SATHYABAMAUNIVERSITY

(Establishedundersection3oftheUGCAct,1956)

Departmentof Mechanical&Production Engineering

LabManual 4thSemester

SPRX4005METALLURGYLAB
Name :______________________________________________________ RegisterNo :______________________________________________________ Batch :______________________________________________________

LISTOFEXPERIMENTS

1 2 3 4 5 6 7 8 9 10 11 12 13

IntroductiontoMetallography StudyOfMetallurgicalMicroscope IdentificationofMicrostuctureofPlainCarbonSteel IdentificationofMicrostuctureofAlloySteel IdentificationofMicrostuctureofHighSpeedSteel IdentificationofMicrostuctureofGreyCastIron IdentificationofMicrostuctureofWhiteCastIron IdentificationofMicrostuctureofSpheroidalGraphiteCastIron IdentificationofMicrostuctureofCopperalloys IdentificationofMicrostuctureofMagnesiumalloys IdentificationofMicrostuctureofAluminiumalloys Heat Treatment of Steel Annealing, Normalising, Hardening And Tempering HardenabilityTestJomnyEndQuenchTesting

ExerciseNo:1

IntroductiontoMetallography

Introduction Metallography or microscopy consists of the microscopic study of the structuralcharacteristicsofametaloranalloy.Themicroscopeisbyfarthemost importanttoolofthemetallurgistfromboththescientificandtechnicalstandpoints. Itispossibletodeterminegrainsizeandthesize,shapeanddistributionofvarious phasesandinclusionswhichhaveagreateffectonthemechanicalpropertiesofthe metal.Themicrostructurewillrevealthemechanicalandthermaltreatmentofthe metal,anditmaybepossibletopredictitsexpectedbehaviourunderagivensetof conditions. The procedure to be followed in the preparation of a specimen is comparatively simple and involves a techique which is developed only after constant practice. The ultimate objective is to produce a flat, scratchfree, mirror likesurface. Sampling: The choice of a sample for microscopic study may be very important. If a failureistobeinvestigated,thesampleshouldbechosenascloseaspossibletothe areaoffailureandshouldbecomparedwithonetakenfromthenormalsection. Roughgrinding: The specimen should be of a size that is convenienttohandle.Asoftsamplemaybemadeflatby slowlymovingitupandbackacrossthesurfaceofaflat smooth file. The soft or hard specimen may be rough groundonabeltsander,withthespecimenkeptcoolby frequent dropping in water during the grinding operation. In all grinding and polishing operations the specimenshouldbemovedperpendiculartotheexisting scratches. The rough grinding is continued until the surface is flat and free of nicks, burrs, etc., and all scratchesduetothehacksaworcutoffwheelarenolongervisible.

 Mounting: Specimens that are small or awkwardly shaped should be mounted to facilitateintermediateandfinalpolishing.Wire,smallrods,sheetmetalspecimens, thin sections,etc., must be appropriately mounted in a suitable material or rigidly clampedinamechanicalmount. Intermediatepolishing: Finepolishing: Thefinepolishingisobtainedbyuseofawetrotating wheel covered with a special cloth that is charged with carefullysizedabrasiveparticles. Etching: Thepurposeofetchingistomakevisiblethemanystucturalcharacteristics of the metal or alloy. The process mus be such that the various parts of the microstucture may be clearly differentiated. This is accomplished by use of an appropriatereagentwhichsubjectsthepolishedsurfacetochemicalaction. Aftermounting,thespecimenispolishedonaseriesof emerypaperscontainingsuccessivelyfinerabrasives.

Specimenpreparationformetallurgicalanalysis: Itisnecessarytoproduceaperfectlyneatandscratchfreesurface,whenthe specimenisviewedthroughthemicroscope.Thisinvolvesgrindingthesurfaceand thenpolishing. Procedure: The mounted specimens are ground with the help of emery paper of finer grade(400Gritsize). The scratches are removed by grinding the specimen against the emery paperinrightangles. Thespecimennowistakentothesingle/doublediscpolishingmachinefor finalpolishing. Aluminapowderissprinkledovertherotatingdiscandthespecimeniskept incontactwiththepowder. The alumina powder acts as an abrasive and removes the very finer scratchesthatwereleftasideduringemerypolishing. Afterobtainingmirrorfinishonthetoplayerofthespecimen,theprocess ofpolishingisstopped. Thespecimenisrinsedwithwater. Respectiveetchantisappliedtothematerial/specimens. Afterapplyingtheetchant,thespecimenisgivenasoakingtimeof2minutes fortheetchanttopenetrate. Nowthespecimeniswashedwithrunningwaterandcleanedwithacetone, ifnecessary. The specimen is dried with the help of drier before taking it under the microscope.

Etchingreagentsformicroscopicexamination: Etchingreagents
Nitricacid (Nital)

Composition

Volumeof Etchant

Uses
Incarbonsteels: Todarkenpearliteandgivecontrast betweenpearlitecolonies. Torevealferriteboundaries To differentiate ferrite from martensite Forallgradesofcarbonsteels: Annealed, normalized, quenched and tempered, spheroidized, austempered. For all low alloy steels attacked by thisreagent. Structure of austenitic nickel and stainlesssteels Generallyusedforcopperandmany ofitsalloys. Copper, brass, bronze, nickel silver, aluminiumbronze General reagent for zinc and its alloys Rapidetchforleadanditsalloys: Very suitable for removing thick layerofworkedmetal General microscopic for aluminium anditsalloys

Whitenitricacid 1 5ml EthylorMethylalcohol 100ml (95%orabsolute) Picricacid 4g EthylorMethylalcohol 100ml (95%orabsolute) 5g 50ml 100ml 5parts 5part 25parts 10g 90ml 200g 15g 1000ml 100g 140ml 240ml 60ml 0.5ml 99.5ml

Picricacid (Picral)

Ferric chloride and Ferricchloride hydrochloricacid Hydrochloricacid Water Ammonium hydroxide Ammoniumhydroxide and hydrogen Water peroxide Hydrogenperoxide Ammoniumpersulfate Ammoniumpersulfate Water Palmertonreagent Chromicoxide Sodiumsulfate Water Ammoniummolybdate Molybdicacid(85%) Ammonium hydroxide Water Filter and add to nitric acid Hydrofluoricacid Hydrofluoricacid H2O

Result: Thus, the specimen preparation for the metallurgical analysis has been studied.

 ExerciseNo:2 Aim: Tostudytheconstructionandworkingofmetallurgicalmicroscope Metallurgicalmicroscopeisthemostimportanttoolusedinmetallurgy.Itis Introduction: used to determine the grain size, shape and distribution of various phases and inclusions.Italsousedformechanicalandthermaltreatmentofthealloys. Workingpriniciple: The microscope involves the examination by the light reflected from specimen surface, since metallurgical specimens are opaque. The plane glass reflector partially reflects the incident light from the light source down on the specimen. The light rays falling on the polished specimen get reflected and pass throughtheobjectiveandtheglassreflectortoformthefinalimageviewedthrough theeyepiece. Diagram: StudyofMetallurgicalMicroscope

Construction: Adrawtubecarryingtheeyepieceatitstopendslideswithinthebodytube ofthemicroscope,withthehelpofarackandpiniondevicebyrotatingthecoarse and fine adjustment knobs, thus helps in the focusing the object. The objective, fitted at the bottom end of the body tube, resolves the structure of the specimen. The eyepiece enlarges the image formed by the objective. The light source inside the microscopetube is diffused using the diffusing discand the width of the light beamiscontrolledbytheirisdiaphragm.Theplaneglassreflectorisplacedat45. Magnification: The metallurgical microscope can provide a maximum magnification of 2000X.Themetallurgicalstructurescanbepermanentlysavedusingphotographic cameramountedabovetheeyepiece. Result: Thustheconstructionandworkingofthemetallurgicalmicroscopehasbeen studied.

ExerciseNo:3 Aim:

IdentificationofMicrostructureofLowCarbonSteel

Toidentifythemicrostructureofplaincarbonsteel. 100X Nital

Magnification: Etchantused:

Microstructuralobservations: Thestructureshowspatchesofpearliteandferrite grains. Steels containing 0.05% 0.35% C are generally known as low carbon steel. When etched with 2% Nital, the structure shows ferrite and pearlite micro constitutions.Thepercentageofferriteappearsaslighter areas. Itpossesseslowstrength,goodmachinability,high ductilityandformability. Result: Thus,theidentificationofmicrostructureoflowcarbonsteelisstudiedand verified.

ExerciseNo:4 Aim: Magnification: Etchantused: 10mlHno3, 15mlHCl, 10mlAcetic,

IdentificationofMicrostructureofStainlessSteel

ToidentifythemicrostructureofStainlessSteel. 100X

3dropsGlycol

Composition: Itcontainsmixture0.05%C,18.5%Crand9.5%Ni. Microstructuralobservations: The structure shows fine austenitic grains with annealing twins. No grain boundary carbide precipitation. The stainless steels aregenerally austenitic. They resistextremecorrosiveenvironments.Theyhavegreaterstrengthandresistance tooxidationevenatelevatedtemperatures.Thepresenceofcarbonabout0.05%to 0.14% increases the strength and cold working. Stainless steel is difficult to machine. Result: Thus, the identification of microstructure of Stainless Steel is studied and verified.

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 ExerciseNo:5 Aim: Magnification: Etchantused: Microstructuralobservations: The structure shows fine tempered with undissolved carbide martensite 100X 4%Nital ToidentifythemicrostructureofHighspeedsteel. IdentificationofMicrostructureofHighSpeedSteel

particles. The high speed steel maintain their hardness at elevated temperatures andresistanttowear. Result: Thus,theidentificationofmicrostructureofHighSpeedSteelisstudiedand verified.

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ExerciseNo:6 Aim: Magnification: Etchantused: Composition:

IdentificationofMicrostructureofGreyCastIron

ToidentifythemicrostructureofGreycastiron. 100X 3%Nital

Itcontains3.1%C,

Microstructuralobservations: The structure shows predominantly type A graphite flakes. 90 % of flakes

areoccuredinpearlitematrix.Inthisiron,thetendencyofcementiteisseparated intographiteandaustenite.Mostgreycastironsarehypoeutecticalloyscontaining between2.5and4%C. Result: Thus, the identification of microstructure of Grey cast iron is studied and verified.

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Ex.No:7IdentificationofMicrostructureofSpheroidalGraphiteCastiron Aim: Toidentifythemicrostructureofspheroidalgraphitecastiron. 100X 2%Nital Magnification: Etchantused: Microstructuralobservations: Thisstructurealsoknownasnodularorductilecastiron.Themicrostucture

shows well performed spheroidal graphite nodules of above 90 % and its size varies about 25. The nodular iron is produced by treating the molten alloy with magnesium,ceriumoracombinationofthetwoelements,followedbyanaddition offerrosilicon.Whenthealloysolidifies,graphitizationoccurstoformnodulesof graphite. Result: Thus,theidentificationofmicrostructureofSpheroidalgraphitecastironis studiedandverified.

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ExerciseNo:8 Aim: Magnification: Etchantused:

IdentificationofMicrostructureofMalleableCastIron

ToidentifythemicrostructureofMalleablecastiron. 100X 3%Nital

Microstructuralobservations: Result: Thus, the identification of microstructure of Malleable cast iron is studied andverified. Unetched Etched The structure shows tempered carbon nodules in perritic matrix. The

malleablecastironismoreductilethangreycastiron.

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ExerciseNo:9 Aim: Magnification: Etchantused:

IdentificationofMicrostructureofCopperalloy

ToidentifythemicrostructureofCopperalloy 100X

Ammoniumhydroxide+H2O2 FerricChloride+Methanol

Microstructuralobservations: The structure consists of small white particles of alpha solid solution in a matrixofbetaphase(variousshadesofgrey).Blackdotsofironrichphasearealso seen. The solid solution alloys of copper are classified into two types (Brass and Bronze). Result: Thus, the identification of microstructure of Copper alloy is studied and verified.

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 ExerciseNo:10 Aim: Magnification: Etchantused: 100X 0.5%HF ToidentifythemicrostructureofAluminiumalloy IdentificationofMicrostructureofAluminiumalloy

Microstructuralobservations: Result: Thus,theidentificationofmicrostructureofAluminiumalloy isstudiedand verified. Thestructureshowssmallangularrefinedgreyprimaryparticlesofsilicon. Thealloysappearedintheformofdendritestructure.

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ExerciseNo:11

HeatTreatmentofSteelAnnealing,Normalizing, Hardening&Tempering

Aim: Heattreatment Heattreatmentprocess: Aheattreatmentprocessconsistsoffollowingsteps: 1. Heatingthesteeltoahighpredeterminedtemperature,calledaustenitising temperature. 2. Soaking,i.e.,holdingthesteelatthistemperatureforsomeperiodoftimeto obtain a homogeneous austenite throughout the cross section of the steel part. 3. The steel is then cooled to room temperature at a particular cooling rate whichdependsonthepropertiestobedevelopedinthesteel. Thescienceofheattreatmentdealswiththefactorsandmechanismswhichcontrol the microstructures of metals and alloys, and also to develop an understanding betweenthemicrostructuresandtheresultingproperties. Annealing: Annealingoperationconsistsofheatingthesteeltoacertainpredetermined temperature, holding it at that temperature for a sufficient time to allow the necessarychangestooccurandthencoolingslowlyatapredeterminedrate. Whenthesteelisheated,thepearliteareaswilltransformtosmallgrainsof austenite by means of the eutectoid reaction, but the original ferrite grains will remainunchanged. A combination of heating and cooling operations timed and applied to a metal,oralloyinthesolidstateinawaythatwillproducedesiredproperties. To study the heat treatment process of annealing, normalizing, hardening andtempering.

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Thepurposeofannealingmaybecarriedtoobtainthefollowingproperties: 1. To relieve internal stresses induced by previous treatment such as rolling, forging,casting,etc., 2. Toimprovemachinability 3. Tosoftenthesteels 4. Torefineandhomogenisethestructure. 5. Toremovegases. Normalizing: Thisprocessconsistsinheatingthesteeltothepropertemperatureandthe cooling in air to room temperature. The purpose of normalizing is to produce a harder and stronger steel than full annealing, so that for some applications normalizingmaybeafinalheattreatment. Normailizingmayalsobeusedtoimprovemachinability,modify andrefine castdendriticstructures,andrefinethegrainandhomogenize themicrostructure inordertoimprovetheresponseinhardeningoperations. Hardening: Hardening is the process which improves the hardness of steel. In this process,thehypereutectoidsteelsareheatedabovethelowercriticaltemperature say30Cto50C,heldatthattemperatureforsufficienttimeandthenquenchedin water, oil or brine solution. Due to this, the austenite changes into a micro constituentcalledmartensitewhichisveryhardandbrittleandthisimpartshigh hardnesstosteelafterhardeningtreatment. Thepurposeofhardeningistoobtainthefollowingproperties: 1. Toincreasethehardnessofsteelandtoolsteelsarehardenedtoimprovetheir cuttingability. 2. Toimprovewearresistanceofsteels 3. Toimprovemagneticproperties.

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Tempering: Hardeningofsteelbyquenchingproducesthemicrostructuresconsistingof martensite and retained austenite. The martensite formed during quenching is highly brittle, hard and stressed. The hardened steel is not used in this condition because cracking and distortion occurs. Therefore, hardening is almost always followedbytempering. Tempering consists of heating the hardened components below the lower critical temperature, holding at the temperature for a specified period and then coolingtoroomusuallyinair. Thepurposeoftemperingisasfollows: 1. Torelieveinternalstressesinducedbyquenching. 2. Toreducehardnessandtoincreaseductilityandtoughness. 3. Toeliminateretainedaustenite. Result: Thusthevariousheattreatmentprocesseswerestudied.

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ExerciseNo:12 Aim: Procedure:

HardenabilityTestJominyEndQuenchTest

Tocheckthehardenabilityofthegivenspecimen. JominyEndQuenchtestapparatus.

Apparatus:

1. Prepare a test specimen as per IS/BS standards. The specimen should have a collarforseatingintheapparatus. 2. Austenisethespecimen(accordingtoaustenitizingtemperature). 3. FillwaterintheEndQuenchapparatusfromthetoptank,fillthewatertillthe water reaches the bottom sump and overflows through the side overflow tap. (providedatthesideoftheapparatusreservoirtank) 4. Seethatthequickreleasingvalueisatclosedpositionwhilefillingwater. 5. Switchinthemotorandcheckwhetherthepumpisworking. 6. Thenopenthequickreleasingvalve,bykeepinginopenposition. 7. Aftercompletingthesteps3to6closethevalve. 8. Keepthespecimenchargingchamberopen,letthemotorberunning. 9. Transfer the specimen from the furnace to the specimen holder and quickly open the quick releasing valve. The specimen gets quenched at one end at specifiedconditionsofflowwater. 10. Takethespecimenoutaftercoolingandconductthehardnesssurveytest. Diagram:

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Precautions: 1. This instrument has been designed and manufactured as per IS and BS standards. 2. ThespecimenmustpreparedasperISandBSspecifications. 3. Keep the equipment dry when not in use by draining the water through wateroutlet. 4. Dontusehardwaterasscalesmayformwithnozzlesandcopperconduits. 5. Usedeionisedwaterorreasonablesoftwater. Result: Thus, the hardenability of the given specimen has been determined using JominyEndQuenchTestapparatus.

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