THEAMERICANUNIVERSITYINCAIRO

MENG3207/327
EngineeringMaterials
LabReport:MicrostructureCharacterization

Submittedby:CherifChokeir
ID:
900140712

DateofSubmission:17/4/2016

Dr.HanadiSalem
TA:AhmedSamir

Abstract

Thepurposeofthisstudyistoexaminethemicrostructurefeaturesofmartensiticsteelspecimen
usinganopticalmicroscope.Appropriatesurfacepreparationincludingsectioning,mounting,
grinding,polishingandetchinghelptorevealthemicrostructure.Thestudyofsomefeatureslike
thepresenceofsingleandmultiphases,theexistenceofcolumnarorequiaxedgrainsisofa
majorimportanceinmaterialsciencesinceithelpstounderstandthedifferentmaterialproperties
andtheirrelationshiptomicrostructure.

TableofContents

PageNumber
ListofFigures

#4

Introduction

#5

Objective

#6

Procedure

#7

Results

#15

Conclusions&Recommendations

#18

References

#19

Listoffigures

Fig.1SectioningMachine...8
Fig.2Mountedspecimen.....8
Fig.3GrindingMachine.10

Fig4SiliconCarbideGrindingPaper.10
Fig.5GrindingProcess.10
Fig.6Evolutionofthespecimensurfacewhenusingfinerabrasivepaper...11
Fig.7PolishingMachine...12
Fig.8EtchingPrinciple.13

Fig.9Overetchedcopperspecimen...13
Fig.10MicroscopicObservationprinciple...14
Fig.11OpticalMicroscope...14
Fig.12SinglePhasemetal...15
Fig.13Multiphasemetal..15
Fig.14Equiaxedvs.Columnargrains..16
Fig.15Differenceinmicrostructurebetweenpureandimpurezinc.17

Introduction
Metallographyisthestudyofthemicrostructurefeaturesofthemetalsinorderto
understandtherelationshipbetweenthesestructuresandthedifferentpropertiesofmaterial.In
fact,thematerialisgreatlyaffectedbythedifferentfeaturespresentonthemicronscale.
Theexaminationofthesestructureshelpsalsotovisualizethepresenceofimperfectionsor
defects,controlthepercentofsoluteinanalloy,assurethedesiredpropertiesareacquired.

Microscopyisthestudyofthemicrostructurefeaturesofthematerialsusinga
microscope(Callister,2007).Differenttypesofmicroscopescouldbeusedtoobservethe
microstructuredependingontherequiredmagnification.Thescanningelectronmicroscope
(SEM)couldyieldupto20,000X.Transmissionelectronmicroscopes(TEM)helptogetupto
100,000X.(Experiment:MetallographySpecimenPreparationandExamination)
Thescanningprobemicroscopeshelptogettopographicalimagesofthemicrostructureandthus
areofgreatimportance(Callister,2007).Inthisexperiment,opticalmicroscopesareusedto
revealthemicrostructureofmartensiticsteelspecimen.Theyarebasedontheilluminationbya
lightbeamofthesurfaceofthespecimenandthedifferenceinreflectivityofthedifferent
featureshelpedtoidentifythem.

Priortotheuseofmicroscope,propersurfacepreparationisofamajorimportance.
Theprocessesinvolvesectioning,mounting,grinding,polishingandetching.Thishelptoreveal
themicrostructure.
Theidentificationofsomefeaturesliketheexistenceofsingleormultiphase,the
columnarorequiaxedgrainshelpedtounderstandthematerialspropertiesandthusareofmajor
importance.

Objectives:
A.

Studythesamplepreparationformicroscopicobservation.

B.

Examinethemicrostructureofamartensiticsteelsample

C.

Understandtherelationshipbetweenmicrostructureandmechanical
properties

D.

Understandthedifferencebetweenpureandimpuremetalsandbetween
singleandmultiphaseones.

Procedure:

Inordertoobservethemicrostructurefeaturesofthemartensiticsteelspecimen,itisimportant
toperformsomesamplepreparationwhichhelpstorevealthegrainandgrainboundariesofthe
specimenunderthemicroscope.Thedirectobservationofaspecimenunderthemicroscope
withoutanysamplepreparationwontrevealanyfeatures.

1) Sectioning
Thepurposeofthesectioningoperationistoselectasampleofthespecimentoobservewhich
couldbeeasilycontrolled.Thesectioningalsohelptoreducethedamagecausedbysome
externaleffectslikeshearstresses,whichifnotminimizedwouldaffectthemicrostructure
featuresofthespecimenandthusleadtoafalsecharacterizationofthespecimenunderthe
microscope.
Thesectioningoperationisdonebyusingabrasivecuttingwheels,whichshouldbemadeofa
materialharderthanthespecimeninorderforthesectiontobeflat.Thewheelsaremadeof
abrasivegrainslikeSiliconCarbideandAluminumOxidewhicharebondedtorubber.Inorder
forthesectioningoperationtobesuccessful,appropriatespeedsofthewheelshouldbechosen
dependingonthematerialscharacteristics.Inordertoavoidtheheatcausedbyfrictionduring
theoperationwhichmightaffectthemicrostructure,acoolantshouldbeused.Inthisexperiment,
theuseofdistillatewaterisappropriatesinceitislightandhasahighspecificheatcapacitysoit
couldabsorbtheheat.Itisalsoinviscidflowandthuscouldbeeasilyused.Thespecimenshould
beappropriatelyplacednearthecuttingwheelandsecured.Thecoolantmustbeappliedduring
thewholeprocessinordertocoolthespecimenbutalsotowashitssurface.

Fig.1SectioningMachine

2)Mounting
Thepurposeofthemountingoperationistobeabletoeasilycontrolthespecimen,specially
whenitssectionissmall.Anotherimportantobjectiveistoprovideprotectiontothespecimens
edgeforappropriatecharacterization.Themountingoperationisdonegenerallyusinga
polymericmaterial(plastic).Themountingoperationcouldbeachievedbyeithercompression
moldingorcoldmolding(doneatroomtemperature).Thespecimenislocatedinsideamounting
cylinderwhichisthenplacedinpowdersofpolymericmaterial.Forthecoldmolding,epoxyis
usedtosurroundthemetalandproducesthemountedspecimen.Theprocessofcoldmounting
mighttakeapproximatelyonehour.Butinthecaseofcoldmountingspecialcautionshouldbe
madeasadhesionislessbetweenepoxyandthespecimenwhichmightleadtogapformation.

Fig.2Mountedspecimen

Themountingprocedureisasfollows:
1. Centerthespecimeninthemountingringorcylinder.Thesurfacetobeexaminedshould
bepointingdownward
2. Pourtheepoxyresininsidethemountingring
3. Waitanhourthengentlyremovethemountingring

3)Grinding
Thepurposeofthegrindingoperationistogetasmoothandflatsurfacefreeofscratchesandto
eliminatetheeffectofcoldworkingthataffectsthespecimenssurfaceduringsectioningand
mountingoperations.Theseoperationscouldinfactcausedeformationinthematerial:the
grindinghelpstoeliminatethedeformedlayerinordertohavelessdistortioninthematerialand
thusbeabletopropercharacterizationandtobeabletovisualizethegrainsandgrain
boundaries.
Thegrindingoperationisdoneonstages.Atfirst,thecoarsegrindinghelpstoobtainthefirstflat
surfaceforthefollowinggrindingandthenpolishingprocesses.Thegrindingisdoneusing
siliconcarbidegrindingpaperordisk.Inthecoarsegrindingstage,paperofsize120180(which
isthesizeoftheparticles)isusedtoremovetheroughdeformedsurface.Duringthedifferent
grindingsteps,allscratchesshouldbeofthesamedimensionsandparallel.Afterfinishingthe
coarsegrinding,itisthentimetodothefinegrindingbyusingfinersiliconcarbidepapergrit.
Thestepsare240,320,400,600andeven8001000formaterialslikesteel.Passingfroma
grindingstagetotheothershouldbedoneafterallthescratchesfromthepreviousoneare
removed.Theimportantthingistousefinergrindingpaperinordertoobtainsmoothersurface.
Itiscrucialtowashthespecimenwithdistilledwaterbetweenthedifferentgrindingstagesto
avoidthepersistenceofscratchesfrompreviousstages.Ataspecificstage,thegrindingangleis
fixedbutthespecimenmustberotatedthrough90betweendifferentstages.Inthefinegrinding,
wetgrindingcouldbeapplied.Thepurposeistoeliminatetheeffectofheatwhichmightaffect
thespecimensmicrostructure.

Fig.3GrindingMachine

Fig4SiliconCarbideGrindingPaper

Fig.5GrindingProcess

Fig.6Evolutionofthespecimensurfacewhenusingfinerabrasivepaper
(Samplepreparation)

4)Polishing
Thepurposeofthepolishingstageistoobtainaverysmoothmirrorlikesurfaceforproper
characterizationandexamination.Thisisdonebyusingabrasivesinawatersolutiononawheel
thatiscoveredbyacloth.Thepolishingcouldbedoneusingaluminumoxidepowder.Priorto
polishingthespecimenmustbewashedanddried:thesmallestdustparticles

mightaffectthe
specimenssurfaceiftheygetontothecloth.

Polishingisalsodoneonstages.Herealsofiner
aluminumoxideparticlesareusedatstageswherethespecimeniscarefullywashedbetweenthe
differentstages.Thepolishingstagesaredoneusingfinerparticlesize(onthecloth).Atfirst,the
surfaceremainingfromgrindingshouldberemoved.Thenlighterpressureofthewheelshould
beappliedandthetimeshouldbeminimizedatthefinalstageasthespecimenwillmaintainthe

shapeithasatthisstageunderthepressureofthewheel.Thelessthespeedofthewheel,the
morepolishing

Theprocedureforpolishingisasfollows:
1. Washinghandsandthespecimenpriortoanypolishing
2. Adjustthewaterlevel
3. Usealuminumoxidepowderonthecloth
4. Thenstartthefirstpolishingstage.Thisstageisroughandthustakebetween12
minutes.
5. Makesuretoholdthespecimenwithbothhandsandapplyamoderatepressureonthe
specimenbythewheel
6. Washthespecimenwithwaterbeforebeginningthenextpolishingstage
7. Repeattheabovestepsforthedifferentpolishingstages
8. Afterthefinalpolishingstage,washthespecimenandbecarefulnottotouchit

Fig.7PolishingMachine

5)Etching
Etchingisachemicalreactionthatisappliedtothespecimenssurfaceinordertoreveal
microstructurefeaturessuchasgrainandgrainboundaries.Anunetchedspecimenwillonly
showsomestructuresasvoids,cracksorinclusions.Tobeabletovisualizethedifferentphases
andgrains,anetchantwhichisusuallyanalkalineoranacidisusedtochemicallyattackthe
surfaceofthespecimen.Thishelpedtoremovethefinaldeformedsurfacefrompolishingstage.
Inthisexperiment,theetchantwasHCLtowhichwasaddedsomedistilledwater.Theideais
thataccordingtothedifferenceinreactivitywithetchantandtheorientationoftheattackthis
willhelptorevealthedifferentmicrostructures.Forexample,grainboundariesaremorereadily
attackedbyetchantandappeardarkerinmicroscopicexamination.Thetimeshouldbesmall
(around0.51minute)toavoidoveretchingwhichmightaffectthespecimensobservation.

Fig.8EtchingPrinciple

Fig.9Overetchedcopperspecimen

(SamplePreparation)
Theprocedureforetchingisasfollows:
1. Placethepolishedspecimenatthetopofthetablewiththesurfaceup
2. Applyetchantdropstothespecimen
3. Wait50seconds1minuteandthenwashthespecimen
4. Incasethesurfacefeaturescannotappear,youmightwanttodofurtheretching
5. Incaseyouoveretchedthespecimen,manyscratchesmightappear,youwillneedtogo
backtothegrindingstage
6. Drythespecimenwithairblower

Afterperformingthespecimenpreparation,itisnowpossibletodothemicroscopicobservation.
Inthisexperiment,anopticalmicroscopewasusedtostudythemicrostructurefeaturesofthe
martensiticsteelandtounderstandthedifferencebetweenpureandimpuremetals.
Thespecimenshouldbeplacedonthemicroscopestageinawaythatthesurfaceofobservation
istobeperpendiculartotheopticalaxisofthemicroscope.Themicroscopeshouldhavesome
differentcharacteristicsinordertobeabletoviewthedetails:
Magnification
Resolution
Flatnessoffield

Fig.10MicroscopicObservationprinciple Fig.11OpticalMicroscope(andersonmaterials)
(KPShah)

(Experiment:MetallographySpecimenPreparationandExamination)
(DonaldZipperianMetallographicSpecimenPreparationBasics)

Resultsanddiscussion:

Thesurfacepreparationformicroscopicorganizationhelpedtoobservethemicrostructure
featuresforthemartensiticsteelspecimenandtounderstandthedifferencesbetweensingleand
multiphasemetalsaswellaspureandimpurespecimens.

Theobservationwiththemicroscopehelpedtoidentifytwotypesofmetalspecimenbasedon
thepresenceofasingleormultiphase.

Fig.12SinglePhasemetalFig.13Multiphasemetal

AphasecouldbedefinedasAhomogeneousportionofasystemthathasuniformphysical
andchemicalcharacteristics(Callister,
MaterialsScienceandEngineeringAnIntroduction)

Inmultiphasecrystals,themicrographshowsdifferentregions(darkandclear).Eachoneof
themcorrespondstoaphasewhichhasitsproperphysicalandchemicalcharacteristics.Itis
separatedfromtheotherphasesbyaboundarythatmarksanabruptchangeinthephysical
and/orchemicalproperties.Similarly,incaseofapolymorphicmaterial,thedifferentstructures
constitutedifferentphasessincetheydifferintheirphysicalorchemicalproperties.Mostofthe
metalsandalloysaremultiphasesystems.
(Callister,2007)

Asinglephasecrystalischaracterizedbythepresenceofoneonlyphasethushavingauniform
physicalandchemicalproperties.

AgraincouldbedefinedasAnindividualcrystalinapolycrystallinemetalorceramic
(Callister,2007).Inagrainatomsarearrangedrelativelyinthesamecrystallographicorientation
andtheyareseparatedbygrainboundaries,aregionofatomicmismatchbetweenthem.

Asinglegraincouldcontaindifferentphases:theatomsarearrangedinthesamemannerbutthe
differentphaseshavedifferentphysicalandchemicalproperties.

Anotherimportantcomparisonisbetweenequiaxedandcolumnargrains
Duringcrystallizationofalloys,animportantnumberofstablenucleiformandthereisafast
extractionoftheheatofthemeltingliquid.Whenamoltenmetalcomesincontactwithamold
thatisatroomtemperature,smallequiaxedgrainsforminthechillzonewherethereisafastrate
ofcooling.Thisfastrateofcoolingleadstosmallgrainsize.

Atthispoint,someofthesesmallgrainsbegintogrowinanoppositedirectiontothatoftheheat
propagation.Thiswillresultincolumnargrainswhichareelongatedinaspecificdirection.
(CHAPTER4SOLIDIFICATION,CRYSTALLINEIMPERFECTIONS,ANDDIFFUSION
INSOLIDS).Columnargrainsformatalowtemperaturegradient.Thenwhenthelatentheatis
propagatedthroughthematerial,undercoolingwillstopgrowthofthesegrains.Coolingofthe
moltenmetalinthemiddleofthemoldwillresultintheformationoflargerequiaxedgrains.
Thegrowthofthecrystalsoccurindendriteform
(
Kopeliovich
,
Solidification
)

Fig.14Equiaxedvs.Columnargrains.
Inanalloy,itisimportanttoreducecolumnargrainssincetheycauseductilitywiththeirlarge
size.(unlesswewantdirectionalproperties.)Theequiaxedgrains,ontheotherhand,aresmaller
andthusimparthardnessandstrength.Tomakeequiaxedgrainsfromcolumnarones,itis

possibletousenucleatingagentswhichhelptocausegrowthofnucleiwithoutreactingwith
material

Theexperimentalsohelpedtounderstandthedifferencebetweenpureandimpurematerialsin
termsofmicrostructure.

Fig.15Differenceinmicrostructurebetweenpureandimpurezinc

Themicrostructureofpurezincisformedofcolumnargrainswhileimpurezinciscomposedof
equiaxed(almostspherical)grains.Whenintentionallyaddedduringalloying,thesolutehelpsto
strengthenthematerialthroughtheprocessofsolidsolutionstrengthening.

ConclusionandRecommendations

Toconclude,thepurposeofthisstudywastounderstandthemicrostructurefeaturesof
martensiticsteelspecimeninordertofindtherelationshipbetweenthemechanicalproperties
andthemicrostructure.Thiswasdonebymicroscopicobservation.
Priortotheobservationappropriatesurfacepreparationshouldbedone.Thisinvolvesthe
processesofsectioningthespecimen,mountingittobeabletohandleit,grindingittoobtainthe
smoothsurface,polishingitssurfacetoamirrorlikeshapeandetching,whichisachemical
reactionusedtorevealthedifferentmicrostructurefeatureslikegrainandgrainboundaries.
Theobservationofthemicrostructurehelpedtoidentifythedifferencebetweensingle
andmultiphasecrystals:asinglephasecrystaliscomposedofonlyonehomogenousportionthat
hashomogenousphysicalandmechanicalproperties,whilemultiphaseoneiscomposedof
differentonesthathavedifferentproperties
Theidentificationofequiaxedandcolumnargrainsduringsolidificationprocessisalsoof
majorimportance:equiaxedgrainsareequalinalldirectionswhilecolumnarareelongatedina
specificone.Thecolumnargrainsformatlowtemperaturegradientatalowcoolingrate.The
columnargrainsappearinpurematerialwhileimpureonesaremorecomposedofequiaxedones.
Thecolumnargrainsneedtobereducedsincetheirlargesizecauseductilitytomaterial
Furthermore,theobservationofthemicrostructurefeaturesofamaterialisofmajor
importanceandhelpstounderstanddifferentmechanicalpropertiesthatcouldnotbeunderstood
elsewise.

References:
Callister,
MaterialsScienceandEngineering:AnIntroduction
2007.

Chapter4Solidification,CrystallineImperfections,ANDDiffusioninsolids
Retrievedfrom
http://web.nuu.edu.tw/~hsuch/download/material_science_cht04%20and%20cht08.pdf

Experiment:MetallographySpecimenPreparationandExamination.
Retrievedfrom
http://mimoza.marmara.edu.tr/~altan.turkeli/files/1sample_preparation.pdf
Kopeliovich,Dmitri
Solidification
Retrievedfrom
http://www.substech.com/dokuwiki/doku.php?id=solidification

Zipperian,Donald
MetallographicSpecimenPreparationBasics
Retrievedfrom
http://www.metallographic.com/Technical/Basics.pdf