【摘要】：多年來,Fe-Mo及其復(fù)合材料在冶金行業(yè)、工業(yè)催化等領(lǐng)域有廣泛的應(yīng)用。近年來,廣泛的前沿研究也表明,Fe-Mo及其復(fù)合材料具有獨(dú)特的結(jié)構(gòu)與性質(zhì),尤其是在電磁、催化和傳感器等方面都具有重要的應(yīng)用和價(jià)值。目前,Fe-Mo材料的制備方法有:溶膠凝膠法,液相共沉淀法,固相反應(yīng)法等。此中,鐵鉬催化劑的制備方法在工業(yè)上主流的方法有兩種:以氯化鐵為原料的沉淀法和以硝酸鐵為原料的凝膠法。本論文采用雙室陽(yáng)離子膜電解法制備鉬酸鐵(Fe2(MoO4)3)粉體,對(duì)其物理及電催化性能作了相關(guān)表征。并探究了鉬酸鐵粉體與葡萄糖混合鍛燒,制備出碳復(fù)合的Fe-Mo材料并將其應(yīng)用在超級(jí)電容器方面,測(cè)試其電化學(xué)性能。論文主要內(nèi)容:1、采用雙室陽(yáng)離子膜電解槽,電解制備三種形貌的鉬酸鐵粉體。并使用X-射線衍射技術(shù)(XRD)、掃描電子顯微鏡(SEM)、高分辨透射電鏡分析(TEM)、熒光光譜(PL)、比表面積分析(BET)、光電子能譜分析(XPS)等分析手段對(duì)產(chǎn)物粉體進(jìn)行物理化學(xué)性能表征。還使用Material Studio軟件分別模擬三種形貌鉬酸鐵的晶體結(jié)構(gòu)。2、采用三電極體系,將三種形貌鉬酸鐵粉體進(jìn)行甲醇的電催化性能測(cè)試,三種工作電極 Sphere-Fe2(MoO4)3/GCE,Nanorod--Fe2(MoO4)3/GCE 和 Nanotube-Fe2(MoO4)3/GCE在循環(huán)伏安曲線正向掃描的峰值電流密度分別為0.75mA/cm2,1.72mA/cm2和3.27mA/cm2,通過峰值電流密度的對(duì)比,將三種粉體制備的測(cè)試電極進(jìn)行比較,并且可以得知與鉑電極進(jìn)行對(duì)比,Nanotube--Fe2(MoO4)3/GCE電極峰值電流是其 1.1 倍,220 次循環(huán)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為 91%,92%,88%。3、鉬酸鐵粉體與葡萄糖混合鍛燒,制備出碳復(fù)合的Fe-Mo材料,使用X-射線衍射技術(shù)(XRD)、掃描電子顯微鏡(SEM)、高分辨透射電鏡分析(TEM)、熒光光譜(PL)、比表面積分析(BET)、光電子能譜分析(XPS)等分析手段對(duì)產(chǎn)物粉體進(jìn)行物理化學(xué)性能表征。然后將其應(yīng)用于超級(jí)電容器中,通過CV, GCD、循環(huán)性能的測(cè)試,2mV/s時(shí),電極在1M的硫酸鋰、氫氧化鈉、硫酸電解液中,容量分別為380.8F/g,190.2F/g和260.9F/g,5A/g條件下,一萬次充放電循環(huán)后,在1M的硫酸鋰、氫氧化鈉、硫酸電解液中容量保持率分別為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.
【學(xué)位授予單位】：上海應(yīng)用技術(shù)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：TB33;TM53

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