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    Biosynthesis and characterization of mesoporous organic–inorganic hybrid iron phosphate

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    MaterialsChemistryandPhysics116(2009319–322
    ContentslistsavailableatScienceDirect
    MaterialsChemistryandPhysics
    journalhomepage:www.elsevier.com/locate/matchemphys
    Materialssciencecommunication
    Biosynthesisandcharacterizationofmesoporousorganic–inorganichybridironphosphate
    WeijiaZhoua,WenHea,b,∗,XudongZhanga,HongshiZhaoa,ZhengmaoLia,ShunpuYana,XiuyingTiana,XiananSuna,XiuxiuHana
    ab
    DepartmentofMaterialsScienceandEngineering,ShandongInstituteofLightIndustry,Jinan250353,PRChinaBiomaterialsResearchCenter,SouthChinaUniversityofTechnology,Guangzhou510640,PRChina
    articleinfoabstract
    Mesoporousorganic–inorganichybridironphosphatehasbeensynthesizedbyaprecipitationmethodwithyeastcellsasbiotemplate.Theyeastcellsareusedtoregulatethenucleationandgrowthofironphosphate.Thesmall-angleX-raydiffraction(SXRDpatternsshowashort-rangeorderedstructureinthedriedandcalcinedsamples.TheBJH(Barrett–Joyner–Halendamodelsrevealthattheaverageporesizesareat13.9nmfordriedsampleandat14.8nmforcalcinedsample.Thesamplecalcinedat300◦Chasthehighestspecificsurfaceareaof146.2m2g−1.Transmissionelectronmicroscopy(TEManalysesrevealawormhole-likemesoporousstructureinthesamples.Fouriertransforminfrared(FT-IRspectraareusedtoanalyzethechemicalbondlinkagesinhybridmesoporousFePO4materials.TheFePO4coatedcarbonhashigherconductivitythanuncoatedone,whichhaspotentialuseforlithiumbatterymaterials.
    CrownCopyright©2009PublishedbyElsevierB.V.Allrightsreserved.
    Articlehistory:
    Received26October2008
    Receivedinrevisedform2April2009Accepted5April2009Keywords:Biomaterials
    MicroporousmaterialsSurfacepropertiesElectricalconductivity
    1.Introduction
    SinceMCM-41silicamolecularsieveswerefirstreportedin1992[1,2],theresearchinthefieldofmesoporousmaterialswithhighspecificsurfaceareahasbeenaveryhottopic.Overthepastfewdecades,mesoporousmetalphosphateshaveattractedmuchattentionbecauseoftheirimportantapplicationsincatalysis,adsorptionandseparation[3–6].Comparedwithphosphate-basedmesoporousmaterials(Al,Ti,ZrandCe[7–10],onlyafewsyntheticmethodshavebeenreportedforthepreparationofmesoporousironphosphates[11–13].Insomeopen-frameworkironphosphates,thespacesbetweenparticlescanbefilledwithorganicmolecules,suchasorganic–inorganichybridmesoporousironoxophenylphosphatesynthesizedusingsodiumdodecylsulfateasatemplate[12].Ironphosphatehasbeenreportedasagoodcatalystforselectiveoxi-dationreactions,e.g.oxidativedehydrogenationofisobutyricacidtomethacrylicacid[14],andfortheselectiveoxidationofmethanewhenitwassupportedbyMCM-41orSBA-15[15,16].Inparticular,ironphosphateisausefullithiumbatterymaterial[17,18].
    Templateiscommonlyemployedforcontrollingproductionofmaterialswithorderedstructureanddesiredproperties.Examplesofthetemplatesvaryingfromcopolymerstoorderedlatexparticles
    havebeenconsiderablyreported,butonlyafewsyntheticmethodshavebeenreportedforthepreparationofmesoporousmaterialsusingmicrobecellsasatemplate[19].Here,wehavepreparedmesoporousorganic–inorganichybridironphosphatebyasimpleprecipitationmethodusingyeastcellsasbiotemplate.Themeso-porousstructureofthesynthesizedmaterialsisthermallystableupto300◦C.Themesoporousorganic–inorganichybridironphos-phatecanbeusedasLiFePO4/CcathodematerialforLi-ionbatteryaftercalcinationinreducingatmosphere[20].
    2.Experimental
    2.1.Materialsandmethods
    Thestartingmaterialsusedinthisstudyincludedferricchloride(FeCl3·6H2O,99.0%,SinopharmChemicalReagentCo.,Ltd,disodiumhydrogenphosphate(Na2HPO4·12H2O,99.0%,TianjinBodiChemicalCo.,Ltd,sodiumacetate(CH3COONa·3H2O,99.0%,TianjinBodiChemicalCo.,Ltdandbaker’syeastcells(instantdryyeast,AngelYeastCo.,Ltd.Allchemicalreagentswereinanalyticalgrade.
    Quantitativeyeastcellswerecultivatedin30mlglucoseaqueoussolutionfor30minat36◦C.0.01molFeCl3·6H2Owasdissolvedin20mldistilledwater,and0.01molNa2HPO4·12H2Owasdissolvedin50mldistilledwater.TheFeCl3solutionwasdroppedintotheyeastcellssolutionwithvigorousstirring.TheFeCl3/yeastsolutionwascontinuouslystirredatroomtemperaturefor2htoobtainaFe-cellssuspension.TheNa2HPO4solutionwasaddedtotheFe-cellssuspensionunderaconstantstirringcondition,andsuperfluoussodiumacetateaqueoussolutionwasusedtoadjustpHvalueto5.5(thebestactivityofyeastcells,thenthemixturewashomogenizedfor2handagedfor48h.Thereactioncanbedescriptedasfollows(Eq.(1:
    FeCl3+Na2HPO4+NaAC→FePO4+3NaCl+HAC
    (1
    ∗Correspondingauthorat:DepartmentofMaterialsScienceandEngineering,ShandongInstituteofLightIndustry,Jinan250353,PRChina.Tel.:+86053188522792;fax:+86053188522792.
    E-mailaddress:hewen1960@126.com(W.He.
    0254-0584/$–seefrontmatter.CrownCopyright©2009PublishedbyElsevierB.V.Allrightsreserved.doi:10.1016/j.matchemphys.2009.04.013

    320W.Zhouetal./MaterialsChemistryandPhysics116(2009319–322
    Table1
    TheBETspecificsurfaceareaofhybridironphosphatewithvariedyeastcellsamounts.
    Yeastcellsweight(g0
    BET(m2g−1
    90.3
    0.4103.2
    0.8120.2
    1.2106.3
    1.682.9
    2.052.5
    3.036.7
    Theresultantmaterialswerewashedwithdistilledwaterandethanol,andcol-lectedusingcentrifugationmethod.Thewetsamplewasthenfreeze-driedandlappingfinish.TheresultanthybridFePO4sampleswereheatedatdifferenttem-peratures80,300,400,500,600and700◦Cfor2h,andtheBETspecificsurfaceareaandconductivitiesoftheproductsweredetermined.2.2.Characterizations
    Thesmall-angleX-raydiffraction(SXRDtechniquewasperformedonanX-raydiffractometerwithCuK␣(

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