隨著奈米科技研究風潮的興起，許多奈米尺度下的特殊物理與化學性質，逐漸被人所發現。其中，一維奈米結構具有蓮花效應、高比表面積以及良好的電子發射特性，而結構呈現二維規則排列時，還將擁有光子晶體、蛾眼效應等特性。目前可用於定義奈米級圖案的微影技術，有電子束(Electron beam)、深紫外光(Deep ultraviolet, DUV)、X光(X-ray)等微影技術，但都有著設備昂貴的共通缺點，同時必須搭配感應耦合電漿反應性離子蝕刻(Inductively coupled plasma reactive ion etching, ICP-RIE)、電子迴旋共振式反應性離子蝕刻(Electron cyclotron resonance reactive ion etching, ECR-RIE)高成本之特殊設備與製程，才能製作高深寬比之矽質奈米結構陣列，此項門檻將使得學術界與中小型企業難以投入相關的研究。聚苯乙烯奈米球具有自組裝效應，能輕易定義出奈米等級的圖形陣列，稱之為自組裝奈米球微影(Self-assembled nanosphere lithography, SANSL)技術；而光輔助電化學蝕刻(Photo-assisted electrochemical etching, PAECE)技術，有著易於形成奈米級孔洞的優點，其蝕刻之深寬比可超過50:1，優於感應耦合電漿反應性離子蝕刻術的蝕刻效果，因而非常適合用於製作高深寬比之奈米結構。因此，本研究結合自組裝奈米球微影以及光輔助電化學蝕刻兩項技術之優點，用以實現低成本製作高深寬比的奈米結構陣列。
研究結果顯示，本研究以旋轉塗佈與震盪塗佈的方式，可獲得趨近完美排列的單層奈米球膜於1.8 ∗1.8 cm2的試片上。利用反應性離子蝕刻術(Reactive ion etching, RIE)將奈米球圖形轉移至氮化矽之上，以形成光輔助電化學蝕刻所需之蝕刻窗(Etching window)。而在HF濃度2.5 wt%的蝕刻液中進行光輔助電化學蝕刻實驗，使用蝕刻幕罩可獲得規則排列且深度較大的奈米孔洞。將界面活性劑SDSS加入光輔助電化學蝕刻液中，可降低蝕刻液的接觸角並避免孔洞產生擴孔現象。當使用1 V的蝕刻電壓與，經過12.5分鐘的蝕刻後，能夠產生深度5.69 μm，直徑為90 nm的孔洞，而孔洞的深寬比可達到63:1。若增加蝕刻電壓時，孔洞的寬度將隨之增加，同時蝕刻深度則逐漸減少。當施以2 V的蝕刻電壓時，經過5分鐘的蝕刻後，可製作出高度為2 μm，直徑為100 nm的柱體，而柱體的深寬比可達到20:1。且奈米柱將隨著奈米球的定義而排列，因此具有陣列化的排列現象。
將具有生物樣本之溶液滴入奈米柱間隙中，將影響穿越奈米結構光源的極化光變化，並產生特定極化光參數。研究結果顯示，將純水加入於入奈米柱結構時，極化光參數分別為極化度0.981、方位角4.86°，而橢圓率為2.83°。而含有5 μg/ml大腸桿菌的溶液加入奈米柱結構時，極化光參數分別變為極化度0.957、方位角7.7°，而橢圓率為3.99°。由此可知，極化光參數的變化與溶液中的生物樣本濃度有關。因此將極化光測試系統結合奈米柱陣列，可應用於光子晶體生物感測器之研發。此外，利用本研究所開發出的奈米孔洞結構陣列，製作太陽能電池的抗反射結構。結果顯示當結構越深時，抗反射效能越佳。其中使用1 V與5分鐘光輔助電化學蝕刻參數的試片，於280-890 nm波段範圍，可將矽的加權平均反射率降低至1.73 %。再配合200 Å的氮化矽抗反射膜，可使加權平均反射率可進一步降低至0.878 %。最後，本研究亦利用不同的光輔助電化學蝕刻電壓，產生表面積不同的奈米結構陣列，用於製作燃料電池電極。研究顯示當試片表面積越大時，電極的催化反應效果越佳。本研究利用1.5 V與1.75 V之兩階段蝕刻，可製作出的表面積約為14.2 cm2的奈米柱，約為平板電極的50.2倍。當奈米柱體表面沉積1000 Å的白金時，可產生10.2 mA的催化反應電流，為平板電極的72.9倍。

With the raise of nanotechnology researching, many special physical and chemical properties were found gradually in nanoscale. Among them, the one-dimension nanostructure owns high specific surface area and excellent electron emission properties. Moreover, the two-dimension arrayed nanostructure has the characteristics of photonic crystal and moth-eye effect. Currently, advanced lithographic methods such as electron beam (E-beam) or deep ultraviolet (DUV) lithography and X-ray lithography are adopted to define periodic nanoscale patterns. But these lithographic equipment are too expensive. Moreover, costly etching methods such as inductively coupled plasma reactive ion etching (ICP-RIE) or electron cyclotron resonance reactive ion etching (ECR-RIE) must be used to form arrayed silicon nanostructure with high aspect ratios. The nanoscale array patterns can be defined on the surface of the silicon wafer by the self-assembly of a polystyrene nanosphere. The photo-assisted electrochemical etching (PAECE) has the advantage of forming nanopore, and the aspect ratio of etched nanopores can be as high as 50:1 which is better than ICP-RIE. Therefore, PAECE is very suitable to fabricate nanostructure. This high-cost drawback makes most of academias and small/medium enterprises hard to invest in nanotechnology. This study combines the self-assembly nanosphere lithography (SANSL) process and photo-assisted electrochemical etching to fabricate a nanostructure array with a high aspect ratio on the surface of a silicon wafer.
Experimental results show that the nanosphere array with a nearly perfect arrangement can be obtained in the sample of 1.8 ∗1.8 cm2 by spin coating and vibration coating. Using reactive ion etching (RIE) can transfer the nanosphere array pattern to the silicon nitride layer, and form the etching window of PAECE. The concentration of the HF electrolyte used in PAECE was 2.5 wt%. When PAECE was performed with etching mask can produce deeper and periodic nanopores. The surfactant of SDSS added in the HF electrolyte of PAECE can reduce the contact angle of electrolyte and avoid the phenomenon of hole-reaming. When the voltage of 1 V is used to etch for 12.5 min, the etching depth of the nanopore array structure is about 5.69 μm and its diameter is about 90 nm, such that the aspect ratio of the pore can reach about 63:1. If the etching voltage was increased, the width of pore will be increased and the depth of pore will be reduced gradually at the same time. When the etching voltage of 2 V is applied to etch for 5 min, the etching height of the nanopillar is about 2 μm and its diameter is about 100 nm, such that the aspect ratio of the pillar can reach about 20:1. The nanopillar was arranged periodically according to the definition of nanosphere, therefore the arrayed nanopillar can be realized successfully.
Dropping the solution which has biological samples into the gap of nanopillar, it will affect the light which goes through the nanostructure and produce specific parameters of polarization. The results showed that when the DI water was dropped into the nanopillar structure, the degree of polarization (DOP) is 0.981, azimuth is 4.86° and ellipticity is 2.83°. When the solution which has alkaline lysis plasmid of 5 μg/ml was dropped into the nanopillar structure, the DOP is 0.957, azimuth is 7.7° and ellipticity is 3.99°. The result shows that the change of polarization parameter has the relations with the concentration of biological samples in solution. Therefore, the measure system can be combined with nanopillar array to develop the photonic crystal biosensor. This study also applies the developed nanopore nanostructure array to fabricate sub-wavelength antireflection structure of solar cell. Experimental results show that the deeper in structure and then the better in antireflective effect. After performing 1 V PAECE for 5 min, the weighted mean reflectance can be reduced to 1.73% under the wavelength range of 280–890 nm. Further coating of a silicon nitride layer on the surface of a nanostructure array reduces the weighted mean reflectance even to 0.878 %. Finally, this study also uses various voltage of PAECE to produce nanostructure array with different surface area for the electrode fabrication of fuel cell. Experimental results show that the larger in surface area of sample and then the better in catalysis effect. Two-staged PAECE of 1.5 V and 1.75 V can yield nanopillar with surface area of 14.2 cm2 , which is about 50.2 times higher than a planar electrode. When the surface of such a nanopillar array is coated with platinum of 1000 Å, the reaction current of nanopillar array is 10.2 mA, which is 72.9 times higher than that obtained by only a planar electrode.

總目錄 I
圖目錄 V
表目錄 XII
摘要 XIII

第一章 緒論
1.1 前言 1
1.2 微機電系統簡介 2
1.3 奈米科技簡介 4
1.3.1 奈米科技之市場前景 5
1.3.2 奈米結構的應用 7
1.4 文獻回顧 12
1.4.1奈米結構陣列製作技術 12
1.4.1.1 微影蝕刻法 12
1.4.1.2 奈米顆粒微影蝕刻法 14
1.4.1.3 氣液固法 16
1.4.1.4 模板成形法 17
1.4.2 奈米級微影技術 21
1.4.2.1 由上而下微影法 21
1.4.2.2 由下而上微影法 23
1.4.3 矽基高深寬比蝕刻技術 27
1.4.3.1 感應耦合電漿反應性離子蝕刻術 27
1.4.3.2 光輔助電化學蝕刻術 28
1.5 本論文之研究動機與架構 32
第二章 奈米結構陣列製作
2.1 前言 35
2.2 多孔矽的形成模型 37
2.2.1 Beale模型 37
2.2.2 Zhang模型 39
2.2.3 擴散機制模型 40
2.3實驗程序與實驗設備 44
2.3.1 實驗條件與方法 44
2.3.2 史托克(Stokes)參數與邦加球(Poincarè sphere) 47
2.3.3 實驗設備 50
2.3.4 實驗程序 53
2.4 實驗結果與討論 60
2.4.1 奈米球微影製程 60
2.4.2 光輔助電化學蝕刻製程 69
2.4.2.1 界面活性劑的影響 69
2.4.2.2有無蝕刻幕罩的蝕刻效果比較 76
2.4.2.3 蝕刻時間與蝕刻速率的關係 80
2.4.2.4 蝕刻電壓與蝕刻速率的關係 84
2.4.3 光子晶體之極化光檢測程序 92
2.5 結論與討論 96
第三章 奈米孔洞陣列應用於次波長抗反射結構製作
3.1 前言 98
3.2 文獻回顧 103
3.2.1太陽能電池抗反射結構 103
3.2.2次波長結構之探討 105
3.3實驗程序與實驗設備 107
3.3.1 實驗條件與方法 107
3.3.2 抗反射膜最佳厚度計算 108
3.3.3 加權平均抗反射率計算 109
3.3.4 實驗設備 113
3.3.5 實驗程序 113
3.4 實驗結果與討論 115
3.4.1 結構深度對反射率之影響 115
2.4.2 抗反射膜對反射率之影響 118
3.5 結論 124
第四章 奈米結構陣列應用於燃料電池電極板製作
4.1 前言 126
4.2 文獻回顧 130
4.3實驗程序與實驗設備 132
4.3.1 實驗條件與方法 132
4.3.2 實驗程序 132
4.3.3 實驗設備 133
4.4 實驗結果與討論 136
4.4.1 不同奈米陣列結構對催化的影響 136
4.4.2 觸媒厚度對催化反應之影響 142
4.5 結論 148
第五章 總結與未來展望
5.1 總結 149
5.2 未來展望 151
參考文獻 153

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