Unit 4 MSE Heat Treatment of Metals

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Introduction

Prof. A.V.Dube
Most of the images are
courtesy of the book

“ Manufacturing
Engineering and
Technology” by Serope
Kalpakjian, Steven Schmid.

“Material Science and Engg.


an Introduction” by
William D. Callister, Jr. &
David G. Rethwisch.

Few were adopted from “Fundamentals of Modern


Manufacturing: Materials, Processes, and Systems” by
Mikell P Groover

Images collected from Wikipedia and google images were also used.
Basic Concepts
• Alloy
• A metal made by combining two or more elements, at least one of which is metallic.
Basic Concepts
• Alloy
• A metal made by combining two or more elements, at least one of which is metallic.
• categories of alloys are
• Solid solutions and
• Intermediate phases.

• Solid Solution: one element is dissolved in another to form a single-phase structure.


Phase diagram
Phase : A region of material having uniform physical and chemical properties

• Solid phase: represented by α, β, ϒ, δ etc


• Liquid phase : represented by L
Equilibrium phase diagram- Complete solid solubility
• Nickel and Copper form a complete solid solution
• Nickel’s melting point : 1453⁰C
• Copper’s melting point : 1084⁰C

Two phase region

Single liquid phase region • Solid phase: represented by α, β, ϒ, δ etc


• Liquid phase : represented by L

Single solid phase region


Equilibrium phase diagram- Complete solid solubility
• Nickel and Copper form a complete solid solution
• Nickel’s melting point : 1453⁰C
• Copper’s melting point : 1084⁰C
Liquid phase
Two phase region

Single liquid phase region

Single solid phase region


Equilibrium phase diagram- Complete solid solubility
• Nickel and Copper form a complete solid solution
• Nickel’s melting point : 1453⁰C
• Copper’s melting point : 1084⁰C
Liquid phase
Two phase region

Single liquid phase region


Solid +Liquid
phase

Single solid phase region


Equilibrium phase diagram- Complete solid solubility
• Nickel and Copper form a complete solid solution
• Nickel’s melting point : 1453⁰C
• Copper’s melting point : 1084⁰C
Liquid phase
Two phase region

Single liquid phase region


Solid +Liquid
phase

Single solid phase region

Solid phase
Equilibrium phase diagram- Complete solid solubility
• Nickel and Copper form a complete solid solution
• Nickel’s melting point : 1453⁰C
• Copper’s melting point : 1084⁰C
Liquid phase
Two phase region

60 % Ni 40% Cu
Single liquid phase region

Single solid phase region


Single liquid phase region

Single solid phase region

Cl Cα
Single liquid phase region

53% Liquid of Ni, 47% of Cu


68% solid of Ni, 32% of Cu

Single solid phase region

Cl Cα
Single liquid phase region

Single solid phase region


Single liquid phase region

60% of Ni, 40% Cu

Single solid phase region


The Tin–Lead Alloy System
α and β: solid phase 327⁰C
232⁰C/
Eutectic temperature: 183⁰C / 362 ⁰C 449⁰F

Lead Tin
The Tin–Lead Alloy System
The Liquid
Tin–Lead Alloy System
Liquid
10 wt% of Sn
The Tin–Lead Alloy System

10
Liquid
10 wt% of Sn
The Tin–Lead Alloy System
α+ L
7 wt% Sn

10
Liquid
10 wt% of Sn
The Tin–Lead Alloy System
α+ L
7 wt% Sn

α
10 wt% Sn

10
Liquid
10 wt% of Sn
The Tin–Lead Alloy System
α+ L
7 wt% Sn

α
10 wt% Sn

α+ β
β

10
The Tin–Lead Alloy System
Liquid
The
LiquidTin–Lead Alloy System
40% wt of Sn
60% wt of Pb
The
Liquid
Tin–Lead Alloy System
40% wt of Sn
60% wt of Pb

α+ L
The
Liquid
Tin–Lead Alloy System
40% wt of Sn
60% wt of Pb

α+ L
α : 18% wt of Sn & 82% wt of Pb
L : 58 % wt of Sn & 62 % wt of Pb

CL

The
Liquid
Tin–Lead Alloy System
40% wt of Sn
60% wt of Pb

α+ L

α : 18% wt of Sn & 82% wt of Pb


L : 50 % wt of Sn & 50 % wt of Pb

α+ β
α : 8% wt of Sn
β : 92% wt of Pb
Cα CL
The
Liquid
Tin–Lead Alloy System
40% wt of Sn
60% wt of Pb

α+ L

α : 18% wt of Sn & 82% wt of Pb


L : 50 % wt of Sn & 50 % wt of Pb

α+ β
α : 8% wt of Sn
β : 92% wt of Pb
Cα CL
DEVELOPMENT OF MICROSTRUCTURE
The Iron Carbon System
Ferrite: α Ferrite is a solid solution of Body Centered Cubic (BCC) iron,
• Relatively soft and ductile
• Magnetic from room temperature to 768⁰C,
• Maximum solid solubility of 0.022% C at a temperature of 727◦C
Austenite: γ –iron: FCC structure
• Denser than ferrite
• Solid solubility of up to 2.11%Cat 1148◦C.
• Single-phase FCC structure is ductile at elevated temperatures
• Non magentic

Cementite: 100 % Fe3C : carbon content 6.67%


• Hard and brittle
The Iron Carbon System
Ferrite: α Ferrite is a solid solution of Body Centered Cubic (BCC) iron,
• Relatively soft and ductile
• Magnetic from room temperature to 768⁰C,
• Maximum solid solubility of 0.022% C at a temperature of 727◦C
Austenite: γ –iron: FCC structure
• Denser than ferrite
• Solid solubility of up to 2.11%Cat 1148◦C.
• Single-phase FCC structure is ductile at elevated temperatures
• Non magentic

Cementite: 100 % Fe3C : carbon content 6.67%


• Hard and brittle
The Iron Carbon System A4
Ferrite:α Ferrite is a solid solution of Body Centered Cubic (BCC) iron, δ
• Relatively soft and ductile
• Magnetic from room temperature to 768⁰C,
Austenite: γ –iron: FCC structure
• Denser than ferrite
• Single-phase FCC structure is ductile at elevated
temperatures
• Non magentic
Cementite: 100 % Fe3C : carbon content 6.67%
• Hard and brittle

A3

A1
A2
The
Ferrite:
Iron Carbon System
α Ferrite is a solid solution of Body Centered Cubic (BCC) iron,
Austenite: γ –iron: FCC structure

900⁰ ϒ Austenite
C

α+ϒ

Ferrite + ϒ + Fe3 C
A Hypoeutectoid steel, As the temperature drops, the precipitation of Austenite Austenite + Cementite
ferrite increases progressively, and the amount of the remaining austenite
727⁰C
decreases progressively its carbon content being increased. α

ϒ + Fe3 C

Pearlite with excess ferrite Pearlite with excess cementite

0.2 0.8 2

Carbon wt %
The Iron Carbon System
Ferrite: α Ferrite is a solid solution of Body Centered Cubic (BCC) iron, γ
Austenite: γ –iron: FCC structure

A eutectoid steel, when cooled at very slow rates from temperatures within the Eutectoid Point
austenitic field, undergoes no change until at eutectoid temperature is reached, then
pearlite is formed

Eutectoid Temp.
𝛾 ⇌ 𝛼 (0.022 wt% C) + Fe3C

Pearlite

0.8
Heat Treatment

Fe3 C Hard & Brittle Fe3 C Hard


α soft & ductile

Steel Hardness Wt % C Microstructure Heat


HRC
Treatment
A 15 0.8 Coarse Pearlite
Annealing
B 30 0.8 Fine Pearlite
Normalizing
C 45 0.8 Bainite
Austempering
D 55 0.8 Tempered
Martensite Tempering

E 65 0.8 Martensite
Quenching
Heat Treatment of
Metal
Prof. A.V.Dube
This Photo by Unknown Author is licensed under CC BY-SA
Assignment
• You have to prepare a notes based on class lectures
• Open book questions will be given.

No readymade notes will be given.


What are you going to learn?
• Purpose of heat treatment
• Design parameters of heat treatment
• Heat treatment process
This Photo by Unknown Author is licensed under CC BY-SA
Heat Treatment
Temperature

5
3 2 1
4

Time

1 Annealing Slow Cooling (Furnace) Coarse Pearlite

2 Normalizing Faster Cooling (Air) Fine Pearlite

3 Austempering Interrupted Quench Bainite

Tempering Heating after Quench Tempered Martensite


4
5 Quenching Fast Cooling (Water) Martensite
900⁰C ϒ Austenite

α+ϒ
Ferrite + Austenite ϒ + Fe3 C
Austenite + Cementite
727⁰C
α
α + Fe3 C

Pearlite with excess ferrite Pearlite with excess cementite

0.2 Hypoeutectoid steel 0.8 Hyper eutectoid steel 2


Carbon wt %
The Fe-C phase diagram- at equilibrium
ϒ Austenite
• Equilibrium transformation are driven by diffusion 900⁰
C
of atoms

• Microstructure transformation depends on time α+ϒ

Ferrite + ϒ + Fe3 C
Austenite Austenite + Cementite
727⁰C
α

ϒ + Fe3 C

Pearlite with excess ferrite Pearlite with excess cementite

0.2 0.8 2

Carbon wt %
900⁰ ϒ Austenite
C

α+ϒ

Ferrite + ϒ + Fe3 C
Austenite Austenite + Cementite
727⁰C
α

α + Fe3 C

Pearlite with excess ferrite Pearlite with excess cementite

0.2 0.8 2

Carbon wt %
The Fe-C phase diagram- at equilibrium
• Microstructure transformation depends on time Austenite ϒ

Coarse Pearlite Fine Pearlite

Annealing Normalizing

Slow Cooling Fast Cooling


(Furnace cooling) (air cooling)
Non equilibrium phases and steel microstructure

Austenite ϒ

Moderate Rapid
Slow Cool Quench
Cool

Martensite
Pearlite Bainite (BCT phase,
(α+ Fe3C layer) (α+ Fe3C needles) diffusionless
transformation)

Martensite is time independent

Microstructures in a eutectoid steel: (a) Pearlite formed at 720 °C; (b) bainite formed at 290 °C; (c) bainite formed at 180 °C; (d) martensite.

M.J. Peet, 6 - Bainitic steels and alloys for power plants, Editor(s): Amir Shirzadi, Susan Jackson, In Woodhead Publishing Series in Energy, Structural Alloys for Power Plants, Woodhead Publishing, 2014, Pages 153-187, ISBN 9780857092380,
Non equilibrium phases and steel microstructure

Austenite ϒ

Moderate Rapid
Slow Cool Quench
Cool

Martensite
Pearlite Bainite (BCT phase,
(α+ Fe3C layer) (α+ Fe3C needles) diffusionless
transformation)
Reheat

Spheroidite

Microstructures in a eutectoid steel: (a) Pearlite formed at 720 °C; (b) bainite formed at 290 °C; (c) bainite formed at 180 °C; (d) martensite.

M.J. Peet, 6 - Bainitic steels and alloys for power plants, Editor(s): Amir Shirzadi, Susan Jackson, In Woodhead Publishing Series in Energy, Structural Alloys for Power Plants, Woodhead Publishing, 2014, Pages 153-187, ISBN 9780857092380,
Non equilibrium phases and steel microstructure

Austenite ϒ

Moderate Rapid
Slow Cool Quench
Cool

Martensite
Pearlite Bainite (BCT phase,
(α+ Fe3C layer) (α+ Fe3C needles) diffusionless
transformation)
Reheat
Reheat
Spheroidite
Microstructures in a eutectoid steel: (a) Pearlite formed at
720 °C; (b) bainite formed at 290 °C; (c) bainite formed at Tempered Martensite
180 °C; (d) martensite.
(α+ very fine Fe3C
particle)

M.J. Peet, 6 - Bainitic steels and alloys for power plants, Editor(s): Amir Shirzadi, Susan Jackson, In Woodhead Publishing Series in Energy, Structural Alloys for Power Plants, Woodhead Publishing, 2014, Pages 153-187, ISBN 9780857092380,
Non equilibrium phases and steel microstructure

Microstructure Phases present Arrangement of phases Mechanical properties (relative)


Spheriodite α+Fe3C Relatively small Fe3C spherelike High toughness, lower hardness than pearlite,
particles in an 𝛼-ferrite matrix prevent cracking, used in cold work

Coarse pearlite α+Fe3C Alternating layers of 𝛼-ferrite Harder and stronger than
and Fe3C that are relatively spheroidite, but not as ductile
thick as spheroidite

Fine pearlite α+Fe3C Alternating layers of 𝛼-ferrite Harder and stronger than coarse pearlite, but not as
and Fe3C that are relatively ductile as coarse pearlite
thin

Bainite α+Fe3C Very fine and elongated particles of Harder and stronger than fine
Fe3C in an 𝛼-ferrite matrix pearlite; less hard than
martensite; more ductile than
martensite

Tempered α+Fe3C Very small Fe3C spherelike Strong; not as hard as martensite,
martensite particles in an 𝛼-ferrite matrix but much more ductile than
martensite

Martensite Body-centered, Needle-shaped grains Very hard and very brittle


tetragonal, single
phase

M.J. Peet, 6 - Bainitic steels and alloys for power plants, Editor(s): Amir Shirzadi, Susan Jackson, In Woodhead Publishing Series in Energy, Structural Alloys for Power Plants, Woodhead Publishing, 2014, Pages 153-187, ISBN 9780857092380,
Non equilibrium phases and steel microstructure

Austenite ϒ

Moderate Rapid
Slow Cool Quench
Cool

Martensite
Pearlite Bainite (BCT phase,
(α+ Fe3C layer) (α+ Fe3C needles) diffusionless
transformation)
Reheat
Reheat
Spheroidite

Tempered Martensite
(α+ very fine Fe3C
particle)
Non equilibrium phases and steel microstructure

Austenite ϒ

Moderate Rapid
Slow Cool Quench
Cool

Martensite
Pearlite Bainite (BCT phase,
(α+ Fe3C layer) (α+ Fe3C needles) diffusionless
transformation)

Reheat

Tempered Martensite
(α+ very fine Fe3C
particle)
Time Temperature Transformation Diagram
• For Eutectoid Steel (0.8 wt % C)

900⁰C ϒ Austenite

Stable ϒ
α+ϒ

Ferrite + Austenite ϒ + Fe3 C Unstable ϒ ts Start tf


Austenite + Cementite Finish
727⁰C

Temperature
α Pearlite Pearlite
α + Fe3 C

Pearlite with excess ferrite Pearlite with excess cementite

0.2 0.8 2
Log Time
Carbon wt %
Time Temperature Transformation Diagram
• For Eutectoid Steel (0.8 wt % C)

900⁰ ϒ Austenite
C

Stable ϒ
α+ϒ

Ferrite + ϒ + Fe3 C Unstable ϒ ts Start tf Finish


Austenite Austenite + Cementite
Coarse Annealing
727⁰C
Pearlite

Temperature
α ϒ + Pearlite
Pearlite
ϒ + Fe3 C

Pearlite with excess ferrite Pearlite with excess cementite

0.2 0.8 2
Log Time
Carbon wt %
Annealing
• Process Annealing
• Stress Relief

Process
annealing
Annealing
• Process Annealing
• Stress Relief

Cracking due to internal residual stress

https://www.metallurgyfordummies.com/do-you-know-the-stress-corrosion-cracking.html
Annealing
• Process Annealing
• Stress Relief

Cracking due to internal residual stress

https://www.protoxrd.com/applications/pipelines

Oviedo, Jose & Payer, Joe & Lewandowski, John. (2000). Environmental Assisted Cracking of AISI 305, AISI 410 Stainless Steels and Low Alloy Steel Bolts/Fasteners in Chloride Containing Environments.
Annealing
• Process Annealing
• Stress Relief
• Full Annealing
Annealing
• Process Annealing
• Stress Relief
• Full Annealing
• Spheroidizing
Time Temperature Transformation Diagram
• For Eutectoid Steel (0.8 wt % C)

Stable ϒ Annealing
727⁰C Normalizing
Unstable ϒ ts Start tf Finish
Coarse Pearlite
Temperature

ϒ + Pearlite
Fine Pearlite
Pearlite

Austempering Bainite

Ms Martensite Start
Quench ϒ + Martensite
Mf Martensite Finish
Martensite
Log Time
Austempering
Stable ϒ

727⁰C

Unstable ϒ ts Start tf Finish

Coarse Pearlite
ϒ + Pearlite
Fine Pearlite

Temperature
Pearlite

Austempering
Bainite

Ms Martensite Start
ϒ + Martensite
Mf Martensite Finish
Martensite
Log Time
Time Temperature Transformation Diagram
• For Eutectoid Steel (0.8 wt % C)

Stable ϒ

Unstable ϒ ts Start tf Finish


Coarse Annealing
Pearlite
Temperature

ϒ + Pearlite
Quench Fine Pearlite
Normalizing Pearlite

Ms Martensite Start
ϒ + Martensite
Mf Martensite Finish
Martensite
Log Time
Quenching

The quenching step involves cooling the austenite rapidly


enough so austenite is transformed into martensite.

Same composition as austenite

Austenite : FCC
Martensite BCT

The slower cooling rate reduces the


possibility of hardening defects
Martempering (Marquenching)
• Martempering is a form of heat
treatment applied as an interrupted Stable ϒ
quench of steels typically in a
molten salt bath at a temperature Unstable ϒ ts Start tf Finish
Annealing
right above the martensite start Coarse
Pearlite

Temperature
ϒ + Pearlite
temperature. Fine Pearlite
Pearlite
• The purpose is to delay the cooling
for a length of time to equalise the
temperature throughout the piece.
• This will minimise distortion,
cracking and residual stress. Quench

Log Time
Tempering
• Tempering is a heat treatment applied to
hardened steels to reduce brittleness,
increase ductility and toughness, and
relieve stresses in the martensite structure.

http://threeplanes.net/martensite.html
Pan, L.; Kwok, C.T.; Lo, K.H. Effect of Multiple-Pass Friction Stir Processing on Hardness and Corrosion Resistance of Martensitic Stainless Steel. Coatings 2019, 9, 620. https://doi.org/10.3390/coatings9100620
Patenting
• Patenting of steel wire is a common process
whereby the wire is heated to ∼950°C to
form austenite, and then rapidly quenched in
molten lead held at ∼500°C. The fine-grained
structure so formed.
• This process is conducted with the aim of
obtaining a fine-grained uniform pearlitic
structure which will be susceptible to plastic
deformation in drawing processes
Patenting
• Patenting of steel wire is a common process
whereby the wire is heated to ∼950°C to
form austenite, and then rapidly quenched in
molten lead held at ∼500°C. The fine-grained
structure so formed.
• This process is conducted with the aim of
obtaining a fine-grained uniform pearlitic
structure which will be susceptible to plastic
deformation in drawing processes
TTT Diagram for eutectoid
composition Coarse

Fine

Coarse

Fine

A: Austenite
P: Pearlite
B: Bainite
M: Martensite
TTT Diagram for eutectoid
composition
Specify the nature of the final microstructure (% bainite,
martensite, pearlite etc) for the alloy that is subjected to the
following time–temperature treatments

A: Austenite
P: Pearlite
B: Bainite
M: Martensite
TTT Diagram for eutectoid
composition
Specify the nature of the final microstructure (% bainite,
martensite, pearlite etc) for the alloy that is subjected to the
following time–temperature treatments

50% Pearlite 50% Bainite


50% Martensite
A: Austenite 50% Martensite
P: Pearlite
B: Bainite
M: Martensite
TTT Diagram for eutectoid
composition
Specify the nature of the final microstructure (% bainite, 50% Pearlite
50% Austenite
martensite, pearlite etc) for the alloy that is subjected to the
following time–temperature treatments
50% Pearlite
50% Bainite

50% Pearlite
50% Austenite

50% Pearlite
A: Austenite 50% Bainite
P: Pearlite
B: Bainite
M: Martensite
The Jominy End-Quench Test

Hardenability
• The influence of alloy composition on the
ability of a steel alloy to transform to
martensite for a particular quenching
treatment is related to a parameter called
hardenability.
• The term Hardenability is used to measure
the depth of hardness achieved
Hardenability
Hardenability
Case Hardening
1. Carburizing (gas, liquid, and pack carburizing)
2. Carbonitriding
3. Cyaniding
4. Nitriding
5. Boronizing
6. Flame hardening
7. Induction hardening
8. Laser-beam hardening
Carburizing
• most common surface-hardening treatment
• Heating a part of low carbon steel in the presence of a carbon-rich environment so that C
is diffused into the surface
• the surface is converted to a high carbon steel, capable of higher hardness than the low-C
core
• Methods
• Pack carburizing: use of carbonaceous materials such as charcoal or coke packed in a closed container
with the parts.
• gas carburizing, uses hydrocarbon fuels such as propane (C3H8) inside a sealed furnace to diffuse
carbon into the parts.
• liquid carburizing, which employs a molten salt bath containing sodium cyanide (NaCN), barium
chloride (BaCl2), and other compounds to diffuse carbon into the steel.
• Typical carburizing temperatures are 875° to 925°C (1600°–1700°F), well into the austenite range
Nitriding
• Nitrogen is diffused into the surfaces of special alloy steels to produce a thin hard casing
without quenching
• steel must contain certain alloying ingredients such as aluminum (0.85–1.5%) or
chromium (5% or more) to form nitride compound.
• gas nitriding: steel parts are heated in an atmosphere of ammonia (NH3) or other nitrogen-rich gas
mixture;
• liquid nitriding, in which the parts are dipped in molten cyanide salt baths.
• processes are carried out at around 500°C (950°F)
• Case thicknesses range as low as 0.025 mm (0.001 in) and up to around 0.5 mm (0.020
in), with hardnesses up to HRC 70.
Carbonitriding
• Both carbon and nitrogen are absorbed into the steel surface, usually by heating in a
furnace containing carbon and ammonia.
• Case thickness is usually 0.07 to 0.5 mm (0.003–0.020 in), with hardness comparable with
those of the other two treatments.
Flame hardening
• heating the work surface by means of one or more torches followed by rapid quenching.
• Normally, case depth up to 3mm can be achieved.

https://www.thermexmetal.com/flame-hardening
Induction heating
• application of electromagnetically induced energy supplied by an induction coil to an electrically conductive work part.
• The hardened depth decreases with increasing frequency in induction hardening, the heating time is usually a few seconds.
Immediately after heating water jets are activated to quench the surface
• Martensite is produced at the surface, making it hard and wear resistant.
Influence of Other Alloying Elements
Heat Treatment of Nonferrous Alloys
• Nonferrous alloys and some stainless steels cannot be heat
treated by the techniques described for ferrous alloys.
• Nonferrous alloys do not undergo phase transformations
like those in steels
• PRECIPITATION HARDENING.
• Small particles of a different phase, called precipitates, are
uniformly dispersed in the matrix of the original phase
• Precipitates form because the solid solubility of one element
(one component of the alloy) in the other is exceeded.
Solution heat

• Age Hardening treatment

• Delaying the PRECIPITATION HARDENING time


Precipitation
Age hardening
heat treatment
Relation of Design to Heat Treatment
• Sharp internal or external corners should be avoided, as otherwise stress concentrations at these corners may
raise the level of stresses high enough to cause cracking.
• The part should have its thicknesses as nearly uniform as possible.
• The transition between regions of different thicknesses should be made smooth.
• Parts with holes, grooves, keyways, splines, and asymmetrical shapes may be difficult to heat treat, because they
may crack during quenching.
• Large surfaces with thin cross-sections are likely to warp.
• Hot forgings and hot steel-mill products may have a decarburized skin which may not respond successfully to
heat treatment.
Reading material
• Chapter 4 from Book: “ Manufacturing Engineering and Technology” by Serope
Kalpakjian, Steven Schmid.
• Chapter 10: Section 10.5 onwards, from Book ““Material Science and Engg. an
Introduction” by William D. Callister, Jr. & David G. Rethwisch.
• Chapter 11: Section 11.8 onwards from Book ““Material Science and Engg. an
Introduction” by William D. Callister, Jr. & David G. Rethwisch.
Annealing

Normalizing

Tempering
Uniform coarse pearlite Non -Uniform coarse pearlite

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