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先进材料znfe2o4FULLPAPER1.IntroductionRechargeablelithium-ionbatteries(LIBs),whichareregardedasoneofthemostpromisingdevicesforenergystorageandconversion,haveattractedtremen-dousattentioninthepastdecades.[1–4]Asweallknow,almostalltheanodesofcommercialLIBsarebasedongraphite-basedmaterials,unfortunately,theystillexhibitarelativelylowLi-storagecapacityof≈372mAhg?1andpotentialsafetyissuesasananode,[5]whichcannotmeetthegreatdemandofhigh-energyappli-cationsincurrentplatforms,suchaselectricvehicles(EVs),hybridEVs,elec-tricitygridstoragedevices,andsoon.[1–6]Therefore,ithasbecomeanurgentandsigni?canttasktoextensivelyexploreevenhighercapacityanodematerialsforthenext-generationLIBs.Attractively,transitionmetaloxides(TMOs)standoutfromversatilenovelanodematerialsowingtotheirlowcost,wideavailability,andespeciallyhighertheoreticalspeci?ccapacities(600mAhg?1).[5,7–11]Further-more,TMOsprovidemuchmoreexcitingchoicestorealizelargereversiblecapacitiesviavariouswaysinvolvingalloying/dealloyingprocesses,insertion/extractionmechanismsand/orconversionreactions.[1–4,12,14]Recently,?neassemblyoftwodistinctTMOsintoahierarchicalnano-hybrids,particularlywithhighlyhomogenerousdispersionatthenanoscale,[9,14]wouldallowustomakethebestofinherentinteractionofeachcomponentforbetterelectrochemicalper-formanceinLIBs,affordingafascinatingavenueto?nelytailor,andfurthergeneratehighlypromisinganodesforhigh-performanceLIBs.[5,9,13]Basedontheappealingconcept,afewofhybridarchitecturesconstructedfromdifferentTMOshavebeententativelyexaminedforLIBs,suchas,Co3O4/Fe2O3,[5]NiFe2O4/Fe2O3,[8]CoO/CoFe2O4,[9]Fe2O3/MnO2,[10]andZnO/ZnFe2O4,[14]whichallverifythattheseuniquehybridanodesareendowedwithevenbetterLi-storageperformance(largerspeci?ccapacity,morestablecyclingperformance,etc.)thananysingleone.[5,8–10,13,14]Self-Sacri?ceTemplateFabricationofHierarchicalMesoporousBi-Component-ActiveZnO/ZnFe2O4Sub-MicrocubesasSuperiorAnodeTowardsHigh-PerformanceLithium-IonBatteryLinruiHou,LinLian,LonghaiZhang,GangPang,ChangzhouYuan,*andXiaogangZhangInthework,afacileyetef?cientself-sacri?cestrategyissmartlydevelopedtoscalablyfabricatehierarchicalmesoporousbi-component-activeZnO/ZnFe2O4(ZZFO)sub-microcubes(SMCs)bycalcinationofsingle-resourcePrussianblueanalogueofZn3[Fe(CN)6]2cubes.ThehybridZZFOSCMsarehomogeneouslyconstructedfromwell-dispersednanocrstallineZnOandZnFe2O4(ZFO)subunitesatthenanoscale.AfterselectivelyetchingofZnOnanodomainsfromthehybrid,porouslyassembledZFOSMCswithintegratearchitectureareobtainedaccordingly.WhenevaluatedasanodesforLIBs,bothhybridZZFOandZFOsamplesexhibitappealingelectrochemicalper-formance.However,theas-synthesizedZZFOSMCsdemonstrateevenbetterelectrochemicalLi-storageperformance,includingevenlargerinitialdischargecapacityandreversiblecapacity,higherratebehaviorandbettercyclingperformance,particularlyathighrates,comparedwiththesingleZFO,whichshouldbeattributedtoitsuniquemicrostructurecharacteristicsandstrikingsynergisticeffectbetweenthebi-component-active,well-dispersedZnOandZFOnanophases.Ofgreatsigni?cance,lightisshedupontheinsightsintothecorrelationbetweentheelectrochemicalLi-storagepropertyandthestruc-ture/componentofthehybridZZFOSMCs,thus,itisstronglyenvisionedthattheelegantdesignconceptofthehybridholdsgreatpromisefortheef?cientsynthesisofadvancedyetlow-costanodesfornext-generationrechargeableLi-ionbatteries.DOI:10.1002/adfm.202102827Prof.L.Hou,L.Lian,L.Zhang,Dr.G.Pang,Prof.C.YuanSchoolofMaterialsScienceandEngineeringAnhuiUniversityofTechnologyMa’anshan243002,P.R.ChinaE-mail:ayuancz@(CAS)KeyLaboratoryofMaterialsforEnergyConversionHefei230026,P.R.ChinaFULLPAPER2[4,12,13]besidesthestrikingeffectofmulti-compo-nentsmentionedabove.Aswellestablishedpreviously,uniquerobustmicro-/nanostruc-tures,asauniquehigher-levelsecondarysuperstructure,typicallyofmicro-/sub-micrometerdimensionsbutinternallycon-sistingofnano-buildingblocksand/ornano-domains,offertheexceptionaladvantagesofbothnanometer-sizedbuildingblocks/nano-domainsandmicro-/submicrometer-sizedassembliesthemselves.[4,5,14–17]Inspe-ci?c,thenano-scaledbuildingblocks/nano-domains,withalargespeci?csurfacearea(SSA)andahighsurface-to-bulkratio,offernegligiblediffusiontimeandarethekeystofavorablekineticsandhighspeci?ccapaci-ties.Andthehigher-levelassemblies,withdesirablemechanicalpropertiesandhightapdensity,guaranteegoodstabilityandpracticalfabrication.[4,18]Inparticular,whenhierarchicalmicro-/nanostructures,especiallywithdesirablemesoporosity,ofhybridhetero-components,werewellconstructedasexpected,remarkableelectrochemicalperformancethencouldbehighlyantici