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13 fromthesilicateororganosilicatedielectricfilmviasilyla tion;saidcontactingbeingconductedunderconditionssuffi cientto(i)or(i)or(i): (i)addcarboncontainingmoietiestothesilicateororgano silicatedielectricfilm,or (i)sealSurfaceporesofthesilicateororganosilicatedielec tricfilm,whenthefilmisporous;or (i)firstaddcarboncontainingmoietiestothesilicateor organosilicatedielectricfilm,andthensealSurfaceporesof thesilicateororganosilicatedielectricfilm,whenthefilmis porous. 10 14 ethylsilyl)acetamide, 2-(trimethylsilyl) acetic acid, n-(trimethylsilyl)imidazole, trimethylsilylpropiolate, trim ethylsilyl(trimethylsiloxy)-acetate, nonamethyltrisilaZane, hexamethyldisiloxane, trimethylsilanol, triethylsilanol, triphenylsilanol,t-butyldimethylsilanol,diphenylsilanediol, trimethoxysilane,triethoxysilane,trichlorosilane,andcom binationsthereof.Inonenoteworthyembodiment,thesurface modificationagentismethyltriacetoxysilane.Inapreferred embodimenttheSurfacemodificationagentisdimethyldiac etoxysilane. AdditionalSurfacemodificationagentsincludemultifunc tionalSurfacemodificationagentsasdescribedindetailin U.S.Pat.No.6,208,014,incorporatedbyreferenceherein,as described above. Such multifunctional surface modification agentscanbeappliedineithervaporform,gaseousform,or bychemicalvapordepositing,optionalywithorwithout co-solvents. Suitable co-solvents include, e.g., ketones, such as acetone,disopropylketone,2-heptanone,3-pentanone,and others,asdescribedindetailinco-ownedU.S.Pat.No.6,395, 651,thedisclosureofwhichisincorporatedbyreference herein. Forexample,asdescribedindetailinU.S.Pat.No.6,208, 014,certainpreferedsurfacemodificationagentswilhave twoormorefunctionalgroupsandreactwithSurfacesilanol functionalgroupswhileminimizingmasspresentoutsidethe structuralframeworkofthefilm,andinclude,e.g.,Surface silanolsmaycondensewithSuitablesilanolssuchas A Suitable Surface modification agent composition includesoneormoreSurfacemodificationagentsableto15 removesilanolgroupsfromtheSurfaceofanetchedand/or ashedorganosilicateglasdielectricfilmthatitisdesiredto renderhydrophobic.Thesemaybesilane,silaZane,silanols, orcarboxysilyl.Forexample,aSurfacemodificationagentis acompoundhavingaformulaselectedfromtheFormulas: (1)—SiRNR' inwheren-2andmaybecyclic;(2) RSiNR'SiR,(3)(RSi)N;(4)RSiNR';(5)RSi(NR): (6)RSi(NR),(7)R,SiCl,(8)R,Si(OH),(9)RSiOSiR's, (10)R,Si(OR),(1)R,Si(OCOR),(12)R,SiH,(13)R,Si25 OC(R')—R" andcombinationsthereof, US 7,678,712B2 whereinXisanintegerrangingfrom1to3,yisaninteger rangingfrom1to3Suchthaty=4-X;eachRisanindepen dentlyselectedfromhydrogenandahydrophobicorganic moiety.TheRgroupsarepreferablyindependentlyselected30 fromthegroupoforganicmoietiesconsistingofalkyl,aryl andcombinationsthereof.TheR'groupmaybeH,alkyl,aryl, whereinx=1-3,andeachRisindependentlyselectedmoi orcarbonylsuchasCOR,CONR,COR.TheR"maybealkyl orcarbonylsuchasCOR,CONR,COR ForalSurfacemodificationagents,thereactivesilylgroup35 mustcontainahydrolyzableleavinggroupSuchasbutnot limitedto—Cl,—Br.—I,—OR, NR (wherex=1-2), OCOR, OCOR, NRCOR, NRCOR, NR CONR,—SR, SOR.Forreactionofthesurfacemodifi cationagent,hydrolysismayoccurspontaneouslywithmois40 turepresentduringtheSurfacemodificationagentaplication andproces,orpre-hydrolysismaybeforcedduringthefor mulationproces. Thealkylmoietyiseitherfunctionalizedornon-function alizedandisderivedfromgroupsofStraightalkyl,branched45 alkyl,cyclicalkylandcombinationsthereof,andwhereinsaid alkylmoietyrangesinsizefromC toaboutCs.Thefunc tionalizationmaybeacarbonyl,ahalide,anamine,analco hol,anether,asulfonylorsulfide.Thearylmoietyissubsti tutedorunsubstitutedandrangesinsizefromCstoaboutCs.50 PreferablytheSurfacemodificationagentisanacetoxysilane, or,forexample,amonomercompoundSuchasacetoxysilane, acetoxytrimethylsilane, diacetoxysilane, triacetoxysilane, acetoxytrimethylsilane,diacetoxydimethylsilane,methyltri acetoxysilane,phenyltriacetoxysilane,diphenyldiacetoxysi55 lane,methyltriethoxysilane,dimethyldiethoxysilane,trim ethylethoxysilane, methyltrimethoxysilane, dimethyldimethoxysilane,trimethylmethoxysilane,methyl trichlorosilane, dimethyldichlorosilane, trimethylchlorsi lane,methylsilane,dimethylsilane,trimethylsilane,hexam60 ethyldisilaZane, hexamethylcyclotrisilaZane, bis (dimethylamino)dimethylsilane, bis(diethylamino) dimethylsilane, tris(dimethylamino)methylsilane, tris (dimethylamino)phenylsilane, tris(dimethylamino)silane, dimethylsilyldiformamide,dimethylsilyldiacetamide,dim65 ethylsilyldisocyante,trimethylsilylisocyanate,methylsilyl trisocyanate, 2-trimethylsiloxypent-2-ene-4-one, n-(trim eties.SuchasHand/oranorganicmoietySuchasanalkyl,aryl orderivativesofthese.WhenRisanalkyl,thealkylmoietyis optionalySubstitutedorunsubstituted,andmaybestraight, branchedorcyclic,andpreferablyrangesinsizefromCto aboutCs,orgreater,andmorepreferablyfromC toabout Cs.WhenRisaryl,thearylmoietypreferablyconsistsofa singlearomaticringthatisoptionalySubstitutedorunsub stituted,andrangesinsizefromCstoaboutCs,orgreater, andmorepreferablyfromCstoaboutCs.Inafurtheroption, thearylmoietyisaheteroaryl. Inanotherembodiment,alkoxysilanesmaybeusedasthe Surfacemodificationagent,e.g.SuitablealkoxysilanesSuch aS RSi(OR) whereinRareindependentlyselectedmoieties,suchasH and/oranorganicmoietysuchasanalkyl,arylorderivatives ofthese:Rareindependentlyselectedalkylorarylmoieties. When RorR'isanalkyl,thealkylmoietyisoptionaly Substitutedorunsubstituted,andmaybestraight,branchedor cyclic,andpreferablyrangesinsizefromC toaboutCs,or greater,andmorepreferablyfromC toaboutCs.WhenRor R"isaryl,thearylmoietypreferablyconsistsofasingle aromaticringthatisoptionalySubstitutedorunsubstituted, andrangesinsizefromCstoaboutCs,orgreater,andmore preferablyfromCstoaboutCs.Inafurtheroption,thearyl moiety is a heteroaryl. Thus, the R groups independently selectedfromH.methyl,ethyl,propyl,phenyl,and/orderiva tivesthereof,providedthatatleastoneRisorganic.Inone embodiment,bothRgroupsaremethyl,andatri-functional Surfacemodificationagentismethyltrimethoxysilane. Inanotherembodiment,asuitablesilaneaccordingtothe inventionhasthegeneralformulaofPDF Image | VAPOR PHASE TREATMENT OF DELECTRIC MATERALS
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