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Heat Treatment

R. Manna
AssistantProfessor
CentreofAdvancedStudy
DepartmentofMetallurgicalEngineering
InstituteofTechnology

BanarasHinduUniversity
Varanasi221005,India
rmanna.met@itbhu.ac.in

TataSteelTRAERFFacultyFellowshipVisitingScholar
DepartmentofMaterialsScienceandMetallurgy

UniversityofCambridge

PembrokeStreet,Cambridge,CB23QZ
rm659@cam.ac.uk

HEATTREATMENT
Fundamentals
FeCequilibriumdiagram.Isothermalandcontinuous
coolingtransformationdiagramsforplaincarbonand
alloysteels.Microstructureandmechanicalpropertiesof
pearlite,bainiteandmartensite.Austeniticgrainsize.
Hardenability,itsmeasurementandcontrol.
Processes
Annealing,normalisingandhardeningofsteels,
quenchingmedia,tempering.Homogenisation.
Dimensionalandcompositionalchangesduringheat
treatment.Residualstressesanddecarburisation.

SurfaceHardening
Casecarburising,nitriding,carbonitriding,inductionandflamehardening
processes.
SpecialGradeSteels
Stainlesssteels,highspeedtoolsteels,maragingsteels,highstrengthlow
alloysteels.
Castirons
White,grayandspheroidalgraphiticcastirons
NonferrousMetals
Annealingofcoldworkedmetals.Recovery,recrystallisationandgrain
growth.Heattreatmentofaluminum,copper,magnesium,titaniumand
nickelalloys.Temperdesignationsforaluminumandmagnesiumalloys.
ControlledAtmospheres
Oxidizing,reducingandneutralatmospheres.

SuggestedReading
R.E.ReedHillandR.Abbaschian:PhysicalMetallurgy
Principles,PWS,PublishingCompany,Boston,ThirdEdition.
VijendraSingh:HeattreatmentofMetals,StandardPublishers
Distributors,Delhi.
AnilKumarSinha:PhysicalMetallurgyHandbook,McGrawHill
Publication.
H.K.D.H.BhadeshiaandR.W.K.Honeycombe:Steels
MicrostructureandProperties,ButterworthHeinemann,Third
Edition,2006
R.C.Sharma:PrinciplesofHeatTreatmentofSteels,NewAge
International(P)Ltd.Publisher.
CharlieR.Brooks:HeatTreatment:StructureandPropertiesof
NonferrousAlloys,A.S.M.Publication.
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Definition of heat treatment


Heat treatment is an operation or combination of operations
involving heating at a specific rate, soaking at a temperature
for a period of time and cooling at some specified rate. The
aim is to obtain a desired microstructure to achieve certain
predetermined properties (physical, mechanical, magnetic or
electrical).

Objectives of heat treatment (heat treatment processes)


The major objectives are
to increase strength, harness and wear resistance (bulk
hardening, surface hardening)
to increase ductility and softness (tempering, recrystallization
annealing)
to increase toughness (tempering, recrystallization annealing)
to obtain fine grain size (recrystallization annealing, full
annealing, normalising)
to remove internal stresses induced by differential deformation by
cold working, non-uniform cooling from high temperature during6

toimprovemachineability(fullannealingandnormalising)
toimprovecuttingpropertiesoftoolsteels(hardeningand
tempering)
toimprovesurfaceproperties(surfacehardening,corrosion
resistancestabilisingtreatmentandhightemperature
resistanceprecipitationhardening,surfacetreatment)
toimproveelectricalproperties(recrystallization,tempering,
agehardening)
toimprovemagneticproperties(hardening,phase
transformation)
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Fecementitemetastablephasediagram(Fig.1)consistsof
phasesliquidiron(L),ferrite,oraustenite,ferriteand
Fe3Corcementiteandphasemixtureofpearlite
(interpenetratingbicrystalsofferriteandcementite)(P)and
ledeburite(mixtureofausteniteandcementite)(LB).
Solid phases/phase mixtures are described here.

Fig.1:FeCementitemetastablephasediagram (microstructural)
+L

A5=1495C

0.09

0.53

0.17

1227C

L+I

2.11

910C

A2
=668/
770C

A3
I+

cm

A B

0.77

+CmIII
0.00005

4.30

I+LB

L+CmI

LB+CmI

I(II+CmII)+LB (eu(II
+CmII)+Cmeu)

II+CmII

0.0218
I+ (P(ed P(ed+Cmed)
+CmII
+Cmed)
Pearlite

Temperature, C

1394C

L=liquid, Cm=cementite, LB=ledeburite, =delta ferrite, =


alpha ferrite, = alpha ferrite(0.00005 wt%C) =austenite,
P=pearlite, eu=eutectic, ed=eutectoid, I=primary, II=secondary,
III=tertiary

(P(ed+Cmed)+CmII)+ LB (P(ed+Cmed)
+CmII+Cmeu)

I(+CmIII)+ P( (
(P(ed(ed+CmIII)+Cmed) +CmII)+
ed
ed
(P(ed(ed+C +Cm )+Cm ) LB ((P( ( +Cm )+Cm )
III
ed
ed
ed
III
ed
mIII)+Cmed) +Cm
+Cm
)+Cm
)
II
II
eu

Weight percent carbon

Ledeburite=LB(eu+Ceu)

1539C

LB (eu(II
+CmII)+Cmeu)
+CmI

A4=1147C

F
Cm

LB (P(ed+Cmed)
+CmII)+Cmeu)+CmI

A1=727C

LB ((P(ed(ed+CmIII)
+Cmed) +CmII)+ Cmeu)
+CmI
Ao=210C
6.67
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ferrite:
Interstitial solid solution of carbon in iron of body centred
cubic crystal structure (Fig .2(a)) ( iron ) of higher lattice
parameter (2.89) having solubility limit of 0.09 wt% at
1495C with respect to austenite. The stability of the phase
ranges between 1394-1539C.
Fig.2(a):Crystalstructureofferrite

This is not stable at room temperature in plain carbon steel.


However it can be present at room temperature in alloy steel
speciallyduplexstainlesssteel.

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phase or austenite:
Interstitial solid solution of carbon in iron of face centred cubic
crystal structure (Fig.3(a)) having solubility limit of 2.11 wt% at
1147C with respect to cementite. The stability of the phase ranges
between 727-1495C and solubility ranges 0-0.77 wt%C with respect
to alpha ferrite and 0.77-2.11 wt% C with respect to cementite, at 0 wt
%C the stability ranges from 910-1394C.

Fig.3(a):Crystalstructureofausteniteisshownatright
side.

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Fig.3(b):Polishedsampleheldataustenitisationtemperature.Groovesdevelopattheprioraustenitegrain
boundariesduetothebalancingofsurfacetensionsatgrainjunctionswiththefreesurface.Micrograph
courtesyofSaurabhChatterjee.

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-ferrite:
Interstitial solid solution of carbon in iron of body centred
cubic crystal structure ( iron )(same as Fig. 2(a)) having
solubility limit of 0.0218 wt % C at 727C with respect to
austenite.
The stability of the phase ranges between low temperatures to
910C, and solubility ranges 0.00005 wt % C at room
temperature to 0.0218 wt%C at 727C with respect to
cementite.
There are two morphologies can be observed
under equilibrium transformation or in low under
undercooling condition in low carbon plain carbon
steels. These are intergranular allotriomorphs ()
(Fig. 4-7) or intragranular idiomorphs(I) (Fig. 4,
Fig. 8)
13

Fig.4:Schematicdiagramofgrainboundaryallotriomoph
ferrite,andintragranularidiomorphferrite.

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Fig.5:Anallotriomorphofferriteinasamplewhichispartially
transformedintoandthenquenchedsothattheremaining
undergoesmartensitictransformation.Theallotriomorphgrows
rapidlyalongtheaustenitegrainboundary(whichisaneasy
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diffusionpath)butthickensmoreslowly.

Fig.6:AllotriomorphicferriteinaFe0.4Csteelwhichisslowlycooled;the
remainingdarketchingmicrostructureisfinepearlite.Notethatalthough
someparticlesmightbeidentifiedasidiomorphs,theycouldrepresent
sectionsofallotriomorphs.MicrographcourtesyoftheDOITPOMSproject.
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Fig.7:Theallotriomorphshaveinthisslowlycooledlowcarbonsteelhave
consumedmostoftheaustenitebeforetheremaindertransformsintoasmall
amountofpearlite.MicrographcourtesyoftheDoITPOMSproject.Theshape
oftheferriteisnowdeterminedbytheimpingementofparticleswhichgrow
fromdifferentnucleationsites.
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Fig.8:Anidiomorphofferriteinasamplewhichispartially
transformedintoandthenquenchedsothattheremaining
undergoesmartensitictransformation.Theidiomorphis
crystallographicallyfacetted.
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Therearethreemoreallotropesforpureironthatformunder
differentconditions
iron:
Theironhavinghexagonalclosepackedstructure.Thisforms
atextremepressure,110kbarsand490C.Itexistsatthecentre
oftheEarthinsolidstateataround6000Cand3million
atmospherepressure.
FCTiron:
Thisisfacecentredtetragonaliron.Thisiscoherently
depositedirongrownasthinfilmona{100}planeofcopper
substrate
Trigonaliron:
Growingirononmisfiting{111}surfaceofafacecentred
cubiccoppersubstrate.

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Fe3C or cementite:
Interstitial intermetallic compound of C & Fe with a carbon content
of 6.67 wt% and orthorhombic structure consisting of 12 iron atoms
and 4 carbon atoms in the unit cell.
Stability of the phase ranges from low temperatures to 1227C

Fig.9(a):Orthorhombiccrystalstructureofcementite.Thepurple
atomsrepresentcarbon.Eachcarbonatomissurrondedbyeightiron
atoms.Eachironatomisconnectedtothreecarbonatoms.
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Fig.9(b): The pearlite is resolved in some regions where the


sectioning plane makes a glancing angle to the lamellae. The
lediburiteeutecticishighlightedbythearrows.Athightemperatures
thisisamixtureofausteniteandcementiteformedfromliquid.The
austenitesubsequentlydecomposestopearlite.
Courtesy of BenDennisSmither,FrankClarkeandMohamedSherif
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Critical temperatures:
A=arret means arrest
A0= a subcritical temperature (<A1) = Curie temperature of
cementite=210C
A1=Lower critical temperature=eutectoid temperature=727C
A2=Curie temperature of ferrite=768/770C
A3=upper critical temperature=+ / phase field boundary
=composition dependent=910-727C
A4=Eutectic temperature=1147C
A5=Peritectic temperature=1495C
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Acm=/+cementite phase field boundary=composition dependent =727-1147C


In addition the subscripts c or r are used to indicate that the temperature is measured
during heating or cooling respectively.
c=chaffauge means heating, Ac
r=refroidissement means cooling, Ar

Types/morphologies of phases in Fe-Fe3C system


Cementite=primary (CmI), eutectic (Cmeu), secondary (CmII)(grain boundary
allotriomophs, idiomorphs), eutectoid (Cm ed) and tertiary(CmIII).
Austenite= austenite()(equiaxed), primary (I), eutectic (eu), secondary (II)
(proeutectoid),
-ferrite=ferrite () (equiaxed), proeutectoid or primary (grain boundary
allotriomorphs and idiomorphs)(I), eutectoid(eu) and ferrite (lean in carbon)
().

Phase mixtures
Pearlite (P) and ledeburite(LB)
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Important Reactions
Peritectic reaction
Liquid+Solid1Solid2
L(0.53wt%C)+(0.09wt%C)(0.17wt%C) at 1495C
Liquid-18.18wt% +-ferrite 81.82 wt%100 wt%

Fig.10:ferriteindendriteforminascastFe0.4C
2Mn0.5Si2Al0.5Cu,CoutesyofS.Chaterjeeetal.
M.Muruganath,H.K.D.H.Bhadeshia
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Eutectic reaction
LiquidSolid1+Solid2
Liquid (4.3wt%C) (2.11wt%C) + Fe3C (6.67wt%C) at 1147C
Liquid-100 wt% 51.97wt% +Fe3C (48.11wt%)
The phase mixture of austenite and cementite formed at eutectic
temperature is called ledeburite.

Fig.11:Microstructureofwhitecastironcontaining
massivecementite(white)andpearliteetchedwith4%
nital,100x.AfterMrs.JaninaRadzikowska,Foundry
ResearchlnstituteinKrakw,Poland

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Fig.12:Highmagnificationview(400x)ofthewhitecastiron
specimenshowninFig.11,etchedwith4%nital.AfterMrs.
JaninaRadzikowska,FoundryResearchlnstituteinKrakw,
Poland

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Fig.13:Highmagnificationview(400x)ofthewhitecast
ironspecimenshowninFig.11,etchedwithalkalinesodium
picrate.AfterMrs.JaninaRadzikowska,FoundryResearch
lnstituteinKrakw,Poland

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Eutectoid reaction
Solid1Solid2+Solid3
(0.77wt%C) (0.0218wt%C) + Fe3C(6.67wt%C) at 727C
(100 wt%) (89 wt% ) +Fe3C(11wt%)
Typical density
ferrite=7.87 gcm-3
Fe3C=7.7 gcm-3
volume ratio of - ferrite:Fe3C=7.9:1

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Fig.14:Theprocessbywhichacolonyofpearlite
evolvesinahypoeutectoidsteel.
29

Fig.15:Theappearanceofapearlitic
microstructureunderopticalmicroscope.
30

Fig.16:Acabbagefilledwithwateranalogyofthethree
dimensional structure of a single colony of pearlite, an
interpenetratingbicrystalofferriteandcementite.
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Fig.17:Opticalmicrographshowingcolonies
ofpearlite.CourtesyofS.S.Babu.
32

Fig.18:Transmissionelectronmicrograph
ofextremelyfinepearlite.
33

Fig.19:Opticalmicrographofextremelyfine
pearlitefromthesamesampleasusedto
createFig.18.Theindividuallamellaecannot
nowberesolved.
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Evolutionofmicrostructure(equilibriumcooling)
Sequenceofevolutionofmicrostructurecanbedescribedby
theprojectedcoolingoncompositionsA,B,C,D,E,F.
AtcompositionA
L+L++I+CmIII
AtcompositionB
L+LL+II+ I+ (P(ed+Cmed)
I(+CmIII)+(P(ed(ed+CmIII)+Cmed)

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AtcompositionC
L
L+I

II+CmII

P(ed+Cmed)+CmII

P(ed(ed+CmIII)+Cmed)+CmII
AtcompositionD
L L+I
I+LB

I(II+CmII)+LB(eu(II+CmII)+Cmeu)

(P(ed+Cmed)+CmII)+LB(P(ed+Cmed)+CmII+Cmeu)

(P(ed(ed+CmIII)+Cmed)+CmII)+LB((P(ed(ed+CmIII)+Cme
+CmII)+Cmeu)

36

AtcompositionE
L+CmI
LB(eu+Cmeu+CmI
L
LB(eu(II+CmII)+Cmeu)+CmI
LB(P(ed+Cmed)+CmII)+Cmeu)+CmI
LB((P(ed(ed+CmIII)+Cmed)+CmII)+Cmeu)+CmI
AtcompositionF
LFe3C

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Limitationsofequilibriumphasediagram
Fe-Fe3C equilibrium/metastable phase diagram
Stability of the phases under equilibrium condition only.
It does not give any information about other metastable
phases. i.e. bainite, martensite
It does not indicate the possibilities of suppression of
proeutectoid phase separation.
No information about kinetics
No information about size
No information on properties.
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