三维石墨烯空心球的制备及电化学性能研究
发布时间：2018-07-31 15:44
【摘要】：石墨烯是一种只有单层原子厚度的二维材料,具有优异的机械性能以及物理化学性能,因而受到研究者的关注。但是二维的结构,大大降低了石墨烯与溶液的接触面积,因此石墨烯在电化学传感器方面的应用受到了较大的限制。三维(3D)石墨烯空心球(hollow graphene balls)具有三维中空的结构,相比于二维的石墨烯,在保留二维石墨烯优异性能外,具有大的比表面积且形变场稳定,与溶液的接触面积更大,电化学性能优异。本文通过还原氯化镍的方法制备球形镍颗粒模板,然后通过碳化包覆法将石墨烯包覆在镍颗粒模板表面,刻蚀镍,制备三维石墨烯空心球。采用扫描电子显微镜(SEM)和透射电镜(TEM)对三维石墨烯空心球进行形貌及尺寸的表征,并进行了 X射线衍射(XRD)与拉曼光谱(Raman)表征,确定三维石墨烯空心球的结构以及缺陷。SEM图和TEM图中可以看出三维石墨烯空心球球形结构完整,尺寸约为100 nm,分散性较好。XRD分析结果显示三维石墨烯空心球纯净无杂质。Raman光谱证明三维石墨烯空心球为少层结构且低缺陷。将三维石墨烯空心球通过自动喷涂设备喷涂在ITO导电玻璃表面,构建三维石墨烯空心球/ITO电极,用于生物传感器中左旋多巴(L-DOPA)的检测。采用循环伏安(CV)与差分脉冲循环伏安(DPV)对三维石墨烯空心球/ITO电极进行电化性能测试。实验结果表明三维石墨烯空心球/ITO电极在浓度为0-80μM的范围下,对L-DOPA检测的灵敏度为0.48 μAμM-1。在UA干扰下的DPV测试,证明该电极具有优异的选择性。同时,该电极具有优异的重复性及稳定性,因此三维石墨烯空心球/ITO电极可以用于电化学生物传感器中对L-DOPA的检测。
[Abstract]:Graphene is a kind of two-dimensional material with the thickness of single layer atoms. It has excellent mechanical and physical and chemical properties, so it has attracted the attention of researchers. However, the two-dimensional structure greatly reduces the contact area between graphene and solution, so the application of graphene in electrochemical sensor is limited. Three-dimensional (3D) graphene hollow spheres (hollow graphene balls) have three-dimensional hollow structure. Compared with two-dimensional graphene, (hollow graphene balls) has large specific surface area, stable deformation field and larger contact area with solution, in addition to preserving the excellent properties of two-dimensional graphene. Excellent electrochemical performance. In this paper, the spherical nickel particle template was prepared by reducing nickel chloride, and then graphene was coated on the surface of nickel particle template by carbonization, and the three-dimensional graphene hollow spheres were prepared by etching nickel. The morphology and size of three-dimensional graphene hollow spheres were characterized by scanning electron microscope (SEM) (SEM) and transmission electron microscopy (TEM). X-ray diffraction (XRD) and Raman spectroscopy (Raman) were used to characterize the morphology and size of the hollow spheres. The structure of the three-dimensional graphene hollow spheres and the defects. SEM and TEM diagrams show that the spherical structure of the three-dimensional graphene hollow spheres is complete. The size of the hollow spheres is about 100 nm. The results of XRD analysis show that the three-dimensional graphene hollow spheres are pure and impurity free. Raman spectra show that the three-dimensional graphene hollow spheres are of small layer structure and low defects. Three-dimensional graphene hollow spheres were sprayed on the surface of ITO conductive glass by automatic spraying equipment. Three-dimensional graphene hollow spheres / ITO electrodes were constructed for the detection of left dopa (L-DOPA) in biosensor. Cyclic voltammetry (CV) and differential pulse cyclic voltammetry (DPV) were used to test the electrochemical properties of 3D graphene hollow spheres / ITO electrodes. The experimental results show that the sensitivity of the three dimensional graphene hollow spheres / ITO electrode to L-DOPA detection is 0.48 渭 A 渭 M-1 in the concentration range of 0-80 渭 M. The DPV test under UA interference shows that the electrode has excellent selectivity. At the same time, the electrode has excellent repeatability and stability, so the three-dimensional graphene hollow sphere / ITO electrode can be used for the detection of L-DOPA in electrochemical biosensor.
【学位授予单位】：哈尔滨理工大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TQ127.11
[Abstract]:Graphene is a kind of two-dimensional material with the thickness of single layer atoms. It has excellent mechanical and physical and chemical properties, so it has attracted the attention of researchers. However, the two-dimensional structure greatly reduces the contact area between graphene and solution, so the application of graphene in electrochemical sensor is limited. Three-dimensional (3D) graphene hollow spheres (hollow graphene balls) have three-dimensional hollow structure. Compared with two-dimensional graphene, (hollow graphene balls) has large specific surface area, stable deformation field and larger contact area with solution, in addition to preserving the excellent properties of two-dimensional graphene. Excellent electrochemical performance. In this paper, the spherical nickel particle template was prepared by reducing nickel chloride, and then graphene was coated on the surface of nickel particle template by carbonization, and the three-dimensional graphene hollow spheres were prepared by etching nickel. The morphology and size of three-dimensional graphene hollow spheres were characterized by scanning electron microscope (SEM) (SEM) and transmission electron microscopy (TEM). X-ray diffraction (XRD) and Raman spectroscopy (Raman) were used to characterize the morphology and size of the hollow spheres. The structure of the three-dimensional graphene hollow spheres and the defects. SEM and TEM diagrams show that the spherical structure of the three-dimensional graphene hollow spheres is complete. The size of the hollow spheres is about 100 nm. The results of XRD analysis show that the three-dimensional graphene hollow spheres are pure and impurity free. Raman spectra show that the three-dimensional graphene hollow spheres are of small layer structure and low defects. Three-dimensional graphene hollow spheres were sprayed on the surface of ITO conductive glass by automatic spraying equipment. Three-dimensional graphene hollow spheres / ITO electrodes were constructed for the detection of left dopa (L-DOPA) in biosensor. Cyclic voltammetry (CV) and differential pulse cyclic voltammetry (DPV) were used to test the electrochemical properties of 3D graphene hollow spheres / ITO electrodes. The experimental results show that the sensitivity of the three dimensional graphene hollow spheres / ITO electrode to L-DOPA detection is 0.48 渭 A 渭 M-1 in the concentration range of 0-80 渭 M. The DPV test under UA interference shows that the electrode has excellent selectivity. At the same time, the electrode has excellent repeatability and stability, so the three-dimensional graphene hollow sphere / ITO electrode can be used for the detection of L-DOPA in electrochemical biosensor.
【学位授予单位】：哈尔滨理工大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TQ127.11
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