Fe-Mo与其碳复合材料的电化学合成及其应用研究
发布时间：2018-08-26 18:24
【摘要】：多年来,Fe-Mo及其复合材料在冶金行业、工业催化等领域有广泛的应用。近年来,广泛的前沿研究也表明,Fe-Mo及其复合材料具有独特的结构与性质,尤其是在电磁、催化和传感器等方面都具有重要的应用和价值。目前,Fe-Mo材料的制备方法有:溶胶凝胶法,液相共沉淀法,固相反应法等。此中,铁钼催化剂的制备方法在工业上主流的方法有两种:以氯化铁为原料的沉淀法和以硝酸铁为原料的凝胶法。本论文采用双室阳离子膜电解法制备钼酸铁(Fe2(MoO4)3)粉体,对其物理及电催化性能作了相关表征。并探究了钼酸铁粉体与葡萄糖混合锻烧,制备出碳复合的Fe-Mo材料并将其应用在超级电容器方面,测试其电化学性能。论文主要内容:1、采用双室阳离子膜电解槽,电解制备三种形貌的钼酸铁粉体。并使用X-射线衍射技术(XRD)、扫描电子显微镜(SEM)、高分辨透射电镜分析(TEM)、荧光光谱(PL)、比表面积分析(BET)、光电子能谱分析(XPS)等分析手段对产物粉体进行物理化学性能表征。还使用Material Studio软件分别模拟三种形貌钼酸铁的晶体结构。2、采用三电极体系,将三种形貌钼酸铁粉体进行甲醇的电催化性能测试,三种工作电极 Sphere-Fe2(MoO4)3/GCE,Nanorod--Fe2(MoO4)3/GCE 和 Nanotube-Fe2(MoO4)3/GCE在循环伏安曲线正向扫描的峰值电流密度分别为0.75mA/cm2,1.72mA/cm2和3.27mA/cm2,通过峰值电流密度的对比,将三种粉体制备的测试电极进行比较,并且可以得知与铂电极进行对比,Nanotube--Fe2(MoO4)3/GCE电极峰值电流是其 1.1 倍,220 次循环后,Sphere-Fe2(MoO4)3/GCE,Nanorod--Fe2(MoO4)3/GCE 和 Nanotube--Fe2(MoO4)3/GCE 催化活性保持率依次为 91%,92%,88%。3、钼酸铁粉体与葡萄糖混合锻烧,制备出碳复合的Fe-Mo材料,使用X-射线衍射技术(XRD)、扫描电子显微镜(SEM)、高分辨透射电镜分析(TEM)、荧光光谱(PL)、比表面积分析(BET)、光电子能谱分析(XPS)等分析手段对产物粉体进行物理化学性能表征。然后将其应用于超级电容器中,通过CV, GCD、循环性能的测试,2mV/s时,电极在1M的硫酸锂、氢氧化钠、硫酸电解液中,容量分别为380.8F/g,190.2F/g和260.9F/g,5A/g条件下,一万次充放电循环后,在1M的硫酸锂、氢氧化钠、硫酸电解液中容量保持率分别为81.8%, 75.4%和 56.8%。
[Abstract]:For many years, Fe-Mo and its composites have been widely used in metallurgical industry, industrial catalysis and other fields. In recent years, extensive frontier studies have also shown that the Fe-Mo and its composites have unique structures and properties, especially in electromagnetic, catalytic and sensor applications. At present, the preparation methods of Fe-Mo materials include sol-gel method, liquid phase coprecipitation method, solid state reaction method and so on. There are two main methods for the preparation of Fe-Mo catalyst in industry: precipitation with ferric chloride as raw material and gel method with ferric nitrate as raw material. Iron molybdate (Fe2 (MoO4) 3) powders were prepared by double chamber cationic membrane electrolysis, and their physical and electrocatalytic properties were characterized. The carbon composite Fe-Mo material was prepared by calcination of ferric molybdate powder and glucose, and was applied to supercapacitors to test its electrochemical properties. In this paper, three kinds of ferromolybdate powders with different morphologies were prepared by electrolysis in a two-chamber cationic membrane electrolytic cell. The physical and chemical properties of the powders were characterized by means of X-ray diffraction (XRD),) scanning electron microscope (XRD), high resolution transmission electron microscopy (SEM), specific surface area analysis (PL), specific surface area analysis (BET), photoelectron spectroscopy (XPS), etc. The crystal structure of ferric molybdate with three morphologies was simulated by Material Studio software, and the electrocatalytic properties of methanol were tested by using the three-electrode system. The peak current density of Sphere-Fe2 (MoO4) 3 / GCEO Nanorod-Fe _ 2 (MoO4) 3/GCE and Nanotube-Fe2 (MoO4) 3/GCE in the forward scanning of cyclic voltammetry curves were 0.75 Ma / cm ~ (2) 路cm ~ (2) and 3.27 Ma / 路cm ~ (2) respectively. By comparing the peak current density, the test electrodes prepared by the three kinds of powders were compared. It was also found that the peak current of Nanotube-Fe _ 2 (MoO4) 3/GCE electrode was 1.1 times higher than that of platinum electrode. After 220 cycles, Sphere-Fe2 (MoO4) _ 3 / GCEOD-Fe _ 2 (MoO4) 3/GCE (MoO4) and Nanotube--Fe2 (MoO4) 3/GCE kept the catalytic activity of 92288.3The Fe _ (2) molybdate powder was calcined with glucose, and the carbon composite Fe-Mo material was prepared. X-ray diffraction (XRD) technique (XRD), scanning electron microscope (XRD),) high resolution transmission electron microscopy (SEM),) was used to characterize the physical and chemical properties of the product by means of (TEM), fluorescence spectrum (PL), specific surface area analysis (BET), photoelectron spectrum analysis (XPS) etc. Then it was applied to supercapacitors. When the CV, GCD, cycle performance was measured by 2mV / s, the electrode capacity was 380.8F / g, 190.2F / g and 260.9F / g / g in 1m lithium sulfate, sodium hydroxide and sulfuric acid electrolyte, respectively, after 10,000 charge-discharge cycles. The capacity retention rates of lithium sulfate, sodium hydroxide and sulphuric acid electrolyte at 1m were 81.8%, 75.4% and 56.8%, respectively.
【学位授予单位】：上海应用技术大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TB33;TM53
本文编号：2205773
[Abstract]:For many years, Fe-Mo and its composites have been widely used in metallurgical industry, industrial catalysis and other fields. In recent years, extensive frontier studies have also shown that the Fe-Mo and its composites have unique structures and properties, especially in electromagnetic, catalytic and sensor applications. At present, the preparation methods of Fe-Mo materials include sol-gel method, liquid phase coprecipitation method, solid state reaction method and so on. There are two main methods for the preparation of Fe-Mo catalyst in industry: precipitation with ferric chloride as raw material and gel method with ferric nitrate as raw material. Iron molybdate (Fe2 (MoO4) 3) powders were prepared by double chamber cationic membrane electrolysis, and their physical and electrocatalytic properties were characterized. The carbon composite Fe-Mo material was prepared by calcination of ferric molybdate powder and glucose, and was applied to supercapacitors to test its electrochemical properties. In this paper, three kinds of ferromolybdate powders with different morphologies were prepared by electrolysis in a two-chamber cationic membrane electrolytic cell. The physical and chemical properties of the powders were characterized by means of X-ray diffraction (XRD),) scanning electron microscope (XRD), high resolution transmission electron microscopy (SEM), specific surface area analysis (PL), specific surface area analysis (BET), photoelectron spectroscopy (XPS), etc. The crystal structure of ferric molybdate with three morphologies was simulated by Material Studio software, and the electrocatalytic properties of methanol were tested by using the three-electrode system. The peak current density of Sphere-Fe2 (MoO4) 3 / GCEO Nanorod-Fe _ 2 (MoO4) 3/GCE and Nanotube-Fe2 (MoO4) 3/GCE in the forward scanning of cyclic voltammetry curves were 0.75 Ma / cm ~ (2) 路cm ~ (2) and 3.27 Ma / 路cm ~ (2) respectively. By comparing the peak current density, the test electrodes prepared by the three kinds of powders were compared. It was also found that the peak current of Nanotube-Fe _ 2 (MoO4) 3/GCE electrode was 1.1 times higher than that of platinum electrode. After 220 cycles, Sphere-Fe2 (MoO4) _ 3 / GCEOD-Fe _ 2 (MoO4) 3/GCE (MoO4) and Nanotube--Fe2 (MoO4) 3/GCE kept the catalytic activity of 92288.3The Fe _ (2) molybdate powder was calcined with glucose, and the carbon composite Fe-Mo material was prepared. X-ray diffraction (XRD) technique (XRD), scanning electron microscope (XRD),) high resolution transmission electron microscopy (SEM),) was used to characterize the physical and chemical properties of the product by means of (TEM), fluorescence spectrum (PL), specific surface area analysis (BET), photoelectron spectrum analysis (XPS) etc. Then it was applied to supercapacitors. When the CV, GCD, cycle performance was measured by 2mV / s, the electrode capacity was 380.8F / g, 190.2F / g and 260.9F / g / g in 1m lithium sulfate, sodium hydroxide and sulfuric acid electrolyte, respectively, after 10,000 charge-discharge cycles. The capacity retention rates of lithium sulfate, sodium hydroxide and sulphuric acid electrolyte at 1m were 81.8%, 75.4% and 56.8%, respectively.
【学位授予单位】：上海应用技术大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TB33;TM53
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