本文選題：通孔PAA模板　切入點(diǎn)：快速制備　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】：高度有序的多孔陽極氧化鋁(Porous Anodic Alumina,PAA)模板被廣泛用于各種納米功能材料的制備中,但通孔PAA模板的快速制備仍是一個(gè)挑戰(zhàn)。本文為了構(gòu)建鋁納米柱陣列的電介質(zhì)電容器,著重研究了大小孔間距(孔徑)PAA模板的快速制備方法和通孔工藝,并利用PAA通孔模板,采用真空熔融壓注法,通過優(yōu)化壓注工藝參數(shù),成功地制備出大面積高度有序的鋁納米柱陣列,并通過陽極氧化法在納米柱表面形成一層電介質(zhì)薄膜,構(gòu)建了納米電容器。首先,在不同濃度草酸溶液中不同氧化電壓下進(jìn)行高場恒壓陽極氧化,探究影響PAA膜有序度的主要因素,結(jié)果表明:提高電解液濃度和氧化電壓均能有效地提高PAA膜的有序度(Ordering degree)。其中在62 V、0.75 molL-1草酸電解液中單面陽極氧化所得的PAA膜最為規(guī)整,有序度達(dá)75.6%,生長速率高達(dá)134.54μm-1;對62 V單面氧化的PAA膜和48 V雙面氧化的PAA膜分別進(jìn)行單向腐蝕150 min和40 min后均可得到完全通孔的PAA模板。其次,在磷酸的乙醇溶液、低濃度草酸溶液中可實(shí)現(xiàn)在常溫下大孔間距PAA模板的制備,但仍存在生長速率偏慢,PAA膜孔道不規(guī)整等問題。在單取代磷酸酯溶液中可實(shí)現(xiàn)大孔徑PAA模板的快速制備,在該電解液體系中,電壓可調(diào)控范圍非常廣(200-380 V)、PAA膜的生長速率為磷酸溶液中的30-60倍。對340 V氧化的PAA膜進(jìn)行單向腐蝕8 h可得到完全通孔的PAA模板。另外,為了構(gòu)建納米電容器,先在拋光的鋁基體上研究陽極氧化鋁電介質(zhì)膜的形成工藝和性能。結(jié)果表明檸檬酸氫二銨和硼酸銨溶液中所得的電介質(zhì)膜的漏電流較小;在40℃下所得的電介質(zhì)膜的綜合介電性能較好;在同等氧化電壓下檸檬酸氫二銨中加入少量磷酸單丁酯可以得到"污染層"更薄的氧化鋁膜,因此可以明顯降低致密膜的漏電流,并且隨著添加劑濃度的增加氧化鋁致密膜的漏電流越小。最后,以不同孔徑的通孔PAA模板,利用不同的壓注工藝制備出不同直徑的鋁納米柱陣列,研究不同工藝方法對鋁納米柱陣列的影響。結(jié)果表明,所加的壓力應(yīng)以65 MPa為宜,壓注溫度應(yīng)低于鋁的熔點(diǎn)(660℃),其中在200℃下開始施加壓力至65 MPa,其后在保壓的同時(shí)升溫至400℃,保溫保壓一段時(shí)間后再緩慢升溫至650℃可以制備大面積較為規(guī)整的鋁納米柱陣列,對該工藝條件下制備的鋁納米柱陣列利用陽極氧化法在納米柱表面形成一層電介質(zhì)膜,構(gòu)建了納米結(jié)構(gòu)的電介質(zhì)電容器,在測試頻率為50 Hz時(shí),與平面結(jié)構(gòu)電介質(zhì)電容器相比,其比容提高了 20.8倍。
[Abstract]:Porous Anodic aluminum oxide (PAA) templates with highly ordered order have been widely used in the preparation of various nano-functional materials, but the rapid preparation of through pore PAA templates is still a challenge. In this paper, the rapid preparation method and through pore technology of large and small pore spacing (PAA) template are studied. By using PAA through pore template and vacuum melt pressing method, the process parameters of pressure injection are optimized. A large area and highly ordered aluminum nanocolumn array was successfully prepared, and a layer of dielectric film was formed on the surface of the nanocrystalline column by anodizing method to construct the nanocrystalline capacitor. High field constant voltage anodic oxidation was carried out in oxalic acid solution with different concentrations. The main factors affecting the order of PAA films were investigated. The results show that increasing electrolyte concentration and oxidation voltage can effectively improve the ordering degree of PAA film, and the PAA film obtained by anodic oxidation on one side is the most regular in 62 V ~ 0.75 molL-1 oxalic acid electrolyte. The order degree was 75.6 and the growth rate was 134.54 渭 m ~ (-1). After unidirectional corrosion of 62V PAA film and 48V double-sided oxidation PAA film for 150 min and 40 min respectively, the PAA template could be obtained. Secondly, in the ethanol solution of phosphoric acid, the through pore PAA template could be obtained. In low concentration oxalic acid solution, the large pore spacing PAA template can be prepared at room temperature, but there are still some problems such as slow growth rate and irregular pore channel. The rapid preparation of large pore size PAA template can be realized in monosubstituted phosphate solution. In this electrolyte system, the voltage adjustable range is very wide. The growth rate of the film is 30-60 times as high as that in the phosphoric acid solution. The PAA film with 340V oxidation can be corroded in one direction for 8 hours. In addition, a fully porous PAA template can be obtained. In order to construct nanocrystalline capacitors, the formation process and properties of anodic alumina dielectric films were studied on polished aluminum substrates. The results showed that the leakage current of dielectric films obtained in the solution of diammonium citrate and ammonium borate was small. The dielectric film obtained at 40 鈩，

本文編號(hào)：1582842