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US 7,678,712B2 56 dielectricmaterials.One materialwithalowdielectriccon stantissilicawhichcanbeappliedasafoameddielectric material.Forthelowestposibledielectricvalues,airisintro duced into silica dielectric materials. Air has a dielectric constantof1,andwhenairisintroducedintoasilicadielectric materialintheformofnanoporousornanometer-scalepore structures,relativelylowdielectricconstantsareachieved.It shouldbeunderstoodthatunlesthe“SiO,”functionalgroup isspecificalymentionedwhentheterm“silica”isemployed, theterm“silica”asusedherein,forexample,withreference10 toporousandnon-porousdielectricfilms,isintendedtorefer tosilicateandorganosilicatedielectricfilmspreparedfroman organicorinorganicglasbasematerial,e.g.,anySuitable startingmaterialcontainingoneormoresilicon-baseddielec15 tricprecursors.Itshouldalsobeunderstoodthattheuseof singulartermshereinisnotintendedtobesolimited,but, whereapropriate,alsoencompassestheplural,e.g.,exem plaryprocessesoftheinventionmaybedescribedasapplying toandproducinga“film'butitisintendedthatmultiplefilms canbeproducedbythedescribed,exemplifiedandclaimed proceses,asdesired.Theterm,“film'asusedhereinwith regardtothedielectricmaterialsisintendedtoencompassany othersuitableformorshapeinwhichsuchsilicadielectric materialsareoptionalyemployed.Nanoporoussilicais25 atractivebecauseitemployssimilarprecursors,including organic-Substituted silanes, e.g., tetramethoxysilane (“TMOS)and/ortetraethoxysilane(“TEOS),asareused forthecurentlyemployedspin-on-glases(“SOG”)and chemicalvapordisposition(“CVD)silicaSiO.Asused30 herein,theterms“void’and“pore”meanafrevolumein whichamassisreplacedwithagasorwhereavacuumis generated.Thecompositionofthegasisgenerallynotcriti cal,andappropriategasesincluderelativelypuregasesand mixturesthereof,includingair.Thenanoporouspolymermay35 compriseapluralityofpores.Poresaretypicalyspherical, butmayalternativelyoraditionalyhaveanysuitableshape, includingtubular,lamelar,discoidal,orothershapes.The poresmaybeuniformlyorrandomlydispersedwithinthe porouspolymer.Itisalsocontemplatedthattheporesmay40 haveanyappropriatediameter.Itisfurthercontemplatedthat atleastSomeporesmayconnectwithadjacentporestocreate astructurewithasignificantamountofconnectedor“open’ porosity. Nanoporoussilicafilmshavepreviouslybeenfabricatedby45 anumberofmethods.Suitablesilicon-basedprecursorcom positionsandmethodsforformingnanoporoussilicadielec tricfilms,aredescribed,forexample,bythefollowingco owned U.S. Pat. Nos. 6,048,804, 6,022,812; 6,410,149: 6,372,666;6,509,259;6,218,497;6,143,855,6,037,275;50 6,042,994; 6,048,804: 6,090,448; 6,126,733; 6,140,254; 6,204.202:6,208,041;6,318,124and6,319,855alincorpo ratedhereinbyreferenceherein. Otherdielectricandlowdielectricmaterialscompriseinor ganic-basedcompounds,suchasthesilicon-baseddisclosed55 incommonlyassignedpendingU.S.patentaplicationSer. No.10/078,919filedFeb.19,2002:(forexampleNANO GLASSR)andHOSPR)productscommerciallyavailable fromHoneywellInternationalInc.).Thedielectricandlow dielectricmaterialsmaybeappliedbyspincoatingthemate60 rialontotheSurface,dipcoating,spraycoating,chemical vapordeposition(CVD),rolingthematerialontothesurface, drippingthematerialontotheSurface,and/orspreadingthe materialontothesurface.Dielectricsusefulforthisinvention includeCVDdepositedmaterials,suchascarbondoped65 oxidesforexample,BlackDiamond,commerciallyavailable fromAppliedMaterials,Inc.,Coral,commerciallyavailable fromNovellus,Aurora,whichiscommerciallyavailablefrom ASM,andOrion,whichiscommerciallyavailablefrom Trikon. Asusedherein,thephrases'spin-onmaterial','spin-on organicmaterial','spin-oncomposition'and'spin-oninor ganiccomposition'maybeusedinterchangeableandreferto thosesolutionsandcompositionsthatcanbespun-ontoa SubstrateorSurfaceusingthespincoatingaplicationpro ces.Examplesofsilicon-basedcompoundscomprisesilox anecompounds,suchasmethylsiloxane,methylsilsesquiox ane, phenylsiloxane, phenylsilsesquioxane, methylphenylsiloxane,methylphenylsilsesquioxane,sila Zanepolymers,silicatepolymersandmixturesthereof.A contemplatedsilaZanepolymerisperhydrosilaZane,which hasa“transparentpolymerbackbonewherechromophores canbeatached.Spin-on-glassmaterialsalsoincludessilox anepolymersandblockpolymers,hydrogensiloxanepoly mersofthegeneralformula(Ho-SiOs-o),andhydrogen silsesquioxanepolymers,whichhavetheformula(HSiOs), whereXisgreaterthanaboutfour.Alsoincludedarecopoly mersofhydrogensilsesquioxaneandanalkoxyhydridosilox ane or hydroxyhydridosiloxane. Spin-on glas materials aditionalyincludeorganohydridosiloxanepolymersofthe generalformula(Ho-LoSiOS-2.o),(Ro-oSiOS-20), and organohydridosilsesquioxanepolymersofthegeneralfor mula(HSiOs),(RSiOs),wheremisgreaterthanZeroand theSumofnandmisgreaterthanaboutfourandRisalkylor aryl.Someusefulorganohydridosiloxanepolymershavethe sumofnandmfromaboutfourtoabout5000whereRisa C-C alkylgrouporaC-C arylgroup.Theorganohydri dosiloxaneandorganohydridosilsesquioxanepolymersare alternativelydenotedspin-on-polymers.Somespecific examplesincludealkylhydridosiloxanes,suchasmethylhy dridosiloxanes,ethylhydridosiloxanes,propylhydridosilox anes,t-butylhydridosiloxanes,phenylhydridosiloxanes;and alkylhydridosilsesquioxanes,suchasmethylhydridosilses quioxanes,ethylhydridosilsesquioxanes,propylhydridosils esquioxanes,t-butylhydridosilsequioxanes,phenylhydri dosilsesquioxanes,andcombinationsthereof.Severalofthe contemplatedspin-onmaterialsaredescribedinthefollow ingissuedpatentsandpendingaplications,whichareherein incorporatedbyreferenceintheirentirety:U.S.Pat.Nos. 6,506,497;6,365,765;6,268.457;6,177,199;6,358,559; 6,218,020; 6,361,820; 6,218,497; 6,359,099: 6,143,855; 6,512,071,U.S.patentaplicationSer.No.10/001,143filed Nov. 10, 2001; PCT/US00/15772 filed Jun. 8, 2000, and PCT/US00/00523filedJan.7,1999. Solutionsoforganohydridosiloxaneandorganosiloxane resinscanbeutilizedforformingcagedsiloxanepolymer filmsthatareusefulinthefabricationofavarietyofelectronic devices,micro-electronicdevices,particularlysemiconduc torintegratedcircuitsandvariouslayeredmaterialsforelec tronicandsemiconductorcomponents,includinghardmask layers,dielectriclayers,etchstoplayersandburiedetchstop layers.Theseorganohydridosiloxaneresinlayersarecompat iblewithothermaterialsthatmightbeusedforlayeredmate rialsanddevices,suchasadamantane-basedcompounds,dia mantane-based compounds, silicon-core compounds, organicdielectrics,andnanoporousdielectrics.Compounds thatareconsiderablycompatiblewiththeorganohydridosi loxaneresinlayerscontemplatedhereinaredisclosedinU.S. Pat.Nos.6,214,746;6,171,687;6,172,128;6,156,812,U.S. ApplicationSer.No.60/350,187filedJan.15,2002;U.S. patentaplicationSer.No.09/538,276;U.S.patentapplica tionSer.No.09/544,504;U.S.patentaplicationSer.No. 09/587,851;andU.S.60/347,195filedJan.8,2002:PCT ApplicationPCT/US01/32569filedOct.17,2001;PCTPDF Image | VAPOR PHASE TREATMENT OF DELECTRIC MATERALS
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