海洋用电化学传感器的制备及研究

发布时间：2018-01-03 07:37

  本文关键词：海洋用电化学传感器的制备及研究　出处：《华东师范大学》2017年硕士论文　论文类型：学位论文

  更多相关文章： 海水 Ir/IrO_2pH电极 Ag/Ag_2S H_2S电极 金汞齐电极

【摘要】：21世纪是海洋世纪,研究海洋环境中的各种理化性质关乎人类生存和发展。原位测试能够及时反馈测试环境的理化参数的变化情况,因而是研究海洋的学者们关注的热点。本课题主要制备了几种具有体积小巧、操作简单、便于微型化、灵敏度高、可原位测试等特点,并能用于海洋环境测试的电化学传感器,主要内容如下:(1)采用熔融碳酸盐法和NaOH循环热氧化法制备Ir/IrO2 pH电极,并对电极的表面形貌、成分含量、电极的响应时间、可逆性和稳定性等工作性能进行综合分析,认为NaOH循环热氧化法是较适合的制备Ir/IrO2电极的方法。在此基础上,首次提出采用水热水化法改进电极的稳定性。实验结果表明:水热水化处理后的电极具有响应速率快(3s)、灵敏度高(70.5mV/pH)、重复性好、滞后性小、使用寿命长等优点。在长达一个多月的连续测试中,电势漂移小于5 mV。该水热处理方法有效地解决了Ir/IrO2 pH电极长期以来存在的电势漂移现象,提高了电极的稳定性。(2)选用Ag丝作为金属基体,分别采用硫化钠法、蘸取银浆法和硫代乙酰胺(CH3CSNH2)法制备Ag/Ag2S电极。并从中筛选出适合海洋环境使用的Ag/AgaS电极的制备方法。实验结果表明:后两种方法所制备的电极均具有响应速率快、灵敏度高、检测范围广的特点,有效改进了硫化钠法制备的电极的性能。但是考虑到敏感膜与金属基体之间的附着作用,硫代乙酰胺法制备的电极硫化程度更高与基体之间的结合更加紧密,因而更适合使用在特殊环境下使用。(3)在模拟海洋环境中的应用:制备出适合检测海洋离子的金汞齐电极,并应用于Mn2+、Cu2+和S2-等多种离子的检测。同时将电极应用到在高达80℃的环境中进行应用,仍然能获得较好的溶出伏安曲线。因此金汞齐电极具有高温环境下工作的应用前景。并将前期制备的Ir/Ir02 pH和Ag/Ag2S H2S电极在高达150℃的高温高压下进行测试。实验结果表明:所制备的电极内对温度和浓度的变化呈现出较理想的能斯特响应,可以初步应用于高温高压环境。
[Abstract]:In 21th century, the ocean century, the study of various physical and chemical properties in the marine environment is related to the survival and development of human beings. In situ testing can timely feedback changes in the physical and chemical parameters of the test environment. Therefore, it is a hot topic for the scholars to study the ocean. In this paper, we have prepared several kinds of characteristics, such as small size, simple operation, easy to miniaturize, high sensitivity, in situ testing and so on. The electrochemical sensor which can be used in marine environment testing, the main contents are as follows: 1) the Ir/IrO2 pH electrode was prepared by melting carbonate method and NaOH cyclic thermal oxidation method. The surface morphology, composition content, response time, reversibility and stability of the electrode were analyzed. It is considered that NaOH cyclic thermal oxidation is a more suitable method for preparing Ir/IrO2 electrode. It is the first time to improve the stability of the electrode by the method of hydrothermal treatment. The experimental results show that the electrode after hydrothermal treatment has a fast response rate of 3sN, high sensitivity of 70.5 MV / pH ~ (-1) and good reproducibility. Small lag, long service life and so on. In more than a month of continuous testing. The potential drift is less than 5 MV. The method of hydrothermal treatment effectively solves the phenomenon of potential drift of Ir/IrO2 pH electrode for a long time. The stability of the electrode was improved. (2) Ag wire was used as the metal matrix and sodium sulfide method was used respectively. Dipping silver paste and thioacetamide CH3CSNH2). The preparation method of Ag/AgaS electrode suitable for marine environment was selected. The experimental results showed that the electrode prepared by the latter two methods had a fast response rate. Because of its high sensitivity and wide detection range, the performance of the electrode prepared by sodium sulphide method is improved effectively, but the adhesion between the sensitive film and the metal substrate is considered. The sulfidation degree of the electrode prepared by thioacetamide method is higher than that of the substrate. Therefore, it is more suitable for use in special environment. 3) in simulated marine environment: the gold amalgam electrode suitable for ocean ion detection is prepared and applied to Mn2. Cu2 and S2- are used to detect many kinds of ions. At the same time, the electrode is applied in the environment as high as 80 鈩，

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