氮摻雜石墨烯負(fù)載鈷系金屬氧化物的制備及其超級(jí)電容器電極性能研究
發(fā)布時(shí)間：2018-08-01 15:37
【摘要】：目前人類(lèi)社會(huì)在能源與發(fā)展方面面臨日漸尖銳的挑戰(zhàn),尋找一種清潔高效能源和存儲(chǔ)能源材料的需求越發(fā)急迫。超級(jí)電容器因與普通電容器、傳統(tǒng)電池相比在放電時(shí)間、放電電流、使用壽命以及環(huán)境保護(hù)方面更有優(yōu)勢(shì)而備受關(guān)注。在各種金屬氧化物中,成本更加低廉、儲(chǔ)量更加豐富、環(huán)境更加友好、毒害更加輕微的四氧化三鈷及鈷酸鎳成為了研究的重點(diǎn)。然而金屬氧化物導(dǎo)電能力差、易團(tuán)聚、與電解液接觸界面面積小等不足制約著其在電容器實(shí)際應(yīng)用方面的前景。石墨烯是碳原子以sp2雜化排列形成的一種二維蜂窩狀碳材料,具有更高的強(qiáng)度、極佳的導(dǎo)電性以及超大的比表面積。石墨烯具有極佳的化學(xué)穩(wěn)定性并且在力學(xué)、光學(xué)、熱力學(xué)、電化學(xué)等領(lǐng)域應(yīng)用前景廣闊。研究者為了進(jìn)一步研究和發(fā)掘石墨烯的潛能在其表面進(jìn)行摻雜引入異種元素以此來(lái)合成新的石墨烯基材料。氮摻雜石墨烯在保持石墨烯原有結(jié)構(gòu)的前提下能夠修復(fù)部分石墨烯的結(jié)構(gòu)缺陷,從而增加石墨烯表面的活性位點(diǎn),增強(qiáng)石墨烯的儲(chǔ)電能力。將金屬氧化物與氮摻雜石墨烯復(fù)合不僅可以發(fā)揮各自的性能優(yōu)勢(shì),還可以產(chǎn)生電子轉(zhuǎn)移協(xié)同效應(yīng),進(jìn)一步增強(qiáng)復(fù)合材料的電容器性質(zhì)。所以研發(fā)出性能可靠的超級(jí)電容器材料具有重要的研究意義和實(shí)用價(jià)值。本文的主要內(nèi)容如下:1.以聚丙烯酰胺(PAM)為表面活性劑,通過(guò)微波-煅燒法制備得到Co_3O_4納米粒子氮摻雜石墨烯復(fù)合物。利用XRD、FTIR、Raman、TEM、XPS、ICP、電化學(xué)工作站測(cè)試等方法對(duì)Co_3O_4/NG復(fù)合物的結(jié)構(gòu)、形貌和電化學(xué)性能進(jìn)行表征。實(shí)驗(yàn)結(jié)果表明,在950 W功率下微波加熱15 min后將產(chǎn)物在750℃下煅燒3 h,Co_3O_4納米粒子能夠均勻的分散在氮摻雜石墨烯表面,在1 A g-1的電流密度下測(cè)得的比電容為1288.2 F g-1。Co_3O_4/NG復(fù)合物優(yōu)良的電化學(xué)活性主要?dú)w因于Co_3O_4納米顆粒與氮摻雜石墨烯之間的協(xié)同作用。2.以六亞甲基四胺(HMT)、尿素(Urea)為堿源,通過(guò)水熱-煅燒法制備的到NiCo_2O_4納米管氮摻雜石墨烯復(fù)合物。利用XRD、TGA、FTIR、Raman、TEM、XPS、ICP、電化學(xué)工作站測(cè)試等方法對(duì)NiCo_2O_4/NG復(fù)合物的結(jié)構(gòu)、形貌和電化學(xué)性能進(jìn)行表征。實(shí)驗(yàn)結(jié)果表明,以六亞甲基四胺作為堿源,在180℃下水熱24 h后將產(chǎn)物在350℃下煅燒3 h,形成管徑均一的NiCo_2O_4晶體沉積在氮摻雜石墨烯表面,在1 A g-1的電流密度下測(cè)得的比電容為2147.4 F g-1。NiCo_2O_4/NG復(fù)合物出色的電容性能歸因于NiCo_2O_4納米管與氮摻雜石墨烯活性位點(diǎn)之間的協(xié)同效應(yīng),還得益于三維空間介孔結(jié)構(gòu)的NiCo_2O_4納米管晶體能夠極大的增加金屬氧化物與電解液的接觸面積,從而展現(xiàn)出更加優(yōu)良的電容性能。3.以六亞甲基四胺作為堿源、聚丙烯酰胺作為表面活性劑,通過(guò)水熱-煅燒法制備得到雙金屬?gòu)?fù)合的Co_3O_4@NiCo_2O_4納米粒子氮摻雜石墨烯復(fù)合物。通過(guò)XRD、Raman、FTIR、ICP、TEM、XPS、電化學(xué)測(cè)試等方法對(duì)Co_3O_4@NiCo_2O_4/NG復(fù)合物的形貌結(jié)構(gòu)以及電化學(xué)性能進(jìn)行表征。實(shí)驗(yàn)結(jié)果表明,適量的六亞甲基四胺和少量的聚丙烯酰胺表面活性劑有利于三明治形狀的雙金屬氮摻雜石墨烯復(fù)合物,在180℃下水熱24 h后將產(chǎn)物在350℃下煅燒3 h,形成片狀的NiCo_2O_4晶體表面生長(zhǎng)有Co_3O_4納米顆粒并與氮摻雜石墨烯復(fù)合形成三明治狀的空間結(jié)構(gòu),在1 A g-1的電流密度下測(cè)得的比電容為2387.5 F g-1。Co_3O_4@NiCo_2O_4/NG復(fù)合物的卓越性能得益于三明治狀的特殊三維空間結(jié)構(gòu)和金屬氧化物與氮摻雜石墨烯間的進(jìn)一步電子協(xié)同作用。
[Abstract]:At present, human society is facing an increasingly acute challenge in energy and development. It is more and more urgent to find a clean and efficient energy and energy storage material. Supercapacitor is concerned about the advantages of discharge time, discharge current, service life and environmental protection compared with conventional capacitors and traditional batteries. In the metal oxides, the cost is lower, the reserves are more abundant, the environment is more friendly, and the toxicity of the four oxidation of cobalt and nickel cobalt oxide is the focus of the study. However, the poor conductivity of the metal oxide, the easy reunion and the small contact interface with the electrolyte restrict its application in the practical application of the capacitor. A two-dimensional honeycomb carbon material formed by SP2 hybrid arrangement of carbon atoms, with higher strength, excellent conductivity and large specific surface area. Graphene has excellent chemical stability and is widely used in the fields of mechanics, optics, thermodynamics and electrochemistry. In order to further study and explore graphene The potential on its surface is doped with heterologous elements to synthesize new graphene based materials. Nitrogen doped graphene can repair the structural defects of some graphene on the premise of maintaining the original structure of graphene, thus increasing the active site of the graphene surface, enhancing the power storage capacity of graphene, and doping metal oxide and nitrogen. Graphene composite can not only give play to its own performance advantages, but also produce the synergistic effect of electron transfer, and further enhance the properties of the capacitor of the composite. Therefore, it is of great significance and practical value to develop a reliable supercapacitor material. The main contents of this paper are as follows: 1. the surface of polyacrylamide (PAM) is the surface. Co_3O_4 nanoparticle nitrogen doped graphene complex was prepared by microwave calcination. The structure, morphology and electrochemical properties of the Co_3O_4/NG complex were characterized by XRD, FTIR, Raman, TEM, XPS, ICP, and electrochemical workstation testing. The experimental results showed that the product was 750 after microwave heating of 15 min at 950 W power. Calcined 3 h at C, Co_3O_4 nanoparticles can be dispersed uniformly on the surface of nitrogen doped graphene. The excellent electrochemical activity of the specific capacitance of 1288.2 F g-1.Co_3O_4/NG complexes under the current density of 1 A g-1 is mainly attributed to the synergistic effect of Co_3O_4 nanoparticles and nitrogen doped graphene,.2. with six methylene four amine (HMT), and urine. XRD, TGA, FTIR, Raman, TEM, XPS, ICP, and electrochemical workstations were tested by XRD, TGA, FTIR, Raman, TEM, XPS, ICP, and electrochemical workstations. The experimental results showed that six methylene four amine was used as the base source, and 180 was used as the base source. After 24 h, the product was calcined at 350 centigrade for 3 h, and the uniform diameter of the NiCo_2O_4 crystal was deposited on the surface of nitrogen doped graphene. The excellent capacitance of the specific capacitance of 2147.4 F g-1.NiCo_2O_4/NG under the current density of 1 A g-1 was attributed to the synergy between the NiCo_2O_4 nanotubes and the active site of nitrogen doped graphene. The effect, also benefited from the NiCo_2O_4 nanotube crystal in the three-dimensional mesoporous structure, can greatly increase the contact area of the metal oxide and the electrolyte, thus showing a better capacitive performance.3. with six methylene four amine as the base source and the polyacrylamide as the surfactant to prepare the bimetallic composite by the hydrothermal calcination method. The morphology and electrochemical properties of the Co_3O_4@NiCo_2O_4/NG complex were characterized by XRD, Raman, FTIR, ICP, TEM, XPS, electrochemical testing and other methods. The results showed that a proper amount of six methylene four amines and a small amount of polyacrylamide surfactants were beneficial to three. The Meiji form of bimetallic doped graphene complex, after 24 h water heat at 180 C, calcined the product at 3 h at 350 C, formed a sheet like NiCo_2O_4 crystal with Co_3O_4 nanoparticles and formed a sandwich space structure with nitrogen doped graphene, and the specific capacitance measured at 1 A g-1 was 2387.5 F g-1.C. The excellent performance of the o_3O_4@NiCo_2O_4/NG complex is attributed to the sandwich shaped special three-dimensional space structure and the further electronic synergy between the metal oxide and the nitrogen doped graphene.
【學(xué)位授予單位】：江蘇大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類(lèi)號(hào)】：TB332;TM53
本文編號(hào)：2158039
[Abstract]:At present, human society is facing an increasingly acute challenge in energy and development. It is more and more urgent to find a clean and efficient energy and energy storage material. Supercapacitor is concerned about the advantages of discharge time, discharge current, service life and environmental protection compared with conventional capacitors and traditional batteries. In the metal oxides, the cost is lower, the reserves are more abundant, the environment is more friendly, and the toxicity of the four oxidation of cobalt and nickel cobalt oxide is the focus of the study. However, the poor conductivity of the metal oxide, the easy reunion and the small contact interface with the electrolyte restrict its application in the practical application of the capacitor. A two-dimensional honeycomb carbon material formed by SP2 hybrid arrangement of carbon atoms, with higher strength, excellent conductivity and large specific surface area. Graphene has excellent chemical stability and is widely used in the fields of mechanics, optics, thermodynamics and electrochemistry. In order to further study and explore graphene The potential on its surface is doped with heterologous elements to synthesize new graphene based materials. Nitrogen doped graphene can repair the structural defects of some graphene on the premise of maintaining the original structure of graphene, thus increasing the active site of the graphene surface, enhancing the power storage capacity of graphene, and doping metal oxide and nitrogen. Graphene composite can not only give play to its own performance advantages, but also produce the synergistic effect of electron transfer, and further enhance the properties of the capacitor of the composite. Therefore, it is of great significance and practical value to develop a reliable supercapacitor material. The main contents of this paper are as follows: 1. the surface of polyacrylamide (PAM) is the surface. Co_3O_4 nanoparticle nitrogen doped graphene complex was prepared by microwave calcination. The structure, morphology and electrochemical properties of the Co_3O_4/NG complex were characterized by XRD, FTIR, Raman, TEM, XPS, ICP, and electrochemical workstation testing. The experimental results showed that the product was 750 after microwave heating of 15 min at 950 W power. Calcined 3 h at C, Co_3O_4 nanoparticles can be dispersed uniformly on the surface of nitrogen doped graphene. The excellent electrochemical activity of the specific capacitance of 1288.2 F g-1.Co_3O_4/NG complexes under the current density of 1 A g-1 is mainly attributed to the synergistic effect of Co_3O_4 nanoparticles and nitrogen doped graphene,.2. with six methylene four amine (HMT), and urine. XRD, TGA, FTIR, Raman, TEM, XPS, ICP, and electrochemical workstations were tested by XRD, TGA, FTIR, Raman, TEM, XPS, ICP, and electrochemical workstations. The experimental results showed that six methylene four amine was used as the base source, and 180 was used as the base source. After 24 h, the product was calcined at 350 centigrade for 3 h, and the uniform diameter of the NiCo_2O_4 crystal was deposited on the surface of nitrogen doped graphene. The excellent capacitance of the specific capacitance of 2147.4 F g-1.NiCo_2O_4/NG under the current density of 1 A g-1 was attributed to the synergy between the NiCo_2O_4 nanotubes and the active site of nitrogen doped graphene. The effect, also benefited from the NiCo_2O_4 nanotube crystal in the three-dimensional mesoporous structure, can greatly increase the contact area of the metal oxide and the electrolyte, thus showing a better capacitive performance.3. with six methylene four amine as the base source and the polyacrylamide as the surfactant to prepare the bimetallic composite by the hydrothermal calcination method. The morphology and electrochemical properties of the Co_3O_4@NiCo_2O_4/NG complex were characterized by XRD, Raman, FTIR, ICP, TEM, XPS, electrochemical testing and other methods. The results showed that a proper amount of six methylene four amines and a small amount of polyacrylamide surfactants were beneficial to three. The Meiji form of bimetallic doped graphene complex, after 24 h water heat at 180 C, calcined the product at 3 h at 350 C, formed a sheet like NiCo_2O_4 crystal with Co_3O_4 nanoparticles and formed a sandwich space structure with nitrogen doped graphene, and the specific capacitance measured at 1 A g-1 was 2387.5 F g-1.C. The excellent performance of the o_3O_4@NiCo_2O_4/NG complex is attributed to the sandwich shaped special three-dimensional space structure and the further electronic synergy between the metal oxide and the nitrogen doped graphene.
【學(xué)位授予單位】：江蘇大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類(lèi)號(hào)】：TB332;TM53
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