稻谷壳制备石墨烯纳米片及结构表征  

Preparation and structural characterization of graphene by rice husk

作　　者：程金生 万维宏[1] 陈信炎 郑启祥[1] 

机构地区：[1]嘉应学院医学院客家养生保健研究所,梅州514031

出　　处：《农业工程学报》2015年第12期288-294,共7页Transactions of the Chinese Society of Agricultural Engineering

基　　金：广东自然科学基金项目(S2013010012676);广东医学科学基金(A2014825);2014广东扬帆计划拔尖人才项目

摘　　要：为了充分利用南方丰富的稻谷壳资源,制备附加值较高的石墨烯纳米材料。该文采用稻谷壳可再生资源经高温炭化、过筛、透析等工艺等制备活性炭,将其在高纯氩保护下高温催化石墨化后制备的石墨微晶作为石墨烯的新型碳源。应用具有较大离子半径的硫酸根离子（0.295 nm）为插层剂预处理该石墨微晶,经水热及微波工艺制备石墨烯纳米片。采用透射电镜、扫描电镜、原子力显微镜、红外光谱、拉曼光谱及X射线衍射（X-ray diffraction spectroscopy,XRD）等技术对样品进行了形貌、结构和谱学等表征。原子力图表明,该石墨烯纳米片厚度范围为0.8~1.75 nm,为单层或双层石墨烯;由红外光谱可以观察到1 550 cm-1左右的石墨烯特征碳碳双键骨架振动峰。但未观察到传统Hummers氧化及水合肼法常出现,与石墨烯氧化后缺陷度有关的3 000~3 600 cm-1之间峰及1 250 cm-1左右振动峰。XRD数据显示所制备材料在24.7°亦具有石墨烯特征峰。拉曼光谱分析则显示,该方法所制备材料的与石墨烯层数相关的2D峰峰高接近G带的2倍,而与石墨烯缺陷度有关的D带峰峰高较小。该方法可成功制备单层或双层石墨烯纳米片,研究结果为高效制备基于稻谷壳可再生资源的石墨烯开辟了一条新路。Graphene possesses excellent chemical,physical,mechanical and thermal properties,which has attracted much attention in the past several years.Traditional Hummers-hydrazine hydrate method,mechanical stripping method,chemical vapor deposition（CVD） method,SiC substrate dependence epitaxial growth or other methods for graphene preparation use expensive graphite or gases,leading to high price of graphene.A case of point is Hummers-hydrazine hydrate method,by using the strong oxidants of KMnO 4 and H2O2,graphene is prepared and has many defects（such as vacancy defect,Stone-Wales defect,doped defect and atomic absorption defect） in its structure,which would limit its application prospects.Husk,cornstalk or bagasse are common renewable biomass resources in Southern China（including Guangdong Province,Fujian Province,Hainan Province and Guangxi Zhuang Autonomous Region）,which have had poor utilization ratio in the past decades.In this work,we tried to use the renewable husk resource with low price as the starting material,and by successive sulfate ions intercalation,N,N-dimethylacetamide（DMAC） thermal dispersion,microwave and ice splashing treatments,the husk-derived graphene with high added-value could be obtained.Acticarbon was prepared by high temperature carbonization,washing,vacuum drying,mesh screening and dialysis processes of husk renewable resource,which was graphitized under high-purity argon flow and high temperature（1 800℃） in the presence of Fe2O3,forming graphite crystallite with a size range of 4-25 μm.In this work,the sulfate ions with large ionic radius（0.295 nm） were used as intercalation reagent of the resulted graphite crystallite,and by successive DMAC thermal dispersion,microwave and ice splashing treatments,graphene nanosheets could be obtained readily.The characteristics of the prepared material were measured by transmission electron microscopy（TEM）,scanning electron microscopy（SEM）,atomic force microscopy（AFM）,Fourier transform infrared spectrometry（FTIR）,

关 键 词：废弃物 活性炭 工艺 稻谷壳 石墨烯 

分 类 号：O652.6[理学—分析化学]