采用两步炭化法和熔盐模板法制备N、S共掺杂煤基硬炭及共储钠性能.pdf
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1、Cite this:NewCarbonMaterials,2024,39(2):297-307DOI:10.1016/S1872-5805(24)60842-5N,S co-doped coal-based hard carbon prepared by two-step carboniz-ation and a molten salt template method for sodium storageNIUHui-zhu1,WANGHai-hua1,2,3,*,SUNLi-yu1,YANGChen-rong1,WANGYu4,CAORui1,YANGCun-guo1,WANGJie1,SH
2、UKe-wei1,*(1.School of Chemistry and Chemical Engineering,Shaanxi University of Science and Technology,Xian 710021,China;2.Xian Key Laboratory of Advanced Performance Materials and Polymers,Shaanxi University of Science and Technology,Xian 710021,China;3.Shaanxi Key Laboratory of Chemical Additives
3、for Industry,Shaanxi University of Science and Technology,Xian 710021,China;4.Xian North Huian Chemical Industry Co,Xian 710302,China)Abstract:Hardcarbon,knownforitsabundantresources,stablestructureandhighsafety,hasemergedasthemostpopularan-odematerialforsodium-ionbatteries(SIBs).Amongvarioussources
4、,coal-derivedhardcarbonhasattractedextensiveattention.Inthiswork,NandSco-dopedcoal-basedcarbonmaterial(NSPC1200)wassynthesizedthroughacombinationoftwo-stepcarboniza-tionprocessandheteroatomdopingusinglong-flamecoalasacarbonsource,thioureaasanitrogenandsulfursource,andNaClasatemplate.Thetwo-stepcarbo
5、nizationprocessplayedacrucialroleinadjustingthestructureofcarbonmicrocrystalsandexpandingtheinterlayerspacing.TheNandSco-dopingregulatedtheelectronicstructureofcarbonmaterials,endowingmoreactivesites.Ad-ditionally,theintroductionofNaClasatemplatecontributedtotheconstructionofporestructure,whichfacil
6、itatesbettercontactbetweenelectrodesandelectrolytes,enablingmoreefficienttransportofNa+andelectrons.Underthesynergisticeffect,NSPC1200exhibitedexceptionalsodiumstoragecapacity,reaching314.2mAhg1at20mAg1.Furthermore,NSPC1200demonstratedcom-mendablecyclingstability,maintainingacapacityof224.4mAhg1even
7、after200cycles.Thisworksuccessfullyachievesthestra-tegictuningofthemicrostructureofcoal-basedcarbonmaterials,ultimatelyobtaininghardcarbonanodewithexcellentelectrochem-icalperformance.Key words:Hardcarbon;Sodium-ionbattery;Coal-derivedcarbon;Two-stepcarbonization;NandSco-doped1IntroductionLithium-io
8、n batteries(LIBs)stand as the mostwidelyusedsecondarybatteriesinenergystoragesys-tems.However,limitedresourcesofLianditschal-lengingextractionprocesseshaveconstrainedfurtherdevelopmentsinLIBs.Sodium,ontheotherhand,isnot only abundantly available and inexpensive butalsoshows similar chemical properti
9、es to lithium,makingsodiumionbatteries(SIBs)standoutasavi-talsupplementorpotentialsubstituteforLIBsinre-searchandindustrialization13.However,thedevel-opmentandapplicationofelectrodesinSIBsareintheearlystages.GraphiteisusuallyusedastheLIBsanode,butitisnotsuitableforSIBsduetothelargerionicradiusofsodi
10、um45.Therefore,findingsuitableelectrodematerialsiscrucialforthefuturedevelop-mentofSIBs.Researchershaveexploredvariousanodemateri-alsfor SIBs,each accompanied by its set of chal-lenges.Common alloying reaction anode materials,such as Na-P6,Na-Ge7 and Na-Sb8,exhibit highspecific capacity.However,thes
11、e materials undergovolumeexpansionduringtheintercalationandde-in-tercalationprocessesofNa+,resultinginfasterspecif-iccapacitydecayandreducedcyclingperformance.Carbonmaterialsbasedonintercalationreaction,suchas graphene,hard and soft carbon,are significantlyadvantageousconsideringtheirlowcost,highsta
12、bil-ityandotheraspects910.Therefore,carbonmaterialscontinuetobethemainstreamchoiceforanodesinSIBs.Amongthem,coalanditsby-productspresentawiderangeofoptionsandhighcarboncontent,mak-Received date:2023-12-04;Revised date:2024-01-27Corresponding author:WANGHai-hua,Professor.E-mail:;SHUKe-wei,AssociatePr
13、ofessor.E-mail:Author introduction:NIUHui-zhu,Ph.Dcandidate.E-mail:Supplementarydataassociatedwiththisarticlecanbefoundintheonlineversion.Homepage:http:/ coal-based carbon materials can not onlymeetthegrowingdemandforsecondarybatteriesbutalsoreduceenvironmentalpollutionandachievethehigh-valueutiliza
14、tionofcoal.Wangetal.12synthes-izedcoal-basedporouscarbonusingpotassiumper-manganate(KMnO4)as oxidant,sodium hydroxide(NaOH)asanactivatorandsodiumchloride(NaCl)asatemplate.Itexhibitedasodiumstoragecapacityof150.4mAhg1after1000cycles.Similarly,Gaoetal.13preparedcoal-basedcarbonnanofibers(CCNF)througha
15、spinningmethodusingoxidizedcoal(OC),polyacrylonitrile(PAN)anddimethylformamide(DMF)asrawmaterials.Itdemonstratedacapacityof109mAhg1evencyclingover1000times.Thesefindings collectively affirm the viability of coal-de-rivedcarbonmaterialsinSIBs.Previousstudieshaveproventhattheintroduc-tionofheteroatoms
16、canpromoteelectricalconductiv-ityandgeneratemoreactivesites,therebyimprovingelectrochemical performance1417.Ou et al.18 pre-paredaporousN-dopedcarbonmaterialusingchrys-anthemumascarbonsource,exhibitingaspecificca-pacityof205mAhg1after200cyclesat0.1Ag1.Yanetal.10utilizedphosphorustrichloride(PCl3)asa
17、phosphorussourceandcyclohexane(C6H12)asacar-bonsourcetoobtainanultra-highP-dopedcarbonma-terial(UPC).Itexhibitedhighreversiblecapacityof510.4mAhg1at100mAg1.Thus,improvingtheso-diumstorageperformancethroughheteroatomdopingisparticularlybeneficialforcoal-basedcarbonmateri-als.Long-flamecoal,knownaslow
18、-rankbituminouscoal,istypicallyusedaspowercoalandbringsinevit-able environmental pollution.Utilizing long-flamecoalasacarbonsourceforpreparingcoal-basedcar-bonmaterialscanachieveitshigh-valueutilization.Inthiswork,wepreparedN,Sco-dopedcoal-basedhardcarbon(NSPC1200)withextendedinterlayerspacingbyacom
19、binationoftwo-stepcarbonizationandhet-eroatomdoping.TheNSPC1200exhibitedoutstand-ingelectrochemicalperformanceowingtothecom-binedeffectofexpandedinterlayerspacinganddop-ing.It achieved a sodium storage capacity of314.2mAhg1at20mAg1.Evenafter200cyclesat100 mA g1,it still maintained a capacity of224.4
20、mAhg1.2Experimental 2.1 Material preparationLong-flame coal(Huangyuchuan Coal Mine inOrdos)servedastherawmaterial(TableS1).Hydro-chloricacid(HCl)(coal:HCl=110)andhydrofluor-icacid(HF)(coal:HF=15)wereusedtotreatthelong-flamecoalat60Cfor3htocleanupimpurit-ies.Afterwashinganddrying,apurifiedcoalprecurs
21、-orwasobtainedandnamedasCY.NSPC1200 was prepared through heteroatomdopingbytwo-stepcarbonizationofCYat700Cinargonatmosphere.First,theCYpowderwascarbon-izedinatubefurnaceat1200Cfor2htoobtainPC1200.Subsequently,PC1200,thiourea and NaClweremixedwitharatioof1510intubefurnacefortwo-stepcarbonizationat700
22、Cfor2hataheat-ingrateof3Cmin1.ThetargetsampleNSPC1200wasobtainedafterwashinganddrying.2.2 CharacterizationsTransmission electron microscopy(TEM,FEITecnai G2 F20)and scanning electron microscopy(SEM,FEIVerios460)wereusedtoexaminethemi-crostructure of PC1200 and NSPC1200.The X-raydiffractometer(XRD,Br
23、uker D8 Advance)and Ra-manspectroscopy(THEMDXRxi)wereemployedtocharacterizethecrystallinityandgraphitizationofcar-bonmaterials.Theelementalcompositionandbond-ingstateweredetectedbyX-rayphotoelectronspec-troscopy(XPS,AXISSUPRA).N2adsorption/desorp-tiontestswereconductedusingafullyautomatedsur-faceare
24、aandporesizeanalyzer(BET,MicromeriticsASAP2460)underliquidnitrogenconditions.2.3 Electrochemical measurementThe coal-based carbon materials,super carbonblackandPVDFwerehomogeneouslymixedinNMPwithamassratioof811.Afterdrying,thework-ingelectrode was obtained.The batteries were as-sembledwithsodiumshee
25、tsarethecounterelectrodeand glass fiber separators.The electrolyte was298新型炭材料(中英文)第39卷1molL1NaClO4inamixtureofdimethylcarbonate(DMC)andethylenecarbonate(EC)(11;v/v).Andthe charging/discharging curves were performed onbatterytesting system(CT-4000).Cyclic voltam-metry(CV)measurements were taken on e
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