【摘要】：石墨烯是一種只有單層原子厚度的二維材料,具有優(yōu)異的機械性能以及物理化學性能,因而受到研究者的關注。但是二維的結構,大大降低了石墨烯與溶液的接觸面積,因此石墨烯在電化學傳感器方面的應用受到了較大的限制。三維(3D)石墨烯空心球(hollow graphene balls)具有三維中空的結構,相比于二維的石墨烯,在保留二維石墨烯優(yōu)異性能外,具有大的比表面積且形變場穩(wěn)定,與溶液的接觸面積更大,電化學性能優(yōu)異。本文通過還原氯化鎳的方法制備球形鎳顆粒模板,然后通過碳化包覆法將石墨烯包覆在鎳顆粒模板表面,刻蝕鎳,制備三維石墨烯空心球。采用掃描電子顯微鏡(SEM)和透射電鏡(TEM)對三維石墨烯空心球進行形貌及尺寸的表征,并進行了 X射線衍射(XRD)與拉曼光譜(Raman)表征,確定三維石墨烯空心球的結構以及缺陷。SEM圖和TEM圖中可以看出三維石墨烯空心球球形結構完整,尺寸約為100 nm,分散性較好。XRD分析結果顯示三維石墨烯空心球純凈無雜質。Raman光譜證明三維石墨烯空心球為少層結構且低缺陷。將三維石墨烯空心球通過自動噴涂設備噴涂在ITO導電玻璃表面,構建三維石墨烯空心球/ITO電極,用于生物傳感器中左旋多巴(L-DOPA)的檢測。采用循環(huán)伏安(CV)與差分脈沖循環(huán)伏安(DPV)對三維石墨烯空心球/ITO電極進行電化性能測試。實驗結果表明三維石墨烯空心球/ITO電極在濃度為0-80μM的范圍下,對L-DOPA檢測的靈敏度為0.48 μAμM-1。在UA干擾下的DPV測試,證明該電極具有優(yōu)異的選擇性。同時,該電極具有優(yōu)異的重復性及穩(wěn)定性,因此三維石墨烯空心球/ITO電極可以用于電化學生物傳感器中對L-DOPA的檢測。
[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.
【學位授予單位】：哈爾濱理工大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：TQ127.11

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