新型溶解氧检测仪探头的研制
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摘要
在本论文中,我们研制了一种新型溶解氧检测仪的探头部分,在实现快速灵敏检测的基础上,具有简单的结构和相对较小的外观尺寸。我们对其中涉及到的工作电极的制备及修饰方法进行研发,并对探头的装配进行了优化及实际测试,具体包括以下几个部分:
1.基于实验室条件,开发了机器辅助制备微阵列电极的方法,成功的制备了微阵列电极,可以实现规模化生产。我们从简单入手,首先开发了手工制备微阵列电极的方法和质量检测手段;在此基础上,针对手工方法的诸多缺点进行了改进,进而实现了机器辅助的方法;
2.基于上述电极制备方法,优化了探头装配方法,制备出用于检测溶解氧的探头,并对其性能进行了比较全面的测试和评价,与合作厂家共同研发出了溶解氧检测仪样机;
3.建立了一种无模板无表面活性剂的简单方法,用于制备树枝状金纳米结构,进行了详细的表征,推断了其形成机理及实验条件对形貌的影响,将其用于溶解氧的催化,获得了良好的效果;
4.建立了一种快速简便的方法,实现对金微盘阵列电极的多孔化和钯纳米粒子的修饰同步完成,并将修饰电极用于溶解氧的检测,获得了良好的效果。
In this dissertation, we have manufactured the probe unit of a new type dissolved oxygen (DO) detector. Beside sensing fast and readily of the DO detector, it has concise structure and relatively small dimension. We have developed the preparation and modification methods of the working electrode involved, and optimized the assembling of the probe unit. Then, we gave detail valuation of its performance. The dissertation covered following aspects:
1. We have developed a method to prepare microelectrode array electrode with the aid of certain kind of equipment based on the laboratory environment. We started the preparation simply using operation by hand-working, and also established the criterion to evaluate the success of the preparation. Further, we improved the preparation approach utilized the modified machine to assist the work;
2. We optimized the assembling of the probe unit, and evaluated its electrochemical performance. We have fabricated prototype of a new DO detector in cooperation with our partner.
3. We have developed a templeteless, surfacantless, simple electrochemical route to prepare dendritic gold nanostructure. The formation mechanism related to experimental conditions was discussed. The as-prepared modified electrode has excellent catalytic activity to oxygen reduction in neutral KCl solution.
4. We have developed a one-step facile route to fabricate Pd modified porous Au films. The as-prepared Pd modified electrode was used to the detection of oxygen and showed a good sensitivity.
1.基于实验室条件,开发了机器辅助制备微阵列电极的方法,成功的制备了微阵列电极,可以实现规模化生产。我们从简单入手,首先开发了手工制备微阵列电极的方法和质量检测手段;在此基础上,针对手工方法的诸多缺点进行了改进,进而实现了机器辅助的方法;
2.基于上述电极制备方法,优化了探头装配方法,制备出用于检测溶解氧的探头,并对其性能进行了比较全面的测试和评价,与合作厂家共同研发出了溶解氧检测仪样机;
3.建立了一种无模板无表面活性剂的简单方法,用于制备树枝状金纳米结构,进行了详细的表征,推断了其形成机理及实验条件对形貌的影响,将其用于溶解氧的催化,获得了良好的效果;
4.建立了一种快速简便的方法,实现对金微盘阵列电极的多孔化和钯纳米粒子的修饰同步完成,并将修饰电极用于溶解氧的检测,获得了良好的效果。
In this dissertation, we have manufactured the probe unit of a new type dissolved oxygen (DO) detector. Beside sensing fast and readily of the DO detector, it has concise structure and relatively small dimension. We have developed the preparation and modification methods of the working electrode involved, and optimized the assembling of the probe unit. Then, we gave detail valuation of its performance. The dissertation covered following aspects:
1. We have developed a method to prepare microelectrode array electrode with the aid of certain kind of equipment based on the laboratory environment. We started the preparation simply using operation by hand-working, and also established the criterion to evaluate the success of the preparation. Further, we improved the preparation approach utilized the modified machine to assist the work;
2. We optimized the assembling of the probe unit, and evaluated its electrochemical performance. We have fabricated prototype of a new DO detector in cooperation with our partner.
3. We have developed a templeteless, surfacantless, simple electrochemical route to prepare dendritic gold nanostructure. The formation mechanism related to experimental conditions was discussed. The as-prepared modified electrode has excellent catalytic activity to oxygen reduction in neutral KCl solution.
4. We have developed a one-step facile route to fabricate Pd modified porous Au films. The as-prepared Pd modified electrode was used to the detection of oxygen and showed a good sensitivity.
引文
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1 Fletcher, S. and M.D. Horne, Random assemblies of microelectrodes (RAM (TM) electrodes) for electrochemical studies. Electrochemistry Communications, 1999. 1(10): p. 502-512.
2 Provent, C., et al., Boron-doped diamond electrodes and microelectrode-arrays for the measurement of sulfate and peroxodisulfate. Electrochimica Acta, 2004. 49(22-23): p. 3737-3744.
3董绍俊,赵峰,王鸣魁。微盘阵列电极的制备方法。ZL. 200310110043.7
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3董绍俊,赵峰,王鸣魁。微盘阵列电极的制备方法。ZL. 200310110043.7
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1 Y. Li, Y.-Y. Song, C. Yang, and X.-H. Xia, Electrochemistry Communications 9:981 (2007).
2 S. Papadimitriou, S. Armyanov, E. Valova, A. Hubin, O. Steenhaut, E. Pavlidou, G. Kokkinidis, and S. Sotiropoulos, Journal of Physical Chemistry C 114:5217 (2010).
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4 J. Yin, J. B. Jia, and L. D. Zhu, International Journal of Hydrogen Energy 33:7444 (2008).
5 W. Zhao, J. J. Xu, C. G. Shi, and H. Y. Chen, Electrochemistry Communications 8:773 (2006).
6 J. B. Jia, L. Y. Cao, and Z. H. Wang, Langmuir 24:5932 (2008).
7 W. Huang, M. H. Wang, J. F. Zheng, and Z. L. Li, Journal of Physical Chemistry C 113:1800 (2009).
8 Y. P. Deng, W. Huang, X. Chen, and Z. L. Li, Electrochemistry Communications 10:810 (2008).
9 A. Kiani and E. N. Fard, Electrochimica Acta 54:7254 (2009).
10 X. Xu, C. Liu, J. Jia, B. Liu, X. Yang, and S. Dong, Electroanalysis 20:797 (2008).
11 W. Zhao, P. Y. Ge, J. J. Xu, and H. Y. Chen, Langmuir 23:8597 (2007).
12 Y. Shen, L. H. Bi, B. F. Liu, and S. J. Dong, New Journal of Chemistry 27:938 (2003).
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