电沉积聚合物和纳米颗粒构造电化学传感器以及纳米电极的研制
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摘要
本论文在对聚合物膜修饰电极以及纳米材料的研究概况进行综述的基础上,开展了PdCu合金纳米、烟酰胺、酚藏花红与Pd纳米复合物等的电化学制备、界面表征:以神经递质多巴胺(DA)、尿酸(UA)、抗坏血酸(AA)和亚硝酸根等为对象,探讨了这些纳米电极的电化学催化作用与传感性能。此外,以电化学刻蚀方法制备了纳米尺寸的会电极,开展了初步的分析应用。具体内容如下:
用电化学共沉积法,在玻碳电极(GCE)表面制备了2维与3维混合结构的PdCu合金纳米簇。在优化的沉积条件下,2维纳米簇,先电沉积形成,颗粒的尺寸约为15mm,多为椭球形,较分散地连接在一起成藤蔓状;3维纳米簇,后电沉积形成,为球状聚集的纳米粒子,直径为50-100nm,像藤蔓上开的花朵。研究发现,2维纳米簇修饰的GCE,能立即降低亚硝酸根氧化反应的过电位,3维纳米簇形成,则主要改善该反应电子传递的可逆性,使氧化峰高增大,电流灵敏度提高。该PdCu纳米簇修饰电极,PdCu/GCE,由于Pd和Cu的协同作用而具有更强的催化能力和更高的电流灵敏度,而且稳定性好。发现合金纳米粒子的催化作用与纳米簇三维结构特征相关的现象,对于深入探讨合金组成-纳米结构-催化效应的关系具有启示意义。
研究了烟酰胺在GCE上的电化学聚合及所形成的修饰电极(poly-VPP/GCE)的电化学特性。发现该电极抗坏血酸(AA)、对多巴胺(DA)、尿酸(UA)以及亚硝酸根等的电化学氧化具有显著的催化作用,过氧化电位降低,氧化峰分别出现在0.034、0.163、0.291和0.78 V(vs.SCE):而且该修饰层对AA具有较强的电性排斥作用,因而进一步降低了测定干扰,可在大量AA共存下同时测定DA和UA的浓度。此电极还可应用于NO_2~-的电化学测定,在很宽的浓度范围内与氧化峰电流有良好的线性关系,响应快速,重现性良好。
用CV法合成了一种新的聚合物金属纳米复合物:聚酚藏花红(PPS)-Pd的纳米复合物(PPS-Pd)。由于实验设计在沉积Pd纳米粒子同时,聚合一层纳米厚度的酚藏花红聚合物覆盖层,使Pd纳米粒子被有效地分散开,防止进一步的聚集,增加了Pd纳米粒子的有效催化表面积。而且,PPS中N原子可与Pd配位,可能改变了PPS/Pd界面的的性质。PPS-Pd修饰的GCE对亚硝酸根有很强的电催化作用,检测范围较宽,检测限较低,体现了Pd纳米粒子与聚酚藏花红之间显著的协同效应。
最后,以电化学刻蚀-电泳漆绝缘的方法制备出了单根的纳米金电极,最细小有效直径达到52nm。对该纳米金电极进行了恒电位阳极化处理,发现对亚硝酸根的氧化具有强烈的电催化作用,DPV峰电位为0.75 V,峰电流与浓度在2～809μmol/L范围成线性关系,检测下限达到0.3μmol/L,重复性良好,可用作亚硝酸盐传感器。
Based on detailed reviews on polymer film modified electrodes and nanoscale materials,research was carried out for electrochemical sensor fabrications by surface modification of various substances involving niacinamide(VPP),PdCu alloy nanoparticles as well as phenosafranin(PS) and Pd nanocomposite.The fabrication of several novel nano-structured electrochemical interfaces by direct electrochemical deposition on GCE is reported.These sensors were used for electrochemical sensing of bioactive molecules including dopamine(DA),uric acid(UA),ascorbic acid(AA), and nitrite.In addition,we obtained nanoscale gold disk electrodes by electrochemical etching and probe into its electroanalytical application.The study is mainly focused on the following aspects:
PdCu alloy nanoclusters were fabricated using electrochemical codeposition on the GCE.We found that the PdCu alloys were consisted of 15nm average sized nanoparticles.Most dispersed nanoparticles were elliptical,linked together but dispersed in a range like twigs and leaves.The fractal nanostructures may be referred to "2D-nanoclusters ".Some spherical clusters of 50-100 nm size,which consisted of closely assembled nanoparticles,can be found on the GCE like flowers.They were referred to "3D-nanoclusters".The 2D- nanoclusters can reduce the overpotentials of nitrite oxidation immediately and the 3D-clusters have weak ability to influence the overpotentials but strong ability to influence the current response.The reproducibility was excellen.Obviously,the PdCu/GCE had higher catalytic activity than singly Pd and Cu deposited electrodes,showing the synergic effect of the two metals in the nano-alloy.These findings indicated that catalytic activities may be related to the structure of nanoclusters.The complicity of the nanostructures may come from the easy variation of alloy compositions in result of several different crystalline structures. These results can be in favor of farther researching the correlations of alloy composition,nanostructures and catalytic activities.
A chemically modified electrode has been prepared successfully by means of electropolymerization of niacinamide(VPP) at a glassy carbon electrode(poly-VPP /GCE).It was found that the polymer catalyzed the electrochemical oxidation of DA,UA,AA and NO_2~-,whose oxidation peak appeared at 0.163 V,0.291 V,0.034 V and 0.78 V(vs.SCE) respectively.Owing to the repulsion between the polymer film and AA,the poly-VPP/GCE has superior exclusive ability for AA.The co-existence of lots of AA did not interfere with the detection of DA or UA.It has been applied to the determination of NO_2~- with satisfactory results.The oxidation current was linearly related to nitrite concentration over wider range.The response was fast and had excellent reproducibility.
The incorporation of Pd into PPS forms a nano-structured metal/polymer composite:PPS- Pd nano composite using cyclic voltammetry(CV).A Pd nanoparticle was formed during one cycle of CV scanning.Each Pd nanoparticle should be covered by a thin-layer of in-situ synthesized PPS film of nano-thickness. The Pd nanoparticles in the composite can be separated effectively and thus increased their effective surface area for the catalytic reaction.Moreover,the nano-Pd can coordinatively bind to PPS through N atoms lead to creat novel interface of Pd/PPS, which will change the properties of both Pd and PPS.The PPS-Pdcomposite modified layer can further reduce the overpotential and can significantly enhance the CV and DPV peak current response of nitrite oxidation in comparison with P.d and PPS individually modified layers.This can be attributed to the cooperative effect of PPS and Pd nanoparticles.Compared with the nitrite oxidation-based nitrite sensor reported previously,this method exhibits wider linear range and lower detecting limit.
Lastly,nanoscale gold electrode was prepared by etching a fine Au wire,which was subsequently coated with electrophoretic paint deposited cathodically.The dimension of microelectrode could reach to 52 nm.And then,electrochemical activation is achieved by polarization at a fixed potential.It was found that the electrode catalyzed the electrochemical oxidation of nitrite.The DPV oxidation peak appeared at 0.75 V.The oxidation current was linearly related to nitrite concentration over the range 2～809μmol/L,with a detection limit of 0.3μmol/L.The response was fast and had excellent reproducibility.It could be found important applications in nitrite sensors.
用电化学共沉积法,在玻碳电极(GCE)表面制备了2维与3维混合结构的PdCu合金纳米簇。在优化的沉积条件下,2维纳米簇,先电沉积形成,颗粒的尺寸约为15mm,多为椭球形,较分散地连接在一起成藤蔓状;3维纳米簇,后电沉积形成,为球状聚集的纳米粒子,直径为50-100nm,像藤蔓上开的花朵。研究发现,2维纳米簇修饰的GCE,能立即降低亚硝酸根氧化反应的过电位,3维纳米簇形成,则主要改善该反应电子传递的可逆性,使氧化峰高增大,电流灵敏度提高。该PdCu纳米簇修饰电极,PdCu/GCE,由于Pd和Cu的协同作用而具有更强的催化能力和更高的电流灵敏度,而且稳定性好。发现合金纳米粒子的催化作用与纳米簇三维结构特征相关的现象,对于深入探讨合金组成-纳米结构-催化效应的关系具有启示意义。
研究了烟酰胺在GCE上的电化学聚合及所形成的修饰电极(poly-VPP/GCE)的电化学特性。发现该电极抗坏血酸(AA)、对多巴胺(DA)、尿酸(UA)以及亚硝酸根等的电化学氧化具有显著的催化作用,过氧化电位降低,氧化峰分别出现在0.034、0.163、0.291和0.78 V(vs.SCE):而且该修饰层对AA具有较强的电性排斥作用,因而进一步降低了测定干扰,可在大量AA共存下同时测定DA和UA的浓度。此电极还可应用于NO_2~-的电化学测定,在很宽的浓度范围内与氧化峰电流有良好的线性关系,响应快速,重现性良好。
用CV法合成了一种新的聚合物金属纳米复合物:聚酚藏花红(PPS)-Pd的纳米复合物(PPS-Pd)。由于实验设计在沉积Pd纳米粒子同时,聚合一层纳米厚度的酚藏花红聚合物覆盖层,使Pd纳米粒子被有效地分散开,防止进一步的聚集,增加了Pd纳米粒子的有效催化表面积。而且,PPS中N原子可与Pd配位,可能改变了PPS/Pd界面的的性质。PPS-Pd修饰的GCE对亚硝酸根有很强的电催化作用,检测范围较宽,检测限较低,体现了Pd纳米粒子与聚酚藏花红之间显著的协同效应。
最后,以电化学刻蚀-电泳漆绝缘的方法制备出了单根的纳米金电极,最细小有效直径达到52nm。对该纳米金电极进行了恒电位阳极化处理,发现对亚硝酸根的氧化具有强烈的电催化作用,DPV峰电位为0.75 V,峰电流与浓度在2～809μmol/L范围成线性关系,检测下限达到0.3μmol/L,重复性良好,可用作亚硝酸盐传感器。
Based on detailed reviews on polymer film modified electrodes and nanoscale materials,research was carried out for electrochemical sensor fabrications by surface modification of various substances involving niacinamide(VPP),PdCu alloy nanoparticles as well as phenosafranin(PS) and Pd nanocomposite.The fabrication of several novel nano-structured electrochemical interfaces by direct electrochemical deposition on GCE is reported.These sensors were used for electrochemical sensing of bioactive molecules including dopamine(DA),uric acid(UA),ascorbic acid(AA), and nitrite.In addition,we obtained nanoscale gold disk electrodes by electrochemical etching and probe into its electroanalytical application.The study is mainly focused on the following aspects:
PdCu alloy nanoclusters were fabricated using electrochemical codeposition on the GCE.We found that the PdCu alloys were consisted of 15nm average sized nanoparticles.Most dispersed nanoparticles were elliptical,linked together but dispersed in a range like twigs and leaves.The fractal nanostructures may be referred to "2D-nanoclusters ".Some spherical clusters of 50-100 nm size,which consisted of closely assembled nanoparticles,can be found on the GCE like flowers.They were referred to "3D-nanoclusters".The 2D- nanoclusters can reduce the overpotentials of nitrite oxidation immediately and the 3D-clusters have weak ability to influence the overpotentials but strong ability to influence the current response.The reproducibility was excellen.Obviously,the PdCu/GCE had higher catalytic activity than singly Pd and Cu deposited electrodes,showing the synergic effect of the two metals in the nano-alloy.These findings indicated that catalytic activities may be related to the structure of nanoclusters.The complicity of the nanostructures may come from the easy variation of alloy compositions in result of several different crystalline structures. These results can be in favor of farther researching the correlations of alloy composition,nanostructures and catalytic activities.
A chemically modified electrode has been prepared successfully by means of electropolymerization of niacinamide(VPP) at a glassy carbon electrode(poly-VPP /GCE).It was found that the polymer catalyzed the electrochemical oxidation of DA,UA,AA and NO_2~-,whose oxidation peak appeared at 0.163 V,0.291 V,0.034 V and 0.78 V(vs.SCE) respectively.Owing to the repulsion between the polymer film and AA,the poly-VPP/GCE has superior exclusive ability for AA.The co-existence of lots of AA did not interfere with the detection of DA or UA.It has been applied to the determination of NO_2~- with satisfactory results.The oxidation current was linearly related to nitrite concentration over wider range.The response was fast and had excellent reproducibility.
The incorporation of Pd into PPS forms a nano-structured metal/polymer composite:PPS- Pd nano composite using cyclic voltammetry(CV).A Pd nanoparticle was formed during one cycle of CV scanning.Each Pd nanoparticle should be covered by a thin-layer of in-situ synthesized PPS film of nano-thickness. The Pd nanoparticles in the composite can be separated effectively and thus increased their effective surface area for the catalytic reaction.Moreover,the nano-Pd can coordinatively bind to PPS through N atoms lead to creat novel interface of Pd/PPS, which will change the properties of both Pd and PPS.The PPS-Pdcomposite modified layer can further reduce the overpotential and can significantly enhance the CV and DPV peak current response of nitrite oxidation in comparison with P.d and PPS individually modified layers.This can be attributed to the cooperative effect of PPS and Pd nanoparticles.Compared with the nitrite oxidation-based nitrite sensor reported previously,this method exhibits wider linear range and lower detecting limit.
Lastly,nanoscale gold electrode was prepared by etching a fine Au wire,which was subsequently coated with electrophoretic paint deposited cathodically.The dimension of microelectrode could reach to 52 nm.And then,electrochemical activation is achieved by polarization at a fixed potential.It was found that the electrode catalyzed the electrochemical oxidation of nitrite.The DPV oxidation peak appeared at 0.75 V.The oxidation current was linearly related to nitrite concentration over the range 2～809μmol/L,with a detection limit of 0.3μmol/L.The response was fast and had excellent reproducibility.It could be found important applications in nitrite sensors.
引文
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