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1、Pilkington浮法玻璃生产介绍Application of Inorganic Chemistry in IndustryFlat Glass and Coatings On GlassDrTroyManningAdvancedTechnologist,On-lineCoatingsPilkingtonEuropeanTechnicalCentreHallLaneLathomUK2OutlineOverviewofFlatGlassindustryandNSG/PilkingtonFlatGlassmanufactureFloatGlassProcessCoatingtechnology
2、withintheglassindustryChemicalVapourDepositionExamplesofonlinecoatingapplicationsLowEmissivity/SolarControlSelfCleaningSummarySuggestedReading3GlobalFlatGlassMarketGlobalMarket37milliontonnes(4.4billionsq.m)BuildingProducts33mtonnes-Automotive4mtonnesOfwhich24million=highqualityfloatglass3million=sh
3、eet2million=rolled8million=lowerqualityfloat(mostlyChina)GlobalValueAtprimarymanufacturelevel15billionAtprocessedlevel50billion4NSGandPilkingtoncombinedAglobalglassleaderthepureplayinFlatGlassCombinedannualsalesc.4billionEqualtoAsahiGlassinscale,mostprofitableinFlatGlassOwnership/interestsin46floatl
4、ines6.4milliontonnesannualoutputWidenedAutomotivecustomerbase36,000employeesworldwideManufacturingoperationsin26countriesSalesin130+countries5TheFloatGlassProcess8Rawmaterials9MeltingFurnace10FloatBath11FloatGlassPlant12TheFloat-GlassProcessFine-grainedingredients,closelycontrolledforquality,aremixe
5、dtomakebatch,whichflowsasablanketontomoltenglassat1500Cinthemelter.Thefurnacecontains2000tonnesofmoltenglass.Afterabout50hours,glassfromthemelterflowsgentlyoverarefractoryspoutontothemirror-likesurfaceofmoltentin,startingat1100Candleavingthefloatbathasasolidribbonat600C.Despitethetranquillitywithwhi
6、chfloatglassisformed,considerablestressesaredevelopedintheribbonasitcools.13RawMaterialsOxide%in glass Raw material sourceSiO272.2SandNa2O13.4Soda Ash(Na2CO3)CaO8.4Limestone(CaCO3)MgO4.0Dolomite(MgCO3.CaCO3)Al2O31.0Impurity in sand,Feldspar or CalumiteFe2O30.11Impurity in sand or Rouge(Fe2O3)SO30.20
7、Sodium sulphateC0.00Anthracite14RawmaterialsSiO2Very durable,BUT high melting point(1700C)!+Na2OMelts at a lower temperature,BUT dissolves in water!+CaOMore durable,BUT will not form in bath without crystallisation+MgOGlass stays as a super-cooled liquid in bath,no crystallisation+Al2O3Adds durabili
8、ty+Fe2O3Adds required level of green colour for customer15ChemistryofGlassImportant glassmaking chemistry:basic reactionsNa2CO3 +SiO2 1500C Na2SiO3 +CO2Na2SiO3 +x SiO2 Na2SO4 (Na2O)(SiO2)(x+1)Digestion16CompositionofGlass17StructureofGlassRandom network of SiO4-tetrahedral units.Na-O enter Si-O netw
9、ork according to valency Network FormersCa and Mg Network Modifiers make structure more complex to prevent crystallisation 18Body-tintedGlassIonResulting Colour of GlassFerrous(Fe2+)BlueFerric(Fe3+)YellowFe2+Fe3+GreenSelenium(SeO2)BronzeCobalt(Co2+)Grey/BlueNickel(Ni2+)Grey19CIELa*b*colourspace20CIE
10、La*b*colourspace21FunctionsofaWindowLightinhomes,officesLightoutshops,museumdisplaysHeatinheatingdominatedclimatesHeatoutcoolingdominatedclimatesCanchangepropertiesofglassbyapplyingcoatingstothesurface22Makingawindowfunctional-coatingsAwidevarietyofcoatingtechnologiesareutilisedbytheglassindustrySpr
11、ayPyrolysisPowderSprayChemical Vapour DepositionSputterCoatingThermalEvaporationCoatingsSolGelCoatingsTheseareappliedOnLinei.e.astheglassisproducedonthefloatlineOffLinei.e.coatingnotnecessarilyproducedatthesamelocation23VariationsofCVDAtmosphericPressureAPCVDLowPressure-LPCVDAerosolAssisted-AACVDMet
12、alorganicMOCVDCombustion/FlameCCVDHotWire/FilamentHWCVD/HFCVDPlasmaEnhanced-PECVDLaserAssistedLACVDMicrowaveAssistedMWCVDAtomicLayerDepositionALD24ChemicalVapourDeposition25ChemicalVapourDepositionMaingasflowregionGasPhaseReactionsSurfaceDiffusionDesorptionofFilmPrecursorByProductsDiffusiontosurface
13、26ChemicalVapourDepositionAnimation kindly supplied by Dr.Warren Cross,University of Nottingham27CVDprocessesandparametersProcessParametersTransportPrecursorsGasphasereactionPressure,temperature,flowconditions,boundarylayerthickness,gasphaseconcentration,precursors,carriergasDiffusionPressure,temper
14、ature,flowconditions,boundarylayerthickness,gasphaseconcentrationAdsorptionTemperature,gasphaseconcentration,numberandnatureofsitesSurfacereactionTemperature,natureofsurfaceDesorptionofby-productsTemperature,pressure,natureofsurfaceDiffusiontolatticesiteTemperature,surfacemobility,numberofvacantsite
15、s28CVDPrecursorPropertiesVolatilegas,liquid,lowmeltingpointsolid,sublimablesolidPureStableundertransportReact/DecomposecleanlytogivedesiredcoatingminimisecontaminantsCanbesinglesourceordual/multi-source29CVDPrecursorsSingleSourcepyrolysis(thermaldecomposition)e.gTi(OC2H5)4TiO2+4C2H4+2H2O(400C)Oxidat
16、ione.gSiH4(g)+O2(g)SiO2(s)+2H2(g)Reductione.g.WF6(g)+3H2(g)W(s)+6HF(g)Dualsourcee.g.TiCl4(g)+4EtOH(g)TiO2(s)+4HCl(g)+2EtOEt(g)30DualSourceandSingleSourcePrecursorsFilmDual SourceSingle SourceGaAsGaCl3+AsH3Me2Ga(AsH2)TiNTiCl4+NH3Ti(NMe2)4WSiWCl6+SiH4W(SiR)4TiO2TiCl4+H2OTi(OiPr)4CdSeCdMe2+H2SeCd(SeR)2
17、31TransportofPrecursorsBubblerforliquidsandlowmeltingsolidsDirectLiquidInjectionsyringeandsyringedriverforliquidsandsolutionsSublimationforsolidshotgaspassedoverheatedprecursorAerosolofprecursorsolutions32EffectofTemperatureonGrowthRateIndependent of temperature33FlowconditionsLaminar Flow regimeTur
18、bulent Flow Regime34ReynoldsNumberDimensionlessnumberdescribingflowconditionsr=r=Mass density related to concn and partial pressureu=average velocitym=viscosityL=relevant length,related to reactor dimensionsIf Re 1000 fully turbulent flowReality is between the two extremes35DimensionlessNumbersReduc
19、esthenumberofparametersthatdescribeasystemMakesiteasiertodeterminerelationshipsexperimentallyForexample:DragForceonaSphereVariables:Force=f(velocity,diameter,viscosity,density)Canbereducedto2“dimensionlessgroups”:Dragcoefficient(CD)andReynoldsnumber(Re)36DimensionlessNumbersLaminar flow regimeTurbul
20、ent flow regimeExperimental values of CD for spheres in fluid flows at various Re37BoundaryLayergasvelocityFrictional forces against reactor walls decrease gas velocity The boundary layer thickness can be estimated from:38BoundaryLayer-temperatureContact with hot surfaces increases temperature39Boun
21、daryLayerprecursorconcentrationDepletion of precursor decreases gas phase concentration40NucleationandGrowthVan der Waals type adsorption of precursor to substratePrecursors then diffuse across surfacePrecursors diffuse across boundary layer to surfaceAnd can be desorbed back into main gas flowOr ca
22、n find low energy binding sites to coalesce into filmMain Gas Flow41NucleationandGrowthSubstrate TemperatureGrowth RateSurface DiffusionCrystallinityLowHighSlowrelativefluxofprecursorsAmorphousnocrystallinestructureHighLowFastrelativetofluxofprecursorsEpitaxialreplicatessubstratestructureIntermediat
23、eIntermediateIntermediatePolycrystalline42GrowthMechanisms(b)Frank-van der MerweLayer growth(c)Stranski-KastanovMixed layered and island growth(a)Volmer-WeberIsland growth43ThinFilmAnalysisManytechniquesareusedtocharacterisethinfilmsExamplesincludeXRDcrystallinity,phaseXRRlayerthickness,layerroughne
24、ssSEM/EDX/WDXmorphology,thickness,compositionRamanphase,bondingFTIRphase,bondingXPScomposition,depthprofiling,dopingSIMScomposition,depthprofiling,dopingAFMroughness,surfacemorphologyTEMcrystallinestructure,crystaldefectsAnalysisoffunctionalproperties44CVDonGlassForon-linecoatingofglasswerequire:Hig
25、hgrowthratesrequiredthicknessin100nm/spossibleLowprecursorefficiency10%SiCxOy(70 nm)SnO2:F(350 nm)GlassSiH4+C2H4+CO2SiCxOy+H2O+otherby-productsUsedascoloursuppressionandbarrierlayer57LowEmissivityCoatingGenerallybasedonSnO2:F(TransparentConductiveOxide)SiCOunderlayerusedascoloursuppressant58Low-Eand
26、SolarControlCoatings59Self-CleaningGlassTwomechanisms:SuperhydrophilicityPhotocatalyticdegradationoforganicmatter.TiO2coating60SuperhydrophilicityOxygen vacanciesTiO-TiOTiHTiTiTiH+TiOTiOTiTiOTiOTiHHH2O(OH-,H+)Water dropletsUniform water filmUV illumination timeContact angleooooooodarkUV61Photocataly
27、ticActivityUltrabandgapirradiationofTiO2GenerationofelectronholeinvalencebandHolemigratestothesurfaceandresultsinoxidationoforganicmaterialValenceBandConductanceBandOxidationReductionAA+BB-h+hn62Semi-conductorPhotocatalysisA.Mills,S Le Hunte,J.Photochem.Photobiol A,1997,108,1-35.63CVDofActivTMSiO2(3
28、0 nm)TiO2(17 nm)GlassSiH4+O2+C2H4 SiO2+by-productsUsed as barrier layer to prevent diffusion of Na ions into TiO2 layerTiCl4+EtOAc TiO2+HCl+organic by-productsLaminar Flow regimeReasonable growth rates and precursor efficiency64ActivTM65ActivTM66ActivTM67Superhydrophilicity15 mins UV Exposure30 mins
29、 UV Exposure45 mins UV ExposureBefore UV Exposure68PhotocatalyticEffect UV-AbsorptionO2-OH*Organic SoilHH2 2O+COO+CO2 2GlassBarrier LayerTiO2-Layer69PhotocatalyticEffectThephotoactivityofthecoatingcanbemeasuredbymonitoringthedecompositionofastandardcontaminantAthinfilmofstearicacid(n-octadecanoicaci
30、d,200)isappliedfromamethanolsolutionontothecoatingStearicacidusedasatypicalorganiccontaminantFTIR(Fouriertransforminfra-redspectroscopy)usedtodetectC-HstretchofstearicacidC-HabsorptionintensitymeasuredaftervaryingUVexposure70StearicAcidDecompositionC-HAbsorptionZeroUVexposureC-HAbsorption60minsUVexp
31、osureUV 0.77W/m2 340nm71PilkingtonActivTM72SummaryScaleoftheGlobalFlatGlassIndustryManufacturingFlatGlassFloatGlassProcessCoatingGlassChemicalVapourDepositionExamplesofcommercialglazingcoatingspreparedbyCVD73RecommendedReadingD.W.SheelandM.E.PembleAtmospheric Pressure CVD Coatings on Glass,ICCG42002 http:/www.cvdtechnologies.co.uk/CVD%20on%20Glass.pdfM.L.Hitchman,K.F.JensenChemical Vapor DepositionAcademicPress,1993W.S.Rees,CVD of Non-metals,VCH,Weinheim,1996M.OhringThe Materials Science of Thin Films,AcademicPress,74First in Glass75