臺灣博碩士論文加值系統

摘 要
本實驗以溶液聚合法（solution polymerization）製備具有低介電常數特性的芳香族聚亞胺。以MIM結構量測聚亞胺之介電常數、崩潰電場和散逸因子，利用TGA量測聚亞胺的熱裂解溫度，並對聚亞胺做黏度和吸濕性測試，量測聚亞胺的固有黏度和吸濕率。黏度量測結果顯示，芳香族聚亞胺的固有黏度範圍是0.45∼0.57 dL/g，在氮氣環境下對聚亞胺所做的熱性質分析結果顯示，聚亞胺5％熱裂解溫度大約486 ~ 498℃，證明聚亞胺具有優良的熱穩定性，實驗結果並顯示聚亞胺具有低介電常數（範圍從2.23∼2.97）、低吸濕性（小於0.6％）和高崩潰電場（範圍從0.86∼3.81 MV/cm）的優點，但散逸因子量測結果顯示，測試頻率超過數個MHz之後，聚亞胺之介電損失特性不盡理想，其有待後續之研究改進。

ABSTRACT
Solution polymerization was applied to prepare the low dielectric constant aromatic polyimines and their physical properties were investigated. We evaluated electrical properties of polyimines including dieletric constant, breakdown voltage and dissipation factor. Thermal decomposed temperature of polyimine was measured by thermal gravimetric analyzer (TGA) to evaluate the thermal stability of the polymer specimens. We also measured the inherent viscosity and moisture absorption index of aromatic polyimines. The aromatic polyimines have inherent viscosities of 0.45 ~ 0.57 dL/g. The TGA results showed that the temperatures of 5% weight loss of aromatic polyimines are in the range of 486 ~ 498℃ in nitrogen ambient, indicating that the aromatic polyimines possess excellent thermal stability. Electrical property is measurement indicated that the aromatic polyimines have lower dielectric constant (ranging from 2.23 to 2.97), lower moisture absorption (＜0.6%), and high breakdown voltage (ranging from 0.86 to 3.81 MV/cm). However, dissipation factor measurement revealed that the dielectric loss property of polyimines remains unsatisfactorily when the frequency exceeds several MHz and further study is required.

目錄
中文摘要………………………………………………………………•Ⅰ
英文摘要………………………………………………………………•Ⅱ
誌謝……………………………………………………………………•Ⅳ
目錄……………………………………………………………………•Ⅴ
圖目錄…………………………………………………………………•Ⅷ
表目錄…………………………………………………………………•Ⅹ
第一章 前言……………………………………………………………•1
第二章 文獻回顧………………………………………………………•3
2.1 聚亞胺（polyimine）簡介……………………………………•3
2.1.1 聚亞胺的聚合方法………………………………………•4
2.1.2 聚亞胺的導電特性………………………………………•7
2.2 介電理論………………………………………………………•9
2.3 低介電常數材料的需求………………………………………•12
2.4 低介電常數材料的發展………………………………………•15
2.4.1 二氧化矽（SiO2）………………………………………•16
2.4.2 氟化矽酸鹽玻璃（FSG）………………………………•17
2.4.3 摻雜碳的二氧化矽………………………………………•17
2.4.4 含氫矽酸鹽類（HSQ）…………………………………•18
2.4.5 含甲烷基矽酸鹽類（MSQ）……………………………•19
2.4.6 聚四氟乙烯（PTFE）…………………………………… 20
2.4.7 氟化聚亞醯胺（FPI）…………………………………… 20
2.4.8 聚芳香烯醚（PAE）……………………………………… 22
2.4.9 Benzocyclobutene（BCB）……………………………… 23
2.4.10 SiLK …………………………………………………… 23
2.5 研究動機………………………………………………………•25
第三章 實驗方法………………………………………………………27
3.1 實驗藥品………………………………………………………•27
3.2 實驗儀器………………………………………………………•31
3.3 實驗流程………………………………………………………•32
3.4 實驗步驟………………………………………………………•33
3.4.1 烘膜方法…………………………………………………•35
3.4.2 下電極的製作……………………………………………•35
3.4.3 介電層的製膜……………………………………………•35
3.4.4 上電極的製作……………………………………………•36
3.5 溶解度測試方法………………………………………………•36
3.6 黏度量測方法…………………………………………………•37
3.7 傅氏紅外線光譜儀（FTIR）量測方法……………………•38
3.8 熱重分析儀（TGA）量測方法…………………………………38
3.9 吸濕性量測方法………………………………………………•39
3.10 抗張強度量測方法…………………………………………•39
3.11 電性量測方法…………………………………………………•42
第四章 結果與討論……………………………………………………43
4.1 聚亞胺的成膜性………………………………………………43
4.2 溶解度測試……………………………………………………46
4.3 黏度測試………………………………………………………49
4.4 FTIR光譜分析…………………………………………………50
4.5 熱性質分析……………………………………………………52
4.6 吸濕性測試……………………………………………………55
4.7 機械性質測試…………………………………………………56
4.8 介電常數量測…………………………………………………58
4.9 散逸因子（tanδ）對頻率特性的量測………………………60
4.10 介電常數對頻率量測…………………………………………63
4.11 崩潰電場量測…………………………………………………65
4.12 未來展望………………………………………………………68
第五章 結論……………………………………………………………69
參考文獻………………………………………………………………72
圖目錄
圖2-1 聚亞胺的聚合時間與固有黏度的關係圖………………………4
圖2-2 MePPD-TA的結構示意圖………………………………………5
圖2-3 聚亞胺的聚合反應式……………………………………………6
圖2-4 導電高分子的導電模式示意圖…………………………………8
圖2-5 四種不同的極化機構…………………………………………•10
圖2-6 極化和頻率的關係圖…………………………………………•11
圖2-7 積體電路中線寬和時間的關係圖……………………………•12
圖2-8 FSG的結構示意圖……………………………………………17
圖2-9 HSQ的結構示意圖……………………………………………19
圖2-10 MSQ的結構示意圖…………………………………………•19
圖2-11 PTFE的結構示意圖…………………………………………•20
圖2-12 BPDA－PDA的結構示意圖…………………………………21
圖2-13 PMDA-TFMOB-6FDA-PDA的結構示意圖…………………21
圖2-14 FLARE 1.0、FLARE 2.0及PAE-2的結構示意圖…………•22
圖2-15 BCB的結構示意圖…………………………………………•23
圖2-16 SiLK的結構示意圖…………………………………………•24
圖3-1 實驗流程圖……………………………………………………•32
圖3-2 實驗的基本反應式……………………………………………•33
圖3-3 實驗裝置圖……………………………………………………•34
圖3-4 尤伯洛德毛細管黏度計………………………………………•37
圖3-5 啞鈴形試片的示意圖…………………………………………•39
圖3-6 工程應力-工程應變曲線圖…………………………………••40
圖4-1 無法成膜之聚亞胺結構示意圖………………………………•45
圖4-2 可以成膜之聚亞胺結構示意圖………………………………•46
圖4-3 對苯二甲醛與各種二胺類的FTIR光譜圖…………………•51
圖4-4 間苯二甲醛與各種二胺類的FTIR光譜圖…………………•52
圖4-5 對苯二甲醛與各種二胺類的熱重損失圖……………………•54
圖4-6 間苯二甲醛與各種二胺類的熱重損失圖……………………•55
圖4-7 介電常數與置放時間的關係圖………………………………•60
圖4-8 四種聚亞胺與Kapton的散逸因子（tanδ）對頻率關係圖…62
圖4-9 四種聚亞胺與Kapton之f × Q對頻率的關係圖……………•63
圖4-10 TPBA和TPBP的介電常數對頻率關係圖…………………•64
圖4-11 IPBA和IPBP的介電常數對頻率關係圖…………………•64
圖4-12 TPBA的漏電流密度對電場圖………………………………66
圖4-13 TPBP的漏電流密度對電場圖………………………………66
圖4-14 IPBA的漏電流密度對電場圖………………………………67
圖4-15 IPBP的漏電流密度對電場圖………………………………67
表目錄
表2-1 製程技術與介電常數的相對關係……………………………13
表2-2 低介電常數材料的基本條件…………………………………14
表2-3 低介電常數材料之介電常數與沈積方式的關係……………15
表2-4 SiO2的沈積方式與特性………………………………………16
表 2-5 SiLK的相關特性………………………………………………25
表4-1 對苯二甲醛與各種二胺類所合成聚亞胺的成膜性…………43
表4-2 間苯二甲醛與各種二胺類所合成聚亞胺的成膜性…………44
表4-3 對苯二甲醛與各種二胺類所合成聚亞胺的溶解度關係……47
表4-4 間苯二甲醛與各種二胺類所合成聚亞胺的溶解度關係……48
表4-5聚亞胺的黏度測試結果………………………………………50
表4-6 聚亞胺5％的熱裂解溫度……………………………………53
表4-7 聚亞胺的吸濕率………………………………………………56
表4-8 聚亞胺與其他低介電常數材料的機械性質…………………57
表4-9 聚亞胺的介電常數值…………………………………………59
表4-10 四種聚亞胺、Kapton和BCB的崩潰電場…………………65

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