三維石墨烯空心球的制備及電化學(xué)性能研究
發(fā)布時(shí)間:2018-07-31 15:44
【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(jī)械性能以及物理化學(xué)性能,因而受到研究者的關(guān)注。但是二維的結(jié)構(gòu),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(xué)傳感器方面的應(yīng)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(jié)構(gòu),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(chǎng)穩(wěn)定,與溶液的接觸面積更大,電化學(xué)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(duì)三維石墨烯空心球進(jìn)行形貌及尺寸的表征,并進(jìn)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(jié)構(gòu)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(jié)構(gòu)完整,尺寸約為100 nm,分散性較好。XRD分析結(jié)果顯示三維石墨烯空心球純凈無雜質(zhì)。Raman光譜證明三維石墨烯空心球?yàn)樯賹咏Y(jié)構(gòu)且低缺陷。將三維石墨烯空心球通過自動(dòng)噴涂設(shè)備噴涂在ITO導(dǎo)電玻璃表面,構(gòu)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(cè)。采用循環(huán)伏安(CV)與差分脈沖循環(huán)伏安(DPV)對(duì)三維石墨烯空心球/ITO電極進(jìn)行電化性能測(cè)試。實(shí)驗(yàn)結(jié)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(duì)L-DOPA檢測(cè)的靈敏度為0.48 μAμM-1。在UA干擾下的DPV測(cè)試,證明該電極具有優(yōu)異的選擇性。同時(shí),該電極具有優(yōu)異的重復(fù)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(xué)生物傳感器中對(duì)L-DOPA的檢測(cè)。
[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(xué)位授予單位】:哈爾濱理工大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2017
【分類號(hào)】: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.
【學(xué)位授予單位】:哈爾濱理工大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2017
【分類號(hào)】:TQ127.11
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