电纺微/纳米纤维修饰电极在电化学传感器中的应用研究
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摘要
一维微/纳米材料具有大的比表面积和长径比，将其修饰在电极表面可以大大提高电极面积，并有利于电子传输，因此利用各种方法制备一维微/纳米材料修饰电极一直备受关注。通过静电纺丝技术直接将一维微/纳米纤维修饰在电极表面是一种有效的制备一维材料修饰电极的方法。本文通过静电纺丝技术制备了基于过渡金属氧化物微米纤维修饰电极的非酶葡萄糖传感器和基于多金属氧酸盐（POM）复合纳米纤维修饰电极的亚硝酸盐传感器。主要的工作如下：
1、掺杂氟的二氧化锡（FTO）电极作为纤维接收屏，电纺包含高含量的硝酸铜的无机盐/高聚物混合前驱溶液，经过煅烧后，制得由CuO纳米粒子组成的CuO微米纤维修饰电极并将其应用于非酶葡萄糖传感器的研究。扫描电镜结果表明，CuO纳米颗粒的大小取决于前驱物中硝酸铜的含量。随着硝酸铜含量的增加，纳米尺寸的CuO粒子逐步取代大尺寸的CuO颗粒来组成CuO微米纤维。这些纳米尺寸的CuO粒子大大提高了电极面积和催化反应活性点，从而增强了其修饰电极对葡萄糖的电催化性能。
2、通过静电纺丝和煅烧技术制得NiO微米纤维修饰FTO电极并将其应用于非酶葡萄糖传感器的研究。伏安法和安培分析法研究结果表明，煅烧温度对NiO微米纤维修饰电极的电催化性能有影响，其电催化性能随着煅烧温度的增加而降低。通过300℃煅烧所获得的NiO微米纤维修饰电极对葡萄糖表现出最好的电催化性能。这是因为随着煅烧温度的增加制得的NiO材料的导电性降低，从而使得低温煅烧得到的NiO微米纤维修饰电极的电催化性能最好。
3、通过静电纺丝和煅烧技术制得CuO掺杂-NiO复合微米纤维修饰FTO电极并将其应用于非酶葡萄糖传感器的研究。伏安法和安培分析法研究结果表明，CuO掺杂-NiO复合微米纤维修饰电极的电催化性能较单纯的NiO微米纤维修饰电极有了大幅度的提高。基于CuO掺杂-NiO复合微米纤维修饰电极的葡萄糖传感器具有极高的灵敏度。这主要是因为CuO的掺杂不仅提高了NiO微米纤维的导电性也增加了NiO对葡萄糖催化时的反应活性点。基于CuO掺杂-NiO复合微米纤维修饰电极的传感器被实际应用于检测人体血样中的葡萄糖浓度，其结果与自动生化分析仪的检测结果吻合。
4、氧化铟-氧化锡（ITO）电极作为纤维接收屏，电纺聚乙烯醇(PVA)和α-K6[P_2W_(18)O_(62)]14H2O (P_2W_(18))混合前驱溶液，制得PVA/P_2W_(18)复合纳米纤维修饰电极。经过热交联处理后，PVA/P2W18复合纳米纤维不再溶于水，从而将PVA/P_2W_(18)复合纳米纤维修饰电极应用于亚硝酸盐传感器的研究。伏安法和安培分析法研究结果表明, PVA/P2W18复合纳米纤维修饰电极对亚硝酸盐表现出非常好的电催化还原性能。同时，电极具有很好的长期稳定性和可重现性。
Due to their high surface-to-volume ratio and high aspect ratio, one dimensional (1D)micro/nanomaterials have been widely applied in many fields, especially in the field ofchemically modified electrode because1D micro/nanomaterials can significantly increaseelectrode surface area and help the electron transfer. Therefore, the preparations of1Dmicro/nanomaterials modified electrode using various techniques have attracted great interest.Electrospinning technique is an efficient method for preparing1D micro/nanofibers modifiedelectrode. In this thesis, transition metal oxides microfibers modified electrodes fornonenzymatic glucose sensors and polyoxometalate (POM) hybrid nanofibers modifiedelectrode for nitrite sensor fabricated by electrospinning technique were investigated. Themain achievements are summarized as follows:
1. Fluorine tin oxide (FTO) electrode modified by CuO microfibers composed ofnumerous interconnected CuO nanoparticles for nonenzymatic glucose sensor was preparedby electrospinning precursor containing high percentage content of copper nitrate withsubsequent calcination. The results of scanning electron microscope (SEM) showed the sizeof CuO particles composing CuO microfibers depended on the percentage content of coppernitrate in precursor solution. With increasing the percentage content of copper nitrate, theinterconnected CuO nanoparticles would gradually replace the large-size CuO particles toaccumulate the CuO microfibers, which have the potential to provide larger surface area andmore reaction sites for electrocatalytic performance toward glucose.
2. NiO microfibers were directly immobilized onto the surface of FTO electrode byelectrospinning and calcination for nonenzymatic glucose sensor. The results of cyclicvoltammetry and amperometry proved that calcination temperature has an influence on theelectrocatalytic performance toward the oxidation of glucose at the NiO microfibers modifiedelectrode. The electrocatalytic performance of the NiO microfibers modified electrodedecrease gradually with increasing the calcination temperature. The NiO microfibers modifiedelectrode prepared at low calcination temperature (300℃) presented remarkableelectrocatalytic performance toward the oxidation of glucose. This is because the decrease ofthe conductivity of NiO with the increase of calcination temperature.
3. An improved nonenzymatic glucose sensor based on CuO-doped NiO compositemicrofibers modified FTO electrode was prepared by electrospinning and calcinationtechnique. The results of cyclic voltammetry and amperometry demonstrated that theCuO-doped NiO composite microfibers modified electrode displayed much higherelectrocatalytic performance than the NiO microfibers modified electrode, which can be mainly attributed to the resulting increase in conductive and reaction sites at NiO microfibersinduced by doping CuO. Additionally, its application for detecting glucose concentration ofhuman serum sample showed good agreement with the results obtained from automaticbiochemical analyzer.
4. POM hybrid nanofibers modified electrode was prepared by electrospinning of amixture of poly (vinyl alcohol)(PVA) and α-K_6[P_2W_(18)O_(62)]14H_2O (P_2W_(18)) onto surface ofindium tin oxide (ITO) electrode. After thermal crosslinking, the P_2W_(18)hybrid nanofibers areinsoluble in aqueous solutions, which ensure that the P2W18hybrid nanofibers modifiedelectrode could be applied as nitrite sensor. The results of cyclic voltammetry andamperometry demonstrated that the P2W18hybrid nanofibers modified ITO electrode exhibitsexcellent electrocatalytic performance toward the reduction of nitrite. Additionally, long-termstability and reproducibility were observed.
1、掺杂氟的二氧化锡（FTO）电极作为纤维接收屏，电纺包含高含量的硝酸铜的无机盐/高聚物混合前驱溶液，经过煅烧后，制得由CuO纳米粒子组成的CuO微米纤维修饰电极并将其应用于非酶葡萄糖传感器的研究。扫描电镜结果表明，CuO纳米颗粒的大小取决于前驱物中硝酸铜的含量。随着硝酸铜含量的增加，纳米尺寸的CuO粒子逐步取代大尺寸的CuO颗粒来组成CuO微米纤维。这些纳米尺寸的CuO粒子大大提高了电极面积和催化反应活性点，从而增强了其修饰电极对葡萄糖的电催化性能。
2、通过静电纺丝和煅烧技术制得NiO微米纤维修饰FTO电极并将其应用于非酶葡萄糖传感器的研究。伏安法和安培分析法研究结果表明，煅烧温度对NiO微米纤维修饰电极的电催化性能有影响，其电催化性能随着煅烧温度的增加而降低。通过300℃煅烧所获得的NiO微米纤维修饰电极对葡萄糖表现出最好的电催化性能。这是因为随着煅烧温度的增加制得的NiO材料的导电性降低，从而使得低温煅烧得到的NiO微米纤维修饰电极的电催化性能最好。
3、通过静电纺丝和煅烧技术制得CuO掺杂-NiO复合微米纤维修饰FTO电极并将其应用于非酶葡萄糖传感器的研究。伏安法和安培分析法研究结果表明，CuO掺杂-NiO复合微米纤维修饰电极的电催化性能较单纯的NiO微米纤维修饰电极有了大幅度的提高。基于CuO掺杂-NiO复合微米纤维修饰电极的葡萄糖传感器具有极高的灵敏度。这主要是因为CuO的掺杂不仅提高了NiO微米纤维的导电性也增加了NiO对葡萄糖催化时的反应活性点。基于CuO掺杂-NiO复合微米纤维修饰电极的传感器被实际应用于检测人体血样中的葡萄糖浓度，其结果与自动生化分析仪的检测结果吻合。
4、氧化铟-氧化锡（ITO）电极作为纤维接收屏，电纺聚乙烯醇(PVA)和α-K6[P_2W_(18)O_(62)]14H2O (P_2W_(18))混合前驱溶液，制得PVA/P_2W_(18)复合纳米纤维修饰电极。经过热交联处理后，PVA/P2W18复合纳米纤维不再溶于水，从而将PVA/P_2W_(18)复合纳米纤维修饰电极应用于亚硝酸盐传感器的研究。伏安法和安培分析法研究结果表明, PVA/P2W18复合纳米纤维修饰电极对亚硝酸盐表现出非常好的电催化还原性能。同时，电极具有很好的长期稳定性和可重现性。
Due to their high surface-to-volume ratio and high aspect ratio, one dimensional (1D)micro/nanomaterials have been widely applied in many fields, especially in the field ofchemically modified electrode because1D micro/nanomaterials can significantly increaseelectrode surface area and help the electron transfer. Therefore, the preparations of1Dmicro/nanomaterials modified electrode using various techniques have attracted great interest.Electrospinning technique is an efficient method for preparing1D micro/nanofibers modifiedelectrode. In this thesis, transition metal oxides microfibers modified electrodes fornonenzymatic glucose sensors and polyoxometalate (POM) hybrid nanofibers modifiedelectrode for nitrite sensor fabricated by electrospinning technique were investigated. Themain achievements are summarized as follows:
1. Fluorine tin oxide (FTO) electrode modified by CuO microfibers composed ofnumerous interconnected CuO nanoparticles for nonenzymatic glucose sensor was preparedby electrospinning precursor containing high percentage content of copper nitrate withsubsequent calcination. The results of scanning electron microscope (SEM) showed the sizeof CuO particles composing CuO microfibers depended on the percentage content of coppernitrate in precursor solution. With increasing the percentage content of copper nitrate, theinterconnected CuO nanoparticles would gradually replace the large-size CuO particles toaccumulate the CuO microfibers, which have the potential to provide larger surface area andmore reaction sites for electrocatalytic performance toward glucose.
2. NiO microfibers were directly immobilized onto the surface of FTO electrode byelectrospinning and calcination for nonenzymatic glucose sensor. The results of cyclicvoltammetry and amperometry proved that calcination temperature has an influence on theelectrocatalytic performance toward the oxidation of glucose at the NiO microfibers modifiedelectrode. The electrocatalytic performance of the NiO microfibers modified electrodedecrease gradually with increasing the calcination temperature. The NiO microfibers modifiedelectrode prepared at low calcination temperature (300℃) presented remarkableelectrocatalytic performance toward the oxidation of glucose. This is because the decrease ofthe conductivity of NiO with the increase of calcination temperature.
3. An improved nonenzymatic glucose sensor based on CuO-doped NiO compositemicrofibers modified FTO electrode was prepared by electrospinning and calcinationtechnique. The results of cyclic voltammetry and amperometry demonstrated that theCuO-doped NiO composite microfibers modified electrode displayed much higherelectrocatalytic performance than the NiO microfibers modified electrode, which can be mainly attributed to the resulting increase in conductive and reaction sites at NiO microfibersinduced by doping CuO. Additionally, its application for detecting glucose concentration ofhuman serum sample showed good agreement with the results obtained from automaticbiochemical analyzer.
4. POM hybrid nanofibers modified electrode was prepared by electrospinning of amixture of poly (vinyl alcohol)(PVA) and α-K_6[P_2W_(18)O_(62)]14H_2O (P_2W_(18)) onto surface ofindium tin oxide (ITO) electrode. After thermal crosslinking, the P_2W_(18)hybrid nanofibers areinsoluble in aqueous solutions, which ensure that the P2W18hybrid nanofibers modifiedelectrode could be applied as nitrite sensor. The results of cyclic voltammetry andamperometry demonstrated that the P2W18hybrid nanofibers modified ITO electrode exhibitsexcellent electrocatalytic performance toward the reduction of nitrite. Additionally, long-termstability and reproducibility were observed.
引文
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