荧光二硫化钼纳米材料的制备及其用于环境中某些离子的检测

发布时间：2018-06-15 17:49

本文选题：荧光二硫化钼纳米片 + 化学计量学　；参考：《南昌大学》2017年硕士论文

【摘要】：本文以钼酸钠和硫脲为原材料辅以水热法制备荧光二硫化钼纳米片,把荧光二硫化钼纳米片作为荧光探针或纳米酶,并结合光谱法和化学计量学,对环境中常见的离子(Pb~(2+)、S2-和Fe~(2+))进行分析检测。文中所提出的方法绿色环保,操作简单,选择性好,灵敏度高,且快速,能运用到实际样品中。本论文的主要内容如下:第一章:阐述了二维纳米材料过渡金属硫属化物—二硫化钼纳米片的制备方法,物理化学性质以及在分析检测中的应用研究;简单的描述了检测对象以及创新点;展望了荧光二硫化钼纳米片在其它领域中的发展前景。第二章:以钼酸钠和硫脲为原材料辅以水热法制备荧光二硫化钼纳米片,采用透射电子显微镜,X-射线能谱,X-射线衍射,扫描电子显微镜,紫外-可见光谱和红外光谱等表征手段对其形貌结构和化学性质进行分析。荧光二硫化钼纳米片最佳激发和发射波长分别为250 nm和405 nm,当Pb~(2+)加入荧光二硫化钼纳米片中能诱导荧光增强,随后加入S2-荧光猝灭,以此构建“turn on-off”荧光传感器来对Pb~(2+)和S2-进行检测。第三章:以上合成的二硫化钼纳米片被证明具有类过氧化物酶的催化活性,在有过氧化氢的条件下能够催化氧化邻苯二胺生成黄色产物2,3-二氨基吩嗪。进一步加入Fe~(2+)到纳米片中,能够显著地增强二硫化钼纳米片的类过氧化物酶的催化活性,据此原理构建出一种无标记比色纳米酶传感器,实现对Fe~(2+)的灵敏检测。同时采用多元曲线分辨-交替最小二乘(MCR-ALS)对反应过程中的动力学光谱数据进行解析,发现Fe~(2+)增强二硫化钼纳米片的类过氧化物酶的催化活性的原因是使其反应速率常数增大。第四章:以上二硫化钼纳米片催化过氧化氢氧化邻苯二胺产生的黄色产物2,3-二氨基吩嗪同时具有很强的荧光,基于产物的荧光性质,构建了荧光检测Fe~(2+)的传感器。同时采用一种化学计量学“二阶校正”方法—平行因子分析法(PARAFAC)来消除实际湖水样中的背景干扰,从而实现在未知背景干扰物质的存在下对湖水中的Fe~(2+)的检测。本文研究的创新点主要有:(1)合成荧光二硫化钼纳米片,构建几种光学传感器实现对环境中几种离子的检测,并且具有良好的选择性和灵敏度;(2)将化学计量学工具应用到荧光二硫化钼纳米片传感器中,解释传感器响应过程中的可能机理问题以及增加传感器在实际样品中应用的性能。
[Abstract]:In this paper, we use sodium molybdate and thiourea as raw materials to prepare molybdenum disulfide nanoscale with hydrothermal method, and take the fluorescent nano disulfide nanosulfide as a fluorescent probe or nanoscale, and combine the spectrometric method and chemometrics to analyze the common ions (Pb~ (2+), S2- and Fe~ (2+)) in the environment. The method proposed in this paper is green and operation. The main contents of this paper are as follows: first chapter: the preparation method, the physical and chemical properties and the application of the molybdenum disulfide nanosulfide nanomaterials are described in the first chapter. The second chapter: using sodium molybdate and thiourea as raw materials to prepare molybdenum disulfide nanosulfide by hydrothermal method and using transmission electron microscope, X- ray energy spectrum, X- ray diffraction, scanning electron microscope, ultraviolet visible spectrum and infrared spectrum. The optimum excitation and emission wavelengths of the phosphor disulfide nanometers are 250 nm and 405 nm respectively. When Pb~ (2+) is added to the fluorescent nano disulfide nanoscale, the fluorescence enhancement can be induced, and then S2- fluorescence quenching is added to construct the "turn on-off" fluorescence sensor to detect Pb~ (2+) and S2-. The third chapter: the above synthesized molybdenum disulfide nanosulfide has been proved to have the catalytic activity of the peroxidase, and can catalyze the oxidation of phthalamine to produce the yellow product 2,3- two amino phenazine under the condition of hydrogen peroxide. Further addition of Fe~ (2+) to the nanoscale can significantly enhance the peroxidase of molybdenum disulfide nanoscale. On the basis of the catalytic activity, a colorless nano enzyme sensor was constructed to detect the Fe~ (2+) sensitively. At the same time, the kinetic spectral data of the reaction process were analyzed by multivariate curve resolution alternating least squares (MCR-ALS), and the catalytic activity of Fe~ (2+) enhanced molybdenum disulfide like peroxidase was found. The reason is that the rate constant of the reaction is increased. The fourth chapter: the yellow product of 2,3- two amino phenazine produced by the oxidation of o-phthalamine by the molybdenum disulfide nanoscale has very strong fluorescence. Based on the fluorescence properties of the product, a sensor for fluorescence detection of Fe~ (2+) is constructed. At the same time, a chemometrics "two order correction" is used. "Method parallel factor analysis (PARAFAC) method (PARAFAC) is used to eliminate the background interference in the actual lake water, so as to realize the detection of Fe~ (2+) in the lake water under the presence of unknown background interferences. The main innovations of this paper are as follows: (1) synthesis of fluorosulfide nanosulfide nanoscale and several optical sensors to realize several ions in the environment Detection, and has good selectivity and sensitivity; (2) the chemometrics tool is applied to the fluorescence sensor of molybdenum disulfide nanoscale, to explain the possible mechanism problems in the response process of the sensor and to increase the performance of the sensor in the actual sample.
【学位授予单位】：南昌大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：X830;O657.3;TB383.1

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