基于一维纳米结构的电化学传感器研究
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摘要
本论文工作主要包括基于一维纳米结构的化学与生物传感器的设计与研究,具体工作包括以下几个方面:
第一,基于束状硅纳米线的谷胱甘肽电化学传感器的研究。利用去除氧化层的硅纳米线表面对金属离子的还原性,将三价金离子还原在硅纳米线表面,在硅纳米线表面形成稳定均匀的金纳米颗粒,并且利用金纳米颗粒易于与巯基反应的特点,将氨基为末端的有机小分子巯基乙胺修饰在金纳米颗粒表面。修饰后的硅纳米线由于其独特的成束性、较大的比表面积、金颗粒的修饰对硅纳米线传导性增强的特点,与化学修饰后所具有的氨基末端与三肽生物分子谷胱甘肽末端的羧基的相互作用,被用作检测谷胱甘肽的直接电化学传感器。实验结果表明,基于硅纳米线的谷胱甘肽传感器具有低浓度线性响应(0.33-2.97μM)、灵敏度高(48.5 mA.mmol-1)、以及检测底限浓度较低(0.33μM,measured)的优点。
第二,硅纳米线在溶液中的分散与葡萄糖电化学传感器的研究。分别以磷酸缓冲溶液、乙醇溶液与水溶性全氟取代聚合物Nafion溶液作为溶剂,研究了硅纳米线在溶液中的分散。实验结果表明,去除掉氧化层的硅纳米线与金纳米颗粒修饰的硅纳米线在Nafion溶液中可以形成稳定均匀的分散液,在其它溶剂中难以分散;而未经表面处理的硅纳米线在几种溶液中均难以形成分散液。金纳米颗粒修饰的硅纳米线分散液被用于酶电极的修饰,制备了葡萄糖电化学传感器,电化学实验结果表明,硅纳米线的修饰对葡萄糖的传感具有明显的增强作用。根据实验结果,我们提出了去掉氧化层的硅纳米线由于表面的Si-H与Nafion的磺酸基之间的作用而使之易于溶剂化进而在溶液中分散的机理。
第三,基于硅纳米线阵列的细胞色素c电化学传感器的研究。利用化学刻蚀法由硅片制备了硅纳米线阵列,经过表面去氧化层处理后,制备了检测蛋白质细胞色素c的电化学传感器。实验表明,硅纳米线阵列电极对细胞色素c有良好的电化学响应,并且在低浓度条件下具备线性响应的特点,灵敏度为2.75μA.mM-1。根据与未经表面处理的硅纳米线阵列电极的实验结果相对比,提出了细胞色素c所具备的羧基末端与硅纳米线阵列电极表面的Si-H相互作用从而改善传感性能的检测机理。
第四,基于表面修饰ZnO纳米管阵列的葡萄糖电化学传感器的研究。在本实验室发展的电化学沉积法制备氧化锌纳米管阵列的基础上,利用氧化锌表面与葡萄糖氧化酶(GOx)之间的静电吸引作用,将GOx修饰在氧化锌纳米管阵列的表面,并引入Nafion以达到进一步固化GOx与增强传感器抗干扰能力的目的,制备了基于氧化锌纳米管阵列的葡萄糖电化学传感器。实验结果证明,由于ZnO纳米管的独特结构使其比表面积相对较大,电化学沉积的方法使ZnO纳米管与基底电极ITO玻璃之间的接触较好,可以改善ZnO结构与基底电极之间的电子传输效率,传感器具备灵敏度高(30.85μA.cm-2.mM-1),线性范围较宽(10μM-4.2 mM),检测底限浓度较低(10μM,measured),响应时间较短(<5s)等优点。
The fabrication and properties of chemical sensors and biosensors based modified one-dimensional nanomaterials have been studied in this doctorial dissertation. The main results can be concluded as follows:
First, the functionalized SiNWs, chemically modified with Au nanoparticles, and with amino-terminated organic molecules anchored on the surface of the nanoparticles, were fabricated into the electrochemical biosensors for glutathione (GSH). The biosensor showed good linear response to GSH of low concentration (0.33-2.97μM), high sensitivity (48.5 mA.mmol-1), and a low limit of detection (0.33μM, measured) by virtue of strong sorption ability and high electrical conductivity of the modified SiNWs based electrode.
Second, the dispersion of silicon nanowires in Nafion toward the fabrication of amperometric biosensors for glucose was studied. We demonstrated a convenient method of the dispersion of SiNWs in solvent in virtue of the interaction between Nafion and the surface of SiNWs. The dispersion of the HF-etched SiNWs and Au nanoparticles modified SiNWs exhibited homogeneous and long time steady properties. Moreover, the Au nanoparticles modified SiNWs could be used to modify the enzyme-electrode as the biosensors for glucose sensing, which proved to have an effect of enhancement for the detection of glucose. The present method of the dispersion of the SiNWs and the modification of electrode could be extended to the construction of the one-dimensional nanostructures based nanodevices.
Third, the direct electrochemical biosensor for cytochrome c based on the silicon nanowire arrays was fabricated. The silicon nanowire arrays were prepared from the etched silicon wafer, which were then treated with nitrohydrochloric acid and HF to remove the cladding silicon oxide sheath. The modified silicon nanowire arrays were further used as the electrode for fabricating the direct electrochemical biosensors for the detection of cytochrome c, which exhibited linear response to cytochrome c at low concentration and high sensitivity of 2.75μA.mM-1 due to the vast surface-to-bulk ratio of the silicon nanowire arrays and the interaction between the carboxyl group of cytochrome and Si-H group provided by the surface of the modified silicon nanowire arrays.
Fourth, an amperometric biosensor based on enzyme-modified ZnO nanotube arrays for the sensitive detection of glucose was demonstrated. The ZnO nanotube arrays based electrode exhibited high sensitivity of 30.85μA cm-2 mM-1 , wide linear detection range from 10μM to 4.2 mM and the low limit of detection (LOD) of 10μM (measured) for the glucose detection, which benefited from the coupling of the vast surface-to-bulk ratio and the uniquely tubular morphology with the good contact between the substrate electrode (ITO-coated glass) and ZnO nanotube arrays. The fabrication methodology of the present biosensor could be extended to other biosensors based oxidase, such as those for detection of acetylcholine, cholesterol, phenol, etc.
第一,基于束状硅纳米线的谷胱甘肽电化学传感器的研究。利用去除氧化层的硅纳米线表面对金属离子的还原性,将三价金离子还原在硅纳米线表面,在硅纳米线表面形成稳定均匀的金纳米颗粒,并且利用金纳米颗粒易于与巯基反应的特点,将氨基为末端的有机小分子巯基乙胺修饰在金纳米颗粒表面。修饰后的硅纳米线由于其独特的成束性、较大的比表面积、金颗粒的修饰对硅纳米线传导性增强的特点,与化学修饰后所具有的氨基末端与三肽生物分子谷胱甘肽末端的羧基的相互作用,被用作检测谷胱甘肽的直接电化学传感器。实验结果表明,基于硅纳米线的谷胱甘肽传感器具有低浓度线性响应(0.33-2.97μM)、灵敏度高(48.5 mA.mmol-1)、以及检测底限浓度较低(0.33μM,measured)的优点。
第二,硅纳米线在溶液中的分散与葡萄糖电化学传感器的研究。分别以磷酸缓冲溶液、乙醇溶液与水溶性全氟取代聚合物Nafion溶液作为溶剂,研究了硅纳米线在溶液中的分散。实验结果表明,去除掉氧化层的硅纳米线与金纳米颗粒修饰的硅纳米线在Nafion溶液中可以形成稳定均匀的分散液,在其它溶剂中难以分散;而未经表面处理的硅纳米线在几种溶液中均难以形成分散液。金纳米颗粒修饰的硅纳米线分散液被用于酶电极的修饰,制备了葡萄糖电化学传感器,电化学实验结果表明,硅纳米线的修饰对葡萄糖的传感具有明显的增强作用。根据实验结果,我们提出了去掉氧化层的硅纳米线由于表面的Si-H与Nafion的磺酸基之间的作用而使之易于溶剂化进而在溶液中分散的机理。
第三,基于硅纳米线阵列的细胞色素c电化学传感器的研究。利用化学刻蚀法由硅片制备了硅纳米线阵列,经过表面去氧化层处理后,制备了检测蛋白质细胞色素c的电化学传感器。实验表明,硅纳米线阵列电极对细胞色素c有良好的电化学响应,并且在低浓度条件下具备线性响应的特点,灵敏度为2.75μA.mM-1。根据与未经表面处理的硅纳米线阵列电极的实验结果相对比,提出了细胞色素c所具备的羧基末端与硅纳米线阵列电极表面的Si-H相互作用从而改善传感性能的检测机理。
第四,基于表面修饰ZnO纳米管阵列的葡萄糖电化学传感器的研究。在本实验室发展的电化学沉积法制备氧化锌纳米管阵列的基础上,利用氧化锌表面与葡萄糖氧化酶(GOx)之间的静电吸引作用,将GOx修饰在氧化锌纳米管阵列的表面,并引入Nafion以达到进一步固化GOx与增强传感器抗干扰能力的目的,制备了基于氧化锌纳米管阵列的葡萄糖电化学传感器。实验结果证明,由于ZnO纳米管的独特结构使其比表面积相对较大,电化学沉积的方法使ZnO纳米管与基底电极ITO玻璃之间的接触较好,可以改善ZnO结构与基底电极之间的电子传输效率,传感器具备灵敏度高(30.85μA.cm-2.mM-1),线性范围较宽(10μM-4.2 mM),检测底限浓度较低(10μM,measured),响应时间较短(<5s)等优点。
The fabrication and properties of chemical sensors and biosensors based modified one-dimensional nanomaterials have been studied in this doctorial dissertation. The main results can be concluded as follows:
First, the functionalized SiNWs, chemically modified with Au nanoparticles, and with amino-terminated organic molecules anchored on the surface of the nanoparticles, were fabricated into the electrochemical biosensors for glutathione (GSH). The biosensor showed good linear response to GSH of low concentration (0.33-2.97μM), high sensitivity (48.5 mA.mmol-1), and a low limit of detection (0.33μM, measured) by virtue of strong sorption ability and high electrical conductivity of the modified SiNWs based electrode.
Second, the dispersion of silicon nanowires in Nafion toward the fabrication of amperometric biosensors for glucose was studied. We demonstrated a convenient method of the dispersion of SiNWs in solvent in virtue of the interaction between Nafion and the surface of SiNWs. The dispersion of the HF-etched SiNWs and Au nanoparticles modified SiNWs exhibited homogeneous and long time steady properties. Moreover, the Au nanoparticles modified SiNWs could be used to modify the enzyme-electrode as the biosensors for glucose sensing, which proved to have an effect of enhancement for the detection of glucose. The present method of the dispersion of the SiNWs and the modification of electrode could be extended to the construction of the one-dimensional nanostructures based nanodevices.
Third, the direct electrochemical biosensor for cytochrome c based on the silicon nanowire arrays was fabricated. The silicon nanowire arrays were prepared from the etched silicon wafer, which were then treated with nitrohydrochloric acid and HF to remove the cladding silicon oxide sheath. The modified silicon nanowire arrays were further used as the electrode for fabricating the direct electrochemical biosensors for the detection of cytochrome c, which exhibited linear response to cytochrome c at low concentration and high sensitivity of 2.75μA.mM-1 due to the vast surface-to-bulk ratio of the silicon nanowire arrays and the interaction between the carboxyl group of cytochrome and Si-H group provided by the surface of the modified silicon nanowire arrays.
Fourth, an amperometric biosensor based on enzyme-modified ZnO nanotube arrays for the sensitive detection of glucose was demonstrated. The ZnO nanotube arrays based electrode exhibited high sensitivity of 30.85μA cm-2 mM-1 , wide linear detection range from 10μM to 4.2 mM and the low limit of detection (LOD) of 10μM (measured) for the glucose detection, which benefited from the coupling of the vast surface-to-bulk ratio and the uniquely tubular morphology with the good contact between the substrate electrode (ITO-coated glass) and ZnO nanotube arrays. The fabrication methodology of the present biosensor could be extended to other biosensors based oxidase, such as those for detection of acetylcholine, cholesterol, phenol, etc.
引文
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