硅基底上纳米棒电极的制备及其应用
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摘要
随着近年来全世界范围的能源危机和环境污染的加剧,节能而又环保的新能源系统的开发受到了越来越多的关注,这其中直接甲醇燃料电池(DMFC)和电化学电容器是研究的比较多的。但是无论是直接甲醇燃料电池还是电化学电容器,它的成本及使用寿命都在很大程度上的受器件的电极结构及电极材料的限制。本论文提出了一种新型的纳米棒电极结构,并研究了纳米棒电极作为直接甲醇燃料电池及电化学电容器电极时的电化学性质,主要内容如下:
1.利用射频溅射制备Al/Ti/Si基片,然后用二次阳极氧化法把有序模板成功生长在了硅基底上,优化实验参数可以获得AAO/Ti/Si模板。与单一的AAO模板相比,AAO/Ti/Si模板具有较高的硬度,较好的耐高温性。另外,AAO/Ti/Si模板还具有独特的电化学沉积特性,使沉积材料与基底之间具有很好的结合力。
2.利用直流电沉积在Si基底上成功制备了Pt及PtRu合金纳米棒,用扫描电子显微镜(SEM)、透射电子显微镜(TEM)和X射线能量谱(EDX)表征了纳米棒的形貌结构特征及元素成分。电化学性质测试表明,Pt纳米棒电极比Pt薄膜电极有着更大的催化电流密度,而PtRu纳米棒电极由于Ru元素的引入,使其比初期制备的Pt纳米棒电极有着更好的防碳氧化合物毒化的作用。
3.为了进一步降低DMFC阳极催化剂的成本,我们制备了PtNi纳米棒电极,用FESEM、TEM、EDS和X射线光电子能谱(XPS)表征了纳米棒的形貌结构特征及元素成分。电化学性质测试表明PtNi纳米棒电极比传统方法制备的Pt/C电极有着更大的活性面积,同时循环伏安测试和长时间恒电位极化还表明PtNi纳米棒电极比Pt/C电极有着更好的抗中毒能力。
4.通过直流电沉积的方法在硅基底上制备了聚苯胺(PANI)及钴锰氧化物(CMO)纳米棒。电化学测试表明在电流密度为5 Ag~(-1)时,PANI纳米棒电极的比容量为1142 Fg~(-1),PANI纳米棒电极经过500圈的循环充放电后电极的比容量降低了大约5%,证明这种电极的电化学性质比较稳定。对于CMO纳米棒电极而言,经过100℃热处理的CMO纳米棒电极显示了比较好的电容行为,比容量可达396 Fg~(-1)。
New energy systems which is more energy saving and environmentally friendly are attracting more and more concern because of the energy crisis and environmental pollution in the whole world.In all the systems,DMFC and supercapacitors have attracted the most concern.However,the cost and the life of DMFC and supereapacitors are restricted by the structure and the materials of the electrodes.In this work,new electrode architecture with nanorod structure is proposed.And the electrochemical performance of the electrodes is studied when they act as the electrodes of DMFC and supercapacitors.The main results are as follows:
1.Al/Ti/Si substrates were fabricated by radio frequency sputtering.Then the ordered AAO templates were successfully transfered to silicon substrates by a two-step electrochemical anodization.AAO/Ti/Si substrates with different diameters were obtained by optimizing the experimental conditions.Compared with the single AAO templates,the AAO/Ti/Si substrates have the properties of good mechanical strength and durability against heat treatment at higher temperature.In addition,the AAO/Ti/Si substrates have also unique electrodeposition properties and could bond well with the deposited materials.
2.Pt and PtRu nanorod electrodes were fabricated on the Si substrate direct current(DC) electrodeposition,respectively.The structure and the composition of the electrodes were characterized by SEM,TEM and EDS.The electrochemical characterization showed that Pt nanorod electrodes have sharper catalysis current than Pt film electrodes.And PtRu nanorod electrodes have better defending effect to the poison of carbonic oxide than Pt nanorod electrodes for the join of Ru element.
3.PtNi nanorod electrodes were fabricated on the Si substrate to reduce the cost. The structure and the composition of the electrodes were characterized by SEM,TEM and EDS.The result of the electrochemical characterization showed that PtNi nanorod electrodes have larger active area than Pt/C electrodes which were fabricated with traditional method.Cyclic voltammograms and chronoamperograms showed that PtNi nanorod electrodes have better defending effect to the poison of carbonic oxide than Pt/C electrodes.
4.PANI and CMO nanorod electrodes were fabricated on the Si substrate(DC) electrodeposition,respectively.The discharge capacitance of the PANI nanowire arrayed electrode at a current density of 5 Ag~(-1) is 1142 Fg~(-1),and the discharge capacitance loss after 500 consecutive cycles was negligible,at about 5%.The ideal capacitive behavior was obtained from the as-prepared sample heat-treated at 100℃. The specific capacitance of the electrode was 396 Fg~(-1).
1.利用射频溅射制备Al/Ti/Si基片,然后用二次阳极氧化法把有序模板成功生长在了硅基底上,优化实验参数可以获得AAO/Ti/Si模板。与单一的AAO模板相比,AAO/Ti/Si模板具有较高的硬度,较好的耐高温性。另外,AAO/Ti/Si模板还具有独特的电化学沉积特性,使沉积材料与基底之间具有很好的结合力。
2.利用直流电沉积在Si基底上成功制备了Pt及PtRu合金纳米棒,用扫描电子显微镜(SEM)、透射电子显微镜(TEM)和X射线能量谱(EDX)表征了纳米棒的形貌结构特征及元素成分。电化学性质测试表明,Pt纳米棒电极比Pt薄膜电极有着更大的催化电流密度,而PtRu纳米棒电极由于Ru元素的引入,使其比初期制备的Pt纳米棒电极有着更好的防碳氧化合物毒化的作用。
3.为了进一步降低DMFC阳极催化剂的成本,我们制备了PtNi纳米棒电极,用FESEM、TEM、EDS和X射线光电子能谱(XPS)表征了纳米棒的形貌结构特征及元素成分。电化学性质测试表明PtNi纳米棒电极比传统方法制备的Pt/C电极有着更大的活性面积,同时循环伏安测试和长时间恒电位极化还表明PtNi纳米棒电极比Pt/C电极有着更好的抗中毒能力。
4.通过直流电沉积的方法在硅基底上制备了聚苯胺(PANI)及钴锰氧化物(CMO)纳米棒。电化学测试表明在电流密度为5 Ag~(-1)时,PANI纳米棒电极的比容量为1142 Fg~(-1),PANI纳米棒电极经过500圈的循环充放电后电极的比容量降低了大约5%,证明这种电极的电化学性质比较稳定。对于CMO纳米棒电极而言,经过100℃热处理的CMO纳米棒电极显示了比较好的电容行为,比容量可达396 Fg~(-1)。
New energy systems which is more energy saving and environmentally friendly are attracting more and more concern because of the energy crisis and environmental pollution in the whole world.In all the systems,DMFC and supercapacitors have attracted the most concern.However,the cost and the life of DMFC and supereapacitors are restricted by the structure and the materials of the electrodes.In this work,new electrode architecture with nanorod structure is proposed.And the electrochemical performance of the electrodes is studied when they act as the electrodes of DMFC and supercapacitors.The main results are as follows:
1.Al/Ti/Si substrates were fabricated by radio frequency sputtering.Then the ordered AAO templates were successfully transfered to silicon substrates by a two-step electrochemical anodization.AAO/Ti/Si substrates with different diameters were obtained by optimizing the experimental conditions.Compared with the single AAO templates,the AAO/Ti/Si substrates have the properties of good mechanical strength and durability against heat treatment at higher temperature.In addition,the AAO/Ti/Si substrates have also unique electrodeposition properties and could bond well with the deposited materials.
2.Pt and PtRu nanorod electrodes were fabricated on the Si substrate direct current(DC) electrodeposition,respectively.The structure and the composition of the electrodes were characterized by SEM,TEM and EDS.The electrochemical characterization showed that Pt nanorod electrodes have sharper catalysis current than Pt film electrodes.And PtRu nanorod electrodes have better defending effect to the poison of carbonic oxide than Pt nanorod electrodes for the join of Ru element.
3.PtNi nanorod electrodes were fabricated on the Si substrate to reduce the cost. The structure and the composition of the electrodes were characterized by SEM,TEM and EDS.The result of the electrochemical characterization showed that PtNi nanorod electrodes have larger active area than Pt/C electrodes which were fabricated with traditional method.Cyclic voltammograms and chronoamperograms showed that PtNi nanorod electrodes have better defending effect to the poison of carbonic oxide than Pt/C electrodes.
4.PANI and CMO nanorod electrodes were fabricated on the Si substrate(DC) electrodeposition,respectively.The discharge capacitance of the PANI nanowire arrayed electrode at a current density of 5 Ag~(-1) is 1142 Fg~(-1),and the discharge capacitance loss after 500 consecutive cycles was negligible,at about 5%.The ideal capacitive behavior was obtained from the as-prepared sample heat-treated at 100℃. The specific capacitance of the electrode was 396 Fg~(-1).
引文
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