards Institution
(http://www.bsi-global.com/index.xalter)
EN European Committee for Standardization
(http://www.cenorm.be)
The Most Widely Used System
for Designating Steels SAE-AISI
Unified Numbering System (UNS)
• Developed by ASTM and
SAE
• Not a specification but only
identify an alloy covered
by other standards
• The 5 digits closely related
to the original identification
system. E.g. AISI 1020 =
G10200
• Adopted by the Copper
Development Association
as official identification
system for Cu alloys
METALLURGICAL LABORATORY
Laboratory Facilities
Optical Emission Spectrometer (OES)

For testing chemical


analysis of metal
samples

Highly accurate results


Reproducible
Sample Cutting Machines
Sample Preparation
Equipment
Laboratory Facilities
Inverted Metallurgical (Optical) Microscope

For qualitative and quantitative analysis of micro-structure


Optical Microscope Observation
• Use polished and etched
specimens
• Limited depth of field
• Shows individual grain
structure
Micro-hardness Measurement

Hardness on metallographic
samples (Vicker’s)
Scanning Electron Microscope (SEM) &
Energy Dispersive X-ray Analyzer (EDAX)
• Fractography
• Wear debris
analysis
• Morphology /
Topography
• Elemental
analysis

 Metal samples  Magnification : ~1,00,000X


 Coated non-  Heating stage
metal samples  In-situ tensile stage
SEM Image With EDAX Analysis

Element Weight%
• Individual grains C 2.19
• Large depth of O 51.31
Mg 0.69
field Al 10.72
Si 23.68
• Nature of failure: K 0.36
• inter-granular Ca 8.53
Ti 0.37
Fe 1.53
Pd 0.61
Scanning Electron Microscope (SEM) &
Energy Dispersive X-ray Analyzer (EDAX)
MICROSTRUCTURES
OF
STEELS
Microstructure of Steel
Constituents structure Properties Microscope
apperance
Ferrite  - Iron soft and ductile white
bcc
Pearlite alternate layers of Hard and ductile; dark
 + Fe3C ; gives toughness
Austenite  - Iron Soft and ductile white
fcc

Cementite Fe3C hard and brittle white

Bainite Hard Feathery;


 + Fe3C ; dark
Martensite Distorted BCT Hard & brittle Needle
like; dark
Ferrite
The structure of pure iron.

Has a body-centred cubic (BCC) crystal


structure. It is soft and ductile and
imparts these properties to the steel.
Very little carbon (less than 0.01%
carbon will dissolve in ferrite at room
temperature). Often known as  iron.
Photomicrograph
of 0.1% carbon
steel (mild steel).
The light areas
are ferrite.

Ferrite Microstructure
Austenite
This is the structure of iron at high
temperatures (over 912 deg C).
Has a face-centre cubic (FCC) crystal
structure. This material is important in
that it is the structure from which other
structures are formed when the material
cools from elevated temperatures.
Often known as  iron. Not present at
room temperatures.
Austenite Structure
Cementite
A compound of iron and carbon, iron
carbide (Fe3C).

It is hard and brittle and its presence in


steels causes an increase in hardness
and a reduction in ductility and
toughness.
Pearlite
A laminated structure formed of
alternate layers of ferrite and cementite.

It combines the hardness and strength


of cementite with the ductility of ferrite
and is the key to the wide range of the
properties of steels. The laminar
structure also acts as a barrier to crack
movement as in composites. This gives
it toughness.
Pearlite Microstructure

Two-dimensional view of pearlite, consisting


of alternating layers of cementite and ferrite.
Martensite
A very hard needle-like structure of iron
and carbon.
Only formed by very rapid cooling from
the austenitic structure (i.e. above
upper critical temperature). Needs to
be modified by tempering before
acceptable properties are reached.
The needle-like
structure of
martensite, the
white areas are
retained
austenite.

Martensite Microstructure
50 m
Martensite Microstructure
Bainite

Bainite formed at 348oC and at 278oC


 →  + Fe3C**
 Nucleation and growth
 Acicular, accompanied by surface distortions
** Lower temperature →
carbide could be ε carbide (hexagonal structure, 8.4% C)
 Bainite plates have irrational habit planes
 Ferrite in Bainite plates possess different orientation relationship
relative to the parent Austenite than does the Ferrite in Pearlite
Martensite Transformation
 The martensitic transformation occurs without composition change
 The transformation occurs by shear without need for diffusion
 The atomic movements required are only a fraction of the
interatomic spacing
 The shear changes the shape of the transforming region
→ results in considerable amount of shear energy
→ plate-like shape of Martensite
 The amount of martensite formed is a function of the temperature
to which the sample is quenched and not of time
 Hardness of martensite is a function of the carbon content
→ but high hardness steel is very brittle as martensite is brittle
 Steel is reheated to increase its ductility - process is called
TEMPERING
Effect of Carbon Content
In steels none of the carbon is present
as free carbon. It is all dissolved in the
iron as part of the previously described
structures.
Increasing the carbon content
decreases the amount of ferrite and
increases the proportion of pearlite in
the structure.
0.1% Carbon Steel 0.2%

Note the increased amount of pearlite


compared with the 0.1% ‘dead mild’ steel
60
Hardness (Rc) →

Hardness of Martensite as a
40 function of Carbon content

20 % Carbon →
Properties of 0.8% C steel
0.2 0.4 0.6
Constituent Hardness (Rc) Tensile strength
(MN / m2)
Coarse pearlite 16 710
Fine pearlite 30 990
Bainite 45 1470
Martensite 65 -
Martensite tempered 55 1990
at 250oC
EFFECTS OF ALLOYING
ELEMENTS
Effects of Alloying Elements
Typical Principle Effects
ranges (%)
Al <2 Aids nitriding, grain refining,
removes O in steel melting
S, P <0.5 Adds machinability, reduces
weldability, ductility and
toughness
Cr 0.3-4 Increases corrosion resistance,
hardenability, high-T strength;
form hard wear resistant carbide
Effects of Alloying Elements
Typical Principle Effects
ranges (%)
Ni 0.3-5 Austenite former, increase
hardenability and toughness
Cu 0.2-0.5 Aid atmospheric corrosion
resistance
Mn 0.3-2 Austenite former, increase
hardenability; combine with S to
reduce its adverse effects

Si 0.2-2.5 Removes O in steel making,


increase hardenability and
toughness
Effects of Alloying Elements
Typical ranges Principle Effects
(%)
Mo 0.1-0.5 Grain refinement, increases
hardenability, high-T strength
V 0.1-0.3 Grain refinement, increases
hardenability, form wear-resistant
carbide
B 0.0005-0.003 Increase hardenability
Pb <0.3 Aid machinability
N <0.1 Acts like C in strengthening
ALLOYING STEEL WITH MORE ELEMENTS

• Teutectoid changes: • Ceutectoid changes:

Ceutectoid (wt%C)
0.8

0.6 Ni
Cr
0.4
TEutectoid (°C)

1200 Ti Si Si
Mo W Mn
0.2 W
1000 Ti Mo
Cr 0
800 0 4 8 12
Mn wt. % of alloying elements
600 Ni
0 4 8 12
wt. % of alloying elements
24
MORE MICROSTRUCTURES
Carbon Steel
Banded structure
Bainite
Structure
Martensite structure
Austenite Structure
Graphitisation
Sensitized microstructure
Sensitisation
Creep
Damage
Oxide filled crack
Internal Surface Oxide scale
Oxide Scale
Thermal Fatigue cracks
Copper particles in Internal deposit
IPW DMW Joint
Corrosion pits
Corrosion pit
Weld Pores
Remaining Life Assessment
(RLA)
VISUAL INSPECTION HARDNESS MEASUREMENT
-Dimension Portable Hardness Testers
-Documentation -Rebound technique
-Ultrasound technique
NDT TECHNIQUES
-Ultrasonic Test MECHANICAL
-DPT MEASUREMENT
-MPI, etc RLA -Portable ball indentation
-Small punch testing

CHEMICAL ANALYSIS MICROSTRUCTURE


CHARACTERIZATION
XRF ANALYZER ACCURACY -Optical
REPEATABILITY -SEM
RELIABILITY
SKILL
INTERPRETATION
Thermal degradation Index in Alloy
Steels - Qualitative
• Spheroidization tendency of pearlite /
bainite in alloy steels
• Coarsening of particles in ferrite matrix
and grain boundaries
• Broadening of de-nuded zones (no
precipitates) along grain boundaries
• One or more of the above is an indication
of overheating exposure
Neubauer schematic assessment of the microstructure
Grade of Structural Evolution observed by metallography
Evolution
0 Normal microstructure for new component

1 Normal micro for service conditions; incipient or advanced


microstructure transformation or precipitation
2 a) Chain shaped oriented carbides on grain boundaries
b) Isolated micro-pores (cavities on grain boundaries)
irregularly distributed
c) Few micropores irregularly distributed
3 Incipient creep damage
a) Micro-pores orientation
b) Grain boundaries separation
4 Advanced creep damage micro-cracks identifiable

5 Structural loosening (grain dis-integration)


Macro cracks (length in millimeter range)
Simplified Neubauer classification
(ISPESL)
2 Presence of isolated 3 Directionally oriented
micro- cavities micro- cavities
5 Presence of macro- cracks

4 Presence of micro- cracks


VGB Guidelines Classification
ISPESL – Classification of
microstructure evolution

LEVEL A LEVEL B LEVEL C

LEVEL D LEVEL E LEVEL F


Creep Damage Classification
Comparison of Hardness Measurements
ASTM MEASURE
TEST TEST METHOD TEST FORCE INDENTER TYPE METHOD METHOD
ROCKWELL REGULAR 60,100,150 Kgs CD & SB E 18 DEPTH
SUPERFICIAL 15,30,45 Kgs CD & SB E 18 DEPTH
LIGHT LOAD 3,5,7 Kgs T- CD N/A DEPTH
MICRO 500, 100 grams SMALL TA - CD N/A DEPTH
MACRO 500 TO 3000 Kgs 5MM, 10MM BALL E 103 DEPTH
MICRO- 136° PYRAMID
HARDNESS VICKERS 5 TO 2000 grams DIAMOND E 384 AREA
1300 X 1720°
KNOOP 5 TO 2000 grams DIAMOND E 384 AREA
ROCKWELL
TYPE 500, 3000 grams T- CD N/A DEPTH
DYNAMIC 0.01 TO 200 gramsTA-DIAMOND N/A DEPTH
BRINELL OPTICAL 500 TO 3000 Kgs 5MM, 10MM BALL E 10 AREA
DEPTH 500 TO 3000 Kgs 5MM, 10MM BALL E 103 DEPTH

CONICAL DIAMOND (CD) & SMALL BALL (SB); TRUNCATED (T); TRIANGULAR (TA)
THANK YOU