本文基本上分為兩大部分，包括：製作多孔性氧化鋁薄膜當作模板以及鎳鈷合金電化學沉積。
此研究以混合脈衝波電壓技術在室溫及靜止電解液環境之下，利用二次陽極處理以低純度(99%)鋁箔在0.05 M草酸電解液裡製作規則性與高密度多孔性氧化鋁薄膜。根據實驗結果，最佳參數為利用pulse reverse在第一階段陽極處理作為預成孔圖案。在第二階段以pulse所做出來的奈米孔洞陣列之直徑範圍為30-60 nm。製程中的控制參數，陽極氧化時間及電壓波形皆直接影響到奈米孔洞之結構與形貌，除此之外鋁的純度也是最主要的考量。
另一方面，透過自組化模板之介電崩潰，利用定電流方形脈衝波在較高溫環境之下(55℃)，增加金屬離子在鍍浴裡之游動率，可製作出鎳鈷合金奈米線。
使用不同電流波形對電鑄的鎳鈷金屬進行表面處理，不管何種波形的脈衝波，只要波形中含有緩衝時間 (relaxation time)，鍍層的表面粗糙度皆較為優異，尤其電鑄高深寬比結構所面臨到的問題在於金屬離子不易補充入溝槽內，造成電鑄效率大幅降低。pulse current 會讓金屬離子在鍍浴裡趁Toff的時候游離至陰極表面附近，改變離子擴散的現象，來改善此高深寬比結構內金屬離子不足的影響。
在合金電鍍過程中，還原電位較小之金屬其電沉積速率大於還原電位較高之金屬，稱為異常共鍍，如鎳(-0.257 V) 之還原電位較鈷 (-0.277 V) 低，但在電鍍過程中鈷析鍍量較鎳多。本研究選取特定鍍液 (complex sulfamate chloride bath)，並發現電鍍過程中電流密度及溫度的改變為影響異常共鍍效果的主因，而異常共鍍效果進一步對鍍層中鈷含量及薄膜硬度產生影響。在這兩個條件變化之下，隨著電流密度與溫度的上昇，鍍層中鈷含量的原子百分比 [Co at% = Co/(Ni+Co) × 100%]大約從25%下降到15%並導致硬度從556 Hv下降到413 Hv。

This study is divided into two main parts basically, including fabrication of porous anodic alumina films which act as a template and Nickel-Cobalt (Ni-Co) alloys electrodeposition on those self assembled porous anodic alumina (PAA) films. Through the electrical breakdown of the template, Ni-Co nanowires could be obtained by constant current square wave form at high temperature (55°C) to increase the mobility of metal ion in electrolyte.
In order to avoid burning and powdering effect, we introduce the hybrid pulse technique to fabricate PAA films at room temperature in quiescent solution. Highly ordered hexagonal of parallel pore arrays were produced from commercial purity of 99% aluminum (Al) foils via two-step anodization process in 0.05 M oxalic acid. From experiment results showed that by utilizing pulse reverse voltage at the 1st step anodization as pre-pattern purpose, and pulse voltage subsequently is the best combined parameter. The diameter of resulting nanopore arrays could reach 30-60 nm. Process parameters, such as duration of anodization and types of voltage would greatly affect the structure and morphology of anodic films. Besides, purity of aluminum substrate is also one of the major considerations.
On the other side, Ni-Co nanowires were prepared via template-guided electrodeposition. Moreover, when two or more elements are deposited simultaneously would encounter the effect of so-called anomalous codeposition behavior. The variation of current densities and temperature resulted in different Co atomic percentage [Co at% = Co/(Ni+Co) × 100%] in atomic ratio of the deposited films as well as the microhardness and morphology sequentially. Co at% in Ni-Co films gradually decreased with increasing current density and temperatures with variation from approximately 25 % to 15 % and lead to changes of microhardness from 556 Hv to 413 Hv.

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