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27 EXAMPLE 9 Inordertounderstandthetemperaturedependenceofthe silanizationreactionontheSurface,thedepositiontempera ture was varied from 110° C. to 400° C. The different tem peraturewouldresultinvariationinmoisturecontentandgas molecularactivityontheSurface,whichinturn,resultin diferentchemistrytoocur.Processconditionsused:ammo niaflowrate20sccm(or80sccm),DMDAS reservoirtem perature,55°C.,totalpressure1.5tor,bakeat350°C.oven Substratetemperature, Contact Dielectric Carbon 28 ammoniaflowrate50sccm,totalpressure2.0tor,wafer temperature,300°C.Reservoirtemperature55°C. Dielectric Carbon Defectcount Bakecondition ContactAngle constant restoration (defectdensity) oC. 200,6,(7) 300,8,(9) 400,13,(12) angle constant restoration 78,(83) 2.67,(2.60) 102(57) 2.54,(2.64) 20(12) 84,(85) 2.52,(2.47) 31(14) 10 15 Slightdecreaseincontactangleandcarbonrestorationusing P5000forfinalthermaltreatmentcomparedtoTEL HP. SlightincreaseindielectricconstantusingP5000insteadof TELHP. Whilethepresentinventionhasbeenparticularlyshown anddescribedwithreferencetopreferedembodiments,it wilbereadilyappreciatedbythoseofordinaryskilintheart thatvariouschangesandmodificationsmaybemadewithout departingfromthespiritandscopeoftheinvention.Itis intendedthattheclaimsbeinterpretedtocoverthedisclosed embodiment,thosealternativeswhichhavebeendiscussed aboveandalequivalentsthereto. What isclaimed is: 1.Amethodfortreatingasilicateororganosilicatedielec tricfilmonasubstrate,whichsilicateororganosilicatedielec tricfilmeithercomprisessilanolmoietiesorwhichsilicateor organosilicatedielectricfilmhashadatleastsomepreviously presentcarboncontainingmoietiesremovedtherefrom,the methodcomprising: (a)optionalydehydratingatleastaportionofasilicateor organosilicatedielectricfilmonasubstrate;then (b)optionalyapplyinganactivatingagentforaSurface modificationagentcompositiontothesilicateororga nosilicatedielectricfilm;then (c)contactingthesilicateororganosilicatedielectricfilm withaSurfacemodificationagentcompositioninavapor orgaseousstate,whereintheSurfacemodificationagent compositioncomprisesacomponentcapableofalkylat ingorarylatingsilanolmoietiesorbondscreatedby removalofcarboncontainingmoietiesfromthesilicate ororganosilicatedielectricfilmviasilylation;wherein theSurfacemodificationagentcompositioncomprisesat leastonecompoundhavingaformulaselectedfromthe groupconsistingof SiRNR' ,wheren>2andmay becyclic;RSiNR'SiR (RSi)N;RSiNR';RSi (NR'); RSi(NR'); RSiOC(R)—R"), RSi (NCOR), RSi(NCO), RSi(OH), andcombi nationsthereof,whereinXisanintegerrangingfrom1to 3,eachRisindependentlyselectedfromhydrogenanda hydrophobicorganicmoiety;R ishydrogen,oran organicmoiety,andR"isanalkylorcarbonylgroup;and whereintheSurfacemodificationagentcompositionfur thercomprisesanactivatingagentselectedfromthe groupconsistingofammoniumcompounds,phospho nium compounds, Sulfonium compounds, iodonium compounds,alkylamines,arylamines,alcoholamines, primary amines, secondary amines, tertiary amines, ammonia,quaternaryammoniumsalts,tetramethylam moniumacetate,tetrabutylammoniumacetate,acombi nationsoftetramethylammoniumacetateandtetrabuty lammonium acetate, sodium hydroxide, potassium hydroxidelithiumhydroxideandammoniumhydrox ide;saidcontactingbeingconductedunderconditions suficientto(i)or(i)or(i): (i)addcarboncontainingmoietiestothesilicateororga nosilicatedielectricfilm,or Thehigherthetemperature,thelowertheKvalue. EXAMPLE 10 Inordertounderstandtheefectofgasdoseonthesilaniza tionreaction,aflowrateofthesilanegaswasvaried.Flow ratewascalculatedbychangingreservoirtemperatureofthe silanesolutionandapressureinthechamber.Thereservoir temperaturewasvariedbyheatingthereactantSolutionina pyrexcontainer.Processconditionsused:ammoniaflowrate30 80sccm,totalpressure1.5tor,bakeat350°C.oven,wafer temperature,400°C. Gasflowrate,scom 65,4 55,12 Contact Dielectric Carbon Defectcount angle constant restoration (defectdensity) 89 2.46 24 85 2.47 27 25 35 40 45 50 55 60 65 NodiferenceinKvaluebyvaryingreservoirtemperature EXAMPLE11 Inordertounderstandtheefectofgasdoseonthesilaniza tionreaction,aflowrateoftheammoniagaswasvaried.The reservoirtemperaturewasvariedbyheatingthereactantSolu tioninapyrexcontainer.Processconditionsused:totalpres sure1.5tor,bakeat350°C.oven,wafertemperature,400° C.,DMDAS reservoir55°C. Contact Gasflowrate,scom angle Dielectricconstant restoration 20,13 84 2.52 32 80,12 85 2.47 27 Thehighertheammoniagasflowrate,thelowertheKvalue. EXAMPLE 12 Tounderstandtheefectofbakecondition(in-situand oven)onKvalue,theprocessedwaferswerebakedineither thechamber(in-situ)orTELoven.Processconditionsused: US 7,678,712B2 Carbon Chamber,12 TEL HP,12 86 2.47 72 88 2.45 86PDF Image | VAPOR PHASE TREATMENT OF DELECTRIC MATERALS
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