基于微细加工技术的微电极的制备及其在废水生物处理中的应用
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摘要
微电极是对环境生物样品进行微区分析的有力工具,在反应机理探索中发挥着重要应用,其中金属和金属-金属氧化物固态微电极应用最为广泛。基于玻璃毛细管拉制的微电极传统制作方法存在着很多缺陷,如:制作步骤繁琐、成品率低、重复性差、对制作人员的技术要求高等,妨碍了它在环境领域中的应用。而微细加工技术精度高、可靠性强、重复性好,非常适合用于微电极及其阵列的制作。本论文研究基于紫外曝光、离子束溅射镀膜和离子束刻蚀等微细加工技术,成功制作了一种新型的针状集成微电极,建立了一种简洁、灵活、高效、可靠的微电极制作新方法。该新型微电极的针尖为75μm宽、100μm厚和5 mm,该针尖上集成了参比电极、对电极和工作电极。电化学表征和抗干扰能力测试结果表明,该集成微电极具有很好的稳定性和电化学活性,能够用于电化学分析测量以及化学修饰以拓展其功能。由于采用负性光刻胶SU-8作为电极支撑材料,电极的外形可以通过修改光刻掩模而重新设计,使得新制作技术具有较大的自由度和广泛的适用性。
化学修饰电极是拓展电极功能最有效的方法。本论文通过在工作微电极尖端修饰一层Pt-Fe纳米颗粒,使之能够定量分析溶液中的亚硝酸盐浓度:在工作电极尖端修饰一层特殊的三维银纳米结构,可以使之同时定量分析溶液中的溶解氧和硝酸盐浓度。通过循环伏安法表征了修饰电极的电化学活性,修饰后的微电极分别对溶解氧、亚硝酸盐和硝酸盐具有很好的线性响应,能够用于实际样品的测量。利用电子扫描显微镜(SEM)观察了修饰电极表面的微观结构,探讨了电极表面结构和组成与其电化学性质之间的关系。修饰电极具有很好的电化学稳定性,能作为溶解氧、亚硝酸盐和硝酸盐传感器。同时该化学修饰微电极具有很强的抗干扰能力。
好氧微生物颗粒是近年来废水处理研究领域的热点之一,它有望取代传统的活性污泥絮体,成为新一代的废水生物处理技术的核心。因此,对它的内部结构和反应机制的研究具有重要的意义。本论文利用制备的化学修饰微电极测定了好氧硝化颗粒内部的溶解氧、亚硝酸盐和硝酸盐浓度的微区分布。观察到溶解氧值在颗粒表面迅速降低,在颗粒内部存在微量的溶解氧;亚硝酸盐和硝酸盐浓度则在颗粒表面较高,内部较低。这表明氨氧化细菌和硝化细菌主要集中在颗粒表层的300微米范围内,且在所测定的颗粒内部不存在反硝化反应。
地下饮用水中存在的硝酸盐对人体具有极大危害,高效、无二次污染地去除地下水中的硝酸盐是环境领域重要的研究方向。本论文利用全息曝光技术与微细加工技术相结合,制备了一种400 nm宽的金丝电极阵列,通过电化学沉积的方法在其表面制备了一层具有较大表面积的特殊三维银纳米结构。通过SEM和同步辐射硬X-ray三维成像表征了此三维银纳米结构。该银纳米结构能够在无外加试剂的条件下电化学还原水体中的硝酸盐。本研究为地下饮用水中硝酸盐的去除提供了一个新的技术路线。
微生物燃料电池(MFC)在处理废水的同时能够利用微生物进行发电,是一种具有良好前景的环境污染控制与清洁能源生产的新技术。微型MFC由于其体积小、产电量高而极具实用价值,有望在军事、国土安全及医学领域发挥重要的作用。本论文采用微细加工技术,成功制作了一种新型的微型MFC金丝电极阵列,并组装了一种微型MFC反应器。利用该微型MFC研究了希瓦氏菌Shewanellaoneidensis MR-1在该MFC中的产电能力,其最大功率密度可达2499 mW/m~2。它相对于以碳电极作为基底的微型MFC,具有较大的产电能力,展现出极为广阔的应用前景。
Microelectrodes(MEs) are regarded as a powerful tool for micro-scale measurements and are used for analysis of environmental samples in the past decades. Because of their properties of sturdy nature,metal and metal-metal oxide-based MEs have been widely used.Although many efforts have been made to improve the fabrication methods,some inherent disadvantages still exist,such as complicated fabrication procedures,low success rate,poor reproducibility,non-renewability and difficulty in making multi-sensor device.Microfabrication techniques,which are used for manufacturing small electrodes of any required planar patterns with excellent reproducibility,good stability and good accuracy,have attracted increasing interests. In this thesis,a needle-type gold-based integrated ME was fabricated by using microfabrication techniques including photolithography,ion-beam deposition and ion-beam etching techniques.A simple,efficient and reliable procedure for fabricating ME was established.The integrated ME tip contained a reference ME,a working ME and a counter ME with 70μm wideth,100μm thickness and 5 mm length.The electrochemical properties and anti-interference ability were investigated,and the results indicate that the integrated MEs had a good stability and an electrochemical activity.Furthermore,the integrated MEs could be used to electrochemical analysis and chemically modified to expanding their functions.An innovative procedure based on the utilization of a negative photoresist,SU-8,was proposed,following which mieroeleetrodes of any desired entire shape could be constructed by using photo-mask at micron-scale readily and reproductively.This new fabrication procedure had a large freedom and a wide range of applicability.
Chemically modified electrode(CME) was one of the most effective way to expand the electrode function.In this thesis,a thin layer Pt-Fe nanoparticles was co-deposited on the tip of the working microelectrode,and this CEM could be used to quantitatively analyze the nitrite concentration.A three-dimensional nano-structured dendritic silver was deposited on the working microelectrode tip,and this CEM could be used to quantitatively analyze nitrate and dissolved oxygen(DO) concentrations simultaneously.The electrochemical properties of the CMEs were investigated by using cyclic voltammetry and the CMEs were found to have a good linear response to nitrite,nitrate and DO.Thus,the CMEs could be used to analyze the samples.The micro-structure of the CMEs surface was observed with scanning electron microscope, and the electrochemical properties of the CMEs were found to be related to their structures and composition.The CMEs had good stability,strong anti-interference ability and could be used as a nitrite,nitrate and DO sensor.
Recently,aerobic microbial granules have received increasing interests because they have a dense structure,good settling ability,and microbial diversity,compared with activated sludge flocs.Evaluation of the distributions of concerned substances in aerobic granules will produce a better understanding of their characteristics in bioreactors.In this thesis,the distribution of nitrite,nitrate and DO was measured by using the CMEs.The DO level decreased at the granule surface and did not become depleted in the granule inner layer.Meanwhile,nitrite and nitrate concentrations were higher in the surface than those in the inner layer.This result suggests that the active ammonia-oxidizing bacteria and nitrite-oxidizing bacteria were mainly located in the upper layer 300μm thickness of the granules,and that denitrification should not occur in the granules.
Nitrogenous substances are widely present in the environments,resulting in a harmless to human health.Efficient and environmentally friendly removal of nitrate in groundwater is an important issue.In this thesis,400 nm-width gold wire microelectrode arrays were fabricated by using holographic lithography and microfabrications techniques,and then three-dimensional nano-structured dendritic silver was electrochemically deposited on the microelectrode array surface.The silver nanostructure was characterized using scanning electron microscope and synchrontron radiation hard X-ray three-dimensional imaging.The microelectrode could electrochemically reduce nitrate in water without dosing of any chemicals.In this way, a new method for nitrate removal in water was established.
Microbial fuel cells(MFCs) could simultaneously generate electricity and treat wastewater.Because of small size and high output,mini-MFCs have a great potential to play an important role in military,homeland security and medical fields.In this thesis,a novel mini-MFC gold wire electrode array was fabricated by using microfabrication techniques,and a new mini-MFC reactor was fabricated with this electrode array.The power generation ability of Shewanella oneidensis MR-1 in this reactor was evaluated.The maximum power density of this reactor was 2499 mW/m~2. This new mini-MFC reactor had a better power generation ability compared to other mini-MFCs based on carbon electrode.Therefore,the fabricated mini-MFC has a great application prospect.
化学修饰电极是拓展电极功能最有效的方法。本论文通过在工作微电极尖端修饰一层Pt-Fe纳米颗粒,使之能够定量分析溶液中的亚硝酸盐浓度:在工作电极尖端修饰一层特殊的三维银纳米结构,可以使之同时定量分析溶液中的溶解氧和硝酸盐浓度。通过循环伏安法表征了修饰电极的电化学活性,修饰后的微电极分别对溶解氧、亚硝酸盐和硝酸盐具有很好的线性响应,能够用于实际样品的测量。利用电子扫描显微镜(SEM)观察了修饰电极表面的微观结构,探讨了电极表面结构和组成与其电化学性质之间的关系。修饰电极具有很好的电化学稳定性,能作为溶解氧、亚硝酸盐和硝酸盐传感器。同时该化学修饰微电极具有很强的抗干扰能力。
好氧微生物颗粒是近年来废水处理研究领域的热点之一,它有望取代传统的活性污泥絮体,成为新一代的废水生物处理技术的核心。因此,对它的内部结构和反应机制的研究具有重要的意义。本论文利用制备的化学修饰微电极测定了好氧硝化颗粒内部的溶解氧、亚硝酸盐和硝酸盐浓度的微区分布。观察到溶解氧值在颗粒表面迅速降低,在颗粒内部存在微量的溶解氧;亚硝酸盐和硝酸盐浓度则在颗粒表面较高,内部较低。这表明氨氧化细菌和硝化细菌主要集中在颗粒表层的300微米范围内,且在所测定的颗粒内部不存在反硝化反应。
地下饮用水中存在的硝酸盐对人体具有极大危害,高效、无二次污染地去除地下水中的硝酸盐是环境领域重要的研究方向。本论文利用全息曝光技术与微细加工技术相结合,制备了一种400 nm宽的金丝电极阵列,通过电化学沉积的方法在其表面制备了一层具有较大表面积的特殊三维银纳米结构。通过SEM和同步辐射硬X-ray三维成像表征了此三维银纳米结构。该银纳米结构能够在无外加试剂的条件下电化学还原水体中的硝酸盐。本研究为地下饮用水中硝酸盐的去除提供了一个新的技术路线。
微生物燃料电池(MFC)在处理废水的同时能够利用微生物进行发电,是一种具有良好前景的环境污染控制与清洁能源生产的新技术。微型MFC由于其体积小、产电量高而极具实用价值,有望在军事、国土安全及医学领域发挥重要的作用。本论文采用微细加工技术,成功制作了一种新型的微型MFC金丝电极阵列,并组装了一种微型MFC反应器。利用该微型MFC研究了希瓦氏菌Shewanellaoneidensis MR-1在该MFC中的产电能力,其最大功率密度可达2499 mW/m~2。它相对于以碳电极作为基底的微型MFC,具有较大的产电能力,展现出极为广阔的应用前景。
Microelectrodes(MEs) are regarded as a powerful tool for micro-scale measurements and are used for analysis of environmental samples in the past decades. Because of their properties of sturdy nature,metal and metal-metal oxide-based MEs have been widely used.Although many efforts have been made to improve the fabrication methods,some inherent disadvantages still exist,such as complicated fabrication procedures,low success rate,poor reproducibility,non-renewability and difficulty in making multi-sensor device.Microfabrication techniques,which are used for manufacturing small electrodes of any required planar patterns with excellent reproducibility,good stability and good accuracy,have attracted increasing interests. In this thesis,a needle-type gold-based integrated ME was fabricated by using microfabrication techniques including photolithography,ion-beam deposition and ion-beam etching techniques.A simple,efficient and reliable procedure for fabricating ME was established.The integrated ME tip contained a reference ME,a working ME and a counter ME with 70μm wideth,100μm thickness and 5 mm length.The electrochemical properties and anti-interference ability were investigated,and the results indicate that the integrated MEs had a good stability and an electrochemical activity.Furthermore,the integrated MEs could be used to electrochemical analysis and chemically modified to expanding their functions.An innovative procedure based on the utilization of a negative photoresist,SU-8,was proposed,following which mieroeleetrodes of any desired entire shape could be constructed by using photo-mask at micron-scale readily and reproductively.This new fabrication procedure had a large freedom and a wide range of applicability.
Chemically modified electrode(CME) was one of the most effective way to expand the electrode function.In this thesis,a thin layer Pt-Fe nanoparticles was co-deposited on the tip of the working microelectrode,and this CEM could be used to quantitatively analyze the nitrite concentration.A three-dimensional nano-structured dendritic silver was deposited on the working microelectrode tip,and this CEM could be used to quantitatively analyze nitrate and dissolved oxygen(DO) concentrations simultaneously.The electrochemical properties of the CMEs were investigated by using cyclic voltammetry and the CMEs were found to have a good linear response to nitrite,nitrate and DO.Thus,the CMEs could be used to analyze the samples.The micro-structure of the CMEs surface was observed with scanning electron microscope, and the electrochemical properties of the CMEs were found to be related to their structures and composition.The CMEs had good stability,strong anti-interference ability and could be used as a nitrite,nitrate and DO sensor.
Recently,aerobic microbial granules have received increasing interests because they have a dense structure,good settling ability,and microbial diversity,compared with activated sludge flocs.Evaluation of the distributions of concerned substances in aerobic granules will produce a better understanding of their characteristics in bioreactors.In this thesis,the distribution of nitrite,nitrate and DO was measured by using the CMEs.The DO level decreased at the granule surface and did not become depleted in the granule inner layer.Meanwhile,nitrite and nitrate concentrations were higher in the surface than those in the inner layer.This result suggests that the active ammonia-oxidizing bacteria and nitrite-oxidizing bacteria were mainly located in the upper layer 300μm thickness of the granules,and that denitrification should not occur in the granules.
Nitrogenous substances are widely present in the environments,resulting in a harmless to human health.Efficient and environmentally friendly removal of nitrate in groundwater is an important issue.In this thesis,400 nm-width gold wire microelectrode arrays were fabricated by using holographic lithography and microfabrications techniques,and then three-dimensional nano-structured dendritic silver was electrochemically deposited on the microelectrode array surface.The silver nanostructure was characterized using scanning electron microscope and synchrontron radiation hard X-ray three-dimensional imaging.The microelectrode could electrochemically reduce nitrate in water without dosing of any chemicals.In this way, a new method for nitrate removal in water was established.
Microbial fuel cells(MFCs) could simultaneously generate electricity and treat wastewater.Because of small size and high output,mini-MFCs have a great potential to play an important role in military,homeland security and medical fields.In this thesis,a novel mini-MFC gold wire electrode array was fabricated by using microfabrication techniques,and a new mini-MFC reactor was fabricated with this electrode array.The power generation ability of Shewanella oneidensis MR-1 in this reactor was evaluated.The maximum power density of this reactor was 2499 mW/m~2. This new mini-MFC reactor had a better power generation ability compared to other mini-MFCs based on carbon electrode.Therefore,the fabricated mini-MFC has a great application prospect.
引文
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