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Characterization postmortemx-raydifractionresultsconfirmedtheconver- Material US 10,991,944B2 18 coin-sizedroomtemperatureNa Scels.Theelectro- surfaceofreservoirandthecathodeswasused.Thedistance chemicaltestswereperformedinanethylenecarbonate/ betweenthereservoirandtheelectrodeswasfoundtoplay propylenecarbonate/fluoroethylenecarbonate-basedelec- akeyroleintheapropriateloadinganddepositionofsulfur. trolyteagainstanNa/Na+anode.Thecyclicvoltametry After24hourstheautoclavewascoledtoroomtempera andchargedischargeresultsshowedasinglepotentialfor 5 tureslowlyinaspanof6-8hours.Theheattreatmentresults conversionofsulfurtoNaS.TheCNF/Scathodesdelivered intheformationofpungentodorsandhencetheautoclave acapacityofabout129mAh/gduringthefirstcyclewith wasopenedinthefumehoodandtheelectrodesweretaken abouta51.1%coulombiceficiency.Thecapacityofthe out.TheelectrodeswereweighedandtransferedinArgon roomtemperatureNa—Scelswasstabilizedatabout350 filedgloveboxviaovernightvacuumdryingintheante mAh/gafterthefirstcycleandwassustainedforupto3010chamber,forbateryfabrication. 17 cycleswithonlyabouta0.03% decayratepercycle.The sionofsulfurtoNa2Sandviceversa.Further,insitu Morphologicalandelementalcharacterizationsofthe nanofibersweredoneusingascaningelectronmicroscope photonelectricspectroscopy(XPS)andgalvanostaticinter-15(SEM)(ZeisSupra50VP,Germany)equipedwithenergy mitenttitrationtechnique(GITT)testswerecariedoutto dispersiveX-rayspectroscopy(EDS)withanin-lensdetec investigatetheunderlyingconversionmechanism.Thepre- torand30umaperturewasusedtoexaminethemorphology liminaryresultsshowedthattheobservedsingleplateauand andobtainmicrographsofthesamples.X-raydifraction long-termcyclingofroomtemperatureNaScelswasthe (XRD)paternswereacquiredonadifractometer(Rigaku convolutedefectofdepositedsulfurandastableSEIlayer20Smartlab,Tokyo,Japan)usingCuK?radiation(40kVand onthecathodeside. 44mA)withastepsizeof0.02°inthe20rangeof10-70°. Thesurfacechemistryofthesampleswasanalyzedbyusing EXAMPLES XPSspectra(PhysicalElectronicsVersaProbe5000spec trometer with monochromatic Al Ka as an excitation Thefolowingexamplesareilustrative,butnotlimiting25source),withaspotsizeof20umandpasenergyof23.5 ofthemethodsandcompositionsofthepresentdisclosure. eVwereusedtoiradiatethesamplesurface.Astepsizeof Thefolowingmaterialswereemployedthroughoutthe 0.5eVwasusedtogatherthehigh-resolutionspectra. examples,Polyacrylonitrile(PAN,Mw150000g/mol),N, CasaXPSVersion2.3.19PR1.0softwarewasusedforspec N-Dimethylformamide(DMF,purity9.8%),Sulfur(S, traanalysis.TheXPSspectrawerecalibratedbysetingthe purity9.98%tracemetalsbasis),Ethylenecarbonate(EC,30valenceedgetozero,whichwascalculatedbyfitingthe purity29%,acid<10ppm,H2O<10ppm),Diethylcarbon- valenceedgewithastep-downfunctionandsetingthe ate(DEC,purity>9%,acid<10ppm,H2O<10ppm)and intersectionto0eV.Thebackgroundwasdeterminedusing Lithiumhexafluorophosphate(LiPF6,Purity:9.9%trace theShirleyalgorithmwhichisabuilt-infunctioninthe metalsbasis,baterygrade)wereobtainedfromSigma CasaXPSsoftware.Thermogravimetricanalysis(TGA)data Aldrich.Alchemicalswereusedwithoutfurtherprocesing.35ofalofthesampleswerecolectedonaTAInstruments SynthesisofCarbonNanofibers(CNFs): 2950(TAInstruments,NewCastle,Del.)underasteady Thefre-standingcarbonnanofibersweremadebyelec- argonflowataheatingramprateof5oC.min-1.Nitrogen trospiningTypicaly,10wt%Polyacrylonitrile,PAN(Mol adsorption-desorptionanalysisofthefrestandingnanofiber wt.150,0,SigmaAldrich)wasaddedtoN,N-Dimethyl- matswasperformedat77Konanautomatedgassorption formamideandstiredovernighttoformapolymericblend.40analyzer(AutoSorbiQ2,QuantachromeInstruments).The ThisblendwasthenloadedintoaBectonDickinson5mL samplewasdegasedovernightat150°C.underN,flow syringewithaLuerlocktipandan18-gaugestainlesstel priortothisanalysis. nedle(HamiltonCorporation).Thesyringewiththenedle Electrochemical wasconectedtoanNE-400modelsyringepump(NewEra Electrochemicalmeasurementswerecariedoutbypre PumpSystems,Inc.)inordertocontrolthefedingrateof45paring2032-typecoincels(MTI andXiamenTMAX thesolution.Thegroundedaluminumcolectorwasplaced bateryequipment)asembledinanargon-filedglovebox 6inchesfromthetipofthenedle.Electrospiningwas (MBraunLabstarpro,MB10G,H20and02<1ppm).As performedatroomtemperaturewithrelativehumiditybelow transferedelectrodeswereusedasworkingelectrodesand 15%.Apotentialdiferenceof7-8KV(SeriesES(30KV), 13mmlithiumdiscspunchedfromLithiumfoil(AlfaAesar, GammaHighVoltageResearch,Inc.)wasapliedbetwen5075mmthick)wereusedascounter/referenceelectrodes.To thecolectorandthetipofthenedle.Theflowrateofthe improvethemassloading,cathodeswerestackedontoeach solutionwaskeptconstantat0.2mL/hr.Theas-spunnano- other.Atypicalweightloadingofaround45-50%wasused fiberswerecolectedandstabilizedinaconvectionovenat withamassloadingofaround0.5-5mg/cm2forelectro 280°C.for6hoursintheair.Finaly,thesestabilized chemicaltesting.Theetherelectrolytewaspreparedby nanofibermatswereactivatedbycarbonizinginnitrogenup5disolving1.8M lithiumtrifluoromethanesulfonateina til90°C.anddweledfor1hourwithCO,flowina solventmixtureof1,2-dioxolane(9.8%,anhydrous,stabi horizontaltubefurnace.Aheatingramprateof2°C./min lizedwith75ppmBHT,AcroSeal)and1,2-dimethoxyethane wasemployedforboththestabilizationandcarbonization (ExtraDry=9%,AcroSeal)in1:1volumeratio.Thecar process. bonateelectrolyteconsistedof1M LiPF6in1:1volume Monoclinic Gamma Phase Sulfur Deposition on Carbon 60 ratio of Ethylene carbonate and Diethyl carbonate (pu Nanofibers(CNFs): rity29%,acid<10ppm,H2O<10pm).Polypropylene Thefre-standingCNFsmatwaspunchedwithstainles membrane(25um,CelgardInc)wasusedasaseparator.The steldie(o=1mm)andweighed.TheCNFsdiscswerethen galvanostaticcharge-dischargemeasurementswerecaried placedinahouse-madeautoclave(Stainlesstel316)and outinapotentialrangeof1.0-3.0VvsLi/Li'usingabatery subjectedto180°C.for24hoursinanoven.Theautoclave 65 cycler (Maccor 4000 and Neware BTS 4000).The CV includedasulfurreservoiratthebotomandperforateddisk measurementswereperformedinapotentialrangeof1.0 forplacingelectrodesatthetop.Agapof1.5cmbetwenthe 3.0Vvs.Li/Litatarangeofscanratesfrom0.01-0.5mV/s electrochemicalimpedancespectroscopy,postmortemx-rayPDF Image | SYNTHESIS OF GAMMA MONOCLINIC SULFUR
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