本文選題：超級(jí)電容器　切入點(diǎn)：氧化鎳　出處：《濟(jì)南大學(xué)》2014年碩士論文　論文類型：學(xué)位論文

【摘要】：隨著全球的能源缺乏和環(huán)境惡化，各種可循環(huán)的電化學(xué)儲(chǔ)能器件愈來(lái)愈受到人們的重視。作為新式能量?jī)?chǔ)存器件的超級(jí)電容器，由于其具有高的功率密度無(wú)污染、循環(huán)時(shí)長(zhǎng)等優(yōu)點(diǎn)，因而受到廣泛關(guān)注與研究。而其性能高低關(guān)鍵在于電極材料的選擇。鑒于金屬氧化物和碳材料作為電極材料的優(yōu)缺點(diǎn)，將金屬氧化物與泡沫鎳集流體、碳材料進(jìn)行負(fù)載制備性能良好的復(fù)合電極材料成為材料研究學(xué)者的首要目標(biāo)。 本論文采用微波水熱法，，圍繞納米氧化鎳的制備以及采用泡沫鎳或活性碳纖維布為載體負(fù)載納米氧化鎳以獲取具有微納米結(jié)構(gòu)的復(fù)合材料的相關(guān)問(wèn)題展開(kāi)研究，采用X射線衍射儀、熱分析、掃描電子顯微鏡等測(cè)試技術(shù)對(duì)材料的結(jié)構(gòu)與形貌進(jìn)行表征與觀察，并通過(guò)循環(huán)伏安法、交流阻抗法對(duì)所制備電極材料的電化學(xué)性能進(jìn)行測(cè)試。主要工作包括以下幾個(gè)方面： 采用微波水熱法，以NiSO4為鎳源，尿素為沉淀劑，分別選用聚乙二醇4000（PEG-4000）和聚醚酰亞胺（PEI)為表面活性劑，通過(guò)改變保溫時(shí)間、表面活性劑種類及添加量合成NiO納米粉體。結(jié)果表明：在微波加熱160℃合成了片狀納米NiO前驅(qū)體，片層厚度約為10nm，經(jīng)過(guò)400℃煅燒2h得到了具有微納米多級(jí)結(jié)構(gòu)的花片狀NiO微球，微球直徑約為2μm，花片狀NiO的厚度為10nm。表面活性劑的添加使NiO微球團(tuán)聚現(xiàn)象明顯減弱，且使微球形狀規(guī)則，尺寸均一。通過(guò)電化學(xué)測(cè)試表明，添加3.7%PEG-4000，保溫30min條件下制備納米NiO電極比電容最大為85.4F/g，經(jīng)過(guò)500次循環(huán)后，比電容僅衰減13.3%，表現(xiàn)出較好的電化學(xué)穩(wěn)定性。 以泡沫鎳為載體，分別以NiSO4和Ni(NO3)2·6H2O為鎳源，通過(guò)改變鎳離子濃度、表面活性劑種類和添加量、反應(yīng)時(shí)間，采用微波水熱原位負(fù)載的方法制備具有微納米多級(jí)結(jié)構(gòu)的NiO/泡沫鎳復(fù)合電極材料樣品。結(jié)果表明：以NiSO4為鎳源合成的納米NiO以花片狀均勻原位生長(zhǎng)在泡沫鎳表面，表面活性劑PEG-4000的添加反而抑制了片狀納米NiO在泡沫鎳上的生長(zhǎng)。測(cè)試結(jié)果表明，保溫30min，無(wú)添加劑條件制備的微納米多級(jí)結(jié)構(gòu)的NiO/泡沫鎳樣品電極獲得的比電容可達(dá)到234.8F/g。以Ni(NO3)2·6H2O為鎳源，保溫60min合成了顆粒狀納米NiO并在泡沫鎳表面均勻生長(zhǎng)，表面活性劑PEG-4000的添加使納米NiO貼附在泡沫鎳表面，不利于離子和電子的傳遞。保溫60min且無(wú)添加劑制備的NiO/泡沫鎳樣品電極比電容最大為224.4F/g。 以活性碳纖維布（ACFC）為載體，以尿素和NiSO4為原料，采用微波水熱法通過(guò)改變反應(yīng)物濃度和反應(yīng)時(shí)間得到不同的NiO/ACFC復(fù)合電極材料，并對(duì)樣品電極進(jìn)行了電化學(xué)特性研究。結(jié)果表明：實(shí)驗(yàn)合成的納米NiO以花片狀結(jié)構(gòu)原位生長(zhǎng)在活性碳纖維布表面，片層厚度約為10nm。在相同的微波合成條件下，表面活性劑PEI添加量和尿素量對(duì)樣品形貌結(jié)構(gòu)和負(fù)載量有較大影響。當(dāng)鎳離子與尿素摩爾比CNi2+:C(NH2)2CO為1:4，添加1ml PEI，保溫60min的NiO/ACFC復(fù)合電極材料電極獲得最大的比電容為190.4F/g，具有良好的電化學(xué)性能和穩(wěn)定性能。
[Abstract]:Along with the global energy shortage and environmental deterioration, the electrochemical cycle device can be getting more and more attention. As a new type of super capacitor energy storage device, because of its high power density has the advantages of no pollution, long cycle, which attracted widespread attention and research. And its performance depends on the electrode the choice of materials. The metal oxides and carbon materials as the advantages and disadvantages of electrode material, metal oxide and nickel foam collector, carbon material load for preparing composite electrode material with good performance has become a prime target for material research scholars.
This paper adopts the microwave hydrothermal method, the nano nickel oxide preparation and the use of nickel foam or activated carbon fiber cloth as the carrier to load nano nickel oxide to obtain micro related problems of composite material with nano structure is studied by X, X-ray diffraction, thermal analysis, scanning electron microscopy, morphology and structure of testing technology the materials were characterized and observation, and through the cyclic voltammetry test on the electrochemical performance of as prepared electrode materials by AC impedance method. The main work includes the following aspects:
By microwave hydrothermal method, using NiSO4 as the source of nickel, urea as precipitant, respectively using polyethylene glycol 4000 (PEG-4000) and polyetherimide (PEI) as the surfactant, by changing the holding time, surfactant type and adding amount of NiO nano powders were synthesized. The results showed that the nano NiO precursor synthesis microwave heating at 160 DEG C, the lamellar thickness is about 10nm, after 400 2H calcined was obtained with micro nano hierarchical structure flower like NiO microspheres, the diameter is about 2 m, the thickness of the NiO flower like to add 10nm. surfactant NiO microspheres aggregation decreased significantly, and the shape of microspheres, uniform size. Through electrochemical tests show that the addition of 3.7%PEG-4000, the preparation of nano NiO electrode specific capacitance 85.4F/g maximum insulation under the condition of 30min, after 500 cycles, the specific capacitance decay is only 13.3%, showing good electrochemical stability.
With nickel foam as the carrier, respectively by NiSO4 and Ni (NO3) 2 - 6H2O as the source of nickel, nickel ions by changing the concentration of surfactant type and dosage, reaction time, using the method of load in situ microwave hydrothermal preparation with micro nano hierarchical structure of NiO/ foam nickel composite electrode material samples. Show that NiSO4 as the source of nickel nano NiO synthesized in situ growth on the surface of uniform flower like nickel foam, adding surfactant PEG-4000 inhibited the NiO nanosheets on nickel foam growth. The test results show that the thermal insulation 30min, NiO/ nickel foam electrode micro nano hierarchical additive preparation conditions the specific capacitance can reach 234.8F/g. to Ni (NO3) 2 - 6H2O as the source of nickel, 60min insulation granular nano NiO was synthesized and grown on nickel foam with uniform surface and surface active agent PEG-4000 is added into NiO nanoparticles attached on the surface of nickel foam, It is not conducive to the transfer of ions and electrons. The maximum specific capacitance of NiO/ foam nickel sample electrode prepared with 60min and no additives is 224.4F/g.
The activated carbon fiber cloth (ACFC) as the carrier, with urea and NiSO4 as raw materials, NiO/ACFC composite electrode materials by changing different reactant concentration and reaction time by microwave hydrothermal method, and the sample electrode were studied. The results showed that the electrochemical properties of nano NiO synthesized by in situ growth in flower like structure the activated carbon fiber cloth surface layer thickness is about 10nm. in microwave synthesis under the same conditions, surfactant dosage of PEI and urea content has a great influence on the morphology and structure of load. When the nickel ion and urea molar ratio of CNi2+: C (NH2) 2CO 1:4, adding 1ml PEI, NiO/ACFC composite electrode materials the maximum insulation 60min electrode specific capacitance is 190.4F/g with good electrochemical performance and stable performance.

【學(xué)位授予單位】：濟(jì)南大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2014
【分類號(hào)】：TM53

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