超微电极的制备及其在扫描电化学显微镜中的应用
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摘要
微电极因其小尺寸表现出许多与常规电极不同的优良性质:高传质速率、小时间常数、低IR降、高信噪比和高电流密度等,因此,微电极成为电化学和电分析化学的前沿领域之一。超微电极的这些优点使其在电化学动力学、伏安检测、修饰纳米微电极、传感器、成像探针和单分子检测等方面都有着广阔的潜在应用背景。因此探讨超微电极的制作及其应用有着重要的意义。本论文包含以下四个部分:
第一章首先对超微电极的基本原理及特点、制作方法、表征方法及应用等方面做了详细介绍。且对扫描电化学显微镜的实验装置、工作模式及应用等也进行了阐述。
第二章用电化学镀和电化学刻蚀相结合的方法制备了不同材料(铂、金、碳纤维)和不同尺寸的超微圆盘电极。并用循环伏安法对其进行表征,它们都有良好的伏安响应。并根据极限电流算出电极的有效半径,其中最小有效半径可达到1.6μm。观察了扫速的变化对循环伏安曲线形状的影响,我们还通过对比超微电极放置四周前后的稳态电流对其稳定性进行了考察,结果证明我们制备的超微电极有很好的稳定性。
第三章HAuCl_4存在的条件下,采用常规铂电极在单一K_3Fe(CN)_6溶液中进行循环伏安扫描沉积普鲁士蓝(PB),同时探讨了K_3Fe(CN)_6浓度、HAuCl_4浓度、及溶液pH值对PB沉积速度的影响。此外,研究了该修饰电极的电化学性质,结果表明Au颗粒的存在大大改善了膜的性能,并用该修饰电极对L-半胱氨酸及溶液中葡萄糖进行检测,分别求出了它们的线性范围和检测限。实验结果表明PB修饰电极对它们都表现出很强的电催化活性。
第四章用第三章中优化了的条件在铂超微电极上沉积PB制成微修饰电极,在KCl溶液中用循环伏安法对修饰电极进行表征,实验证明PB成功地沉积到了铂微电极的表面。该修饰电极在pH 7.0的磷酸缓冲溶液(PBS)中具有良好的化学和电化学稳定性,对H_2O_2表现出强的电催化活性,安培法检测H_2O_2的线性范围为5.6×10~(-7)～3.2×10~(-4)M,检出下限为6.0×10~(-8)M。将所制得的超微电极用作扫描电化学显微镜(SECM)的探针,对自组装上膜过程进行了表征,并对(SECM)渐近线进行拟合,求得了酶催化反应的异相动力学常数。
Microelectrode has a lot of advantages for its small dimension,such as high mass transport,low iR drop,high signal to noise ratio,high current density,low time constant.Therefore,microelectrode is one of the front fields of electrochemistry and electroanalytical chemistry.Because of these properties of microelectrode,the applications in dynamics of electrochemistry,cyclic voltammetric detection,modified electrode,sensor,immaing tip and detection of single molecule of nanoelectrode show a wider potential future.Consequently,investigaton on microelectrode's fabrication and the application have the vital significance.There are four parts in this paper,main contents are as follows:
In chapter one of this paper,the basic principle and characteristic,fabrication method,characterized method and application of microelectrode were first introduced briefly.Then the basic apparatus,operation mode and application of scanning electrochemical microscopy(SECM) were reviewed in detail.
In chapter two,several different material(platinum,gold,carbon fiber) and dimensions ultramicroelectrodes were fabricated by the method of electrochemical plated insulated film and electrochemical etching.The microelectrodes are characterized by CV;they have the good volt-ampere response.We calculated the effective radius by limitted-current,its smallest effective radius to be possible to achieve 1.6μm.The influence factor on the shape of CV curve such as scanning rate is investigated.Finally,we have also observed their stability through contrast the steady current laying aside about four weeks;the results indicated that these microelectrodes have good stability.
In chapter three,the PB-modified electrode is prepared in the single K_3Fe(CN)_6 solution containing HAuCl_4 by electrodeposition.Then,Influencing factors on deposited rate,such as concentration of K_3Fe(CN)_6,HAuCl_4,and PH,are investigated. Moreover,the PB-modified electrode is characterized by CV,the results shows the properties of the PB-modified electrode are improved obviously in present of Au particles.Finally,the L-cysteine and glucose are monitored by the PB-modified electrode,strongly electrocatalytic activities toward L-cysteine and glucose are observed.
In chapter four,we prepared the PB modified platinum microelectrode using the optimum conditions which had been selected in chapter three.Moreover,the PB-modified electrode is characteri2ed by CV in KCl solution.The results indicated that PB deposited on the surface of platinum microelectrode,this PB modified microelectrode had strongly electrocatalytic activity toward the reduction of H_2O_2 in PH7.0 PBS,a linear dependence of the catalytic current versus H_2O_2 concentration was obtained in the range of 5.6×10~(-7)～3.2×10~(-4)M with a detection limit of 6.0×10~(-8)M. We also prepare the SECM tip by the microelectrode we fabricated.We characterize the self-assembled film on the gold electrode by SECM surface topography, furthermore;we useing the probe approaching curve of SECM calculated the kinetic constant of bimolecular interaction.
第一章首先对超微电极的基本原理及特点、制作方法、表征方法及应用等方面做了详细介绍。且对扫描电化学显微镜的实验装置、工作模式及应用等也进行了阐述。
第二章用电化学镀和电化学刻蚀相结合的方法制备了不同材料(铂、金、碳纤维)和不同尺寸的超微圆盘电极。并用循环伏安法对其进行表征,它们都有良好的伏安响应。并根据极限电流算出电极的有效半径,其中最小有效半径可达到1.6μm。观察了扫速的变化对循环伏安曲线形状的影响,我们还通过对比超微电极放置四周前后的稳态电流对其稳定性进行了考察,结果证明我们制备的超微电极有很好的稳定性。
第三章HAuCl_4存在的条件下,采用常规铂电极在单一K_3Fe(CN)_6溶液中进行循环伏安扫描沉积普鲁士蓝(PB),同时探讨了K_3Fe(CN)_6浓度、HAuCl_4浓度、及溶液pH值对PB沉积速度的影响。此外,研究了该修饰电极的电化学性质,结果表明Au颗粒的存在大大改善了膜的性能,并用该修饰电极对L-半胱氨酸及溶液中葡萄糖进行检测,分别求出了它们的线性范围和检测限。实验结果表明PB修饰电极对它们都表现出很强的电催化活性。
第四章用第三章中优化了的条件在铂超微电极上沉积PB制成微修饰电极,在KCl溶液中用循环伏安法对修饰电极进行表征,实验证明PB成功地沉积到了铂微电极的表面。该修饰电极在pH 7.0的磷酸缓冲溶液(PBS)中具有良好的化学和电化学稳定性,对H_2O_2表现出强的电催化活性,安培法检测H_2O_2的线性范围为5.6×10~(-7)～3.2×10~(-4)M,检出下限为6.0×10~(-8)M。将所制得的超微电极用作扫描电化学显微镜(SECM)的探针,对自组装上膜过程进行了表征,并对(SECM)渐近线进行拟合,求得了酶催化反应的异相动力学常数。
Microelectrode has a lot of advantages for its small dimension,such as high mass transport,low iR drop,high signal to noise ratio,high current density,low time constant.Therefore,microelectrode is one of the front fields of electrochemistry and electroanalytical chemistry.Because of these properties of microelectrode,the applications in dynamics of electrochemistry,cyclic voltammetric detection,modified electrode,sensor,immaing tip and detection of single molecule of nanoelectrode show a wider potential future.Consequently,investigaton on microelectrode's fabrication and the application have the vital significance.There are four parts in this paper,main contents are as follows:
In chapter one of this paper,the basic principle and characteristic,fabrication method,characterized method and application of microelectrode were first introduced briefly.Then the basic apparatus,operation mode and application of scanning electrochemical microscopy(SECM) were reviewed in detail.
In chapter two,several different material(platinum,gold,carbon fiber) and dimensions ultramicroelectrodes were fabricated by the method of electrochemical plated insulated film and electrochemical etching.The microelectrodes are characterized by CV;they have the good volt-ampere response.We calculated the effective radius by limitted-current,its smallest effective radius to be possible to achieve 1.6μm.The influence factor on the shape of CV curve such as scanning rate is investigated.Finally,we have also observed their stability through contrast the steady current laying aside about four weeks;the results indicated that these microelectrodes have good stability.
In chapter three,the PB-modified electrode is prepared in the single K_3Fe(CN)_6 solution containing HAuCl_4 by electrodeposition.Then,Influencing factors on deposited rate,such as concentration of K_3Fe(CN)_6,HAuCl_4,and PH,are investigated. Moreover,the PB-modified electrode is characterized by CV,the results shows the properties of the PB-modified electrode are improved obviously in present of Au particles.Finally,the L-cysteine and glucose are monitored by the PB-modified electrode,strongly electrocatalytic activities toward L-cysteine and glucose are observed.
In chapter four,we prepared the PB modified platinum microelectrode using the optimum conditions which had been selected in chapter three.Moreover,the PB-modified electrode is characteri2ed by CV in KCl solution.The results indicated that PB deposited on the surface of platinum microelectrode,this PB modified microelectrode had strongly electrocatalytic activity toward the reduction of H_2O_2 in PH7.0 PBS,a linear dependence of the catalytic current versus H_2O_2 concentration was obtained in the range of 5.6×10~(-7)～3.2×10~(-4)M with a detection limit of 6.0×10~(-8)M. We also prepare the SECM tip by the microelectrode we fabricated.We characterize the self-assembled film on the gold electrode by SECM surface topography, furthermore;we useing the probe approaching curve of SECM calculated the kinetic constant of bimolecular interaction.
引文
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