基于电化学方法的Co_3O_4纳米薄膜材料制备及其性能研究
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摘要
在诸多的过渡金属氧化物中,C0304是一种重要的半导体功能材料,具有稳定的化学性质和特定的磁学性能,因此在许多领域有着重要的应用,诸如能量存储、催化、传感器、场发射材料以及电致变色装置等,因此开发C0304先进功能材料并研究其相应的电磁性能具有重要的意义。
近几十年来在纳米材料技术迅速发展的基础上,研究者们通过多种制备途径开发出形貌和尺寸多样化的C0304纳米材料,并报道了材料在不同应用领域的性能。所采用的方法主要包括化学沉淀法、水热／溶剂热法、溶胶凝胶法、模板法、电化学沉积法、化学气相沉积法、原子层沉积、雾化-热分解法等；所制备的C0304纳米材料的形貌主要有纳米线、纳米棒、纳米立方、纳米管、纳米带、纳米盘以及具有复合结构的纳米材料；所制备材料的尺寸范围分布很广,从几百纳米到小于10纳米不等。在此基础上,研究者们还开发出C0304复合材料,典型的如Co3O4/C(C=石墨烯,其它碳材料等)、MxCo3-xO4(M=Ni, Zn, Mn等)等材料,以期提高材料的性能。在诸多的报道中,具有吸引力和较高应用价值的材料往往满足如下特性之一：(a)具有特定形貌(如线状、片状)的纳米材料；(b)小尺寸(高比表面积,强量子效应)纳米材料；(c)具有多孔结构的纳米材料；(d)具有独立式(Freestanding)纳米结构的薄膜材料；(e)复合材料。具有以上单一特性的材料已多见诸报道,在此基础上,进一步开发具有多种特性的Co3O4纳米材料是一项艰巨而有意义的工作。另外,随着科技的日益发展,社会在能量存储、催化、环境污染治理、传感器、磁性材料等领域对C0304材料的数量和质量必将有进一步的需求,因此探索新的高产量、低成本、操作简便的制备路径仍然是一项具有挑战性并有前景的工作。
基于电化学方法制备C0304纳米材料具有操作简单、方法灵活、条件温和等优点,因此近些年逐渐成为研究的热点之一。本论文从电化学的基本原理出发,以开发新型Co3O4纳米薄膜材料为主要研究方向,探索基于电化学方法制备具有多种特性的C0304纳米材料的新路径,并对所制备材料的电化学性能进行了研究。本论文的主要研究工作如下：
(1)以金属钻作为反应原材料,通过碱液薄膜法制备出独立式C0304六边形纳米薄膜材料。通过XRD、SEM(?)■TEM手段对材料进行了物理学表征,通过观察进一步证明出纳米片内部具有类似泡沫状的多孔(介孔)结构。在电化学测试中,所制备的C0304材料作为锂离子电池负极材料,表现出较高的储锂容量和良好的循环稳定性；作为电化学传感器,该材料对的H202检测表现出较高的灵敏度。
(2)基于电化学沉积／还原的方法制备了小尺寸独立式C0304纳米片薄膜材料。通过Ranman、XRD、XPS、SEM和TEM等手段对材料进行了物理表征。作为电化学传感器,该材料表现出良好的低浓度H202检测能力,实现了对1μmol L-1浓度的检测；作为催化材料,制备的独立式小尺寸C0304纳米片电极在电化学析氧中表现出良好的催化活性、稳定性以及较高的活性物质利用率。
(3)基于电沉积方法制备了沉积均匀、负载量可控的C0304薄膜,研究了不同负载质量的Co3O4/ITO电极对电化学析氧催化的变化规律。通过EIS技术对电极在Tafel区的电极过程动力学变化规律进行了表征,从而得到了电极活性随C0304活性质量的变化规律。
(4)以阳极氧化的Ti02纳米管(内径～70nm,长度5μm)序列为基体,通过光沉积的方法制备出Co3O4/TiO纳米管薄膜电极复合材料。通过XRD、SEM和TEM等手段对材料进行了物理学表征。在电化学测试中,Co3O4/TiO2纳米管复合材料作为锂离子电池负极材料,表现出较高的储锂容量,并在不同放电电流下表现出良好的循环稳定性。
Among all of the transition metal oxides, Co3O4is an important functional semconductive materials with broad applications in variety of fields such as energy storage, catalysis, sensing, field-emission and electrochromic devices, mainly due to their stable chemical properties and specific magnetic properties, thus developing novel strategies to synthesize advanced Co3O4materials and characterizing their electronic/magnetic properties are of importance.
In past decades with the rapid development of nanotechnologies, various synthetic routes have been developped, including chemical precipitation, solvethermal/hydrothermal, sol-gel, electrochemical, chemical vapor deposition, atom layered deposition and spary-pyrolysis, to design and prepare Co3O4nanoparticles with diverse morphologies, such as nanowires, nanorods, nanotubes, nanosheets, nanobelt, nanodisks and other complicated-structured namomaterials. The size of as-synthesized Co3O4nanoparticles could be controlled at a wide range of distribution, from hundreds nm to a very small size even less than10nm in their dimensions. Besides, synthesis of Co3O4-based compsite materials, such as Co3O4/C(C=graphene or other carbon materials), MxCo3-xO4(M=Ni, Zn, Mn, etc) is also an promising objective in order to improving the performance of products. Among all the products according to literatures, one attactive product wih high application value mainly possesses at least one of the following properties:(a) special and uniform morphology (such as wires, sheeets);(b) small size (high specific surface area and strong quantnum effect);(c) porous inside archetecture;(d) freestanding-structured film materials;(e) compsite materials. The products with just one of the abovementioned properties are commonly seen in literatures, however, one possesses combined properties is less reported. Based on this, synthesis of Co3O4nanoparticles with integrative properties is an arduous and significant work. Additionally, with the development of mordern technology, the society will have a further demand for Co3O4nano-products in energy storage, catalysis, decomposition of contaminations, sensors, magnetic material, either in quantity or in quality, thus developing novel synthetic routes with high yield, low cost, easy operation still to be a challenge and promising objective.
Electrochemical-based strategies for synthesizing Co3O4products have advantages of easy and flexible operation in mild condition, thus have attracted attentions in recent years. Herein we pay more attentions on the synthesis of advanced Co3O4nano-film materials based on electrochemical principles, and developing novel synthetic routes to prepare Co3O4nanomaterials with integrative properties and characterizing the electrochemical performances of products. The main work of the thesis is as follows:
(1) By adopting cobalt metallic layer as reagents, we proposed an alkaline thin film-method to synthesize Co3O4fim electrode. According to XRD, SEM and TEM characterization we found that the film products are composed of freestanding hexagonal nanosheet arrays with foam-like mesoporous inside architecture. In the electrochemical test, the products exhibit high lithium storage capacity and good cycle stability. Besides, the as-made film electrode gives high sensitivity for H2O2sensing.
(2) Small-sized freestanding Co3O4nanosheets have been successfully synthesized on substrates via a novel and simple electrochemical deposition&reduction-based strategy. As an electrochemical sensor, the as fabricated Co3O4/ITO electrode shows much higher than previous reports sensitivity for H2O2detecting, and achieves the detecting ability as low as1μmol L-1H2O2. Besides, in the oxygen evolution test, the as-synthesized Co3O4/ITO electrode could perform an enhanced efficiency for oxygen evolution with high catalytic activity and efficiency, and good durability.
(3) A superfine Co3O4film with controllable loading was obtained through an electrochemical deposition method. Based on this we investigated the catalytic activity of spinel Co3O4for oxygen evolution at different loading density of active materials. A clear tendency curve of catalytic activity versus Co3O4loading was obtained via an Electrochemical Impedance Spectroscopy (EIS) technology in the Tafel region of oxygen evolution reaction.
(4) We developed photo-depsition strategy to synthesize Co3O4/TiO2composite materials by adopting TiO2nanotube (-70nm in inner diameter and5μm in length) array film electrode as substrate. As for lithium storage test, the as-prepared Co3O4/TiO2nanotube composite materials exhibit an improved capacity and cycle durability for lithium storage at different current densities. A further electrochemical characterization indicates that the photo-deposited Co3O4could improve the conductivity of TiO2nanotube.
近几十年来在纳米材料技术迅速发展的基础上,研究者们通过多种制备途径开发出形貌和尺寸多样化的C0304纳米材料,并报道了材料在不同应用领域的性能。所采用的方法主要包括化学沉淀法、水热／溶剂热法、溶胶凝胶法、模板法、电化学沉积法、化学气相沉积法、原子层沉积、雾化-热分解法等；所制备的C0304纳米材料的形貌主要有纳米线、纳米棒、纳米立方、纳米管、纳米带、纳米盘以及具有复合结构的纳米材料；所制备材料的尺寸范围分布很广,从几百纳米到小于10纳米不等。在此基础上,研究者们还开发出C0304复合材料,典型的如Co3O4/C(C=石墨烯,其它碳材料等)、MxCo3-xO4(M=Ni, Zn, Mn等)等材料,以期提高材料的性能。在诸多的报道中,具有吸引力和较高应用价值的材料往往满足如下特性之一：(a)具有特定形貌(如线状、片状)的纳米材料；(b)小尺寸(高比表面积,强量子效应)纳米材料；(c)具有多孔结构的纳米材料；(d)具有独立式(Freestanding)纳米结构的薄膜材料；(e)复合材料。具有以上单一特性的材料已多见诸报道,在此基础上,进一步开发具有多种特性的Co3O4纳米材料是一项艰巨而有意义的工作。另外,随着科技的日益发展,社会在能量存储、催化、环境污染治理、传感器、磁性材料等领域对C0304材料的数量和质量必将有进一步的需求,因此探索新的高产量、低成本、操作简便的制备路径仍然是一项具有挑战性并有前景的工作。
基于电化学方法制备C0304纳米材料具有操作简单、方法灵活、条件温和等优点,因此近些年逐渐成为研究的热点之一。本论文从电化学的基本原理出发,以开发新型Co3O4纳米薄膜材料为主要研究方向,探索基于电化学方法制备具有多种特性的C0304纳米材料的新路径,并对所制备材料的电化学性能进行了研究。本论文的主要研究工作如下：
(1)以金属钻作为反应原材料,通过碱液薄膜法制备出独立式C0304六边形纳米薄膜材料。通过XRD、SEM(?)■TEM手段对材料进行了物理学表征,通过观察进一步证明出纳米片内部具有类似泡沫状的多孔(介孔)结构。在电化学测试中,所制备的C0304材料作为锂离子电池负极材料,表现出较高的储锂容量和良好的循环稳定性；作为电化学传感器,该材料对的H202检测表现出较高的灵敏度。
(2)基于电化学沉积／还原的方法制备了小尺寸独立式C0304纳米片薄膜材料。通过Ranman、XRD、XPS、SEM和TEM等手段对材料进行了物理表征。作为电化学传感器,该材料表现出良好的低浓度H202检测能力,实现了对1μmol L-1浓度的检测；作为催化材料,制备的独立式小尺寸C0304纳米片电极在电化学析氧中表现出良好的催化活性、稳定性以及较高的活性物质利用率。
(3)基于电沉积方法制备了沉积均匀、负载量可控的C0304薄膜,研究了不同负载质量的Co3O4/ITO电极对电化学析氧催化的变化规律。通过EIS技术对电极在Tafel区的电极过程动力学变化规律进行了表征,从而得到了电极活性随C0304活性质量的变化规律。
(4)以阳极氧化的Ti02纳米管(内径～70nm,长度5μm)序列为基体,通过光沉积的方法制备出Co3O4/TiO纳米管薄膜电极复合材料。通过XRD、SEM和TEM等手段对材料进行了物理学表征。在电化学测试中,Co3O4/TiO2纳米管复合材料作为锂离子电池负极材料,表现出较高的储锂容量,并在不同放电电流下表现出良好的循环稳定性。
Among all of the transition metal oxides, Co3O4is an important functional semconductive materials with broad applications in variety of fields such as energy storage, catalysis, sensing, field-emission and electrochromic devices, mainly due to their stable chemical properties and specific magnetic properties, thus developing novel strategies to synthesize advanced Co3O4materials and characterizing their electronic/magnetic properties are of importance.
In past decades with the rapid development of nanotechnologies, various synthetic routes have been developped, including chemical precipitation, solvethermal/hydrothermal, sol-gel, electrochemical, chemical vapor deposition, atom layered deposition and spary-pyrolysis, to design and prepare Co3O4nanoparticles with diverse morphologies, such as nanowires, nanorods, nanotubes, nanosheets, nanobelt, nanodisks and other complicated-structured namomaterials. The size of as-synthesized Co3O4nanoparticles could be controlled at a wide range of distribution, from hundreds nm to a very small size even less than10nm in their dimensions. Besides, synthesis of Co3O4-based compsite materials, such as Co3O4/C(C=graphene or other carbon materials), MxCo3-xO4(M=Ni, Zn, Mn, etc) is also an promising objective in order to improving the performance of products. Among all the products according to literatures, one attactive product wih high application value mainly possesses at least one of the following properties:(a) special and uniform morphology (such as wires, sheeets);(b) small size (high specific surface area and strong quantnum effect);(c) porous inside archetecture;(d) freestanding-structured film materials;(e) compsite materials. The products with just one of the abovementioned properties are commonly seen in literatures, however, one possesses combined properties is less reported. Based on this, synthesis of Co3O4nanoparticles with integrative properties is an arduous and significant work. Additionally, with the development of mordern technology, the society will have a further demand for Co3O4nano-products in energy storage, catalysis, decomposition of contaminations, sensors, magnetic material, either in quantity or in quality, thus developing novel synthetic routes with high yield, low cost, easy operation still to be a challenge and promising objective.
Electrochemical-based strategies for synthesizing Co3O4products have advantages of easy and flexible operation in mild condition, thus have attracted attentions in recent years. Herein we pay more attentions on the synthesis of advanced Co3O4nano-film materials based on electrochemical principles, and developing novel synthetic routes to prepare Co3O4nanomaterials with integrative properties and characterizing the electrochemical performances of products. The main work of the thesis is as follows:
(1) By adopting cobalt metallic layer as reagents, we proposed an alkaline thin film-method to synthesize Co3O4fim electrode. According to XRD, SEM and TEM characterization we found that the film products are composed of freestanding hexagonal nanosheet arrays with foam-like mesoporous inside architecture. In the electrochemical test, the products exhibit high lithium storage capacity and good cycle stability. Besides, the as-made film electrode gives high sensitivity for H2O2sensing.
(2) Small-sized freestanding Co3O4nanosheets have been successfully synthesized on substrates via a novel and simple electrochemical deposition&reduction-based strategy. As an electrochemical sensor, the as fabricated Co3O4/ITO electrode shows much higher than previous reports sensitivity for H2O2detecting, and achieves the detecting ability as low as1μmol L-1H2O2. Besides, in the oxygen evolution test, the as-synthesized Co3O4/ITO electrode could perform an enhanced efficiency for oxygen evolution with high catalytic activity and efficiency, and good durability.
(3) A superfine Co3O4film with controllable loading was obtained through an electrochemical deposition method. Based on this we investigated the catalytic activity of spinel Co3O4for oxygen evolution at different loading density of active materials. A clear tendency curve of catalytic activity versus Co3O4loading was obtained via an Electrochemical Impedance Spectroscopy (EIS) technology in the Tafel region of oxygen evolution reaction.
(4) We developed photo-depsition strategy to synthesize Co3O4/TiO2composite materials by adopting TiO2nanotube (-70nm in inner diameter and5μm in length) array film electrode as substrate. As for lithium storage test, the as-prepared Co3O4/TiO2nanotube composite materials exhibit an improved capacity and cycle durability for lithium storage at different current densities. A further electrochemical characterization indicates that the photo-deposited Co3O4could improve the conductivity of TiO2nanotube.
引文
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