水热合成法制备泡沫镍载过渡金属（Mn、Co、Cu）氧化物及其电化学性能研究
发布时间：2019-03-02 07:38
【摘要】：电化学电容器(ECs),作为一种新型的能量存储转化装置,集高功率密度、长循环寿命、可以快速充放电及绿色环保等众优点于一身,拥有非常广泛的应用领域。电极材料作为核心部件之一对电化学电容器的性能具有重要的影响。目前,电化学电容器的电极材料可以分为三大类:碳材料,金属氧化物材料和导电聚合物材料。本论文采用水热合成法制备了锰掺杂钴氧化物材料Mn-Co-O(Mn0.63Co2.37O4)和 CuxO/Cu(1x2)复合材料,并在 CuxO/Cu(1x2)的基础上经煅烧得到了 CuO材料,并将其作为电化学电容器电极材料进行电化学性能研究。本论文采用SEM、TEM、XRD、XPS、EDS对所制备的材料进行物相分析,利用循环伏安、交流阻抗、恒电流充放电对电极物质进行了电化学性能测试。本论文以不同比例(10:10、10:8、10:6、10:4、10:2和10:0)的锰源与钴源为原料通过水热合成法制备Mn-Co-O电极材料,并从中选出最佳的比例。实验数据表明,当锰源与钴源的加入比为1:1时,所制备的电极材料为锰掺杂钴氧化物纳米材料,其中摩尔比Mn:Co=1:3.8,并且呈现出了相互交织的一维纳米线状结构,具有较高的电化学性能和电化学稳定性。当充放电电流密度为j=2.38A/g时,首次放电比容量为580 F/g,经过10次充放电之后,放电比容量升高至611 F/g,经过500次充放电后,容量保持率高达99%,电极材料表现出了较好的电化学性能和较高的循环稳定性。本论文通过水热合成法,以泡沫镍作为基体,通过调节反应时间(8 h、11 h、14 h和17 h)来制备出具有较高的电化学性能的CuxO/Cu(1x2)复合材料。实验数据表明,当反应时间为14 h时所制备的复合材料为Cu20/CuO/Cu复合材料(为了简便起见,以下Cu20/CuO用CuxO代替),其含量比为CuxO:Cu = 83:17,呈现出了立方体形貌,具有较高的电化学性能和电化学稳定性。当充放电电流密度为j=2.5 A/g时,放电比电容最高可达610 F/g,经过500次恒流充放电后,比电容衰减至520 F/g,容量保持率仅有85%,经分析该电极的容量衰减主要是由电极活性物质的溶解及脱落引起的。在得到的CuxO/Cu(1x2)的基础上,通过不同的煅烧温度(200℃、300℃和400℃)煅烧240 min来得到CuO半导体材料。实验数据表明,当煅烧温度为200℃和300℃时会得到纯净的CuO材料,并且200℃煅烧得到的CuO材料表现出了优于300℃得到的CuO材料的电化学性能。实验表明,在电流密度为2.13 A/g时CuO电极的放电比电容仅为198 F/g,经过550次循环寿命测试发现其比电容最高可达213 F/g,最终维持在186 F/g左右,容量保持率为94%。经分析容量的衰减主要是由电极活性物质的溶解及脱落引起的。
[Abstract]:As a new type of energy storage and conversion device, electrochemical capacitor (ECs), has many advantages, such as high power density, long cycle life, fast charge / discharge and environmental protection. It has a wide range of applications. As one of the core components, electrode materials play an important role in the performance of electrochemical capacitors. At present, the electrode materials of electrochemical capacitors can be divided into three categories: carbon materials, metal oxide materials and conductive polymer materials. In this paper, mn-doped cobalt oxide materials Mn-Co-O (Mn0.63Co2.37O4) and CuxO/Cu (1x2) composites were prepared by hydrothermal synthesis and calcined on the basis of CuxO/Cu (1x2) to obtain CuO materials. It is used as electrode material of electrochemical capacitor to study its electrochemical performance. In this paper, the phase analysis of the prepared materials was carried out by SEM,TEM,XRD,XPS,EDS. The electrochemical properties of the electrode materials were tested by cyclic voltammetry, AC impedance and constant current charge / discharge. In this paper, Mn-Co-O electrode materials were prepared by hydrothermal synthesis from manganese and cobalt sources with different ratios (10 ~ 10, 10 ~ 8, 10 ~ (6) 6, 10 ~ (4), 10 ~ (2) and 10:0), from which the optimum proportion was selected. The experimental data show that when the addition ratio of manganese source to cobalt source is 1: 1, the electrode material prepared is mn-doped cobalt oxide nano-material, in which the molar ratio of Mn:Co=1:3.8, is one-dimensional nanowire structure, and the structure of the electrode is interlaced with one-dimensional nanowires. It has high electrochemical performance and electrochemical stability. When the current density of charge and discharge is j=2.38A/g, the specific discharge capacity of the first discharge is 580F / g. After 10 charge and discharge, the specific capacity of discharge is increased to 611F / g. After 500 charge and discharge, the capacity retention rate is as high as 99%. The electrode material exhibits good electrochemical performance and high cycle stability. In this paper, CuxO/Cu (1x2) composites with high electrochemical performance were prepared by hydrothermal synthesis using nickel foam as matrix and adjusting the reaction time (8 h, 11 h, 14 h and 17 h). The experimental data show that when the reaction time is 14 h, the composites are Cu20/CuO/Cu composites (for simplicity, the following Cu20/CuO is replaced by CuxO), and the content ratio of the composites is CuxO:Cu = 83 / 17, showing cubic morphology. It has high electrochemical performance and electrochemical stability. When the current density of charge and discharge is about 2.5 A / g, the specific capacitance of discharge can reach 610 F / g, and after 500 times of constant current charge and discharge, the specific capacitance decreases to 520 F / g, and the capacity retention rate is only 85%. The capacity attenuation of the electrode is mainly caused by the dissolution and shedding of the electrode active material. Based on the obtained CuxO/Cu (1x2), CuO semiconductor materials were obtained by calcining at different temperatures (200 鈩，
本文编号：2432841
[Abstract]:As a new type of energy storage and conversion device, electrochemical capacitor (ECs), has many advantages, such as high power density, long cycle life, fast charge / discharge and environmental protection. It has a wide range of applications. As one of the core components, electrode materials play an important role in the performance of electrochemical capacitors. At present, the electrode materials of electrochemical capacitors can be divided into three categories: carbon materials, metal oxide materials and conductive polymer materials. In this paper, mn-doped cobalt oxide materials Mn-Co-O (Mn0.63Co2.37O4) and CuxO/Cu (1x2) composites were prepared by hydrothermal synthesis and calcined on the basis of CuxO/Cu (1x2) to obtain CuO materials. It is used as electrode material of electrochemical capacitor to study its electrochemical performance. In this paper, the phase analysis of the prepared materials was carried out by SEM,TEM,XRD,XPS,EDS. The electrochemical properties of the electrode materials were tested by cyclic voltammetry, AC impedance and constant current charge / discharge. In this paper, Mn-Co-O electrode materials were prepared by hydrothermal synthesis from manganese and cobalt sources with different ratios (10 ~ 10, 10 ~ 8, 10 ~ (6) 6, 10 ~ (4), 10 ~ (2) and 10:0), from which the optimum proportion was selected. The experimental data show that when the addition ratio of manganese source to cobalt source is 1: 1, the electrode material prepared is mn-doped cobalt oxide nano-material, in which the molar ratio of Mn:Co=1:3.8, is one-dimensional nanowire structure, and the structure of the electrode is interlaced with one-dimensional nanowires. It has high electrochemical performance and electrochemical stability. When the current density of charge and discharge is j=2.38A/g, the specific discharge capacity of the first discharge is 580F / g. After 10 charge and discharge, the specific capacity of discharge is increased to 611F / g. After 500 charge and discharge, the capacity retention rate is as high as 99%. The electrode material exhibits good electrochemical performance and high cycle stability. In this paper, CuxO/Cu (1x2) composites with high electrochemical performance were prepared by hydrothermal synthesis using nickel foam as matrix and adjusting the reaction time (8 h, 11 h, 14 h and 17 h). The experimental data show that when the reaction time is 14 h, the composites are Cu20/CuO/Cu composites (for simplicity, the following Cu20/CuO is replaced by CuxO), and the content ratio of the composites is CuxO:Cu = 83 / 17, showing cubic morphology. It has high electrochemical performance and electrochemical stability. When the current density of charge and discharge is about 2.5 A / g, the specific capacitance of discharge can reach 610 F / g, and after 500 times of constant current charge and discharge, the specific capacitance decreases to 520 F / g, and the capacity retention rate is only 85%. The capacity attenuation of the electrode is mainly caused by the dissolution and shedding of the electrode active material. Based on the obtained CuxO/Cu (1x2), CuO semiconductor materials were obtained by calcining at different temperatures (200 鈩，
本文编号：2432841
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