单分散掺硫碳微球的水热制备及其表征.pdf

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1、第29卷第7期无机化学学报V0I．29No．72013年7月CHINESEJ0URNALOFIN0RGANICCHEMISTRY1391—1399单分散掺硫碳微球的水热制备及其表征郑明涛肖勇张浩然董汉武龚学斌徐汝淳雷炳富刘应亮刘晓瑭(华南农业大学理学院应用化学系，广州510642)摘要：以可溶性淀粉为碳源，采用硫辅助水热碳化法一步制备了平均粒径约为4m的单分散掺硫碳微球。利用扫描电镜、透射电镜、X射线衍射、氮气吸脱附、傅里叶变换红外光谱、x射线光电子能谱、固体核磁共振等手段对掺硫碳微球的结构和性质进行了表征。硫辅助水热碳化法可以在高浓度条

2、件下高产量地制备分散性良好的掺硫碳微球．更重要的是硫原子可以同步进入碳的网络结构巾。与传统水热碳化法相比，采用硫辅助水热碳化法制备的掺硫碳微球具有更高的比表面积．其可能的原因是硫原子的引入产生了大量的化学与结构缺陷：一S—S一、一S一、一SO：一和一S0一等基团构成化学缺陷，而噻吩等五元环取代石墨六元环形成结构缺陷。关键词：碳微球；硫掺杂；水热碳化；表征中图分类号：0611．4；TB383文献标识码：A文章编号：1001—4861(2013)07—1391—09DOI：10．3969~．issn．1001—4861．2013．00．244

3、HydrothermalSynthesisandCharacterizationofSulfur-DopedCarbonMicrospheresZHENGMing—TaoXIAOYongZHANGHao-RanDONGHan-WuGONGXue—BinXURu—ChunLEIBing-FuLIUYing-LiangLIUXiao-Tang(DepartmentofAppliedChemistry,CollegeofScience，SouthChinaAgriculturalUniversity,Guangzhou510642，China)

4、Abstract：Sulfur—dopedcarbonmicrospheresfSCMSs)withmeansizeofabout4Ixmwerepreparedsuccessfullybyasimpleone—stepsulfur—assistedhydrothermalcarbonizationfASHTC)method．Solublestarchwasusedasearb0nprecursorandsublimesulfurassulfursource．Theas—preparedSCMSswerecharacterizedsyst

5、ematicallybymeansofSEM，TEM，XRD，N2absorption—desorptionisotherms，FTIR，XPS，andsolidNMR．TheexistingformsofsulfurinSCMSswerealsodiscussed．Itwasfoundthatmon0disDersedSCMSswithhighoutputcouldbeobtainedunderhighstarchconcentrationf1．0g·mL1andsulfuratomscouldbeintroducedintocarbo

6、nnetworkseasily，indicatingthattheASHTCisapowerfulmethodforSCMSsynthesis．Forcomparison，carbonmicrospheresfCMSs1weresynthesizedbyconventionalhydrothermalearbonizationofstarchintheabsenceofsulfurunderthesamehydrothermalconditions．Experimentalresultsshowthattheas．synthesizedS

7、CMSsexhibitmuchhigherspecificSUrfaceareathanthatofCMSs．ThereasonoftheincreaseofsurfaceareaofSCMSsmaybeduetothestructuralandchemicaldefectsresultedfromthesulfurdoping．ThechemicaIdefectscomefromthe．S．S．．一S一，-SO2-and—SO—groups，whilethestructuraldefectsresultfromthesubstituti

8、onofgraphitehexatomic-ringsbythiophenefive—memberedringsinSCMSs．Keywords：carbonmicrosphere；sulfu