ISO 11505 2025.docx

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1、ISOInternationalStandardISO11505Secondedition2025-06Surfacechemicalanalysis一GeneralproceduresforquantitativecompositionaldepthprofilingbyglowdischargeopticalemissionspectrometryAnalysechimiquedessurfacesModesOperatoiresgenerauxpourIeprofilageenprofondeurCompositionnelquantitatifparSpectrometriedemis

2、sionoptiqueadechargeIuminescenteReferencenumberISO11505:2025(en)COPYRIGHTPROTECTEDDOCUMENTISO2025Allrightsreserved.Unlessotherwisespecified,orrequiredinthecontextofitsimplementation,nopartofthispublicationmaybereproducedorutilizedotherwiseinanyformorbyanymeans,electronicormechanical,includingphotoco

3、pying,orpostingontheinternetoranintranet,withoutpriorwrittenpermission.PermissioncanberequestedfromeitherISOattheaddressbeloworISO,smemberbodyinthecountryoftherequester.ISOcopyrightofficeCP401Ch.deBlandonnet8CH-1214Vernier,GenevaPhone:+41227490111Email:copyrightiso.orgWebsite:www.iso.orgPublishedinS

4、witzerlandContentsPageForewordv1 Scope12 Normativereferences13 Termsanddefinitions14 Principle15 Apparatus25.1 Glowdischargeopticalemissionspectrometer25.1.1 General25.1.2 Selectionofspectrallines25.1.3 Selectionofglowdischargesourcetype26 Adjustingtheglowdischargespectrometersystemsettings36.1 Gene

5、ral.36.2 SettingthedischargeparametersofaDCsource46.2.1 Constantappliedcurrentandvoltage46.2.2 Constantappliedcurrentandpressure56.2.3 Constantappliedvoltageandpressure56.3 SettingthedischargeparametersofanRFsource66.3.1 Constantappliedpowerandpressure66.3.2 ConstantappliedpowerandDCbiasvoltage66.3.

6、3 ConstanteffectivepowerandRFvoltage76.4 Minimumperformancerequirements76.4.1 General76.4.2 Controloflampcleanlinessandstart-upperformance76.4.3 Minimumrepeatabilitry96.4.4 Detectionlimit97 Sampling118 Calibration118.1 General118.2 Calibrationspecimens118.2.1 General118.2.2 Low-alloyironorsteelspeci

7、mens128.2.3 Stainless-steelspecimens128.2.4 High-oxygenspecimens128.2.5 High-carbonspecimens128.2.6 High-nitrogenspecimens128.2.7 High-puritycopperspecimens128.2.8 High-purityzincspecimens138.3 Validationspecimens138.4 Determinationofthesputteringrateofcalibrationandvalidationspecimens138.5 Emission

8、intensitymeasurementsofcalibrationspecimens148.6 Calculationofcalibrationformulae148.7 Validationofthecalibration148.7.1 General148.7.2 Checkinganalyticalaccuracyusingbulkreferencematerials158.7.3 Checkinganalyticalaccuracyusingsurfacelayerreferencematerials158.8 Verificationanddriftcorrection159 An

9、alysisoftestspecimens169.1 Adjustingdischargeparameters169.2 Settingofmeasuringtimeanddataacquisitionrate169.3 Quantifyingdepthprofilesoftestspecimens1610 Expressionofresults1610.1 Expressionofquantitativedepthprofile1610.2 Determinationoftotalcoatingmassperunitarea1710.3 Determinationofaveragemassf

10、ractions1811 Precision1812 Testreport18AnnexA(normative)Calculationofcalibrationconstantsandquantitativeevaluationofdepthprofiles19AnnexB(informative)Suggestedspectrallinesfordeterminationofgivenelements32Bibliography34ForewordISO(theInternationalOrganizationforStandardization)isaworldwidefederation

11、ofnationalstandardsbodies(ISOmemberbodies).TheworkofpreparingInternationalStandardsisnormallycarriedoutthroughISOtechnicalcommittees.Eachmemberbodyinterestedinasubjectforwhichatechnicalcommitteehasbeenestablishedhastherighttoberepresentedonthatcommittee.Internationalorganizations,governmentalandnon-

12、governmental,inliaisonwithISO,alsotakepartinthework.ISOcollaboratescloselywiththeInternationalElectrotechnicalCommission(IEC)onallmattersofelectrotechnicalstandardization.TheproceduresusedtodevelopthisdocumentandthoseintendedforitsfurthermaintenancearedescribedintheISO/IECDirectives,Part1.Inparticul

13、ar,thedifferentapprovalcriterianeededforthedifferenttypesofISOdocumentshouldbenoted.ThisdocumentwasdraftedinaccordancewiththeeditorialrulesoftheISO/IECDirectives,Part2(seeWWW.iso.org/directives).ISOdrawsattentiontothepossibilitythattheimplementationofthisdocumentmayinvolvetheuseof（八）patent(三).ISOtak

14、esnopositionconcerningtheevidence,validityorapplicabilityofanyclaimedpatentrightsinrespectthereof.Asofthedateofpublicationofthisdocument,ISOhadnotreceivednoticeof（八）patent(三)whichmayberequiredtoimplementthisdocument.However,implementersarecautionedthatthismaynotrepresentthelatestinformation,whichmay

15、beobtainedfromthepatentdatabaseavailableatWWW.iso.org/patents.ISOshallnotbeheldresponsibleforidentifyinganyorallsuchpatentrights.Anytradenameusedinthisdocumentisinformationgivenfortheconvenienceofusersanddoesnotconstituteanendorsement.Foranexplanationofthevoluntarynatureofstandards,themeaningofISOsp

16、ecifictermsandexpressionsrelatedtoconformityassessment,aswellasinformationaboutISOsadherencetotheWorldTradeOrganization(WTo)principlesintheTechnicalBarrierstoTrade(TBT工seeWWW.iso.org/iso/foreword.htmLThisdocumentwaspreparedbyTechnicalCommitteeISO/TC201,Surfacechemicalanalysis,SubcommitteeSC8,Glowdis

17、chargespectroscopy.Thissecondeditioncancelsandreplacesthefirstedition(ISe)Il505:2012),whichhasbeentechnicallyrevised.Themainchangesareasfollows: thelistedtypesofarraydetectorshavebeenupdated; advancesinmeasurementtechniquesandapparatushaveexpandedtheapplicablesamplesizes,andmodificationshavebeenmade

18、tooptimizetheoptics,vacuumanddetectionsystems; thetext“settingofthehighvoltageforthedetectors“isreplacedwith“settingoftheparametersfordetectorsensitivitythroughoutthedocuments; theinstructionstooptimizethecratershapehasbeenchangedfrommandatorytooptional.Anyfeedbackorquestionsonthisdocumentshouldbedi

19、rectedtotheusersnationalstandardsbody.AcompletelistingofthesebodiescanbefoundatWWW.iso.org/membnrs.html.SurfacechemicalanalysisGeneralproceduresforquantitativecompositionaldepthprofilingbyglowdischargeopticalemissionspectrometry1 ScopeThisdocumentspecifiesaglowdischargeopticalemissionSpectrometric(G

20、D-OES)methodforthedeterminationofthethickness,massperunitareaandchemicalcompositionofsurfacelayerfilms.TheapplicabilityofthisdocumentislimitedtodescriptionofgeneralproceduresforquantificationofthechemicalcompositionandthicknessinGD-OEScompositionaldepthprofiling.Thisdocumentisnotdirectlyapplicablefo

21、rquantificationofindividualmaterialshavingvariousthicknessesandelementstobedetermined.2 NormativereferencesThefollowingdocumentsarereferredtointhetextinsuchawaythatsomeoralloftheircontentconstitutesrequirementsofthisdocument.Fordatedreferences,onlytheeditioncitedapplies.Forundatedreferences,thelates

22、teditionofthereferenceddocument(includinganyamendments)applies.ISO14707,SurfacechemicalanalysisGlowdischargeopticalemissionspectrometry(GD-OES)Introductiontouse3 TermsanddefinitionsNotermsanddefinitionsarelistedinthisdocument.ISOandIECmaintainterminologydatabasesforuseinstandardizationatthefollowing

23、addresses: ISOOnlinebrowsingplatform:availableathttps:WWW.iso.org/obp IECElectropedia:availableathttps:WWW.electropedia.org/4PrincipleTheanalyticalmethoddescribedinthisdocumentinvolvesthefollowingprocesses:a) cathodicsputteringofthesurfacelayerinadirectcurrentorradiofrequencyglowdischargedevice;b) e

24、xcitationoftheanalyteatomsandionsintheplasmaformedintheglowdischargedevice;c) Spectrometricmeasurementoftheintensitiesofcharacteristicspectralemissionlinesoftheanalyteatomsandionsasafunctionofsputteringtime(qualitativedepthprofile);d) conversionofthequalitativedepthprofileinunitsofintensityversustim

25、etomassfractionversusdepthbymeansofcalibrationfunctions(quantification).Calibrationofthesystemisachievedbymeasurementsoncalibrationspecimensofknownchemicalcompositionandmeasuredsputteringrate.5Apparatus5.1 Glowdischargeopticalemissionspectrometer5.1.1 GeneralTherequiredinstrumentationincludesanoptic

26、alemissionspectrometersystemconsistingofaGrimmtype6orsimilarglowdischargesource(directcurrentorradiofrequencypowered)andasimultaneousopticalspectrometerwhichshallbeinaccordancewithISO14707,capableofprovidingsuitablespectrallinesfortheanalyteelements.Sequentialopticalspectrometers(monochromators)aren

27、otsuitable,sinceseveralanalyticalwavelengthsmustbemeasuredsimultaneouslyathighdataacquisitionspeed.Anarraytypedetector,suchasachargecoupleddevice(CCD)1acomplementarymetal-oxide-semiconductordevice(CMOS)orachargeinjectiondevice(ClD)canalsobeusedforsimultaneousdetectiontocoverawidespectralrangeofthean

28、alyticallines.Theinnerdiameterofthehollowanodeoftheglowdischargesourceshouldbeintherange1mmto8mm.Acoolingdeviceforthinspecimens,suchasametalblockwithcirculatingcoolingliquid,isalsorecommended,butnotstrictlynecessaryforimplementationofthemethod.Sincetheprincipleofdeterminationisbasedoncontinuoussputt

29、eringofthesurfacelayer,thespectrometershallbeequippedwithadigitalreadoutsystemfortime-resolvedmeasurementoftheemissionintensities.Asystemcapableofadataacquisitionspeedofatleast100measurements/secondperspectralchannelisrecommended,but,foralargenumberofapplications,speedsof50measurements/secondperspec

30、tralchannelareacceptable.NOTEPulsedmodeofglowdischargesourceisavailableinsomecommercialinstrumentsandcanbebeneficialintheanalysisofheat-sensitivesamples,forreductionOfsputteringrate.5.1.2 SelectionofspectrallinesForeachanalytetobedetermined,thereexistanumberofspectrallineswhichcanbeused.Suitableline

31、sshallbeselectedonthebasisofseveralfactors,includingthespectralrangeofthespectrometerused,theanalytemassfractionrange,thesensitivityofthespectrallinesandanyspectralinterferencefromotherelementspresentinthetestspecimens.Forapplicationswhereseveraloftheanalytesofinterestaremajorelementsinthespecimens,

32、specialattentionshallbepaidtotheoccurrenceofself-absorptionofcertainhighlysensitivespectrallines(so-calledresonancelines).Self-absorptioncausesnonlinearcalibrationcurvesathighanalytemassfractionlevels,andstronglyself-absorbedlinesshouldthereforebeavoidedforthedeterminationofmajorelements.Suggestions

33、concerningsuitablespectrallinesaregiveninTabIeB.l.Spectrallinesotherthanthoselistedmaybeused,aslongastheyhavefavourablecharacteristics.5.1.3 Selectionofglowdischargesourcetype5.1.3.1 AnodesizeMostGD-OESinstrumentsonthemarketaredeliveredwithoptionstousevariousanodediameters,with2mm,4mmand8mmbeingthem

34、ostcommon.Someolderinstrumentshaveoneanodeonly,usually8mm,whilethemostcommonlyusedanodeinmoderninstrumentsis4mm.Alargeranoderequireslargerspecimensandhigherpowerduringanalysis;therefore,thespecimenisheatedtoagreaterextent.Howeverlalargeranodegivesrisetoaplasmaoflargervolumethatemitsmorelight,resulti

35、nginlowerdetectionlimits(i.e.higheranalyticalsensitivity).Furthermore,alargeranodehelpstomaskinhomogeneitywithinasurfacelayer.Thiscanbeanadvantagedependingontheapplication.Inalargenumberofapplications,the4mmanodeisagoodcompromise.However,insurfaceanalysisapplicationsitisrathercommontoencounterproble

36、msofoverheatingofthespecimensdueto,e.g.surfacelayersofpoorheatconductivityand/orverythinspecimens.Insuchcases,asmalleranodeispreferable(typically2mmor2,5mm),evenifthereissomelossofanalyticalsensitivity.5.1.3.2 TypeofpowersupplyTheglowdischargesourcecanbeeitheratypepoweredbyadirectcurrent(DC)powersup

37、plyoraradiofrequency(RF)type.ThemostimportantdifferenceisthattheRFtypecansputterbothconductiveandnon-conductivespecimens;hencethisistheonlytypethatcanbeusedfor,e.g.polymercoatingsandinsulatingoxidelayers.However,itistechnicallysimplertomeasureandcontroltheelectricalsourceparameters(voltage,current,p

38、ower)ofaDCtype.SeveralcommerciallyavailableGD-OESsystemscanbedeliveredwiththeoptiontoswitchbetweenDCandRFoperation,butRF-onlysystemsalsoexist.Inshort,thereareaverylargenumberofapplicationswhereDCorRFsourcescanbeusedandseveralwhereonlyanRFsourcecanbeused.5.1.3.3 ModeofoperationBothDCandRFsourcescanbe

39、operatedinseveraldifferentmodeswithrespecttothecontroloftheelectricalparameters(current,voltage,power)andthepressure.Thereareseveralreasonsforthis:一“historicalreasons(olderinstrumentshavesimplerbutfunctionalpowersupplies,whilethetechnologyhasevolvedsothatnewermodelshavemorepreciseandeasier-to-operat

40、esourcecontrol); differentmanufacturershavechosendifferentsolutionsforsourcecontrol; therearesomeapplication-relatedissueswhereaparticularmodeofoperationistobepreferred.Thisdocumentgivesinstructionsforoptimizingthesourceparametersbasedonseveralavailablemodesofoperation.Themostimportantreasonforthisi

41、stomaketheseinstructionscomprehensivesoastoincludeseveraltypesofinstruments.Inmostapplications,thereisnomajordifferencebetweenthesemodesintermsofanalyticalperformance,butthereareotherdifferencesintermsofpracticalityandeaseofoperation.Forinstance,asystemequippedwithactivepressureregulationwillautomat

42、icallybeadjustedtothesameelectricalsourceparameterseverytimeaparticularanalyticalmethodisused.Withoutthistechnology,somemanualadjustmentofthepressuretoachievethedesiredelectricalsourceparametersisnormallyrequired.Alternatively,amethodtocorrectforimpedancevariationsbymeansofempiricallyderivedfunction

43、sEcanbeused,provideditisimplementedinthesoftwareoftheGD-OESsystems.NOTEInthiscontext,whatisknownastheemissionyieldformsthebasisforcalibrationandquantificationasdescribedinthisdocument(2.Theemissionyieldhasbeenfoundtovarywiththecurrent,thevoltageand,toalesserextent,thePreSSUreZiii.itisimpossibleinpra

44、cticetomaintainallthreeparametersconstantforalltestspecimens,duetovariationsintheelectricalcharacteristicsofdifferentmaterials.Inseveralinstrumenttypes,theelectricalsourceparameterstheplasmaimpedance)canthereforebemaintainedconstantbymeansofautomaticsystemsthatvarythepressureduringanalysis.6Adjustin

45、gtheglowdischargespectrometersystemsettings6.1 GeneralFollowthemanufacturerlSinstructionsorlocallydocumentedproceduresforpreparingtheinstrumentforuse.RFsourcesdifferfromDCsourcesintherespectthatforseveralinstrumentmodels,onlytheapplied(forward)RFpowercanbemeasured,nottheactualpowerdevelopedintheglow

46、dischargeplasma.TheappliedRFpowerisnormallyintherange10Wto100W,butitneedstobenotedthattheRFpowerlossesinconnectors,cables,etc.varyconsiderablybetweendifferentinstrumentmodels.Typicalpowerlossesareintherange10%to50%oftheappliedpower.Furthermore,thepossibilitiestomeasuretheadditionalelectricalparamete

47、rsvoltageandcurrentintheplasmaaremoreorlessrestrictedduetotechnicaldifficultieswithRFsystems,andseveralexistinginstrumentmodelscanonlymeasuretheappliedRFpower.ThereisnodifferencebetweenDCandRFconcerningthepossibilitiestomeasurethepressure.However,therearelargepressuresdifferentialsinaGrimmtypesource

48、andpressurereadingsobtaineddependonthelocationofthepressuregauge.Someinstrumentmodelshaveapressuregaugeattachedtomeasuretheactualpressureintheplasma,whileothershaveapressuregaugelocatedona“lowpressure1/sideofthesourceclosertothepump.Therefore,thepressurereadingscan,forseveralinstruments,justbeusedtoadjustthesourceparametersofthatparticularinstrument,notasameasureoftheactualoperatingpressureintheplasma.Fortestspecimens,calibrationsamplesandvalidationsamples,itisimportanttoensu