奈米結構材料為現今的人們帶來許多的便利與源源不絕的商機，其中電化學技術又是製備奈米結構材料方法中最為便捷且成本低廉的方式，因此本論文以電化學技術製備奈米結構材料，分析其奈米機械性質、成分分析、結構分析與電性分析。綜觀電化學技術可分為陰極還原與陽極氧化兩大類，因此本論文主要包含此兩大類; 1.電化學沉積鎳與鎳合金鍍層之研究，其中包含脈衝電鍍的鍍層性質分析、脈衝電鍍高深寬比結構分析、合金共鍍分析、合金功函數分析與低溫電鍍之研究；2.室溫脈衝陽極氧化鋁模版製備技術，此研究將脈衝電位技術應用於陽極氧化鋁模板製程中，克服傳統陽極氧化鋁於低溫環境製程的限制，且有助於奈米孔隙的均勻分佈。
論文第一部分為電化學方法沉積奈米結構材料技術。在脈衝電鍍的鍍層性質分析中，先以脈衝電位於50 °C的電解液環境中進行電鍍，鍍層因脈衝電位造成電雙層(double layer)豐富的離子濃度，而還原形成高緻密性的鍍層，奈米壓痕器測試(nano-indentation test)證實，其硬度由傳統鎳金屬的3.90 GPa提升至4.87 GPa (100~200 Hz)。在高深寬比微結構的電鑄技術中，以低功率的二氧化碳雷射蝕刻PMMA形成微米級的結構，並進行脈衝電位電鑄的離子填充性能分析，數值分析與實驗結果顯示，提高脈衝電位至100~200 Hz的範圍時，金屬離子在高深寬比結構底部具有較高濃度與較佳的離子穿透性，可提升微結構電鑄的效率。在鎳基合金的異常共鍍(anomalous co-deposition)方面，鎳鈷合金鍍層的奈米壓痕測試顯示出鍍層在22.53 % 的鈷含量時有最高的硬度 8.72 GPa，且脈衝電位可有效抑制異常共鍍現象的發生。在鎳鈷合金的功函數變異分析中，我們分別以紫外光光譜儀(ultraviolet photoelectron spectroscopy, UPS)與自製凱文探針(Kelvin probe)來分析功函數値，並比較其差異性。結果顯示，藉由製程參數的調整，鎳鈷合金的鈷含量可由22.53 % 變異至13.19 %，紫外光光譜儀所分析的功函數値由3.89 eV 變化至 4.07 eV，凱文探針所分析的功函數値趨勢與紫外光光譜儀的趨勢相同，顯示凱文探針分析功函數的性能良好。在低溫電化學沉積技術方面，低溫環境的沉積條件與室溫甚至高溫(40-60 ˚C)不同，主要是因為電解液中的離子擴散能力不同，使低溫電鍍的困難度提高，結果顯示在5 ˚C以直流電鍍的鍍層硬度值達6.18 GPa，係由於熱殘留應力(thermal residual stress)與細晶強化的影響所造成。
論文第二部分為陽極氧化鋁模板製備技術，我們提出一種可於室溫環境中進行的脈衝電位陽極氧化法，不同於先前技術，陽極氧化鋁製程需在低溫環境中(0~10 °C)進行，此脈衝電位陽極氧化法可在20~30 °C的室溫環境中製備出奈米結構的模板，主要是因為脈衝電位可有效抑制製程中所產生的焦耳熱，而達到室溫環境的製程能力，且奈米孔徑的均勻性更甚於傳統的直流陽極氧化製程，在此部份中將探討製程參數對孔隙結構的影響與脈衝陽極氧化的反應機制。

Nanostructured materials bring business-opportunities and conveniences in life nowadays. Electrochemical technique is one of the most effective and cheap method for producing nanostructured materials. Therefore, this dissertation presents the fabrication of nanostructured material by electrochemical method and the analysis of nanomechanical properties, composition, structure and electronic property of material are also discussed. The main frame of this dissertation can be divided into two parts; one is electrochemical deposition of nickel and nickel-cobalt alloy and the other is anodic oxidation of aluminum.
The first part of dissertation concerns about electrodeposited nanostructured materials. In pulse eletrodeposition of Ni at 50 ˚C, the pulse voltage makes rich in ions within electric double layer for reduction and obtains compact deposits. The results of nano-identation tests show that the hardness of Ni deposits in pulse electrodeposition is 4.87 GPa which is higher than that in direct current (DC) electrodeposition (3.90 GPa). In terms of high-aspect-ratio-micro-structure (HARMS) electrodeposition, we performed the HARMS from PMMA by CO2 laser ablation and analyzing the ion filling ability into micro-cavity via pulse current electrodeposition. Both numerical simulation and experimental results show that higher concentration of ion at cathodic surface and better penetration ability of ion can be obtained in pulse electrodeposition than that in DC electrodeposition. In Ni-Co anomalous co-deposition, the highest hardness which is 8.72 GPa was obatained from the Ni-Co alloy films with 22.53 % Co content. Furthermore, pulse electrodeposition inhibits the anomalous behavior effectively during co-deposition. In part of work function (WF) evaluation, the WF of Ni-Co film was measured via ultraviolet photoelectron spectroscopy (UPS) and the self-made Kelvin probe (KP). The WF of Ni-Co films increases form 3.89 eV to 4.07 eV with decreasing Co content from 22.53 % to 13.19 %, and both UPS and KP presented the identical results. Finally, in low temperature electrodepositon, electrodeposition is difficult to perform at low temperature due to ineffective mass transfer. The results show that the highest hardness of Ni films is 6.18 GPa obtaining at 5 ˚C, the hardness is higher than that in conventional electrodeposited Ni films (~4 GPa) and close to the Ni-Co alloy films (~8 Gpa). Two main strengthenings contribute to the low-temperature electroplated deposits; one is thermal residual stress strengthening and the other is Hall-Petch strengthening.
The second part of dissertation concern about the room temperature (RT) hybrid pulse anodized (HPA) aluminum oxide. Conventional anodic aluminum oxide (AAO) template was performed using potentiostatic method from high-purity (99.999%) aluminum films at low temperatures of 0-10 °C to avoid dissolution effects at relatively high RT of 20-30 °C. The HPA provides ability to process at RT because it inhibits the Joule’s heat generation during the anodization, and thus suppresses the dissolution effect effectively. The HPA not only merits manufacturing convenience and cost reduction but also promotes uniformity of AAO pores distribution. Therefore, the HPA method provides minimized heat fluctuation at RT, improves the uniformity and keeps the growth rate close to DCA

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