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    NullEllipsometry:ABasicExperimentalProcedure

    Submittedto:

    Dr.StephenDucharme

    ProfessorofPhysics

    UniversityofNebraska-Lincoln

    Submittedon:

    May5,2010

    Submittedby:

    JeremyVanDerslice

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    Purpose

    Tolearnthefundamentalsofnullellipsometry

    Introduction

    Ellipsometryisanextremelysensitivetechniqueusedtoanalyzethepropertiesofsurfacesorthinfilms.

    Ellipsometrycanbeusedtofindtheindexofrefraction,extinctioncoefficient,reflectivity,orthickness

    ofasurfaceorthinfilm,amongotherthings.Inbasicterms,ellipsometrymeasuresthechangein

    polarizationthatoccursaslightisreflectedoffofatargetsurface.Withthisinmind,ellipsometrycould

    verywellbecalledpolarimetryexceptthatadifferingtechniquenotrelatedtoellipsometrywasalready

    coinedpolarimetry.Althoughitcanbedisputedwhoactuallyinventedellipsometry,PaulDrudederived

    thefundamentalequationsofellipsometryintheearly1900sandbasedonhisworkAlexanderRother

    thencoinedthetermellipsometryinajournalarticlein1945.Thenamestemsfromthefactthatthe

    mostbasicformofpolarizedlightiselliptic.[1]

    GeneralEllipsometryTheory

    SnellsLaw

    Todefinethegeneralequationofellipsometry,manykeydefinitionsmustfirstbediscussed.First,

    incidentlighttransmittedandreflectedatamediumisdefinedtoactinaplaneofincidence.Theplane

    ofincidenceisshowninFigure1.

    Figure1.Incident,reflected,andtransmittedlightintheplaneofincidence.[1]

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    Snellslawdefineshowlightinteractswithamediumasitpassesthroughit.Snellsrelatesthecomplex

    indexofrefractiontotheanglesofincidenceofthemedium.Theindexofrefractionisacomplex

    argumentdefinedby:

    =+

    Wherenrelatesthespeedoflightinthemediumtothespeedoflightinavacuum, =.Theextinction

    coefficient,k,isdefinedthroughtheabsorptioncoefficient()whichdescribeshowquicklythe

    amplitudeofthelightwavedecreasesasittravelsthroughamedium,

    =,,=4

    Thus,Snellslawcanbeproperlydescribedbythefollowingequation,

    11=22

    Where1istheangleofincidencemeasuredfromtheboundaryunitnormaland 2istheangleof

    transmissionalsomeasuredfromtheunitnormal.Foradielectricmaterialinwhichnolightisabsorbed

    thecomplexportionoftheargumentiszero,thus,forthissimplifiedcase,Snellslawcanbeexpressed

    as,

    11=22

    However,forthesakeofthisderivingthegeneralellipsometryequationsonlythemostgeneralcasewill

    beconsidered.

    FresnelsEquations

    Ellipsometryinvestigatesthephasechangeofthesecomponentswhenreflectedoffasurface.Ingeneral

    thephasechangeisnotthesameforbothcomponentsandtheresultisellipticallypolarizedlight.The

    ellipticallypolarizedlightcanbedefinedbytwocomponents,p-waveands-wave.Thep-wavesis

    definedasthepolarizedwaveparalleltotheplaneofincidencewhiles-waveisdefinedasplane

    polarizedwaveperpendiculartotheplaneofincidence.

    Fresnelreflectioncoefficientsdefinetheamplitudechangebetweentheincidentandreflectedwavesat

    aninterface.Theyaredefinedbythefollowingexpression,

    12=211221+1212=112211+22

    Where1and2areshowninFigure2.

    AzzamfurtheredtheunderstandingoftheFresnelreflectioncoefficientsbydefininghowtheamplitude

    betweentheincidentandreflectedwaveschangewhenthinfilmsarepresent.Hedefinedanoptical

    thicknessasthedistancethewavestravelthroughthethinfilmandthenintegratedthesefindingsto

    withtheFresnelreflectioncoefficientsasfollows,

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    =12+2321+12232=12+2321+12232,

    =222

    Whereistheopticalthickness,disthethicknessofthethinfilm,andisthewavelengthofthelight

    source.

    Figure2.Reflectionandtransmissionoflightatthinfilmboundary.[2]

    GeneralEllipsometryEquation

    Incidentlightreflectingoffasurfaceundergoesachangeinphase.Let 1describethephasedifference

    betweenthes-andp-wavesfortheincidentlightand 2describethephasedifferencebetweenthes-

    andp-wavesforthereflectedlight.Now,letdescribethechangeinphasebetweentheparalleland

    perpendicularcomponentsoftheincidentlightthatoccurswhenitisreflectedfromasurface,

    =12

    Aspreviouslydiscussed,theFresnelequationsdefineamplituderatiosandcanbeuseddefinethe

    changeofamplitudeofthelightwavesastheyarereflected,

    =

    Anewterm,,hasbeenintroducedtoquantifytheamplitudechangethatoccursuponreflection.Usingthepreviousdefinitions,thefundamentalequationofellipsometrycannowdefinedas,

    =

    Thus,thethicknessandcomplexrefractionofathinfilmcanbefoundifthecomplexrefractionofthe

    substrateandtheoutsideenvironment(usuallyair)areknown.[2]

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    NullEllipsometry

    Thepreviousderivationofthefundamentalequationsofellipsometryisvalidforalltypesof

    ellipsometry.However,inthisexperimentonlynullellipsometrywillbeinvestigated.Nullellipsometryis

    oneoftheoldestformsofellipsometryanditisstilloneofthemostaccurate,evenwhendone

    manually.However,itisoftenveryslowandthecalculationsrequiredtoextractandcanbeverytediouswhendonebyhand.

    ThetypicalsetupofanullellipsometerisshowninFigure3.ItisknownasthePCSAconfigurationor

    polarizer-compensator-sample-analyzerconfiguration.Therearemanydifferentwaystosetupanull

    ellipsometer,includingPSCAandPSA,butPCSAisthemostcommon.ThePCSAconfigurationcanbe

    usedfairlysimplytoobtainthetwoellipsometricparametersforthesample.Thebasicprocedure

    consistsoffindingcomponentsettingsthatextinguishthelightatthedetector.Theazimuthsofthe

    polarizerandcompensator(Po&Co)areadjustedtomaketheellipticallypolarizedlightreflectoffthe

    sampleaslinearlypolarizedlight.Thereflectedlightisthenextinguishedbyasuitableanalyzerangle,A o.

    Assumingthelightiscompletelyextinguished,thecomplexreflectanceratiocanbedefinedas

    =ctanPoCo+tanCotanPoCotanCo1tanAo=

    Wherethetransmittanceratioofthecompensatorisdenotedby c.Itisevidentthatthisisafairly

    complexequationbutinthisinvestigationasimplificationwillbeusedinwhichthecompensatorwillbe

    heldconstantataquarter-wave,Co=/4.Withthissimplificationitisknownthatthereflectedlightcan

    beextinguishedwithtwodifferentsettingsP1andA1,andP2andA2.Thesesettingsareknowntobe

    relatedtoeachotherbyP2=P1andA2=-A1.Inaddition,thesemeasurementsarerelatedtothe

    ellipsometricanglesby,

    =1=21+3210(1)

    =1=21+21

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    Figure3.Polarizer-Compensator-Sample-Analyzerconfigurationofanullellipsometer.[3]

    Oncetheellipsometricanglesareknown,theextinctioncoefficient,indexofrefractionandreflectivityof

    thesamplecanbecalculatedfromDrudesapproximationequations[4]

    =tan2(3)

    =2212(4)

    =(1)2+22(+1)2+22(5)

    ExperimentalProcedures

    Equipment

    Thefollowingequipmentwillbeusedforthisexperiment:Highpressuremercurylamp,5461green

    linefilter,Gaertnerspectrometer,rails,adjustablesamplemount,polarizer,analyzer,Soliel-Babinet

    compensator,Gaussianeyepiece,photomultipliertube,picoammeter,acetone,methanol,anda

    crystallinesiliconwafer.

    SetupandCalibration:

    FastensampletoGaertnerSpectrometertableusingopticalplatemount,rails,andadjustablesamplemount.Placehighpressuremercurylampwithfilteratthecollimatorslit.UsingtheGaussianeyepiece,

    adjustthetelescopeontheGaertnerSpectrometeruntilthecross-hairsarecenteredhorizontallyand

    verticallyontheilluminatedgreenrectangleproducedbytheslitonthecollimator.Adjustthevertical

    tiltonthetelescopeifneeded.Turnthelowerrotatabletable,showninFigure4,untilthe0 oline

    matchesupwiththe180olineofthetelescope.Placethesampleontheadjustablesamplemountthat

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    wasconstructed.Carefullycleanthesamplesurfacewithacetoneandthenmethanoltoremoveorganic

    buildup.Slowlyslidethesamplealongtherailuntilitiscenteredbetweenthecollimatorandtelescope.

    Figure4.EssentialcomponentsofPCSAnullellipsometrywithGaertnerSpectrometer.

    Placethepolarizerontheendofthecollimatorandsetitto0 o.AdjustthetelescopetosiliconsBrewster

    Angle(angleofincidenceof152.6o).Rotatetheentirepolarizer(whilekeepingthepolarizersetto0 o)

    untilthephotomultipliertubedetectsaminimumamountoflight.Thepolarizerisnowknowntobe

    orientedsuchthatthe0osettingproduceslightpolarizedvertically.Now,settheangleofincidenceto0 oandplacetheanalyzerontheendofthetelescopeandsetitorthogonaltothepolarizer.Rotatethe

    entireanalyzer(whilekeepingitorthogonaltothepolarizer)untilmaximumextinctionisfoundand

    tightenitdown.Attachthecompensatortothespectrometer.Withthepolarizerat+45 oandthe

    analyzerat-45o,rotatethecompensatoruntilmaximumextinctionisfound.Adjusttheretardationon

    thecompensatorbyturningtheknobtocorrespondwithaquarterwavephaseshift(1.33turns)as

    givenbyTable1.

    PhotomultiplierTube

    Telescope

    LowerRotatableTableUpperRotatableTable

    Analyzer

    Compensator Polarizer

    Collimator

    AdjustableSlit

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    Table1.Soliel-Babinetcalibrationguidetosettheretardanceofthecompensator.Notek=0.987

    [AppendixB]

    Procedure

    Settheangleofincidenceto170o

    byrotatingthetelescope.Next,rotatethepolarizeruntilmaximumextinctionisfound.Then,adjusttheanalyzertofurtherreducethesignalproducedbythe

    photomultipliertube.Continuetoadjusttheanalyzerandpolarizeruntilthemaximumextinctionis

    found.Recordthepolarizerandanalyzerazimuthsettings.Next,adjustthepolarizerandanalyzerto

    allowformaximumtransmission.Now,adjustanalyzerformaximumextinctionandthensequentially

    adjustthepolarizerandanalyzerformaximumextinction.Iftheazimuthsoftheanalyzerandpolarizer

    aredifferentthanthefirstmeasurement,recordthevalues.Iftheyarethesame,adjustthepolarizerto

    anewlocationandbeginagainbyadjustingtheanalyzerformaximumextinction.Oncebothnull

    positionsarefound,reducetheangleofincidenceby10 oandrepeatmeasurementsforanglesof

    incidencebetween170oand60oat10oincrements.Sortthedataintotwoconsistentdatasetsandplot

    thepolarizerandanalyzeranglesasafunctionofangleofincidence.

    ReferencesandAdditionalReading

    [1]Santer,S.(2004,July20).Ellipsometry.Retrievedfromhttp://www.imtek.de/cpi/images/images/vl-

    ofa/OFA-elli.pdf

    [2]Tompkins,Harland,&McGahan,William.(1999).Spectroscopicellipsometryandreflectometry.New

    York:Wiley-Interscience

    [3]Tompkins,Harland,&Irene,Eugene.(2005).Handbookofellipsometry.WilliamAndrew.

    [4]Monk,G.S..(1963).Light:principlesandexperiments.NewYork:DoverPublications.

    [5]Azzam,R.,&Bashara,N.(1987).Ellipsometryandpolarizedlight.NorthHolland.

    *SeeAppendixforcriticalinformationaboutGaertnerNullEllipsometerEquipment

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    CommentsforDr.Ducharme

    Followingtheprocedurethatwaspreviouslyoutlined,rawdatawascollectedasshowninTable2.The

    datacanbecomparedtotheexpectedresultsrememberingthatthetwonullpositionsforeachangleof

    incidenceshouldhavethefollowingrelationship,P2=P1andA2=-A1.Itisquicklyevidentthattheraw

    datacollecteddoesntdirectlyfollowtheguideline.

    Null1 Null2

    2 Analyzer Polarizer Analyzer Polarizer

    170 85 62 41 66 51

    165 82.5 75 54

    160 80 74 31 82 60155 77.5 80 22 88 79

    152 76 79 3 88 90

    150 75 78 7 88 79

    145 72.5 74 24 88 73

    140 70 72 32 82 61

    130 65 67 37 74 51

    Table2.Rawdatacollectedfromanalyzerandpolarizerazimuthmeasurements

    Therawdatashowsthat1!2and2!901.Theanalyzerazimuthmeasurementisthe

    complementaryangletotheonethatisdesiredthus,1=901.

    Aftermakingtheadjustment,2=901and2=901sotherelationshipbetweenthetwonull

    setsofthemeasureddataisslightlydifferentthanthatgivenbyH.Tompkins.Thisdiscrepancyisstill

    underconsideration,butitisthoughtthatthedifferencehassomethingtodowiththescaleonthe

    polarizers.Althoughtheadjustmentsaresimple,thechangesaremadeandshowninTable3forclarity.

    Null1 Null2

    2 Analyzer Polarizer Analyzer Polarizer

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    170 85 28 41 -66 -51

    165 82.5 -75 -54

    160 80 16 31 -82 -60

    155 77.5 10 22 -88 -79

    152 76 11 3 -88 -90150 75 12 7 -88 -79

    145 72.5 16 24 -88 -73

    140 70 18 32 -82 -61

    130 65 23 37 -74 -51

    Table3.Dataaftermodificationsaremadetopreparethemforuseinellipsometricequations

    Theanalyzerandpolarizerazimuthmeasurementsareplottedasafunctionofangleofincidencein

    Figure5.Noticethattheprincipalangleofincidenceislocatedatthedipinthecurves.Theazimuth

    measurementoftheanalyzeratthislocationistheprincipalangleofazimuth.Thisisthelocationand

    measurementthatwillbeusedlaterincalculations.

    Figure5.Analyzerandpolarizeradjustedazimuthmeasurementsasafunctionoftheangleofincidence.

    Now,theextinctioncoefficient,indexofrefraction,andreflectivitycanbeextractedfromthedatausing

    equations(3),(4)&(5).Althoughitseemsthatanyangleofincidencecouldbeusedtoextractthese

    properties,theangleofincidencenearesttoBrewstersangleischosenbecauseitprovidesthegreatest

    changeinpolarizationsothemeasurementcanbefoundwithlesserror.Thecalculatedextinctioncoefficient,indexofrefraction,andReflectivityarecomparedtovaluesgivenbytheSOPRAN&K

    DatabaseinTable4.

    -90

    -70

    -50

    -30

    -10

    10

    30

    50

    65 70 75 80 85

    Pola

    rizer,

    Analyzer

    [deg]

    AngleofIncidence[deg]

    Null1-A

    Null1-P

    Null2-A

    Null2-P

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    SOPRAN&K

    Database

    Measured:Null

    location1

    Rel.

    Error

    Measured:Null

    LocationII

    Rel.

    Error

    k 0.0415 0.404 10x 0.067 68%

    n 4.099 4.254 3.8% 3.901 4.8%

    R .392 0.452 15.3% .400 1.9%

    Table4.Extinctioncoefficient(k),IndexofRefraction(n)andReflectivity(R)asgivenbytheSOPRAN&K

    databaseincomparisontovaluescalculatedfrommeasurements.

    Therelativeerrorinthecalculatedextinctioncoefficientsimmediatelydrawsconcern.However,itwas

    foundthattheextinctioncoefficientisextremelysensitivetotheazimuthoftheanalyzer.Forinstance,

    theNull2analyzerazimuthreadingattheprincipalangleofincidenceis-88 o,whichleadstoanerrorof

    68%.Ifthereadingwouldhavebeenonly1odifferent(-89o)theerrorwouldhaveonlybeen15%.Even

    thoughtheindexofrefractionandreflectivityarefunctionoftheextinctioncoefficient,thedependence

    isweak.Thehugereductionoferror(concerningthehypotheticalcasethat=-89 oratherthan-88o)in

    theextinctioncoefficientonlyimprovestheerrorintheindexofrefractionby0.2%andtheerrorinthe

    reflectivityby1.4%.ThisexplainshowtheindexofrefractionandreflectivityfortheNull1datasetare

    reasonablyclosetoacceptedvalueseventhoughtheextinctioncoefficientisoffby1000%.

    Throughouttheexperimentitwasfoundthatobtainingprecisemeasurementswiththepolarizerand

    analyzerisfairlydifficultleadingtomuchlessprecisioninthenullellipsometryexperimentthan

    advertisedinliterature.Whenreadingthroughsomeliteratureonnullellipsometry,itwasfoundthatamanualnullellipsometertypicallyusepolarizersthatareaccuratewithin0.01o.Thepolarizersusedin

    thisexperimentwereaccurateto0.5owhileactuallyachievingthisaccuracywasoftendifficult.With

    patienceitwasfoundthatthetoleranceontheazimuthmeasurementswasnolessthan2.5 o.Even

    withthislackofprecision,valueswereobtainedthatcomparedreasonablywelltoacceptedvalues.

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    Conclusion(PersonalNotes):

    Mymethodforfindingbothnullpositionsforeachangleofincidenceisnotanexactscience;however,it

    seemedthattheorderinwhichthepolarizerandanalyzerwereadjustedcouldinfluencethenullposition

    thatwasfound.ThisistheprocedureIoutlined,butIadmitthatitdidntalwaysworkwellforme.Im

    slightlyperplexedbyafewthingsintherawdata,namely,therelationshipbetweenthetwonullsets.I

    foundthetheoreticalrelationshipgivenbyTompkinsdoesntdirectlymatchwhatIhave.Ioftensawin

    theliteraturethatpeopleuseananalyzerthathasarangeof-180oto180

    oandapolarizerthathasa

    rangefrom0oto360

    o.ThepolarizerandanalyzerthatIusedrangedfrom0

    oto90

    o.Ithinkthisdifference

    inscalecamouflagesmydatatolookdifferentthanwhatTompkinspredictswhileitisactuallythesame.

    Overall,thiswasafairlycomprehensiveexperimentcoveringarangeofthingsthatwerelearnedduring

    thelabbutitreallyhelpedtosolidifytheconceptswelearnedduringthepolarizationexperiment.

    AssumingthatIveexplainedmyprocedurewellenoughtoreproduce,Ithinkthisentireexperimentcould

    beeasilyduplicatedina2-weeklab,thefirstweekprobablybeingsetupandcalibrationandthesecond

    weekdatacollection.

    CommentsontheClass

    Theclasswasbothinterestingandchallenging.Ireallyappreciatedthefactthatitistaughtbya

    professorratherthanaTA,whichissooftenseenintheengineeringcollege.Youbroughtalotof

    enthusiasmaboutthesubjecttotheclassandthatmadeworkingalittlehardertolearnthingsalot

    easier.Thanksfortheextratimeyouspenthelpingmegetthisextraexperimentgoingaswellasallthe

    rest.Haveagoodsummer.

    Regards,

    Jeremy

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    Appendix