新型掺杂正硅酸乙酯的三维石墨烯/MoS_2气凝胶的制备及其结构表征
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摘要
第一次系统研究了一种在水热条件下制备三维石墨烯/MoS_2(3D-G/MoS_2)组装体的新方法,突破了冷冻干燥得到气凝胶的传统方法,创新性地引入正硅酸乙酯,通过硅化物填充实现3D-G/MoS_2气凝胶的制备,建立了最佳的稳定制备工艺。该方法不需要添加化学交联剂,简单、可控性高。经X射线衍射、红外光谱、扫描电镜、透射电镜、热重分析和拉曼光谱检测分析表明,制备的3D-G/MoS_2样品具有密度低、孔隙率高、机械强度高和稳定性高的特点。与其他方法相比,此制备工艺具有较好的稳定性和重复性,可为构筑其他金属硫化物与石墨烯组装体复合物及其应用研究提供借鉴。
A new method for 3D-G/MoS_2 assembly prepared under hydrothermal conditions for the first was studied,breaking the traditional preparation of freeze-dried to give aerogels with creatively introducing ethyl orthosilicate.By filling silicide achieved 3D-G/MoS_2 assembly,the best and stable preparation process was established.This method did not require adding chemical crosslinking agents,which was highly controllable and maneuverable.The ray diffraction,infrared spectroscopy,scanning electron microscopy,transmission electron microscope,thermal analysis,and Raman spectroscopy detection analysis showed that the preparation of sample had characteristics such as low density,high porosity,high mechanical strength and high stability.Compared with other methods,this preparation had good stability and repeatability,the method can provide a reference for constructing other sulphides-graphene composites and its application and assembly.
A new method for 3D-G/MoS_2 assembly prepared under hydrothermal conditions for the first was studied,breaking the traditional preparation of freeze-dried to give aerogels with creatively introducing ethyl orthosilicate.By filling silicide achieved 3D-G/MoS_2 assembly,the best and stable preparation process was established.This method did not require adding chemical crosslinking agents,which was highly controllable and maneuverable.The ray diffraction,infrared spectroscopy,scanning electron microscopy,transmission electron microscope,thermal analysis,and Raman spectroscopy detection analysis showed that the preparation of sample had characteristics such as low density,high porosity,high mechanical strength and high stability.Compared with other methods,this preparation had good stability and repeatability,the method can provide a reference for constructing other sulphides-graphene composites and its application and assembly.
引文
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[3]Svoronos P D,Bruno T J.Carbonyl sulfide:a review of its chemistry and properties[J].Ind Eng Chem Res,2002,41(22):5321-5336.
[4]Wu Z S,Yang S,Sun Y,et al.3D nitrogen-doped graphene aerogel-supported Fe2O3nanoparticles as efficient electrocatalysts for the oxygen reduction reaction[J].Journal of the A-merican Chemical Society,2012,134(22):9082-9085.
[5]Cong H P,Ren X C,Wang P,et al.Macroscopic multifunctional graphene-based hydrogels and aerogels by a metal ion induced self-assembly process[J].ACS Nano,2012,6(3):2693-2703.
[6]刘湘梅,蒋瑞.层状自组装方法制备三维石墨烯复合材料[J].材料保护,2014,47(增刊1):20-22.
[7]王臻.类石墨烯MoS2/石墨烯复合纳米材料的合成及其电化学储锂性能的研究[D].杭州:浙江大学,2013.
[8]黄国创.过渡金属硫化物与石墨烯复合纳米材料的合成及其电化学储锂性能[D].杭州:浙江大学,2013.
[9]Liu S S,Zhang X B,Shao H,et al.Preparation of MoS2nanofibers by electrospinning[J].Mater Lett,2012,73:223E5.
[10]汤鹏,肖坚坚,郑超,等.类石墨烯二硫化钼及其在光电子器件上的应用[J].物理化学学报,2013,29(4):667-677.
[11]Kim K S,Park S J.Influence of multi-walled carbon nanotubes on the electrochemical performance of graphenenanocomposites for supercapacitor electrodes[J].Electro Chim Acta,2011,56:1629-1635.
[12]Stankovich S,Dikin D A,Piner R D,et al.Synthesis of graphene-based nanosheets via chemical reduction of exfoliated graphite oxide[J].Carbon,2007,45(7):1558-1565.