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11 mentsremoveatleastaportionofpreviouslyexistingcarbon containingmoietiesfromthesilicateororganosilicatedielec tricfilm.Typicallythesetreatmentsremovefromabout5to about95%ofpreviouslyexistingcarboncontainingmoieties. Theinventiveprocessisconductedtoaddbackthesecarbon containingmoietiestothesilicateororganosilicatedielectric film. Inordertoremedythisproblem,theorganosilicateglas dielectricfilmsaremadesubstantialyfreofsilanolsand waterbytreatmentwithasurfacemodificationagentto10 restorecarboncontainingmoietiesandusualyincreasethe hydrophobicityoftheorganosilicateglasdielectricfilm. Thismakesthefilmresistanttostreses,suchasinducedby metalshrinkageduringannealing,stresfromotherdielectric layers,andstresduringpackaging,thusdetersundesirable15 voidsfromforminginsidethedielectricmaterialbetweenthe viasandtrenches. Etching and plasma remove hydrophobic functional groups.Damagetoorganosilicateglasdielectricfilmsdur ingsemiconductormanufacturingprocessesresultsfromthe aplicationofaggressiveplasmasand/oretchingreagentsto etchtrenchesandviasintodielectricfilms.Plasmasarealso usedtoremovephotoresistfilmsduringfabricationofsemi conductordevices.Theplasmasusedaretypicalycomposed25 oftheelementsoxygen,fluorine,hydrogen,carbon,argon, heliumornitrogen(intheformoffreatoms,compounds, ionsand/orradicals). 12 Inordertosolvetheabovementionedproblemstheinven tivetreatmentmethodsimpartingdesirablepropertiesto dielectricfilmspresentonaSubstrateduringtheprocessof fabricatingasemiconductororICdevice. Thefirststepoftheinventiveprocessisanoptionalbut preferedstepofdehydratingatleastaportionofasilicateor organosilicatedielectricfilmonaSubstrate.Suchmaybe donebyanymeansknownintheartSuchasheatingata temperatureoffromabout20°C.toabout450°C.,preferably fromabout100°C.toabout400°C.forfromabout10 secondstoabout4hours,preferablyfromabout1minuteto 120minutes,andmorepreferablyfromabout10secondsto about30minutes.Thedehydrationbakeremovessubstan tialyalofthemoisturewhichmayhavebeenadsorbedinthe dielectricfilm.Removalofmoisturefromthedielectricprior toSurfacemodificationagenttreatmentrenderstheSubse quenttreatmentsmoreefective. Thenextstepoftheinventiveprocessisanoptionalbut preferedstepofapplyinganactivatingagentforaSurface modificationagentcompositiontothesilicateororganosili catedielectricfilm.Usefulactivatingagentsnon-exclusively includeamines,oniumcompoundsandalkalimetalhydrox ides.Usefulactivatingagentsincludeammonium com pounds,phosphoniumcompounds,Sulfoniumcompounds andiodoniumcompounds.Includedareactivatingagents whichmaybealkylamines,arylamines,alcoholaminesand mixturesthereofwhichsuitablyhaveaboilingpointofabout US 7,678,712B2 Dielectricfilmswhichareexposedtotheseplasmasduring 100°C.orhigher,usualyabout125°C.orhigherandmore trench,via,etchand/orphotoresistremovalareeasily30 degradedordamaged.Porousdielectricfilmshaveavery highsurfaceareaandarethereforeparticularlyvulnerableto plasmasdamage.Inparticular,silicabaseddielectricfilms whichhaveorganiccontent(suchasmethylgroupsbondedto Siatoms)arereadilydegradedbyoxygenplasmas.The35 organicgroupisoxidizedintoCO andasilanolorSi-OH groupremainsonthedielectricSurfacewheretheorganic groupformerlyresided.Porousandnon-porouslowdielectric constantsilicafilmsdependonSuchorganicgroups(onSur faces)toremainhydrophobic.Lossofthehydrophobicity40 makesthedielectricconstantrise(thelowdielectricconstant ofsuchfilmsisthekeydesiredpropertyofsuchmaterials). WetchemicaltreatmentsarealsousedinICproductionfor thepurposeofremovingresiduesleftoveraftertrenchorvia etching.Thechemicalsusedareoftensoaggressivetheywil45 atackandremoveorganicgroupsinsilicabaseddielectric films,especialyporoussilicafilms.Again,thisdamagewil causethefilmstolosetheirhydrophobicity.Wetchemical etchantsinclude,forexample,amides,suchasN-methylpyr rolidinone,dimethylformamide,dimethylacetamide:alco50 holssuchasethanoland2-propanol;alcoholaminessuchas ethanolamine;aminessuchastriethylamine;diaminesSuch asethylenediamineandN,N-diethylethylenediamine;tri aminessuchasdiethylenetriamine,diamineacidssuchas ethylenediaminetetraceticacid“EDTA';organicacidssuch55 asaceticacidandformicacid;theammoniumsaltsoforganic acidssuchastetramethylammoniumacetate;inorganicacids SuchasSulfuricacid,phosphoricacid,hydrofluoricacid; fluoridesaltssuchasammoniumfluoride;andbasessuchas ammoniumhydroxideandtetramethylammoniumhydrox60 ide;andhydroxylamine;commercialformulationsdevel opedforpostetchwetcleaningsuchasEKC505,525,450, 265,270,and630(EKCCorp.,HaywardCalif.),andACT CMIandACT-690(AshlandChemical,Hayward,Calif.).to namebutafewart-knownetchants.Ashingagentsinclude 65 plasmasderivedfromhydrogen,nitrogen,helium,argon, oxygen,andmixturesderivedtherefrom,andthelike. usuallyabout150°C.orhigher.Catalystexposuremaybe conductedbyapplyingagasorvaporoftheactivatingagent tothefilmonthesubstrateatatemperatureoffromabout20° C.toabout450°C.,preferablyfromabout100°C.toabout 400°C.forfromabout10secondstoabout30minutes, preferablyfromabout1minuteto30minutes. Usefulamineactivatingagentincludeprimaryamines, secondaryamines,tertiaryamines,ammonia,andquaternary ammonium salts. Useful amines are monoethanolamine, diethanolamine, triethanolamine, monoisopropanolamine, tetraethylenepentamine, 2-(2-aminoethoxy)ethanol: 2-(2- aminoethylamino)ethanolandmixturesthereof.Inadesired embodimentoftheinventiontheactivatingagentcomprises tetramethylammoniumacetate,tetrabutylammoniumacetate orcombinationsthereof.Otheractivatingagentsinclude Sodiumhydroxide,potassiumhydroxide,lithiumhydroxide andammoniumhydroxide.Theactivatingagentmaybe appliedtothefilmbyanyconvenientmethodsuchascoating, spin-on,diping,vaporaplication,chemicalvapordeposi tion,andthelike.Theactivatingagentisusualyappliedtothe filmamountoffromabout0.0001weightpercenttoabout10 weightpercent,moreusualyfromabout0.001weightper centtoabout1weightpercent,andmostusualyfromabout 0.01weightpercenttoabout0.1weightpercent,basedonthe weightoftheSubsequentlyappliedSurfacemodification agentcomposition. Thenextstepintheinventivemethodiscontactingthe silicateororganosilicatedielectricfilmwithasurfacemodi ficationagentcompositioninavapororgaseousstate.For purposesofthisinvention,suchcontactingofthesilicateor organosilicatedielectricfilmwithasurfacemodification agentcompositionisdefinedasacontactingofthefilmwhich eitherhasorhasnotbeenfirstdehydratedandhasorhasnot beencontactedwithanactivatingagentfortheSurfacemodi ficationagent. TheSurfacemodificationagentcompositioncomprisesa componentcapableofalkylatingorarylatingsilanolmoieties orbondscreatedbyremovalofcarboncontainingmoietiesPDF Image | VAPOR PHASE TREATMENT OF DELECTRIC MATERALS
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