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15 16 US 7,678,712B2 whereinX=1-3,RareindependentlyH,alkyland/oraryl. Optionaly,theSurfacemodificationagentcomposition WhenanyRarealkyland/oraryl.Inpreferredembodiments, RisselectedfromH,CH,CHs andRandR arebothCH. Thustri-functionalSurfacemodificationagentsinclude,e.g., tris(dimethylamino)methylsilane,tris(dimethylamino)phe nylsilane,and/ortris(dimethylamino)silane.Inadition,dis ubstitutedsilanesmaybeusedSuchashexamethylcyclotrisi laZane, bisdimethylaminodimethylsilane, and bisdiethylaminodimethylsilane. Inyetanotherembodiment,aSuitablesilaneaccordingto10 theinventionhasthegeneralformulaof RSi(ON=CR2) orRSiOC(R)—R". whereinx=1-3andtheRgroupsareindependentlyH,alkyl and/oraryl,R'maybeH,alkyl,aryl,alkoxyoraryloxy,andR"15 maybealkylorcarbonyl.Thusmodificationagentsinclude, e.g.,methyltris(methylethylketoxime)Silaneor2-trimethylsi loxypent-2-ene-4-onerespectively. includesasolventcompositioncapableofsolubilizingwith thecomponentcapableofalkylatingorarylatingsilanolmoi etiesoftheorganosilicateglasdielectricfilmviasilylation, andtheactivatingagent.Suitablesolventscompositionsnon exclusivelyinclude,forexample,ketones,ethers,esters, hydrocarbons,alcohols,carboxylicacids,amides,andcom binationsthereof.Usefulsolventsnon-exclusivelyinclude 3-pentanone,2-heptanone,gammabutyrolactone,propylene glycolmethyletheracetate,aceticacid,andcombinations thereof.Thesolvent,whenemployed,isusualypresentinthe Surfacemodificationagentcompositioninanamountoffrom about0weightpercenttoabout99.9weightpercent,more usuallyfromabout50weightpercenttoabout99weight percent,andmostusualyfromabout70weightpercentto about97weightpercent.Inanotherembodimentoftheinven tion,theSurfacemodificationagentcompositionincludesa Supercriticalsolvent.SuchasSupercriticalcarbondioxide. Optionaly,theSurfacemodificationagentcomposition includesacorrosioninhibitor,suchasacorrosioninhibitor whichchelateswithcopper.Suchmayincludebenzotriazole, tolyltriazole,andcombinationsthereof.Thecorrosioninhibi tor,whenemployed,isusuallypresentintheSurfacemodifi cationagentcompositioninanamountoffromabout0.001 weightpercenttoabout10weightpercent,moreusualyfrom about0.01weightpercenttoabout5weightpercent,andmost usuallyfromabout0.2weightpercenttoabout1weight percent. TheSurfacemodificationagentcompositionisformedby blendingtheselectedcomponentsintoamixture.TheSurface modificationagentcompositioncontactsthedamagedsilica dielectricfilmasavapor,gas,and/orplasma.Contactingby applyingagasorvaporoftheSurfacemodificationagentto thefilmisprefered.Suchcontactingmaybeconductedata temperatureoffromabout0°C.toabout450°C.,preferably fromabout20°C.toabout450°C.Thecontactingmaybe conductedforfromabout1secondtoabout2hours,prefer ablyfromabout10secondstoabout30minutes.Preferably thecontactingisconductedundercontroledchambercondi tionsusingacariergas.Suchasnitrogen,heliumorargon whichservestocontrolthechamberconditions(presure) andtouniformlydistributethereactants,i.e.thesurface modificationcompositionincludingactivationagentsand solventsused.Preferablythecariergasismisciblewiththese components. TheSurfacemodificationagentcompositionmayalsobe appliedbychemicalvapordepositiontechniques.Chemical vapordepositionprocessesarewellknowntothoseskiledin theartandchemicalvapordepositionreactorsarewidely commerciallyavailable.Onesuitablereactorismodel SK-23-6-93commerciallyavailablefromVactronicEquip mentLabsofBohemia,NewYork.Othersmaybeobtained fromASM International,NovellusSystems,orApplied Materials.Thechemicalvapordepositingisconductedby heatingatarelativelylowtemperatureoffromabout100°C. toabout C.,preferablyfromabout200°C.toabout400°C. andmorepreferablyfromabout350°C.toabout400°C.The heatingduringthechemicalvapordepositingisconductedat arelativelyshorttimeoffromabout30secondstoabout3 minutes.Intheproces,filmonSubstrateisplacedinthe chemicalvapordepositionreactor.Thereactorissealedand evacuatedtolesthanonemilitorofambientbackground gaspresure.Inthepreferredembodiment,aflowofSurface modificationagentcompositionandaninertgas,Suchas nitrogen,heliumorargonisestablishedandthechamberis heateduntilitisstabilizedtothedesiredreactiontemperature andgasflowrate.Thegasflowrangesfrom0toabout5,000 Inyetanotherembodiment,aSuitablesilaneaccordingto theinventionhasthegeneralformulaof RSi(NCOR) orRSi(NCO) whereinx=1-3,RgroupsareindependentlyH,alkyland/or aryl.ThusSurfacemodificationagentsinclude,e.g., dimethylsilyldiformamide,dimethylsilyldiacetamide,dim ethylsilyldisocyante,trimethylsilyltrisocyante. Inyetafurtherembodiment,aSuitablesilaneaccordingto theinventionhasthegeneralformulaof RSiCl whereinx=1-3,isH,alkyloraryl.Inonepreferedembodi ment,RisCH.Thustri-functionalsurfacemodification agentsinclude,e.g., methyltrichlorosilane. Inamorepreferedembodiment,thesurfacemodification agentincludesoneormoreorganoacetoxysilaneswhichhave thefollowinggeneralformula, (R),Si(OCOR2), Preferably,Xisanintegerranginginvaluefrom1to2,and Xandycanbethesameordiferentandyisanintegerranging fromabout2toabout3,orgreater. 25 30 35 40 45 Usefulorganoacetoxysilanes,includingmultifunctional alkylacetoxysilane and/or arylacetoxysilane compounds, include,simplybywayofexampleandwithoutlimitation, methyltriacetoxysilane(“MTAS),dimethyldiacetoxysilane (DMDAS),phenyltriacetoxysilaneanddiphenyldiacetoxysi50 laneandcombinationsthereof. Thecomponentcapableofalkylatingorarylatingsilanol moietiesoftheorganosilicateglasdielectricfilmviasilyla tionisusualypresentintheSurfacemodificationagentcom positioninanamountoffromabout0.1weightpercentto55 about100weightpercent,moreusualyfromabout1weight percenttoabout50weightpercent,andmostusualyfrom about3weightpercenttoabout30weightpercent. TheSurfacemodificationagentcompositionmayoption alycontainoneormoreoftheactivatingagentslistedabove.60 Whenincorporatedwithinthesurfacemodificationagent composition,theactivatingagentisusualypresentinan amountoffromabout0.0001weightpercenttoabout10 weightpercent,moreusuallyfromabout0.001weightper centtoabout1weightpercent,andmostusualyfromabout65 0.01weightpercenttoabout0.1weightpercentofthesurface modificationagentcomposition.PDF Image | VAPOR PHASE TREATMENT OF DELECTRIC MATERALS
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