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US 7,678,712B2 34 availablechemicalcompatiblewiththelow-kdielectric. Additionallyadehydrationbakemaybeperformedbeforethe Surfacemodificationagenttreatment,toincreaseeffective nessoftheSurfacemodificationagenttreatment. Theefectivenesofthesurfacemodificationagenttreat mentcanbeverifiedusingunpatternedlow-kdielectricfilms Subjectedtoetchingandashingprocessingfollowedbythe (b)optionalyapplyinganactivatingagentforasurfacemodi ficationagentcompositiontothesilicateororganosilicate dielectricfilmbychemicalvapordeposition;then (c)contactingthesilicateororganosilicatedielectricfilm withaSurfacemodificationagentcompositionbychemical vapordepositionoftheSurfacemodificationagentcomposi tiontothesilicateororganosilicatedielectricfilm,wherein theSurfacemodificationagentcompositioncomprisesacom ponentcapableofalkylatingorarylatingsilanolmoietiesor bondscreatedbyremovalofcarboncontainingmoietiesfrom thesilicateororganosilicatedielectricfilmviasilylation;said contactingbeingconductedunderconditionsSuficienttoadd carboncontainingmoietiestothesilicateororganosilicate dielectricfilmthroughatleastaportionofadepththereof. The invention further provides a method of imparting hydrophobicpropertiestoasilicateororganosilicatedielec tricfilmonasubstrate,whichsilicateororganosilicatedielec tricfilmeithercomprisessilanolmoietiesorwhichsilicateor organosilicatedielectricfilmhashadatleastsomepreviously presentcarboncontainingmoietiesremovedtherefrom,the methodcomprising: (a)optionalydehydratingatleastaportionofasilicateor organosilicatedielectricfilmonasubstrate;then Surfacemodificationagenttreatment.A sucesfulSurface modificationagenttreatmentresultsinincreasedcarboncon centrationthatcanbemeasuredbyFTIR,EDX,orXPS 10 techniques.Aditionaly,awatercontactangleincreaseis sen,whichdemonstratesthehydrophobicnatureofthepost treatmentSurface.TheSurfacemodificationagenttreatedfilm alsoshowsalowerdielectricconstantcomparedtoanetched/ ashedfilmthatisnottreatedwithSurfacemodificationagent. Inpatternedwafers,theefectivenesofthesurfacemodifi cationagenttreatmentisdemonstratedbyreductionorelimi nationofVoidsinthelow-kdielectricinnarrowspaces betweencoppertrenchesafteracopperannealtreatmentfol lowingelectroplatingofcopper,andalsobylowerprofile changeintrenchesorviasafterexposuretoreactivesolvents. Ithasbeenfoundthattheeffectivenessofsilanebasedsurface modificationagentsisenhancesbyanactivatingagentSuchas anamine,anoniumcompoundoranalkalimetalhydroxide. SUMMARY OF THE INVENTION 25 (b)optionalyapplyinganactivatingagentforasurfacemodi Theinventionprovidesamethodfortreatingasilicateor organosilicatedielectricfilmonaSubstrate,whichsilicateor organosilicatedielectricfilmeithercomprisessilanolmoi30 etiesorwhichsilicateororganosilicatedielectricfilmhashad atleastsomepreviouslypresentcarboncontainingmoieties removedtherefrom,themethodcomprising: (a)optionalydehydratingatleastaportionofasilicateor35 organosilicatedielectricfilmonaSubstrate;then (b)optionalyapplyinganactivatingagentforasurfacemodi ficationagentcompositiontothesilicateororganosilicate dielectricfilm;then 40 (c)contactingthesilicateororganosilicatedielectricfilm withasurfacemodificationagentcompositioninavaporor gaseousstate,whereintheSurfacemodificationagentcom positioncomprisesacomponentcapableofalkylatingor arylatingsilanolmoietiesorbondscreatedbyremovalof45 carboncontainingmoietiesfromthesilicateororganosilicate dielectricfilmviasilylation;saidcontactingbeingconducted underconditionssuficientto(i)or(i)or(i): (i)addcarboncontainingmoietiestothesilicateororgano silicatedielectricfilm,or (i)sealSurfaceporesofthesilicateororganosilicatedielec tricfilm,whenthefilmisporous;or ficationagentcompositiontothesilicateororganosilicate dielectricfilmbychemicalvapordeposition;then (c)contactingthesilicateororganosilicatedielectricfilm withaSurfacemodificationagentcompositionbychemical vapordepositionoftheSurfacemodificationagentcomposi tiontothesilicateororganosilicatedielectricfilm,wherein theSurfacemodificationagentcompositioncomprisesacom ponentcapableofalkylatingorarylatingsilanolmoietiesor bondscreatedbyremovalofcarboncontainingmoietiesfrom thesilicateororganosilicatedielectricfilmviasilylation;said contactingbeingconductedunderconditionssuficientto(i) or(i)or(i): (i)addcarboncontainingmoietiestothesilicateororgano silicatedielectricfilmthroughatleastaportionofadepth thereof,or (i)sealSurfaceporesofthesilicateororganosilicatedielec tricfilm;or (i)firstaddcarboncontainingmoietiestothesilicateor organosilicatedielectricfilmthroughatleastaportionofa depththereof,andthensealsurfaceporesofthesilicateor organosilicatedielectricfilm. (i)firstaddcarboncontainingmoietiestothesilicateor organosilicatedielectricfilm,andthensealSurfaceporesof55 thesilicateororganosilicatedielectricfilm,whenthefilmis porous. FIG.1isaschematicrepresentationofanequipmentcon figurationforperformingtheinventivemethod. FIG.2isaschematicrepresentationofanotherequipment configurationforperformingtheinventivemethod. FIG.3isaschematicrepresentationofyetanotherequip mentconfigurationforperformingtheinventivemethod. DETAILED DESCRIPTION OF THE INVENTION Inthecontextofthepresentinvention,dielectricmaterials havinglowdielectricconstants,typicalybelow3areespe cialydesirablebecausetheytypicalyallowfastersignal propagation,reducecapacitiveefectsandcrostalkbetween conductorlines,andlowerVoltagestodriveintegratedcir cuits.Thisinventionrelatestobothporousandnon-porous Theinventionalsoprovidesamethodofpreventingvoids inadamagedsilicateororganosilicatedielectricfilmona Substrate, which silicate or organosilicate dielectric film eithercomprisessilanolmoietiesorwhichsilicateororgano silicatedielectricfilmhashadatleastsomepreviously presentcarboncontainingmoietiesremovedtherefrom,the methodcomprising: (a)optionalydehydratingatleastaportionofasilicateor organosilicatedielectricfilmonaSubstrate;then 60 65 15 50 BRIEF DESCRIPTION OF THE DRAWINGSPDF Image | VAPOR PHASE TREATMENT OF DELECTRIC MATERALS
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