【摘要】：多孔陽(yáng)極氧化鋁模板（Porous Anodic Aluminum Oxide Template）具有制備工藝簡(jiǎn)單、原材料易得且價(jià)格低廉、孔陣列高度有序且孔徑在一定范圍內(nèi)可調(diào)等優(yōu)點(diǎn)。 本文主要對(duì)微孔徑、小孔間距陽(yáng)極氧化鋁模板的制備方法進(jìn)行了研究，通過大量的實(shí)驗(yàn)對(duì)影響陽(yáng)極氧化鋁模板孔徑、孔間距大小和孔規(guī)整度的工藝（預(yù)處理工藝、電化學(xué)拋光工藝和陽(yáng)極氧化工藝）和工藝參數(shù)（氧電壓值、電流密度、電解液類型及濃度、電解液溫度等）進(jìn)行了探究。成功的制備出了孔徑在20-90nm，氧化膜厚度在200nm-10μ m的高度有序的陽(yáng)極氧化鋁模板。系統(tǒng)的研究了前處理工藝、氧化過程中參數(shù)的調(diào)整、后處理工藝等對(duì)鋁片表面所施加的影響。通過調(diào)整不同的試驗(yàn)參數(shù)獲得最優(yōu)的參數(shù)組合，從而得到最佳的制備工藝。采用不同種類、不同濃度的氧化電解液（硫酸和草酸）條件下，研究了不同電壓對(duì)孔徑、孔間距及規(guī)整度等技術(shù)指標(biāo)的影響，，分析了氧化過程中電流密度的變化、溫度的變化及對(duì)氧化時(shí)間的影響。將采集到的氧化過程中的產(chǎn)生的電壓、電流的變化實(shí)時(shí)數(shù)據(jù)繪成圖表進(jìn)行研究。通過控制陽(yáng)極氧化鋁模板的第一次陽(yáng)極氧化時(shí)間、去除一次氧化膜時(shí)間以及第二次陽(yáng)極氧化時(shí)間來(lái)控制氧化膜表面的形貌。對(duì)所制備的陽(yáng)極氧化鋁模板采用掃描電鏡SEM與原子力顯微鏡AFM進(jìn)行了表征，獲得了精確的測(cè)量參數(shù)。 實(shí)驗(yàn)結(jié)果表明：（1）高溫退火可以有效的去除鋁片內(nèi)部晶界間的應(yīng)力，使晶粒變大,有利于孔核的形成與生長(zhǎng)。電化學(xué)拋光可以有效的去除鋁片表面的氧化層和納米級(jí)以上的缺陷，并且對(duì)鋁片表面起到微觀整平作用，從而得到超平表面。高溫退火以及電化學(xué)拋光等前處理工藝有利于提高模板孔的規(guī)整度和出孔面積。（2）孔徑的大小主要與氧化電壓和氧化電解液類型有關(guān)：孔徑大小和氧化電壓成近似的線性關(guān)系，氧化電壓越大，所形成的孔徑越大。不同類型的氧化電解液所需的最佳氧化電壓高低不等，其高低關(guān)系為硫酸＜草酸＜磷酸。不同類型氧化電解液條件下所制備的模板有序孔的孔徑大小關(guān)系為硫酸＜草酸＜磷酸。（3）第一次氧化對(duì)第二次氧化具有強(qiáng)大的引導(dǎo)作用，適當(dāng)?shù)难娱L(zhǎng)一次氧化的時(shí)間可以提高模板孔的規(guī)整度。二次氧化所用條件應(yīng)與一次氧化條件完全相同，二次氧化時(shí)間長(zhǎng)短關(guān)系到氧化膜的厚度。（4）氧化過程中模板對(duì)于溫度特別敏感，氧化過程中保持溫度穩(wěn)定在適當(dāng)?shù)姆秶鷥?nèi)可以減少缺陷產(chǎn)生，提高制備成功率與模板質(zhì)量。
[Abstract]:Porous anodic alumina template (Porous Anodic Aluminum Oxide Template) has the advantages of simple preparation process, easy availability and low price of raw materials, highly ordered pore array and adjustable pore size in a certain range. In this paper, the preparation method of anodic alumina template with micropore size and pore spacing was studied. The process of influencing the aperture, pore spacing and pore regularity of anodic alumina template was studied by a large number of experiments. The electrochemical polishing process and anodic oxidation process) and process parameters (oxygen voltage, current density, electrolyte type and concentration, electrolyte temperature, etc.) were investigated. A highly ordered anodic alumina template with a pore size of 20-90 nm and an oxide film thickness of 200nm-10 渭 m was successfully prepared. The effects of pretreatment process, parameters adjustment in oxidation process and post-treatment process on the surface of aluminum sheet were systematically studied. By adjusting different experimental parameters, the optimal combination of parameters is obtained, and the best preparation process is obtained. The effects of different voltages on pore diameter, pore spacing and regularity were studied under the conditions of different kinds and different concentrations of oxidized electrolytes (sulfuric acid and oxalic acid), and the change of current density during oxidation was analyzed. The change of temperature and its influence on oxidation time. The real-time data of the voltage and current generated in the oxidation process are graphed for study. The surface morphology was controlled by controlling the first anodizing time of anodic alumina template, removing the first anodizing film time and the second anodizing time. The anodic alumina template was characterized by scanning electron microscope (SEM) and atomic force microscope (AFM). The experimental results show that: (1) the high temperature annealing can effectively remove the stress between grain boundaries in the aluminum sheet, and make the grain size bigger, which is conducive to the formation and growth of the pore nucleus. Electrochemical polishing can effectively remove the oxide layer and the defects above nanometer level on the aluminum sheet surface, and play a micro-leveling role on the aluminum sheet surface, so that the super-flat surface can be obtained. Pre-treatment processes such as high temperature annealing and electrochemical polishing can improve the regularity and area of the template hole. (2) the pore size is mainly related to the oxidation voltage and the type of oxidation electrolyte: pore size and oxidation voltage. In an approximate linear relationship, The larger the oxidation voltage, the larger the pore size. The optimum oxidation voltage for different kinds of electrolytes is different, and the relationship is sulfuric acid < oxalic acid < phosphoric acid. The pore size of the template prepared under different kinds of oxidizing electrolytes is as follows: sulfuric acid < oxalic acid < phosphoric acid. (3) the first oxidation has a strong guiding effect on the second oxidation. The regularity of the template hole can be improved by prolonging the time of primary oxidation. The conditions of secondary oxidation should be exactly the same as that of primary oxidation. The duration of secondary oxidation is related to the thickness of oxide film. (4) the template is particularly sensitive to temperature during oxidation. Keeping the temperature stable in the oxidation process can reduce the production of defects and improve the success rate of preparation and the quality of template.
【學(xué)位授予單位】：內(nèi)蒙古科技大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：TQ133.1;TQ150

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相關(guān)期刊論文 前2條

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