本文選題：電沉積 + SiO_2模板　； 參考：《浙江工業(yè)大學(xué)》2017年碩士論文

【摘要】：隨著生活水平的提高和環(huán)境保護(hù)意識(shí)的日益增強(qiáng),人們渴望尋找新能源以解決化石能源短缺及改善由于濫用化石能源所引起的環(huán)境污染等問(wèn)題。氫能被認(rèn)為是最清潔的能源之一,而電催化分解水是制氫的一種重要途徑。然而,電解水制取氫氣與氧氣過(guò)程中,析氧電位過(guò)高導(dǎo)致能耗增加是制約電解水制備氫氣的瓶頸。貴金屬氧化物IrO_2及RuO_2是公認(rèn)的最佳析氧電極材料。但兩種材料由于其自身具有較大的毒性且儲(chǔ)量稀少、價(jià)格昂貴,限制了其大規(guī)模的商業(yè)化應(yīng)用。近年來(lái),人們一直致力開(kāi)發(fā)成本低且催化性能優(yōu)異的新型催化劑材料以代替貴金屬氧化物,其中過(guò)渡族金屬氧化物,如:錳、鈷、鎳等氧化物或氫氧化物由于分布廣泛,價(jià)格低廉,且在堿性環(huán)境中具有良好的穩(wěn)定性而備受關(guān)注。除此之外,高比表面積也是提升催化劑析氧性能的關(guān)鍵,而模板法可有效提高納米多孔電極材料的比表面積,因而受到人們的重視。本文提出以電沉積Si O_2為模板制備納米多孔鎳鈷基析氧薄膜電極。采用掃描電子顯微鏡(SEM)、透射電子顯微鏡(TEM)、X射線衍射(XRD)、X射線光電子能譜(XPS)等技術(shù)對(duì)薄膜電極的結(jié)構(gòu)和形貌進(jìn)行了表征,并考察了薄膜電極的電催化析氧活性和穩(wěn)定性。第三章以Ni(NO3)2、Co(NO3)2和四甲氧基硅烷(TMOS)為前驅(qū)體溶液,采用恒電流沉積技術(shù)在不銹鋼基體上沉積鎳鈷氫氧化物,經(jīng)熱處理后獲得Ni Co2O4-SiO_2復(fù)合薄膜,并在1.0 mol/L KOH溶液中通過(guò)連續(xù)循環(huán)伏安技術(shù)去除SiO_2組分以得到多孔NiCo2O4薄膜。研究了沉積電流密度、沉積時(shí)間及TMOS體積濃度等參數(shù)對(duì)薄膜電催化析氧活性的影響。結(jié)果表明:在含1.0%TMOS溶液中,-1.0 mA cm-2電流密度下電沉積500s制備的薄膜具有較高的析氧活性和穩(wěn)定性。該薄膜電極析氧反應(yīng)的起始電位為~1.52 V(vs.RHE),電流密度在10mA cm-2和100 mA cm-2時(shí)的析氧過(guò)電位分別為0.293 V和0.358 V,Tafel斜率分別為43和142 mV dec-1。第四章以NiSO4、CoSO4和TMOS為前驅(qū)體溶液,采用恒電位沉積技術(shù)在不銹鋼基體上沉積了Ni-Co-Si O_2復(fù)合薄膜。研究結(jié)果表明,溶液中各組分濃度及電沉積電位和時(shí)間對(duì)合金薄膜電極的微觀形貌及析氧活性具有重要影響。在-0.8 V下電沉積500s制備的多孔鎳鈷合金薄膜電極具有較優(yōu)的電催化性能和穩(wěn)定性能。該薄膜電極析氧反應(yīng)的起始電位為~1.48 V(vs.RHE),電流密度在10 mA cm-2和100 mA cm-2時(shí)的析氧過(guò)電位分別為0.287 V和0.326 V,Tafel斜率分別為65和149 mV dec-1。第五章為解決醇溶性TMOS與諸多無(wú)機(jī)鹽相容性差導(dǎo)致無(wú)法制備復(fù)合薄膜的問(wèn)題,提出以水溶性氟硅酸銨為硅源,制備多孔鎳鈷基薄膜電極,考察了電沉積時(shí)間和溶液中原料組成濃度對(duì)鎳鈷基電極電催化性能的影響。結(jié)果表明:氟硅酸銨與諸多鎳鹽、鈷鹽溶液體系均具有良好的相容性,可有效制備復(fù)合薄膜電極,且該電極的電催化活性均得到提高。該薄膜電極析氧反應(yīng)的起始電位為~1.48 V(vs.RHE),電流密度在10 mA cm-2和100 mA cm-2時(shí)的析氧過(guò)電位分別為0.294 V和0.336 V,Tafel斜率分別為39和137 mV dec-1。
[Abstract]:With the improvement of living standards and the increasing awareness of environmental protection, people are eager to find new energy to solve the problem of shortage of fossil energy and improve the environmental pollution caused by the abuse of fossil energy. Hydrogen energy is considered as one of the most clean energy sources, and the electrocatalytic decomposition of water is an important way of hydrogen production. During the process of hydrogen and oxygen, the high oxygen evolution potential and the increase of energy consumption are the bottlenecks that restrict the preparation of hydrogen by electrolysis. Precious metal oxides IrO_2 and RuO_2 are recognized as the best oxygen evolution electrode materials. However, the two materials have their own large toxicity, scarce reserves and expensive prices, limiting their large-scale commercial applications in recent years. In addition, people have been developing new catalyst materials with low cost and excellent catalytic performance in place of noble metal oxides. In addition, transition metal oxides, such as manganese, cobalt, nickel and other oxides or hydroxides, are widely distributed, and have good stability in alkaline environment. The area is also the key to improve the oxygen evolution performance of the catalyst, and the template method can effectively improve the specific surface area of the nano porous electrode material, so people pay attention to it. In this paper, the nano porous nickel cobalt based oxygen evolution film electrode was prepared by electrodeposition of Si O_2 as a template. The scanning electron microscopy (SEM), transmission electron microscope (TEM) and X ray diffraction were used. The structure and morphology of the thin film electrode were characterized by XRD, X ray photoelectron spectroscopy (XPS) and other techniques. The electrocatalytic activity and stability of the electrocatalysis of the film electrodes were investigated. The third chapter used Ni (NO3) 2, Co (NO3) 2 and tetra methoxy silane (TMOS) as precursors solution to deposit nickel cobalt hydrogen oxidation on stainless steel substrate by constant current deposition. The Ni Co2O4-SiO_2 composite film was obtained after heat treatment, and the SiO_2 components were removed by continuous cyclic voltammetry in 1 mol/L KOH solution to obtain the porous NiCo2O4 film. The effects of the deposition current density, deposition time and TMOS volume concentration on the electrocatalytic activity of the film were investigated. The results showed that the 1.0%TMOS solution contained 1.0%TMOS solution. At -1.0 mA cm-2 current density, the films prepared by electrodeposition of 500s have higher oxygen evolution activity and stability. The initial potential of the oxygen evolution reaction of this film electrode is ~1.52 V (vs.RHE). The current density at 10mA cm-2 and 100 mA cm-2 is 0.293 V and 0.358 respectively, respectively, and the slope is 43 and 142 respectively. O4, CoSO4 and TMOS are precursor solutions, and Ni-Co-Si O_2 composite films are deposited on stainless steel substrate by constant potential deposition. The results show that the concentration of each component in the solution and the electrodeposition potential and time have an important influence on the micromorphology and oxygen evolution activity of the alloy film electrode. Electrodeposition of porous nickel prepared by 500s under -0.8 V The cobalt alloy film electrode has excellent electrocatalytic properties and stability properties. The starting potential of the oxygen evolution reaction of this film electrode is ~1.48 V (vs.RHE). The oxygen evolution overpotential of the current density at 10 mA cm-2 and 100 mA cm-2 is 0.287 V and 0.326 V respectively. The slope of Tafel is 65 and 149 mV dec-1. fifth to solve alcohol soluble and many inorganic compounds. The poor compatibility of salt leads to the problem that the composite film can not be prepared. A polyporous nickel cobalt based film electrode is prepared by using water-soluble ammonium fluorosilicate as the silicon source. The effect of electrodeposition time and the concentration of raw material in solution on the electrocatalytic performance of nickel cobalt base electrode is investigated. The results show that ammonium fluorosilicate is good for many nickel salts and cobalt salt solutions. Good compatibility can effectively prepare a composite film electrode, and the electrocatalytic activity of the electrode is improved. The starting potential of the electrode is ~1.48 V (vs.RHE). The current density at 10 mA cm-2 and 100 mA cm-2 is 0.294 V and 0.336 V respectively, and Tafel slope is 39 and 137 mV dec-1., respectively.
【學(xué)位授予單位】：浙江工業(yè)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類(lèi)號(hào)】：TB383.2;TQ116.2

【參考文獻(xiàn)】

相關(guān)期刊論文 前6條

1 蔡莉;;原位復(fù)合法制備聚吡咯/介孔TiO_2及光催化性能[J];硅酸鹽學(xué)報(bào);2013年04期

2 劉軍梅;王海林;;金屬氧化物涂層鈦陽(yáng)極的研究進(jìn)展[J];電鍍與精飾;2012年11期

3 張衛(wèi)民;胡吉明;;硅烷膜的陰極電化學(xué)輔助沉積及其防護(hù)性能[J];金屬學(xué)報(bào);2006年03期

4 蔡利芳,張永忠,席明哲,石力開(kāi);原位合成法在材料制備中的應(yīng)用及進(jìn)展[J];金屬熱處理;2005年10期

5 陶自春,羅啟富,潘建躍;銥系涂層鈦陽(yáng)極的研究進(jìn)展[J];材料科學(xué)與工程學(xué)報(bào);2003年01期

6 仲維卓,華素坤;納米材料及其水熱法制備(上)[J];上�；�;1998年11期

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