含Mo化合物纳米复合材料的电化学生物传感器的性能研究及应用

发布时间：2018-01-25 18:19

本文关键词： Pt纳米粒子杂多酸氧化石墨烯金属氧化物血清　出处：《东北师范大学》2017年硕士论文　论文类型：学位论文

【摘要】：传感器具有设备简单、体型小、操作简单等特点,其中电化学传感器具有灵敏度高、高效、可多次循环利用、特异性好、成本低廉、检测速度快等优势,因此对于实际样品检测具有重要意义。目前电化学传感器的主要发展方向是制备新材料的修饰电极,以达到检测速度更快,更精准,且材料更简单、环保、易得等效果。本文采用多种复合纳米材料来制备新型修饰电极,利用能量色散X射线谱图(EDX)、扫描电镜(SEM)、红外(IR)、X-射线粉末衍射(XRD)、X射线光电子能谱(XPS)、透射电极(TEM)等手段对合成材料及修饰电极的表面形貌进行了表征。运用循环伏安法(CV)、计时电流法(I-t)、微分脉冲伏安法(DPV)等多种电化学方法对修饰电极的电催化性能进行研究,并对实际样品人体血清中多种生物物质进行测定。首先,Pt/IMo6/GO-GCE的新型多种纳米复合材料修饰电极的制备,并对其电化学催化生物物质进行研究。我们通过电沉积法将石墨烯(GO)、Na5[IMo6O24]?3H2O杂多酸和Pt纳米自组装制备新型复合纳米材料修饰电极(Pt/IMo6/GO-GCE)。通过SEM、IR等方法对材料及修饰电极表面形貌进行表征,同时利用CV、I-t、DPV电化学方法表征修饰电极的电化学行为。结果表明:该纳米材料修饰电极不仅保持了杂多酸电催化活性,同时增大了修饰电极比表面积。与GCE、GO-GCE和IMo6/GO-GCE相比,Pt/IMo6/GO-GCE显示出响应速度快、稳定性好、导电性强、比表面积大、选择性好等优点。在扫速为100 mv/s,电解质溶液为0.05 M稀硫酸溶液中,催化抗坏血酸(AA)、多巴胺(DA)和尿酸(UA)表现出较高的电催化活性。结果表明,三种物质的检测限分别为3.0μM、0.22μM和0.72μM,其对应线性相关系数分别为0.999、0.999和0.998。且证明该纳米复合材料修饰电极可用于同时测定实际样品人体血清中AA、DA和UA的含量。其次,研究了非酶电化学传感器ZnO-MoO3-C/PDDA-GCE对葡萄糖的催化,利用安培法定量测定葡萄糖的含量,并应用于实际样品的检测。通过自组装法利用纳米复合材料制备了修饰电极ZnO-MoO3-C/PDDA-GCE。利用IR、TEM、SEM、XPS、XRD、电化学技术等多种手段对材料及电极表面形貌进行表征。结果表明复合纳米材料及对应修饰电极均制备成功,且表现出良好的催化效果。在100 mv/s扫速,0.1 M NaOH电解质溶液中,修饰电极对葡萄糖表现出良好的电催化活性,与ZnO-C/PDDA-GCE和MoO3-C/PDDA-GCE相比ZnO-MoO3-C/PDDA-GCE灵敏度更高,最低检测限为1.74μM、灵敏度为69.5μAmM-1cm-2、线性范围为6-700μM。总之该修饰电极具有电催化活性强、响稳定性好、响应速度快等特点,已成功应用于测定人体血清中的葡萄糖含量。
[Abstract]:The sensor has the advantages of simple equipment, small size and simple operation, among which the electrochemical sensor has the advantages of high sensitivity, high efficiency, multiple recycling, good specificity, low cost, fast detection speed and so on. At present, the main development direction of electrochemical sensor is the preparation of new materials modified electrode, in order to achieve faster detection, more accurate, more simple materials, environmental protection. In this paper, a new type of modified electrode was prepared by using a variety of composite nanomaterials. Energy dispersive X-ray spectroscopy (EDX), scanning electron microscopy (SEM) and IR (IR) were used to prepare the modified electrode. X ray powder diffractometer XRDX X ray photoelectron spectroscopy (XPS). The surface morphology of the composite and modified electrode was characterized by means of transmission electrode (TEM), cyclic voltammetry (CV) and chronoamperometric method (I-t). Various electrochemical methods such as differential pulse voltammetry (DPVV) were used to study the electrocatalytic properties of the modified electrode and to determine a variety of biomaterials in human serum. The preparation and electrochemical catalytic biomaterials of Pt/IMo6/GO-GCE modified electrode were studied. [IMo6O24]? Preparation of a novel composite nano-material modified electrode PtP / IMo6 / GO-GCEC by self-assembly of 3H2O heteropoly acid and Pt nanocrystalline via SEM. The surface morphology of the modified electrode and the material were characterized by IR and CVFI-t. The electrochemical behavior of the modified electrode was characterized by DPV. The results showed that the modified electrode not only kept the heteropoly acid electrocatalytic activity, but also increased the specific surface area of the modified electrode and GCE. Compared with IMo6/GO-GCE, GO-GCE / IMo6 / GO-GCE shows fast response, good stability, strong conductivity and large specific surface area. The catalytic activity of ascorbic acid (AAA) was obtained in the presence of 100 MV / s sweep speed and 0.05 M dilute sulfuric acid solution. The results showed that the detection limits of the three compounds were 3.0 渭 M 0.22 渭 M and 0.72 渭 M, respectively. The linear correlation coefficients were 0.999 and 0.998.It was proved that the modified electrode could be used for simultaneous determination of AA in human serum. The content of DA and UA. Secondly, the non-enzymatic electrochemical sensor ZnO-MoO3-C/PDDA-GCE was used to catalyze glucose, and the content of glucose was determined by amperometric method. The modified electrode ZnO-MoO3-C / PDDA-GCEwas prepared by self-assembly method, and the modified electrode ZnO-MoO3-C / PDDA-GCEand XPS was used to prepare ZnO-MoO3-C / PDDA-GCE. The surface morphology of materials and electrodes were characterized by XRD and electrochemical techniques. The results showed that the composite nanomaterials and the corresponding modified electrodes were successfully prepared. The modified electrode showed good electrocatalytic activity for glucose in the electrolyte solution of 100 mv/s sweep speed of 0. 1 M NaOH. Compared with ZnO-C/PDDA-GCE and MoO3-C/PDDA-GCE, ZnO-MoO3-C/PDDA-GCE is more sensitive. The lowest detection limit is 1.74 渭 m, the sensitivity is 69.5 渭 AmM-1cm-2, and the linear range is 6-700 渭 M. in short, the modified electrode has strong electrocatalytic activity and good response stability. It has been successfully applied to the determination of glucose in human serum.
【学位授予单位】：东北师范大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TB33;TP212.3

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