纳米材料电化学传感器及环境监测应用研究
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摘要
纳米材料用于催化和分析已成为当前科技领域的一个研究热点。基于纳米材料具有的量子尺寸效应、表面与界面效应、小尺寸效应和宏观量子隧道等效应,使得纳米粒子相对于大块颗粒具有更为独特的物理、化学性质。纳米材料在电化学传感器研究领域得到广泛应用。
目前,用于催化和分析的电化学传感器制备主要有以下两种趋势:一种是负载贵金属纳米颗粒的聚合物膜修饰电极;另一种是双金属或多金属复合修饰电极。双金属或多金属纳米颗粒的催化活性在许多催化反应中要明显优于其所对应的单金属颗粒,这是因为双金属或多金属之间特有的协同作用及电极表面结构变化导致其具有与单金属不一样的催化性能。另外,使用双金属或多金属复合修饰电极可以减少费用,双金属或多金属催化剂中常包含一些非贵金属。尽管双金属纳米颗粒在很多方面呈现出优越的催化活性和选择性,但是由于颗粒过小而产生的团聚使其难以广泛使用。将双金属纳米颗粒负载到催化剂载体,例如聚合物膜或金属氧化物上,与载体的接触界面明显增加,双金属颗粒与载体的作用更为充分,更有利于显著提高催化剂的催化性能。
随着人们对环境质量要求的提高,由甲醛引起的环境污染问题越来越受到人们的关注。甲醛检测技术正朝着快速、灵敏、简便的方向发展。化学传感器法,尤其是纳米贵金属化学传感器,成为目前甲醛速测技术中的研究热点。
本文以实际应用和未来商品化仪器开发为目标,主要研究了单贵金属、双金属纳米材料在聚合物膜或金属氧化物膜上的电化学行为,利用纳米金属和聚合物膜或金属氧化物之间相互作用以及双金属之间的协同作用构建电化学传感器,以提高电化学传感器的灵敏度、选择性、稳定性等,并对甲醛环境污染物进行了检测,也对地下水污染物开展了健康风险评价。本论文的主要研究内容及结果主要体现在以下六个方面:
1.本文研制了基于钯纳米粒子-Nafion修饰玻碳电极(Pd/Nf/GCE)的新型电化学传感器。采用扫描电镜(SEM)对修饰电极表面进行了表征,并采用循环伏安法(CV)和微分脉冲伏安法(DPV)研究了甲醛在该修饰电极上的电催化氧化作用。对修饰电极制备条件和实验条件进行了优化,在此基础上建立了一种测定甲醛的伏安分析方法。
2.通过电化学沉积的方法制备了DNA-纳米金修饰的玻碳电极,用扫描电镜和原子力显微镜(AFM)对该电极进行了形貌表征,实验结果表明,该修饰电极对甲醛具有较高的响应灵敏度。
3.采用循环伏安法在玻碳电极表面依次电沉积纳米二氧化锆和铂纳米微粒,制备了一种新型电化学传感器(Pt/ZrO2/GCE)。用扫描电镜对该修饰电极表面进行了形貌表征。利用循环伏安法和线性扫描伏安法(LSV)研究了甲醛在该修饰电极上的电催化氧化作用,优化了实验参数,并对甲醛进行了定量分析。
4.利用电化学方法将纳米铂和钯共沉积在滴涂有Nafion膜的玻碳电极上,制备了性能优良的甲醛电化学传感器(PtPd/Nf/GCE)。采用扫描电镜和能谱分析(EDS)对电极表面及组分比例进行了表征。用电化学方法对该修饰电极测定了其电化学行为,并用线性扫描伏安法研究了甲醛在该修饰电极上的催化氧化行为。由于Nafion膜对纳米颗粒在电极表面分布影响以及双金属之间的协同作用,修饰电极对甲醛具有很好的催化氧化作用。
5.采用贾凡尼取代反应制备了纳米金钯核壳-Nafion修饰玻碳电极(AuPd/Nf/GCE)。采用扫描电镜和能谱分析对电极表面及组分比例进行了表征。研究了电极在碱性溶液中的电化学行为,并对甲醛进行了检测,发现修饰电极对甲醛具有较好的催化氧化作用。
6.利用健康风险评价方法,按照GB/T 5750-2006《生活饮用水标准检验方法》,对华北某市附近一非规范垃圾填埋场附近五口有代表性的民用水井水样进行了监测,水质检测项目主要包括:甲醛、氨氮、硝酸盐氮、亚硝酸盐氮、挥发酚、锌、六价铬、汞、锰、pH值、氟化物、总硬度,并对其进行了健康风险分析评价。
The use of nanostructured materials for catalysis and analysis is an extremely promising prospect. Due to the quantum size effect, the surface and interface effect, the small size effect and the macroscopic quantum tunnel effect, nanoparticles have drawn much attention for their physical and chemical advantages over bulk materials. Nano-materials have been widely applicated in the reaserch field of electrochemical sensors.
There are two main trends in the field of chemically modified electrodes for catalysis and analysis: one is chemically modified electrodes based on polymer films, the other is bimetallic or multimetallic composite modified electrodes. Bimetallic (or multimetallic) nanoparticles are of greater interest than corresponding monometallic ones for the improvement of the catalytic properties of metal particles. This is because bimetallization can improve catalytic properties of the original single-metal catalysts and create a new property, which can often be explained in terms of synergistic effect associated with changes on electrode surface. Bimetallic (or multimetallic) modified electrodes can also reduce costs by the addition of non-noble metal. Although bimetallic nanoparticles exhibit a high activity and selectivity, particle coalescence greatly limited their application. Hence, bimetallic nanoparticles coated on supporting materials, such as polymer films or metallic oxide, can improve the situation and enhance electron conductivity and catalytic activity of the catalysts.
As the demand of the public for ambient quality advanced, environmental pollution problem caused by formaldehyde is increasingly concerned. The determination techniques of formaldehyde are developing towards fast, sensitive, simple and convenient ones. Nowadays, chemical sensor, espically nano-noble-metal chemical sensor is hotspot in fast determination study field.
To develop a practicable system of electrochemical sensor for the determination of environmental contaminants such as formaldehyde, the voltammetric behavior of monometallic and bimetallic noble nanoparticles modified on polymer films or metallic oxide are investigated. Novel electrochemical sensors are proposed based on the interactions between noble nanoparticles and polymer films or metallic oxide, with aims to develop the sensitivity, selectivity and stability. Health risk assessment (HRA) for groundwater is simply introduced in the end of the paper. In detail, the main results are as follows:
1. Palladium nanoparticles and Nafion film modified glassy carbon electrodes (Pd/Nf/GCE) were electrochemically deposited through cyclic voltammetry (CV). Scanning electron microscope (SEM) was employed to characterize the surface structure. Electrocatalytical behaviors of the modified electrode were investigated by cyclic voltammetry and differential pulse voltammetry (DPV). Experimental conditions were optimized and a voltammetric method for determining formaldehyde was developed.
2. The modified electrode of DNA film and nano-gold was fabricated through electrochemical deposition method and the morphology of electrode surface was characterized by scanning electron microscopy and atomic force microscopy (AFM). Experimental results showed that the modified electrode exhibited a remarked electrocatalytic activity toward formaldehyde.
3. An electrochemical sensor was introduced based on electrodepositing zirconia and Pt nanoparticles on glassy carbon electrode by cyclic voltammetry. Scanning electron microscopy was used to characterize the morphology of electrode surface. The electrocatalytical behaviors of the modified electrode towards formaldehyde were investigated by cyclic voltammetry and linear sweep voltammetry (LSV). Quantitative analysis of formaldehyde was also studied.
4. Platinum-palladium (Pt-Pd) nanoparticles were electrochemically deposited on Nafion (Nf) film coated glassy carbon electrode. Bimetallic (Pt-Pd) nanoparticles were found to be uniformly dispersed on Nafion film, as confirmed by scanning electron microscopic analysis. Energy dispersed X-ray analysis (EDS) was used to characterize the composition of metal present on the nanoparticle-modified electrodes. The electrocatalytical behaviors of the electrode were investigated by cyclic voltammetry and linear sweep voltammetry. Experimental results showed that the electrode exhibited a remarked electrocatalytic activity for the oxidation of formaldehyde, attributed to synergistic effect of the alloy deposit associated with changes in the adsorption features of the Nafion surface.
5. Pd-Au core-shell nanoparticles were deposited onto the Nafion film coated glassy carbon (denited as PdAu/Nf/GC) electrode via galvanic replacement reaction. Scanning electron microscopic analysis and energy dispersed X-ray analysis was used to characterize the composition of metal present on the nanoparticle-modified electrodes. Studies of cyclic voltammetry demonstrated that the modified electrode exhibited a high electrocatalytic activity toward formaldehyde.
6. To assess the health risk of the groundwater pollution caused by a substandard landfill site nearly a city in northern China, the water samples were collected from five representative civil wells situated near the city. Formaldehyde, ammonia nitrogen, nitrite nitrogen, volatile phenol, zinc, sexavalent chrome, mercury, manganese, pH values, fluoride, total hardness of the samples were determined according to the standard determination methods of domestic drinking water GB/T 5750-2006. The assessment of health risk was carried out.
目前,用于催化和分析的电化学传感器制备主要有以下两种趋势:一种是负载贵金属纳米颗粒的聚合物膜修饰电极;另一种是双金属或多金属复合修饰电极。双金属或多金属纳米颗粒的催化活性在许多催化反应中要明显优于其所对应的单金属颗粒,这是因为双金属或多金属之间特有的协同作用及电极表面结构变化导致其具有与单金属不一样的催化性能。另外,使用双金属或多金属复合修饰电极可以减少费用,双金属或多金属催化剂中常包含一些非贵金属。尽管双金属纳米颗粒在很多方面呈现出优越的催化活性和选择性,但是由于颗粒过小而产生的团聚使其难以广泛使用。将双金属纳米颗粒负载到催化剂载体,例如聚合物膜或金属氧化物上,与载体的接触界面明显增加,双金属颗粒与载体的作用更为充分,更有利于显著提高催化剂的催化性能。
随着人们对环境质量要求的提高,由甲醛引起的环境污染问题越来越受到人们的关注。甲醛检测技术正朝着快速、灵敏、简便的方向发展。化学传感器法,尤其是纳米贵金属化学传感器,成为目前甲醛速测技术中的研究热点。
本文以实际应用和未来商品化仪器开发为目标,主要研究了单贵金属、双金属纳米材料在聚合物膜或金属氧化物膜上的电化学行为,利用纳米金属和聚合物膜或金属氧化物之间相互作用以及双金属之间的协同作用构建电化学传感器,以提高电化学传感器的灵敏度、选择性、稳定性等,并对甲醛环境污染物进行了检测,也对地下水污染物开展了健康风险评价。本论文的主要研究内容及结果主要体现在以下六个方面:
1.本文研制了基于钯纳米粒子-Nafion修饰玻碳电极(Pd/Nf/GCE)的新型电化学传感器。采用扫描电镜(SEM)对修饰电极表面进行了表征,并采用循环伏安法(CV)和微分脉冲伏安法(DPV)研究了甲醛在该修饰电极上的电催化氧化作用。对修饰电极制备条件和实验条件进行了优化,在此基础上建立了一种测定甲醛的伏安分析方法。
2.通过电化学沉积的方法制备了DNA-纳米金修饰的玻碳电极,用扫描电镜和原子力显微镜(AFM)对该电极进行了形貌表征,实验结果表明,该修饰电极对甲醛具有较高的响应灵敏度。
3.采用循环伏安法在玻碳电极表面依次电沉积纳米二氧化锆和铂纳米微粒,制备了一种新型电化学传感器(Pt/ZrO2/GCE)。用扫描电镜对该修饰电极表面进行了形貌表征。利用循环伏安法和线性扫描伏安法(LSV)研究了甲醛在该修饰电极上的电催化氧化作用,优化了实验参数,并对甲醛进行了定量分析。
4.利用电化学方法将纳米铂和钯共沉积在滴涂有Nafion膜的玻碳电极上,制备了性能优良的甲醛电化学传感器(PtPd/Nf/GCE)。采用扫描电镜和能谱分析(EDS)对电极表面及组分比例进行了表征。用电化学方法对该修饰电极测定了其电化学行为,并用线性扫描伏安法研究了甲醛在该修饰电极上的催化氧化行为。由于Nafion膜对纳米颗粒在电极表面分布影响以及双金属之间的协同作用,修饰电极对甲醛具有很好的催化氧化作用。
5.采用贾凡尼取代反应制备了纳米金钯核壳-Nafion修饰玻碳电极(AuPd/Nf/GCE)。采用扫描电镜和能谱分析对电极表面及组分比例进行了表征。研究了电极在碱性溶液中的电化学行为,并对甲醛进行了检测,发现修饰电极对甲醛具有较好的催化氧化作用。
6.利用健康风险评价方法,按照GB/T 5750-2006《生活饮用水标准检验方法》,对华北某市附近一非规范垃圾填埋场附近五口有代表性的民用水井水样进行了监测,水质检测项目主要包括:甲醛、氨氮、硝酸盐氮、亚硝酸盐氮、挥发酚、锌、六价铬、汞、锰、pH值、氟化物、总硬度,并对其进行了健康风险分析评价。
The use of nanostructured materials for catalysis and analysis is an extremely promising prospect. Due to the quantum size effect, the surface and interface effect, the small size effect and the macroscopic quantum tunnel effect, nanoparticles have drawn much attention for their physical and chemical advantages over bulk materials. Nano-materials have been widely applicated in the reaserch field of electrochemical sensors.
There are two main trends in the field of chemically modified electrodes for catalysis and analysis: one is chemically modified electrodes based on polymer films, the other is bimetallic or multimetallic composite modified electrodes. Bimetallic (or multimetallic) nanoparticles are of greater interest than corresponding monometallic ones for the improvement of the catalytic properties of metal particles. This is because bimetallization can improve catalytic properties of the original single-metal catalysts and create a new property, which can often be explained in terms of synergistic effect associated with changes on electrode surface. Bimetallic (or multimetallic) modified electrodes can also reduce costs by the addition of non-noble metal. Although bimetallic nanoparticles exhibit a high activity and selectivity, particle coalescence greatly limited their application. Hence, bimetallic nanoparticles coated on supporting materials, such as polymer films or metallic oxide, can improve the situation and enhance electron conductivity and catalytic activity of the catalysts.
As the demand of the public for ambient quality advanced, environmental pollution problem caused by formaldehyde is increasingly concerned. The determination techniques of formaldehyde are developing towards fast, sensitive, simple and convenient ones. Nowadays, chemical sensor, espically nano-noble-metal chemical sensor is hotspot in fast determination study field.
To develop a practicable system of electrochemical sensor for the determination of environmental contaminants such as formaldehyde, the voltammetric behavior of monometallic and bimetallic noble nanoparticles modified on polymer films or metallic oxide are investigated. Novel electrochemical sensors are proposed based on the interactions between noble nanoparticles and polymer films or metallic oxide, with aims to develop the sensitivity, selectivity and stability. Health risk assessment (HRA) for groundwater is simply introduced in the end of the paper. In detail, the main results are as follows:
1. Palladium nanoparticles and Nafion film modified glassy carbon electrodes (Pd/Nf/GCE) were electrochemically deposited through cyclic voltammetry (CV). Scanning electron microscope (SEM) was employed to characterize the surface structure. Electrocatalytical behaviors of the modified electrode were investigated by cyclic voltammetry and differential pulse voltammetry (DPV). Experimental conditions were optimized and a voltammetric method for determining formaldehyde was developed.
2. The modified electrode of DNA film and nano-gold was fabricated through electrochemical deposition method and the morphology of electrode surface was characterized by scanning electron microscopy and atomic force microscopy (AFM). Experimental results showed that the modified electrode exhibited a remarked electrocatalytic activity toward formaldehyde.
3. An electrochemical sensor was introduced based on electrodepositing zirconia and Pt nanoparticles on glassy carbon electrode by cyclic voltammetry. Scanning electron microscopy was used to characterize the morphology of electrode surface. The electrocatalytical behaviors of the modified electrode towards formaldehyde were investigated by cyclic voltammetry and linear sweep voltammetry (LSV). Quantitative analysis of formaldehyde was also studied.
4. Platinum-palladium (Pt-Pd) nanoparticles were electrochemically deposited on Nafion (Nf) film coated glassy carbon electrode. Bimetallic (Pt-Pd) nanoparticles were found to be uniformly dispersed on Nafion film, as confirmed by scanning electron microscopic analysis. Energy dispersed X-ray analysis (EDS) was used to characterize the composition of metal present on the nanoparticle-modified electrodes. The electrocatalytical behaviors of the electrode were investigated by cyclic voltammetry and linear sweep voltammetry. Experimental results showed that the electrode exhibited a remarked electrocatalytic activity for the oxidation of formaldehyde, attributed to synergistic effect of the alloy deposit associated with changes in the adsorption features of the Nafion surface.
5. Pd-Au core-shell nanoparticles were deposited onto the Nafion film coated glassy carbon (denited as PdAu/Nf/GC) electrode via galvanic replacement reaction. Scanning electron microscopic analysis and energy dispersed X-ray analysis was used to characterize the composition of metal present on the nanoparticle-modified electrodes. Studies of cyclic voltammetry demonstrated that the modified electrode exhibited a high electrocatalytic activity toward formaldehyde.
6. To assess the health risk of the groundwater pollution caused by a substandard landfill site nearly a city in northern China, the water samples were collected from five representative civil wells situated near the city. Formaldehyde, ammonia nitrogen, nitrite nitrogen, volatile phenol, zinc, sexavalent chrome, mercury, manganese, pH values, fluoride, total hardness of the samples were determined according to the standard determination methods of domestic drinking water GB/T 5750-2006. The assessment of health risk was carried out.
引文
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