湿化学法合成纳米材料及其在电化学器件中的应用
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摘要
纳米材料由于具有体材料所不具备的独特的物理化学性质,在电化学器件中有着广泛的应用前景,如锂离子电池和电化学传感器。将纳米材料作为电极材料可以有效地提高锂离子电池的比容量和循环性能,为下一代锂离子电池的开发提供理论基础。基于纳米材料构建的新型电化学传感器具有高的灵敏度和快的响应时间,为生物医学检测和环境监测提供了更加高效的方法。本论文采用湿化学法合成了几种特殊结构的纳米材料,并研究了其在锂离子电池和电化学传感器中的应用前景。具体研究内容如下：
1.过渡金属氧化物作为锂离子电池的负极材料,在充放电过程中,会发生体积膨胀导致电池的循环性能下降。通过制备由纳米小颗粒自组装而成的过渡金属氧化物纳米球,充分发挥纳米构建单元和三维空间结构的协同作用,可以实现较高的放电容量和良好的循环性能。在第2章,以乙酸镍和乙二醇为原料,制备了这种三维结构的NiO纳米球。采用恒电流充放电和循环伏安法技术研究了NiO纳米球的电化学性能。在电流密度为100mA/g时,50个充放电循环后,NiO纳米球的放电比容量为573mAh/g,相当于其理论比容量的80%。NiO纳米球具有如此好的电化学性能是来自于它的三维自组装结构。这种结构的NiO纳米球不仅可以缓冲充放电过程中的体积变化以维持材料结构的完整性,而且还缩短了锂离子的扩散路径。
2.Sn02作为锂离子电池的负极材料具有很大的吸引力,比容量是石墨材料的2倍。然而当Sn02和锂反应时会发生巨大的体积膨胀,导致电极材料逐渐粉化,循环性能下降。针对Sn02的这个缺陷,将Sn02和碳材料复合起来可以提高它的循环性能。在第3章,选用了石墨烯这一新型的碳材料与Sn02复合,制备了SnO2/graphene纳米复合物,有效地提高了Sn02的循环性能。在电流密度为50mA/g时,50个充放电循环后,SnO2/graphene纳米复合物的放电比容量为665mAh/g,相当于其理论比容量的86%。SnO2/graphene纳米复合物表现出这么好的性能是由于电极材料中复合了石墨烯。石墨烯纳米片可以抑制Sn02纳米颗粒的团聚,提高电极材料的电导率,增强充放电循环过程中材料结构的稳定性。
3.聚苯胺具有良好的生物相容性和高的电导率,是固定酶分子的理想载体。然而传统的聚苯胺材料在溶液中的分散性很差,不利于材料的加工处理。通过合成纳米结构的聚苯胺可以有效地解决这个问题。在第4章,采用界面聚合法合成了对甲苯磺酸掺杂的聚苯胺纳米纤维,并采用滴涂的方法将聚苯胺纳米纤维和辣根过氧化物酶的混合分散液修饰到玻碳电极上,构建了过氧化氢电化学传感器。包裹在聚苯胺纳米纤维／壳聚糖薄膜中的辣根过氧化物酶较好地保持了生物活性,能有效地催化还原过氧化氢。同时,聚苯胺纳米纤维又具有大的比表面积和高的电导率,可以固定更多的酶分子和加速酶活性中心和电极之间的电子传递。
4.金属纳米颗粒的稳定性、颗粒大小和分散性与它的电催化性能密切相关。石墨烯具有电导率高和化学稳定性好等优点,将它用来固定金属纳米颗粒会起到非常好的效果。在第5章,采用了一种简便的原位合成方法把镍纳米颗粒负载在石墨烯的表面,制备了Ni/graphene纳米复合物(NiGN)。采用滴涂的方法将NiGN和壳聚糖的混合分散液固定到玻碳电极上,构建了非酶葡萄糖电化学传感器。电化学测试结果表明：对于葡萄糖的电催化氧化,NiGN修饰的玻碳电极展现了非常高的电催化活性。葡萄糖传感器的响应电流非常灵敏和稳定,这得益于沉积的镍纳米颗粒具有良好的电催化性能和石墨烯载体拥有快速的电子传递能力。更重要的是,几种干扰物(例如抗坏血酸和尿酸)的存在也不会影响葡萄糖传感器的性能。
Nanomaterials have been extensively applied in electrochemical devices such as lithium ion battery and electrochemical sensor, which are attributed to their novel physical and chemical properties different from their corresponding bulk materials. Nanomaterials as electrode materials can improve the capacity and cycle performance effectively, which provide theoretical basis for exploiting the next generation lithium ion batteries. The novel electrochemical sensors based on nanomaterials have high sensitivity and fast response time, which provide efficient approach for biomedicine detection and environmental monitoring. This dissertation deals primary with the wet chemical synthesis of a few unique structured nanomaterials and investigate their application prospects in lithium ion batteries and electrochemical sensors. The detailed contents are summarized as follows:
1. Transition metal oxides as anode materias for lithium ion battery, show volume expansion in charge/discharge process, leading to cycle performance drop. Based on the synergy effects in both nanostructure unit and three dimensional configurations, preparation of transition metal oxide nanosphere by self-assembly of small nanoparticles could realize high discharge capacity and good cycle performance. In chapter2, three dimensional structured NiO nanospheres were synthesized by using Ni(CH3COO)2·4H2O and ethylene glycol. Electrochemical performance of NiO nanospheres were evaluated by galvanostatic cycling and cyclic voltammetery. At the current density of100mA/g, the NiO nanospheres showed discharge capacity of573mAh/g after50cycles, corresponding80%theoretical capacity. The NiO nanospheres have so good electrochemical performance as anode materials for lithium ion battery, which is attributed to its three dimensional self-assemble structures. The unique structures within NiO nanospheres not only accommodate the volume change of charge/discharge process to maintain the structure integrity of materials, but also shorten Li+diffusion pathways.
2. As anode material for lithium ion battery, SnO2has attracted much attention due to its twice capacity of graphite. However, when SnO2reacts with Li, there is a huge volume expansion, leading to electrode material pulverization and poor cyclability. Aim at this deficiency, hybridizing SnO2with carbon is an effective method to enhance the cyclability of the SnO2anode. In chapter3, a new kind of carbon material, graphene, is chosen to hybridize with SnO2to synthesize SnO2/graphene nanocomposite and improve cycle performance. At the current density of50mA/g, the SnO2/graphene nanocomposite could keep discharge capacity of665mAh/g after50cycles, corresponding86%theoretical capacity. SnO2/graphene nanocomposite showed an excellent cycling performance for lithium ion battery, which was ascribed to the presence of graphene. Graphene nanosheets can suppress the aggregation of active SnO2nanoparticles, enhance the conductivity of electrode material, and increase their structural stability during discharge/charge cycling.
3. Polyaniline is an ideal immobilizing enzyme molecule matrix, due to its good biocompatibility and high electrical conductivity. However, the dispersion of conventional polyaniline in solution is very bad, which is adverse for material processability. Synthesis of nanostructured polyaniline is a feasible method to solve this problem. In Chapter4, polyaniline nanofibers (4-toluenesulfonic acid as dopant) were synthesized by interface polymerization. The mixed dispersion of polyaniline nanofibers and horseradish peroxidase was cast onto the glassy carbon electrode by a drop-coating method, and an electrochemical sensor for hydrogen peroxide was constructed. Horseradish peroxidase entrapped in the polyaniline nanofibers/chitosan film could preferable keep its native bioactivity and effectively catalyze the reduction of hydrogen peroxide. Polyaniline nanofibers modified electrode could lead to more enzyme molecules loading and rapid electron transfer rate between the active centers of enzyme and electrode, because they have large surface area and high electrical conductivity.
4. The electrochemical activities of metal nanoparticles depend heavily on their stability, particle size and distribution. Graphene with high electrical conductivity and good chemical inertia is a wonderful supporting material for immobilizing metal nanoparticles. In chapter5, we employed a facile in situ synthesis approach to load nickel nanoparticles on the graphene surface, prepared Ni/graphene nanocomposite (NiGN). Nonenzymatic glucose sensors were constructed by dropcasting the mixed dispersion of NiGN and chitosan on the glass carbon electrode. The electrochemical measure results showed that NiGN modified electrode exhibited high electrochemical activity for electrocatalytic oxidation of glucose in alkaline medium. The current response of the glucose sensor was highly sensitive and stable, which is attributed to the good electrocatalytic performance of the firmly deposited Ni nanoparticles as well as the efficient electron transfer of graphene matrix. What's more important, the presence of several interferences (such as ascorbic acid and uric acid) cannot affect the performance of the glucose sensor.
1.过渡金属氧化物作为锂离子电池的负极材料,在充放电过程中,会发生体积膨胀导致电池的循环性能下降。通过制备由纳米小颗粒自组装而成的过渡金属氧化物纳米球,充分发挥纳米构建单元和三维空间结构的协同作用,可以实现较高的放电容量和良好的循环性能。在第2章,以乙酸镍和乙二醇为原料,制备了这种三维结构的NiO纳米球。采用恒电流充放电和循环伏安法技术研究了NiO纳米球的电化学性能。在电流密度为100mA/g时,50个充放电循环后,NiO纳米球的放电比容量为573mAh/g,相当于其理论比容量的80%。NiO纳米球具有如此好的电化学性能是来自于它的三维自组装结构。这种结构的NiO纳米球不仅可以缓冲充放电过程中的体积变化以维持材料结构的完整性,而且还缩短了锂离子的扩散路径。
2.Sn02作为锂离子电池的负极材料具有很大的吸引力,比容量是石墨材料的2倍。然而当Sn02和锂反应时会发生巨大的体积膨胀,导致电极材料逐渐粉化,循环性能下降。针对Sn02的这个缺陷,将Sn02和碳材料复合起来可以提高它的循环性能。在第3章,选用了石墨烯这一新型的碳材料与Sn02复合,制备了SnO2/graphene纳米复合物,有效地提高了Sn02的循环性能。在电流密度为50mA/g时,50个充放电循环后,SnO2/graphene纳米复合物的放电比容量为665mAh/g,相当于其理论比容量的86%。SnO2/graphene纳米复合物表现出这么好的性能是由于电极材料中复合了石墨烯。石墨烯纳米片可以抑制Sn02纳米颗粒的团聚,提高电极材料的电导率,增强充放电循环过程中材料结构的稳定性。
3.聚苯胺具有良好的生物相容性和高的电导率,是固定酶分子的理想载体。然而传统的聚苯胺材料在溶液中的分散性很差,不利于材料的加工处理。通过合成纳米结构的聚苯胺可以有效地解决这个问题。在第4章,采用界面聚合法合成了对甲苯磺酸掺杂的聚苯胺纳米纤维,并采用滴涂的方法将聚苯胺纳米纤维和辣根过氧化物酶的混合分散液修饰到玻碳电极上,构建了过氧化氢电化学传感器。包裹在聚苯胺纳米纤维／壳聚糖薄膜中的辣根过氧化物酶较好地保持了生物活性,能有效地催化还原过氧化氢。同时,聚苯胺纳米纤维又具有大的比表面积和高的电导率,可以固定更多的酶分子和加速酶活性中心和电极之间的电子传递。
4.金属纳米颗粒的稳定性、颗粒大小和分散性与它的电催化性能密切相关。石墨烯具有电导率高和化学稳定性好等优点,将它用来固定金属纳米颗粒会起到非常好的效果。在第5章,采用了一种简便的原位合成方法把镍纳米颗粒负载在石墨烯的表面,制备了Ni/graphene纳米复合物(NiGN)。采用滴涂的方法将NiGN和壳聚糖的混合分散液固定到玻碳电极上,构建了非酶葡萄糖电化学传感器。电化学测试结果表明：对于葡萄糖的电催化氧化,NiGN修饰的玻碳电极展现了非常高的电催化活性。葡萄糖传感器的响应电流非常灵敏和稳定,这得益于沉积的镍纳米颗粒具有良好的电催化性能和石墨烯载体拥有快速的电子传递能力。更重要的是,几种干扰物(例如抗坏血酸和尿酸)的存在也不会影响葡萄糖传感器的性能。
Nanomaterials have been extensively applied in electrochemical devices such as lithium ion battery and electrochemical sensor, which are attributed to their novel physical and chemical properties different from their corresponding bulk materials. Nanomaterials as electrode materials can improve the capacity and cycle performance effectively, which provide theoretical basis for exploiting the next generation lithium ion batteries. The novel electrochemical sensors based on nanomaterials have high sensitivity and fast response time, which provide efficient approach for biomedicine detection and environmental monitoring. This dissertation deals primary with the wet chemical synthesis of a few unique structured nanomaterials and investigate their application prospects in lithium ion batteries and electrochemical sensors. The detailed contents are summarized as follows:
1. Transition metal oxides as anode materias for lithium ion battery, show volume expansion in charge/discharge process, leading to cycle performance drop. Based on the synergy effects in both nanostructure unit and three dimensional configurations, preparation of transition metal oxide nanosphere by self-assembly of small nanoparticles could realize high discharge capacity and good cycle performance. In chapter2, three dimensional structured NiO nanospheres were synthesized by using Ni(CH3COO)2·4H2O and ethylene glycol. Electrochemical performance of NiO nanospheres were evaluated by galvanostatic cycling and cyclic voltammetery. At the current density of100mA/g, the NiO nanospheres showed discharge capacity of573mAh/g after50cycles, corresponding80%theoretical capacity. The NiO nanospheres have so good electrochemical performance as anode materials for lithium ion battery, which is attributed to its three dimensional self-assemble structures. The unique structures within NiO nanospheres not only accommodate the volume change of charge/discharge process to maintain the structure integrity of materials, but also shorten Li+diffusion pathways.
2. As anode material for lithium ion battery, SnO2has attracted much attention due to its twice capacity of graphite. However, when SnO2reacts with Li, there is a huge volume expansion, leading to electrode material pulverization and poor cyclability. Aim at this deficiency, hybridizing SnO2with carbon is an effective method to enhance the cyclability of the SnO2anode. In chapter3, a new kind of carbon material, graphene, is chosen to hybridize with SnO2to synthesize SnO2/graphene nanocomposite and improve cycle performance. At the current density of50mA/g, the SnO2/graphene nanocomposite could keep discharge capacity of665mAh/g after50cycles, corresponding86%theoretical capacity. SnO2/graphene nanocomposite showed an excellent cycling performance for lithium ion battery, which was ascribed to the presence of graphene. Graphene nanosheets can suppress the aggregation of active SnO2nanoparticles, enhance the conductivity of electrode material, and increase their structural stability during discharge/charge cycling.
3. Polyaniline is an ideal immobilizing enzyme molecule matrix, due to its good biocompatibility and high electrical conductivity. However, the dispersion of conventional polyaniline in solution is very bad, which is adverse for material processability. Synthesis of nanostructured polyaniline is a feasible method to solve this problem. In Chapter4, polyaniline nanofibers (4-toluenesulfonic acid as dopant) were synthesized by interface polymerization. The mixed dispersion of polyaniline nanofibers and horseradish peroxidase was cast onto the glassy carbon electrode by a drop-coating method, and an electrochemical sensor for hydrogen peroxide was constructed. Horseradish peroxidase entrapped in the polyaniline nanofibers/chitosan film could preferable keep its native bioactivity and effectively catalyze the reduction of hydrogen peroxide. Polyaniline nanofibers modified electrode could lead to more enzyme molecules loading and rapid electron transfer rate between the active centers of enzyme and electrode, because they have large surface area and high electrical conductivity.
4. The electrochemical activities of metal nanoparticles depend heavily on their stability, particle size and distribution. Graphene with high electrical conductivity and good chemical inertia is a wonderful supporting material for immobilizing metal nanoparticles. In chapter5, we employed a facile in situ synthesis approach to load nickel nanoparticles on the graphene surface, prepared Ni/graphene nanocomposite (NiGN). Nonenzymatic glucose sensors were constructed by dropcasting the mixed dispersion of NiGN and chitosan on the glass carbon electrode. The electrochemical measure results showed that NiGN modified electrode exhibited high electrochemical activity for electrocatalytic oxidation of glucose in alkaline medium. The current response of the glucose sensor was highly sensitive and stable, which is attributed to the good electrocatalytic performance of the firmly deposited Ni nanoparticles as well as the efficient electron transfer of graphene matrix. What's more important, the presence of several interferences (such as ascorbic acid and uric acid) cannot affect the performance of the glucose sensor.
引文
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