HighperformanceofacarbonsupportedternaryPdIrNicatalystforethanolelectro-oxidationinanion-exchangemembranedirectethanolfuelcellsShuiyunShen,T.
S.
Zhao,*JianboXuandYinshiLiReceived21stOctober2010,Accepted6thJanuary2011DOI:10.
1039/c0ee00579gInthispaper,wereportthesynthesisofacarbonsupportedternaryPdIrNicatalystfortheethanoloxidationreactioninanion-exchangemembranedirectethanolfuelcells(AEMDEFCs).
WedemonstratethattheuseoftheternaryPdIrNicatalystattheanodeofanAEMDEFCcanincreasethepeakpowerdensitybymorethan122%ascomparedwiththeuseofthemonometallicPdcatalyst,69%ascomparedwiththeuseofthebimetallicPdIrcatalyst,and44%ascomparedwiththeuseofthebimetallicPdNicatalyst.
CyclicvoltammetryandchronopotentiometryanalysesprovethattheternaryPdIrNicatalystiscatalyticallymuchmoreactiveandmorestablethanthemonometallicPdcatalystandthebimetallicPdIrandPdNicatalysts.
1.
IntroductionAnimportantadvantageofanion-exchangemembranedirectalcoholfuelcells(AEMDAFCs)isthatthekineticsofbothalcoholanodicoxidationandoxygencathodicreductioninalkalinemediabecomemuchfasterthaninacidicmedia,makingitpossibletousenon-platinumandlow-costmetalcatalysts.
1,2AmongvariouspossiblefuelsforAEMDAFCs,includingmethanol,ethanol,glycerol,ethyleneglycol,andsoon,ethanolisthebestchoice,asithasahigherenergydensitythanmethanol(8.
0kWhkg1vs.
6.
1kWhkg1),islesstoxicandcanbeproducedinlargequantitiesfromagriculturalproductsorbiomass.
3,4Theuseofpalladiumastheanodecatalystfortheethanoloxidationreaction(EOR)inanion-exchangemembranedirectethanolfuelcells(AEMDEFCs)offerstwosignicantadvan-tagesascomparedwiththeuseofPt.
5,6First,PdshowsbothahighercatalyticactivityandbetterstabilityfortheEORinalkalinemediathanPtdoes.
Secondly,PdismoreabundantthanPtandhasamuchlowerprice,andthusthecostoffuelcelltechnologycanbegreatlyreduced.
However,itisworthnotingthatwithstate-of-the-artanodecatalysts,ethanolisselectivelyoxidizedtoacetateinalkalinemediathroughafour-electronpathwayaccordingto7–10C2H5OH+5OH/CH3COO+4H2O+4e(1)Combiningcyclicvoltammetry(CV)withinsituFouriertransforminfraredspectroscopy,Zhouetal.
8conrmedthatina0.
1MNaOHsolutioncontaining0.
1Methanol,theselec-tivityforethanoloxidationtoCO2wasaslowas2.
5%inthepotentialrangingfrom0.
60Vto0.
0Vvs.
SCE.
Bambagionietal.
9,10employedionicchromatograpyand13C{1H}NMRspectroscopytoanalyzetheanodeexhaustfromAEMDEFCswithPd/MWCNT,Pd/CandPd–(Ni–Zn)/Castheanodecatalyst,respectively,andtheresultsshowedthatduringtheDepartmentofMechanicalEngineering,TheHongKongUniversityofScienceandTechnology,ClearWaterBay,Kowloon,HongKongSAR,China.
E-mail:metzhao@ust.
hk.
Fax:(+852)23581543;Tel:(+852)2358647BroadercontextRecently,attentionhasbeenfocusedontheuseofpalladium(Pd)astheanodecatalystfortheethanoloxidationreaction(EOR)inanion-exchangemembranedirectethanolfuelcells(AEMDEFCs),asPdofferstwosignicantadvantagesascomparedwiththeuseofPt.
First,PdshowsbothahighercatalyticactivityandbetterstabilityfortheEORinalkalinemediathanPt.
Secondly,PdismoreabundantthanPtandhasamuchlowerprice,andthusthecostoffuelcelltechnologycouldbegreatlyreduced.
However,boththecatalyticactivityandstabilityofPdfortheEORinalkalinemedianeedtobefurtherimproved.
Inthisstudy,ahigh-performancecarbonsupportedternaryPdIrNicatalystwassynthesizedfortheEORinalkalinemedia.
InthePdIrNicatalyst,Pdfacilitatesethanoldehydrogenation,whiletheIrandNispeciesconcurrentlycontributetotheremovalofadsorbedethoxyintermediates.
TheuseoftheternaryPdIrNicatalystattheanodeofanAEMDEFCresultsinmuchhigherperformancethantheuseofboththemonometallicPdandbimetallicPdIrandPdNicatalysts.
1428|EnergyEnviron.
Sci.
,2011,4,1428–1433ThisjournalisTheRoyalSocietyofChemistry2011DynamicArticleLinksC1433|1429theanodeelectrode,ananodeinkwasrstpreparedbymixingthePd/C,Pd2Ni3/C,Pd7Ir/CorPd7IrNi12/Ccatalystwith5wt.
%PTFEemulsionasabinderinethanol.
Afterultrasonication,thewelldispersedinkwasbrushedontoanickelfoam(HohsenCorp.
,Japan),whichservedasthebackinglayeroftheanodeelectrode.
Themetal(PdandIr)loadingintheanodewas1.
0mgcm2.
Thecellperformancetestswerecarriedoutat60C,andfuelsolutionwaspumpedtotheanodeatarateof1.
0mlmin1,anddrypureoxygenataowrateof100standardcubiccenti-metersperminute(sccm)wasfedtothecathode.
Thecellperformancedatawerecollectedafteritbecamestable.
3.
Resultsanddiscussion3.
1XRD,TEMandXPScharacterizationThebulkstructuralinformationofthePd7IrNi12/CcatalystwasobtainedbyXRDandisshowninFig.
1.
Therstpeaklocatedatthe2qvalueofabout25referstothegraphite(002)facetofthecarbonpowdersupport.
Thediffractionpeaksatthe2qvaluesof40.
6,47.
06,68.
5,and82.
40areassignedtothe(111),(200),(220)and(311)facetsoftheface-centeredcubic(fcc)crystallinestructure,respectively,andthesefourpeaksarelocatedathigher2qvalueswithrespecttothatofpurePd(JCPDS46-1043),whileatlower2qvalueswithrespecttothatofpureIr(JCPDS06-0598),andthiscanbeattributedtotheincorporationofalowerdspacecrystalstructureofIr(d1112.
217)thanthatofPd(d1112.
246),suggestingtheformationofPdIralloy.
Therealsoexistsanothersmallpeakatthe2qvalueof60.
0,correspondingtotheNi(OH)2(110)facet.
12However,nosinglepeakisobservedatthe2qvalueofabout33.
5fortheNi(OH)2(100)facetinthePd7IrNi12/CcatalystduetosuperpositionofthediffractionpeakofthePd(111)facet,whichiswiderthanthatinthePdNi/Ccatalysts.
12Thisisbecausecitratewasusedasacomplexingagentandstabilizerduringthecatalystsynthesis,andthisresultedinasmallercrystallitesizeofthemetalparticlesonthePd7IrNi12/Ccatalyst.
TheaveragecrystallitesizeofthemetalparticlesonthePd7IrNi12/Ccatalystiscalculatedbasedonthebroadeningofthe(111)diffractionpeaksaccordingtoScherrerequation15d0:9lB2qcosqmax(4)wherelrepresentsthewavelengthoftheX-ray,qistheangleofthemaximumpeak,andB2qisthewidthofthepeakatthehalfheight.
AccordingtotheScherrerequation,theaveragecrystal-litesizeofthemetalparticlesonthePd7IrNi12/Ccatalystis2.
7nm.
Fig.
2showstheTEMimageandhistogramofthemetalparticlesizedistributionofthePd7IrNi12/Ccatalyst.
InFig.
2a,itcanbeobservedthatthemetalparticlesonthePd7IrNi12/Ccatalystexhibitasphericalshapeandarewelldispersedonthecarbonpowdersupportwithoutsevereaggregation.
ThemetalparticlesizedistributionofthePd7IrNi12/Ccatalystwasevalu-atedfromanensembleof200particles.
Basedonthisevaluation,thePd7IrNi12/Ccatalystshowsametalparticlesizedistributionrangingfrom1.
0to4.
6nm,andtheaveragemetalparticlesizeis2.
6nm,whichisalmostthesameasthevaluepredictedfromtheXRDdata.
TheXPStestwasemployedtoanalyzethesurfacecompositionandoxidationstateofthemetalsonthePd7IrNi12/Ccatalyst.
BasedontheintensitiesofXPSpeaks,thesurfaceatomicratioofFig.
1XRDpatternsofthePd7IrNi12/Ccatalyst,JCPDS46-1043leforPd(solidlines)andJCPDS06-0598leforIr(dashedlines).
Fig.
2TEMimage(a)andhistogramofmetalparticlesizedistribution(b)ofthePd7IrNi12/Ccatalyst.
1430|EnergyEnviron.
Sci.
,2011,4,1428–1433ThisjournalisTheRoyalSocietyofChemistry2011Pd:Ir:NiforthePd7IrNi12/Ccatalystis6:1:8,whichshowssomedeviationfromthenominalratiosintheprecursors.
TheIr4fXPSandNi2pXPSspectraofthePd7IrNi12/Ccatalystare,showninFig.
3aandb.
InFig.
3a,itcanbeobservedthatthereexiststhreepeaks;thepeakat68.
0eVcanbeassignedtoNi3p,32whiletheothertwopeakscorrespondtoIr4f,consistingofahighenergyband(Ir4f5/2)at64.
0eVandalowenergyband(Ir4f7/2)at61.
0eV.
33TheIr4fspectrumcanbedeconvolutedintotwodoublets,correspondingtometallicIrandIrO2,respectively;theXPSarearatiosforIrandIrO2are78.
2%and21.
8%.
InFig.
3b,takingtheshake-uppeaksintoaccount,theNi2pspectrumcanbedeconvolutedintofourdoublets,correspondingtometallicNi,NiO,Ni(OH)2andNiOOH;34theXPSarearatiosforthemare4.
8%,5.
9%,62.
0%,and27.
3%,respectively.
3.
2ElectrochemicalpropertyandcellperformanceFig.
4ashowsthestabilizedCVcurves(the20thcycle)oftheEORonthePd/C,Pd2Ni3/C,Pd7Ir/CandPd7IrNi12/Ccatalystsmeasuredinthepotentialrangingfrom0.
926Vto0.
274V;Fig.
4bshowsonlythepositivedirectionscansforclearobservation.
Thescanratewas50mVs1.
AsshowninFig.
4b,boththebimetallicPd2Ni3/CandPd7Ir/CcatalystsshowahighercatalyticactivitythanthemonometallicPd/Ccatalystdoes,andthePd7IrNi12/CcatalystshowsthehighestcatalyticactivityfortheEORinalkalinemediaamongallthecatalysts,intermsofboththeonsetpotentialandthepeakcurrentdensity.
TheonsetpotentialoftheEORonthePd7IrNi12/Ccatalystis0.
71V,0.
59VonPd/C,0.
68VonPd2Ni3/Cand0.
68VonPd7Ir/C;thepeakcurrentdensityoftheEORonthePd7IrNi12/Ccatalystis0.
139Acm2,0.
101Acm2onPd/C,0.
136Acm2onPd2Ni3/Cand0.
103Acm2onPd7Ir/C.
ItisnotedthatcomparedtothePd/Ccatalyst,thePd7Ir/Ccatalystischaracterizedwithamorenegativepeakpotential,thePd2Ni3/Ccatalystischaracterizedwithahigherpeakcurrentdensity,whilebothamorenegativepeakpotentialandahigherpeakcurrentdensityforthePd7IrNi12/Ccatalyst.
AccordingtotheXPSresults,itcanbeconrmedthatthesurfacecompositionandoxidationstateofboththeIrandNispeciesonthePd7IrNi12/CcatalystarealmostthesameasthatinthebimetallicPdIrorPdNicatalysts,12,29andthisindicatesthataconcurrentpromotionfromtheadditionofIr,alongwithNi,accountsforthehighestcatalyticperformanceofthePd7IrNi12/CcatalystfortheEORinalkalinemedia:12,29IradditiontoPdcanfacilitatetheremovalofadsorbedethoxyintermediates,asthehydroxylgroupsaremoreeasilyadsorbedFig.
3Ir4fXPSspectrum(a)andNi2pXPSspectrum(b)ofthePd7IrNi12/Ccatalyst.
Fig.
4CVcurves(a)andpositivedirectionscans(b)oftheEORonthePd/C,Pd2Ni3/C,Pd7Ir/CandPd7IrNi12/Ccatalystsin1.
0MKOH+1.
0Methanol(scanrate:50mVs1).
ThisjournalisTheRoyalSocietyofChemistry2011EnergyEnviron.
Sci.
,2011,4,1428–1433|1431onmetallicIrandIrO2atlowerpotentials;thenickelhydroxides,themaincomponentoftheNispeciesinthePd7IrNi12/Ccatalyst,canfurthercontributetotheEORonPdinalkalinemediathroughareversibleredoxasshownineqn(1).
ThestabilityofthePd/C,Pd2Ni3/C,Pd7Ir/CandPd7IrNi12/CcatalystsfortheEORinalkalinemediawasalsoevaluatedbytheCPtest.
Fig.
5showstheCPcurvesoftheEORonthePd/C,Pd2Ni3/C,Pd7Ir/CandPd7IrNi12/Ccatalysts,inwhichaconstantcurrentdensityof20mAcm2wasappliedfor24000s.
AsshowninFig.
5,thepolarizationpotentialincreasesgrad-uallywithtimeandthroughallthescanningtimethePd7IrNi12/Ccatalystshowsthelowestpolarizationpotentialamongallthecatalysts.
Throughthetimerangingfrom100sto24000s,thePd7IrNi12/Ccatalysthasapotentialdegradationof40mV,whilstitis90mVforPd/C,55mVforPd2Ni3/Cand70mVforPd7Ir/C,indicatingthattheadditionofIr,alongwithNi,toPdcanconcurrentlyfacilitatetheremovaloftheadsorbedethoxyintermediates,hencemakingitmoreresistanttopoisoning.
Fig.
6showsthepolarizationandpower–densitycurvesoftheAEMDEFCwithPd/C,Pd2Ni3/C,Pd7Ir/CandPd7IrNi12/Castheanodecatalyst,andtheinsertisthespecicoperatingconditions.
AscanbeseeninFig.
6,theAEMDEFCwiththePd7IrNi12/Ccatalystastheanodeshowsthehighestperfor-mance.
Theopen-circuitvoltage(OCV)oftheAEMDEFCwiththePd7IrNi12/Ccatalystasanodeis0.
84V,whichis0.
18VhigherthanthatwithPd/C,0.
04VhigherthanthatwithPd2Ni3/C,and0.
14VhigherthanthatwithPd7Ir/C.
ThepeakpowerdensityoftheAEMDEFCwiththePd7IrNi12/Ccatalystasanodeis49mWcm2,whichis122%higherthanthatwithPd/C,44%higherthanthatwithPd2Ni3/Cand69%higherthanthatwithPd7Ir/C.
Fig.
7showsthepolarizationandpower–densitycurvesoftheAEMDEFCwithPd/C,Pd2Ni3/C,Pd7Ir/CandPd7IrNi12/Castheanodecatalystinamodest–highconcentra-tionofsolution,andtheinsertisthespecicoperatingcondi-tions.
FortheAEMDEFCwiththePd7IrNi12/Ccatalystasanode,theOCVis0.
90V,0.
095VhigherthanthatwithPd/C,0.
05VhigherthanthatwithPd2Ni3/C,and0.
04VhigherthanthatwithPd7Ir/C.
ThepeakpowerdensityfortheAEMDEFCwiththePd7IrNi12/Ccatalystastheanodeis92mWcm2,whichis58%higherthanthatwithPd/C,15%higherthanthatwithPd2Ni3/Cand28%higherthanthatwithPd7Ir/C.
4.
ConclusionsInthiswork,acarbonsupportedternaryPdIrNicatalystwithaPd:Ir:Niatomicratioof7:1:12wassynthesizedbythesimultaneousreductionmethod,andcomparedwiththemono-metallicPd/C,bimetallicPd2Ni3/CandPd7Ir/CcatalystsastheanodeinanAEMDEFC.
XPSanalysesshowedthatthesurfacecompositionandoxidationstateofbothIrandNispeciesonthePd7IrNi12/CcatalystwerealmostthesameasthoseinthebimetallicPdIrandPdNicatalysts.
CVandCPresultsprovedthatthePd7IrNi12/CcatalystshowedthehighestperformancefortheEORinalkalinemedia,whichcouldbeattributedtotheconcurrentlyfunctionalmechanismduetotheadditionofIr,alongwithNi.
FuelcellperformancetestsshowedthattheuseofthePd7IrNi12/CcatalystastheanodeofanAEMDEFCcouldyieldapeakpowerdensityof49mWcm2in1.
0MKOHsolutioncontaining1.
0Methanolat60C,whichwas122%higherthanthatwithPd/C,44%higherthanthatwithPd2Ni3/Cand69%higherthanthatwithPd7Ir/C;wheninamodest–highFig.
5CPcurvesoftheEORonthePd/C,Pd2Ni3/C,Pd7Ir/CandPd7IrNi12/Ccatalystsin1.
0MKOH+1.
0Methanol(currentdensity:20mAcm2).
Fig.
6Polarizationandpower–densitycurvesoftheAEMDEFCwithdifferentanodecatalysts(Anode:1.
0MKOH+1.
0Methanol).
Fig.
7Polarizationandpower–densitycurvesoftheAEMDEFCwithdifferentanodecatalysts(Anode:5.
0MKOH+3.
0Methanol).
1432|EnergyEnviron.
Sci.
,2011,4,1428–1433ThisjournalisTheRoyalSocietyofChemistry2011concentrationofsolutionat60C,thepeakpowerdensitywas92mWcm2,whichwas58%higherthanthatwithPd/C,15%higherthanthatwithPd2Ni3/C,and28%higherthanthatwithPd7Ir/C.
AcknowledgementsTheworkdescribedinthispaperwasfullysupportedbyagrantfromtheResearchGrantsCounciloftheHongKongSpecialAdministrativeRegion,China(ProjectNo.
623709).
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