具高深寬比奈米孔特性的陽極氧化鋁(anodic aluminum oxide, AAO)，可做為模板製備奈米線或其他一維奈米材料，並整合於電子或光電奈米製程中。一般AAO製備方法需於低溫下(0-5°C)使用直流電位進行兩階段陽極氧化，相對高的電解液溫度將導致溶解效應而影響其奈米孔洞結構。過去本實驗室發展之複合脈衝陽極氧化技術(hybrid pulse anodization, HPA)藉由搭配微小負電壓週期可於陽極氧化製程中抑制焦耳熱效應，達成常溫製備AAO的可能性。本論文將研究此技術於一階段陽極氧化鋁孔洞品質的改善，並進一步發展鋁薄膜的一階段陽極氧化製程，探討不同濺鍍條件對奈米孔洞成長行為的影響。
在塊材鋁的製程研究中，將比較不同環境溫度下使用脈衝電位與直流電位於草酸溶液中進行一階段陽極氧化的差異。脈衝電位所製備的AAO孔洞尺寸均勻性與真圓度都較直流電位好，脈衝電位製程對環境溫度容忍度較高也有助於提升整體AAO成長速率與獲得較大孔洞。另一方面，在常溫下使用脈衝電位製程對低純度塊材鋁進行陽極氧化的結果則展示了半球彎曲表面的奈米孔洞成長，此部分將針對其成形過程與原因進行驗證探討。在鋁薄膜的陽極氧化製程研究中，首先將藉由不同靶材功率與基板偏壓製備鋁薄膜，探討所形成的不同表面形貌對後續成長AAO孔洞品質的影響。結果指出，於相對低靶材功率並添加基板偏壓可沉積較小平均晶粒尺寸且表面較平整的鋁薄膜，將有助於AAO孔洞尺寸均勻性的提升。基於此結果進一步改變靶材功率，可獲得於50 W形成的平坦表面形貌與185 W所形成的三維表面形貌，並使用脈衝陽極氧化製程成功製備出不同於傳統平面AAO的三維奈米孔洞結構。此外，研究成果也證實鋁薄膜中殘留應力將影響陽極氧化過程的孔洞成長。透過濺鍍製程所製備的不同殘留應力之鋁薄膜實驗發現，殘留張應力會抵消氧化鋁膨脹之壓應力而減少其AAO塑性變形行為，使得孔洞間距變小、孔洞密度增加。本論文最後應用過度蝕刻後的三維奈米孔洞結構沉積P25二氧化鈦材料，應用其高比表面積特性獲得其附著性之改善與整體光催化效能之提升。

Anodic aluminum oxide (AAO) containing high-aspect ratio pore channels is widely used as a template for fabricating nanowires or other one-dimensional nanostructures. Conventional anodic aluminum oxide (AAO) templates were performed using two-step direct current anodization (DCA) at low temperature (0-5°C). A higher electrolyte temperature results in dissolution effects therefore damages the pore structure. This problem is resolved by means of a hybrid pulse anodization (HPA) technique, in which a period of small negative potential is applied to suppress the Joule heating effect during the AAO preparation process. In this dissertation, improvement of AAO quality in single-step anodization was developed by hybrid pulse technique. Moreover, the growth of nanoporous AAO in Al films deposited by various sputtering conditions has been further studied.
In the anodization of bulk Al, the single-step HPA and DCA anodization in oxalic acid and the various environment temperature was investigated. The pore distribution uniformity and circularity of AAO by HPA is much better than DCA. HPA which can sustain higher environment temperature is helpful to increase the growth rate and enlarge the pore size of AAO films. On the other hand, the growth behavior of porous alumina on a hemisphere curved surface has been examined and discussed by an HPA process on low-purity bulk Al at room temperature. In the anodization of Al film, the various Al target power and substrate bias were performed to form different surface morphology of the sputtered Al thin films which were further investigated for the AAO synthesis quality. The Al films with smaller mean grain size and smoother morphology deposited at relatively low target power with bias were beneficial for more uniform pores size distribution. Accordingly, the various Al target powers of 50 to 185 W were performed to form different two-dimensional (2D) and three-dimensional (3D) surface morphologies. The 3D porous structure which is different from general 2D planar AAO has been successfully demonstrated using HPA on the film with greatly rough hillock-surface formed at the highest power of 185 W. In addition, the role and effect of residual stress on pore generation of AAO have been investigated into anodizing the various-residual-stresses aluminium films. The tensile residual stress lessened the compressive oxide growth stress to reduce AAO plastic deformation leading to smaller pore distance and higher pore density. Finally, the enhancement of photocatalytic performance and improvement of adhesion of P25 TiO2 by AAO with over-etched 3D nanoporous structure was demonstrated.

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