Please use this identifier to cite or link to this item: http://hdl.handle.net/11455/9501
標題: 鋁塊材與鋁薄膜陽極氧化之研究
Anodic oxidation of bulk and thin film aluminum
作者: 顏偉倫
Wen-Lun, Yen
關鍵字: bulk aluminum;鋁塊材;aluminum film;electro-polish;anodic oxidation;porous anodic oxidation aluminum films;鋁薄膜;電解拋光;陽極氧化;多孔陽極氧化膜
出版社: 材料工程學研究所
摘要: 
本研究是以電化學陽極氧化方法於高純度(99.999 %)之鋁塊材以及鋁薄膜(Al/TiN/Si)兩種鋁基材上,以40 V直流定電壓模式於0.3 M草酸水溶液製備多孔性陽極氧化鋁膜,並且在相同外加電壓、電解液濃度以及陽極氧化溫度之條件下,比較鋁塊材及鋁薄膜在不同陽極氧化時間下所製備出來之多孔性陽極氧化膜其性質之差異。
不同於文獻常使用之含鉻拋光液,本研究採用磷酸及硫酸混合水溶液為電解拋光液,結果顯示鋁塊材及鋁薄膜在40℃之下,經20 V定電壓模式、電解拋光20分鐘及1分鐘後,表面均生成一含磷酸根及硫酸根之多孔性陽極氧化膜,於鋁薄膜表面之陽極膜厚度達2 μm。直接於試溫、以40 V定電壓模式對鋁塊材以及鋁薄膜做陽極氧化,結果顯示鋁塊材以及鋁薄膜在陽極氧化10、30、60以及90分鐘時,於表面生成較不平整之多孔性陽極氧化鋁膜,且鋁塊材其陽極氧化膜隨時間增加而持續成長,在陽極氧化30、60以及90分鐘時厚度分別為7 μm、10 μm以及12 μm,而鋁薄膜在陽極氧化30分鐘後,原始鋁薄膜因完全氧化而被消耗,所以其陽極氧化膜厚度達到3 μm後便停止成長。
而以X光光電子能譜儀(XPS)分析顯示,在陽極氧化10秒以及60秒時,鋁塊材之陽極氧化膜厚度約115 nm以及393 nm,鋁薄膜之陽極氧化膜厚度約126 nm以及415 nm,配合陽極氧化膜經不同濺射時間之XPS分析結果中,氧化物(Al-O)與金屬(Al)兩者能峰強度之變化,可得知鋁薄膜之陽極氧化速率較快。
陽極氧化之最佳條件方面,在鋁塊材部份本研究採用先以20 V定電壓模式、40℃下,於磷酸及硫酸混合水溶液中電解拋光20分鐘,再以40 V定電壓模式、室溫下於0.3 M草酸溶液中進行陽極氧化,最後將背面金屬鋁及底部障礙層移除,以6 wt%磷酸溶液擴寬孔洞30分鐘,可得平均孔徑約70~80 nm,孔洞排列良好且表面平整之多孔陽極氧化膜,。鋁薄膜部份則以相同條件電解拋光1分鐘,陽極氧化10分鐘,再進行擴寬孔洞30分鐘,結果亦可得一平均孔洞大小約60~70 nm、氧化膜厚度約600 nm之多孔陽極氧化膜。
應用評估上我們以0.2 M硫酸銅以及0.1 M硼酸混合水溶液,於鋁塊材所製備之多孔氧化鋁模板內,以直流定電壓-0.1 V,室溫之下電鍍30分鐘,在移除氧化鋁模板後,可得到長度約5~7 μm之直立陣列奈米銅線。

In this investigation, the porous anodic oxidation aluminum films were prepared by electrochemical method. These films were prepared on the high pure bulk aluminum and aluminum thin film (Al/TiN/Si) by using 40 V DC potentiostatic mode in 0.3 M oxalic acid electrolyte. The characterizations of porous anodic oxidation aluminum films growth on aluminum bulk and thin film aluminum are compared at the same conditions.
The chromium-mixed solution was normally used in electro-polish process. Nevertheless, a solution mixed with phosphoric acid and sulfuric acid was employed in this study. A phosphate and sulfate contain porous anodic oxidation aluminum films with 2 μm thickness is found on the bulk aluminum and aluminum thin film through 20 V potentiostatic electro-polished at 40 oC for 1 min and 20 min, respectively. Moreover, if the potentiostatic was 40 V and the anodic oxidation times were 10, 30, 60 and 90 min, the film surface with more roughness and porous was observed. In this case, when the anodic oxidation times were 30, 60 and 90 min, the depth of oxidation films were 7 μm, 10 μm and 12μm, respectively. After 30 min anodic oxidation, the anodic oxidation of thin film aluminum was depleted and the anodic oxidation film was stopped growing.
Based on the X-ray photoelectron spectroscopy (XPS) analysis, the thickness of oxidation films of bulk aluminum was about 115 nm and 393 nm while on thin film aluminum was about 126 nm and 415 nm, as the anodic oxidation times were 10 sec and 60 sec, respectively. Furthermore, the relative peak intensity of Al-O and Al defined the reaction rate of anodic oxidation by the depth profile of XPS method.
The optimized experimental conditions for the anodic oxidation of aluminum bulk are described as follow. At first, the electro-polish process is done in the mixture solution of phosphoric acid and sulfuric acid for 20 min under 20 V potentiostatic at 40oC. Subsequently, the anodic oxidation is proceeding in the 0.3 M oxalic acid solution, as the potentiostatic 40 V and at room temperature for 60 min. Finally, the smooth surface and order holes of the porous anodic oxidation aluminum films can be obtained via remove the bulk aluminum and barrier layer then enlarge the hole dimension of the films in 6 wt% phosphoric acid solution for 30 min. The average diameter of holes is about 70-80 nm. However, the optimum conditions for anodic oxidation of thin film aluminum are electro-polished for 1 min and anodic oxidation for 10 min under same condition with bulk aluminum. Oxidation film with 60-70 nm average holes diameter and 600 nm thicknesses are obtained after carry out 30 min hole enlargement.
In addition, we employ the porous anodic oxidation aluminum template in 0.2 M copper sulfate and 0.1 M boric acid mixture solution and applied -0.1 V DC potentiostatic for 30 min to electroplate the copper into the holes. After removing the aluminum template, straight copper nano-wires array are successfully obtained.
URI: http://hdl.handle.net/11455/9501
Appears in Collections:材料科學與工程學系

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