基于钒取代磷钨酸盐复合薄膜的制备及传感性质研究

发布时间：2018-03-22 18:32

本文选题：多金属氧酸盐　切入点：复合薄膜　出处：《哈尔滨理工大学》2014年硕士论文　论文类型：学位论文

【摘要】：随着材料科学的不断发展，构建一种具有光、电、磁性质的多功能薄膜成为材料学科的研究重点。本文利用层接层静电自组装技术制备了两种包含钒取代磷钨酸盐的多层复合薄膜{PEI/PSS/[PDDA/P_2W_(17)V-CNTs]10}及{PEI/[P_2W_(17)V-CNTs/PEI-CuO]n/P_2W_(17)V-CNTs}，利用紫外-可见吸收光谱(UV-vis)、循环伏安(CV)、原子力显微镜(AFM)、扫描电子显微镜(SEM)及X-射线光电子能谱(XPS)对复合薄膜的组装、表面形貌、组成进行了可靠的表征，并利用电化学工作站对薄膜的电化学传感性质进行了一系列的研究。具体的研究结果如下：对复合薄膜{PEI/PSS/[PDDA/P_2W_(17)V-CNTs]10}的循环伏安以及安培计时实验研究结果表明，，所制备的薄膜对亚硝酸盐具有很好的催化活性，在0.05M (pH=7)的磷酸盐缓冲溶液中催化电位为+0.9V；同时实验结果显示，10层的复合薄膜具有一个宽的线性范围5×10~(-8)M到2.13×10~(-3)M，较低的检测限0.0367μM，较高的灵敏度0.35mA·mM~(-1)以及非常优异的稳定性，并且在其他可能的干扰物质的存在下仍具有十分杰出的抗干扰性能。此外，该薄膜可作为亚硝酸盐传感器被成功的应用于真实样品中对于NO_2~-的检测，这表明所制备的薄膜在电化学传感器领域具有潜在的应用前景。通过对复合薄膜{PEI/[P_2W_(17)V-CNTs/PEI-CuO]n/P_2W_(17)V-CNTs}电催化性质的研究得出所制备的复合薄膜对于碘酸根具有很好的电催化活性。当在0.5M (pH=2.5) Na_2SO_4-H_2SO_4缓冲溶液中加入碘酸盐后，在大约-0.5V处复合薄膜显示出了对于碘酸盐很明显的响应。加入0.5mM的IO_3~-后，复合薄膜对于IO3-的催化效率为164.12%。通过一系列的实验得到所制备的复合薄膜的检测范围为1.25×10~(-7)M到1.63×10~(-4)M，灵敏度为4.82mA mM~(-1)以及检测限为0.015μM。并且，该传感器对于体系中可能存在的其他干扰物质具有很好的抗干扰性能以及一个很好的稳定性。该传感器已成功应用于真实食盐样品中碘酸根的检测。
[Abstract]:With the continuous development of material science, a kind of material with light, electricity, Multifunctional films with magnetic properties have become the focus of material research. In this paper, two kinds of multilayer composite films {PEI/PSS/ [PDDA/P_2W_(17)V-CNTs] 10} and {PEI/ [P_2W_(17)V-CNTs/PEI-CuO] n/P_2W_(17)V-CNTs} containing vanadium substituted phosphotungstate have been prepared by using laminated electrostatic self-assembly technique. The UV-Vis absorption spectra have been used for the preparation of two kinds of multilayer composite films {PEI/PSS/ [PDDA/P_2W_(17)V-CNTs] 10} and {PEI/ [P_2W_(17)V-CNTs/PEI-CuO] n/P_2W_(17)V-CNTs}. The assembly of composite films by UV-vis, cyclic voltammetry, atomic force microscopy (AFM), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The surface morphology and composition were characterized reliably, and the electrochemical sensing properties of the films were studied by electrochemical workstation. The results are as follows:. The experimental results of cyclic voltammetry and amperometric time of the composite film {PEI/PSS/ [PDDA/P_2W_(17)V-CNTs] 10} show that the film has good catalytic activity for nitrite. The catalytic potential is 0.9V in the phosphate buffer solution of 0.05M ~ (+), and the experimental results show that the composite film has a wide linear range from 5 脳 10 ~ (-8) M to 2.13 脳 10 ~ (-3) 渭 M, a lower detection limit of 0.0367 渭 M, a high sensitivity of 0.35mA MM-1) and excellent stability. In addition, the film can be successfully used as nitrite sensor for the detection of no _ 2O _ 2- in real samples. This indicates that the prepared films have potential applications in electrochemical sensors. The electrocatalytic properties of the composite film {PEI/ [P_2W_(17)V-CNTs/PEI-CuO] n/P_2W_(17)V-CNTs} show that the composite film has good electrocatalytic activity for iodate. When the iodate salt is added to the 0.5 M ~ (-1) pH ~ (2.5) Na_2SO_4-H_2SO_4 buffer solution, the electrocatalytic activity of the composite film is obtained. At about -0.5 V, the composite film showed a significant response to iodate. The catalytic efficiency of the composite film for IO3- is 164.12. The detection range of the composite film is 1.25 脳 10 ~ (-7) M to 1.63 脳 10 ~ (10) ~ (-4) m ~ (-1) and the detection limit is 0.015 渭 M. through a series of experiments. The sensor has a good anti-interference performance and a good stability to other interference substances that may exist in the system. The sensor has been successfully applied to the detection of iodate in real salt samples.
【学位授予单位】：哈尔滨理工大学
【学位级别】：硕士
【学位授予年份】：2014
【分类号】：O611.3;TB383.2

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