為改善玻璃基板上無電鍍銅層附著力，本研究使用二氧化鈦(TiO2)薄膜作為玻璃與銅層間的強化附著層，搭配自行研發之3-氨基丙基三乙氧基矽烷((3-Aminopropyl)triethoxysilane, APTES)包覆之自吸附奈米鈀觸媒，提升金屬銅層之附著力。
首部分將探討使用不同溶劑及還原劑乙醇/硼氫化納、乙二醇/硼氫化鈉以及乙二醇/氫氧化鈉(溶劑/還原劑)合成APTES-Pd對於觸媒的合成流程複雜度及表現。結果顯示，雖在活性以及粒徑方面不分軒輊，但從合成流程及後續發展的角度來看，乙醇/硼氫化納是最好的選擇。接著針對此配方合成之APTES-Pd進行討論，其粒徑小於10 nm，並以氨基朝內與鈀鍵結，矽烷氧基朝外的結構分散於溶液之中。朝外的矽氧基能與玻璃基板或是TiO2薄膜形成Si-O-Si或Si-O-Ti的共價鍵結，APTES-Pd得以在不需任何前處理的情況下吸附於基板之上，達到自吸附的效果。穩定性方面以粒徑、觸媒吸附表現、活性及結構四個方向探討，靜置40天的期間觸媒雖然會有離子化的情況發生，但在粒徑、吸附及活性方面表現穩定，顯示APTES-Pd具有一定的穩定性。此外，相較於商用離子鈀觸媒，APTES-Pd因其結構，能在玻璃基板上有優秀的吸附效果及無電鍍沉積表現。
第二部分探討TiO2強化附著層對於附著力之影響，沉積TiO2薄膜後附著力從72 gf/cm大幅提升至1392 gf/cm，撕裂面分析顯示銅層連帶玻璃被撕起的情況，說明附著力且已達到最高上限。本研究認為TiO2薄膜呈現孔洞結構，後續進行無電鍍銅製程時銅得以滲入孔洞，提升錨定效果，進而提升附著力。利用本研究製程所製造之銅層，與其他方式相比能通過3次的Reflow測試，顯示其可靠性。最後，也對於不同實驗參數如觸媒、TiO2薄膜厚度、退火溫度、孔洞大小以及無電鍍銅厚度對於附著力之影響進行探討。

This study aims to improve the adhesion of Cu film on glass substrate. To achieve this goal, we utilize titanium dioxide (TiO2) thin films as an adhesion promoter, coupled with a self-developed APTES-capped self-adsorption Pd nanoparticles APTES-Pd as an electroless deposition catalyst to enhance the adhesion between Cu film and glass substrate.
The first part of the study discusses characteristic and performance of APTES-Pd which synthesis by different solvents and reducing agents. Results show that ethanol/ sodium borohydride (solvent/reducing agents) is the best formulation. The structure of APTES-Pd facilitates the formation of covalent bond with glass substrates (Si-O-Si) and TiO2 films (Si-O-Ti), enabling APTES-Pd to adsorb onto substrates without any pre-treatment. Stability is evaluated in terms of particle size, adsorption performance, activity and structure. Despite ionization occurring, performance of particle size, adsorption performance and activity still maintain stable, indicating good stability of APTES-Pd. Furthermore, compare to commercial ion-Pd catalyst, APTES-Pd exhibits superior adsorption and copper deposition performance on glass substrates.
The second part of the study focuses on TiO2 thin film coated on glass as adhesion promoter. The adhesion test showed that the average peel strength significantly increased to 1392 gf/cm by spin coating TiO2 thin film on glass. Fracture surface analysis indicate that this adhesion reaches its limit. The study suggests that the porous structure of TiO2 films allows copper to deposit on pore, enhancing anchoring and adhesion. Copper layers produced by this process passed reflow tests three times, demonstrating good reliability. In the end, this study discusses effects of catalyst, porous TiO2 thickness, annealing temperature and pore size on adhesion.

摘要 I
Abstract II
目錄 III
圖目錄 VI
表目錄 X
第一章 緒論 1
1.1 前言 1
1.2 研究目的與動機 2
第二章 文獻回顧 3
2.1 玻璃基板於微電子產業之應用 3
2.1.1 中介層 3
2.1.2 薄膜電晶體液晶顯示器 4
2.1.3 微發光二極體 5
2.2 玻璃基板金屬化 6
2.2.1 濺鍍金屬法 6
2.2.2 蒸鍍金屬法 6
2.2.3 無電鍍金屬法 6
2.2.3.1 無電鍍銅鍍液的組成及特性 7
2.2.3.2 無電鍍銅的反應及觸媒催化機制 9
2.3 玻璃基板上無電鍍金屬化的挑戰與解決方法 12
2.3.1 機械粗化 12
2.3.2 熱退火處理 12
2.3.3 矽烷化合物表面改質 13
2.3.4 金屬氧化物強化附著層 17
2.4 鈀觸媒於無電鍍銅之應用 25
2.4.1 錫鈀膠體觸媒(Sn/Pd Colloid) 25
2.4.2 離子鈀觸媒(Ion-Pd) 26
2.4.3 奈米鈀觸媒 27
2.5 3-氨基丙基三乙氧基矽烷與奈米粒子 29
第三章 實驗 32
3.1 藥品與材料 32
3.2 儀器列表 33
3.3 分析方法及儀器原理 35
3.3.1 水滴接觸角量測儀 (Water Contact angle measurement) 35
3.3.2 原子力顯微鏡 (Atomic Force Microscope, AFM) 36
3.3.3 動態光散射儀 (Dynamic Light Scattering, DLS) 37
3.3.4 掃描式電子顯微鏡(Scanning electron microscope, SEM) 38
3.3.5 X射線光電子能譜儀(X-ray photoelectron spectroscopy, XPS) 39
3.3.6 萬能拉力機(Universal Testing Machine) 41
3.3.7 雙束型聚焦離子束顯微系統（Dual-beam Focused Ion Beam system, DB- FIB） 42
3.3.8 感應耦合電漿原子發射光譜儀（Inductively Couple Plasma Optical Emission Spectrometry, ICP-OES） 43
3.3.9 高解析穿透式電子顯微鏡（High Resolution Transmission Electron Microscope, HRTEM） 45
3.3.10 電化學分析儀(Electrochemical Analyzer) 46
3.3.11 迴焊爐(Reflow oven) 48
3.4 實驗方法 50
3.4.1 奈米鈀觸媒合成 50
3.4.2 無電鍍銅沉積 52
3.4.3 以TiO2為強化附著層之製程 53
3.4.4 玻璃基板高附著銅層之製程 54
第四章 結果與討論 55
4.1.1 不同合成配方之APTES-Pd鈀觸媒比較 55
4.1.2 APTES-Pd基本分析 58
4.1.3 APTES包覆奈米鈀觸媒結構 60
4.1.4 APTES-Pd自吸附於玻璃基板之機制 63
4.1.5 APTES-Pd穩定性分析 66
4.1.6 APTES-Pd與商用離子鈀觸媒 73
4.2 以TiO2為強化附著層之製程 75
4.2.1 TiO2強化附著層形貌 75
4.2.2 附著力結果分析 76
4.2.1 不同APTES-Pd及TiO2附著強化層製程參數之影響 82
第五章 結論 88
第六章 未來展望 90
第七章 參考資料 92

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