電化學(xué)沉積制備納米鋁熱薄膜的研究
本文選題:離子液體 切入點(diǎn):電化學(xué)沉積 出處:《南京理工大學(xué)》2017年碩士論文 論文類型:學(xué)位論文
【摘要】:本文以氯化1-乙基-3-甲基咪唑—三氯化鋁(EMIC-AlCl_3)離子液體為Al的電還原沉積液,進(jìn)行了電化學(xué)沉積制備納米鋁熱薄膜的研究。首先通過配置得到EMIC-AlCl_3離子液體,并以FTO導(dǎo)電玻璃為基板研究了Al的沉積規(guī)律。而后通過膠晶模板法分別制備得到了三維有序Fe_2O_3薄膜及Co_3O_4納米線薄膜,應(yīng)用水熱法在泡沫鎳上制備得到了Co_3O_4納米線薄膜,采用電化學(xué)沉積的方式將Al沉積到各氧化物薄膜上,制備得到了氧化物/Al納米鋁熱薄膜。采用XRD、SEM、TEM、DSC及激光點(diǎn)火等手段對(duì)制備得到的樣品進(jìn)行了相關(guān)表征及測(cè)試。獲得的主要研究結(jié)果如下:配置得到的EMIC-AlCl_3離子液體中,Al2Cl7-能夠穩(wěn)定還原沉積制備Al單質(zhì)的電壓及電流密度分別為0.378V及1mA·cm-2。當(dāng)電流為70mA時(shí),可在FTO導(dǎo)電玻璃上制備得到純度較高、致密性較好的A1,此時(shí)A1的沉積速率為0.8μm·min-1。以聚苯乙烯(PS)球乳液的稀釋液制備得到膠晶模板,以厚度為2μm的膠晶模板制備得到了厚度為1.5μm的三維有序Fe_2O_3薄膜。通過電化學(xué)沉積A1制得了Fe203/Al納米鋁熱薄膜,但沉積的A1無法在Fe_2O_3骨架上直接沉積而只能首先在FTO導(dǎo)電玻璃基板上進(jìn)行沉積,而后逐層向外沉積并填充于Fe_2O_3骨架結(jié)構(gòu)中,直至將整個(gè)Fe_2O_3骨架填充完全。這種復(fù)合方式使得Fe_2O_3/Al納米鋁熱薄膜的熱性能較差,放熱量最高僅為 222.27J·g-1。以膠晶模板結(jié)合草酸的后續(xù)處理成功制備得到了Co_3O_4納米線。電化學(xué)沉積的Al能夠在具有一定導(dǎo)電性的Co_3O_4納米線表面實(shí)現(xiàn)沉積。制備得到的Co_3O_4/Al納米鋁熱薄膜的放熱量可達(dá)724.64 J·-1,遠(yuǎn)高于上述制得的Fe_2O_3/Al納米鋁熱薄膜的反應(yīng)放熱量,激光點(diǎn)火測(cè)試表明該鋁熱薄膜具有發(fā)火能力,且發(fā)火持續(xù)時(shí)間可達(dá)432.9μs。以水熱法在泡沫鎳上制備得到了直立性好、分布均勻的Co_3O_4納米線。電化學(xué)沉積的Al可在Co_3O_4納米線上直接沉積并最終制得Co_3O_4/Al納米鋁熱薄膜。激光點(diǎn)火后的火焰高度及火焰寬度比模板法制備得到的要高。恒電流起爆測(cè)試結(jié)果表明,負(fù)載Co_3O_4/Al納米鋁熱薄膜的泡沫鎳做成的點(diǎn)火橋通電后可發(fā)火,且具有一定的發(fā)火強(qiáng)度,可作為點(diǎn)火器件來研究和應(yīng)用。
[Abstract]:In this paper, the preparation of nanocrystalline aluminothermic films by electrochemical deposition of 1-ethyl-3-methylimidazolium chloride (1-ethyl-3-methylimidazolium trichloride) -EMIC-AlCl3) ionic liquid as Al solution was studied. Firstly, EMIC-AlCl_3 ionic liquid was obtained. The deposition rule of Al on FTO conductive glass substrate was studied, and then three dimensional ordered Fe_2O_3 film and Co_3O_4 nanowire film were prepared by colloidal crystal template method. Co_3O_4 nanowire films were prepared on nickel foam by hydrothermal method. Al was deposited on various oxide films by electrochemical deposition. The oxide / Al nanocrystalline aluminothermic thin films were prepared. The samples were characterized and tested by means of XRDX Sem Tem DSC and laser ignition. The main results obtained are as follows: Al2Cl7-. The voltage and current density of Al prepared by stable reduction deposition are 0.378V and 1mA 路cm-2.When the current is 70mA, A1 with high purity and good densification could be prepared on FTO conductive glass, and the deposition rate of A1 was 0.8 渭 m 路min-1. The colloidal template was prepared from the dilute solution of polystyrene (PS) ball emulsion. Three-dimensional ordered Fe_2O_3 thin films with thickness of 1.5 渭 m were prepared by colloidal template with thickness of 2 渭 m. Fe203/Al nanocrystalline aluminothermic films were prepared by electrochemical deposition of A1. However, the deposited A1 can not be deposited directly on the Fe_2O_3 skeleton. It can only be deposited on the FTO conductive glass substrate first, and then deposited layer by layer and filled in the Fe_2O_3 skeleton structure. Until the whole Fe_2O_3 skeleton is filled, the thermal properties of the Fe_2O_3/Al nanocrystalline aluminothermic films are poor. The maximum heat release was 222.27J 路g-1.The Co_3O_4 nanowires were successfully prepared by gel crystal template and oxalic acid follow-up treatment. The electrochemical deposition of Al on the surface of Co_3O_4 nanowires with certain electrical conductivity could be realized. The Co_3O_4/Al prepared was obtained. The heat release of nanocrystalline aluminothermic films can reach 724.64 J 路-1, which is much higher than the reactive heat release of Fe_2O_3/Al nanocrystalline aluminothermic films. The laser ignition test shows that the film has the ability to ignite, and the firing duration can reach 432.9 渭 s. Co_3O_4 nanowires with uniform distribution. Co_3O_4/Al nanocrystalline aluminothermic films can be directly deposited on Co_3O_4 nanowires by electrochemical deposition. The flame height and flame width after laser ignition are higher than those prepared by template method. The flow initiation test results show that, The ignited bridge made of nickel foam loaded with Co_3O_4/Al nanocrystalline aluminothermic film can be ignited after it is electrified and has a certain ignition intensity, so it can be used as a igniter to study and apply.
【學(xué)位授予單位】:南京理工大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2017
【分類號(hào)】:TQ560.7;TB383.1
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