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研究生： 劉建國
Chien-Kuo Liu
論文名稱： 高分子材料之加馬輻射效應及機械性質之研究
The effect of gamma ray radiation on the physical properties of polymers and their mechanical properties
指導教授： 李三保
Sanboh Lee
胡塵滌
Chen-Ti Hu
口試委員:
學位類別： 博士
Doctor
系所名稱： 工學院 - 材料科學工程學系
Materials Science and Engineering
論文出版年： 2005
畢業學年度： 93
語文別： 中文
論文頁數： 303
中文關鍵詞： 加馬輻射 、對排-聚苯乙烯 、質傳 、聚碳酸酯 、奈米壓痕
外文關鍵詞： gamma ray, syndiotactic polystyrene, mass transport, polycarbonate, nanoindentation
相關次數： 點閱：3  下載：0 
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    • 加馬輻射作用於聚碳酸酯(PC)、聚甲基丙烯酸甲酯(PMMA)及對排-聚苯乙烯(sPS)的光學性質，均造成穿透率下降及截止波長增加，穿透率之下降隨著所受加馬劑量的增加而增加，光學性質的改變可藉由退火處理而回復，但不同照射環境所造成之改變及可回復的程度不同。sPS於氧中受加馬輻射產生之色心均為永久色心，sPS於空氣和真空中受加馬輻射產生的可退火色心及自由基可經由退火過程消失，其色心及自由基消失的動力學均為一級反應過程，sPS於空氣中和真空中因加馬輻射所產生的自由基亦可於退火過程消失，然其動力學分別為一級及二級反應過程。加馬輻射作用對於sPS等溫結晶行為造成影響，其結晶度隨加馬劑量的增加而增加，於氧中受加馬輻射之結晶度大於在真空中受加馬輻射者，sPS於真空中受加馬輻射後之等溫結晶，其 □□□結晶形態隨著加馬劑量增加而增加，而 □□結晶形態則隨加馬劑量增加而稍微減少，於氧氣中受加馬輻射者則呈現相反之趨勢，熔融之sPS於220□C等溫結晶形成 □□□□形態結晶，然而受加馬輻射後之sPS之等溫結晶形態則轉變為 □□□□和 □□ 結晶形態。加馬輻射對於sPS非等溫結晶的過程有抑制的效應，其結晶起始溫度隨所受劑量增加而降低，且於氧中受輻射者下降明顯，其結晶成長維數介於二維和三維之間，加馬輻射對於試片的影響則是降低結晶成長的維數，輻射過程中氧與試片作用的結果，提高了 □□□形態結晶最大速率時的結晶溫度，sPS非等溫結晶過程的活化能值則隨著加馬劑量增加而減小。
    丙酮溶劑與PC之質傳行為為物理作用，且存在厚度及壓縮應力效應，丙酮於施加壓縮應力之PC中質傳所需克服的活化能小於未受應力作用者，但其質傳的活化能隨著厚度減小而增加，丙酮溶劑於質傳過程除了引發PC結晶之外，於35 ~ 20□C的質傳溫度亦使得厚度小於0.8 mm的PC表面產生週期性條紋，條紋的產生與溶劑引起的溶脹應力和結晶有關。本文提出綠豆和紅豆吸水的質傳模型，綠豆和紅豆吸水的質傳行為包括種皮潤濕和種仁的擴散過程，水於種皮潤濕過程中的濃度，隨吸收時間呈指數地增加，但於完全潤濕後則保持為常數，水於種仁中的擴散則遵循擴散定律。
    本文提出黏彈性材料之奈米壓痕負載-位移理論模型，可解釋於奈米壓痕量測過程位移量縮減之前的負載-位移關係，並與五種高分子之實驗數據相當符合，本理論並可解釋高分子等黏彈性材料於奈米壓痕負載-位移曲線中出現之“鼻子”現象。丙酮溶劑引發PC結晶的劈斷面，可分為三層結構，內層為試片玻璃態之心部，為未受溶劑影響之區域，中間層為溶脹層，為吸收溶劑而溶脹但尚未結晶完成之區域，接近試片外緣為結晶層，為溶劑引發結晶完全之區域，溶脹層與試片玻璃態之心部有明顯界線分隔，結晶層與溶脹層則是以晶粒成核和成長區域分界，其結晶為球晶型態，溶劑引發結晶之速率小於溶劑擴散之速率，藉由奈米壓痕量測可以得到溶脹層和結晶層的楊氏模數和硬度值，其楊氏模數及硬度值之大小依序為結晶層 > 溶脹層 > 試片玻璃態之心部。

    第一章 緒論 1.1 高分子與材料的作用 1.1.1 輻射的種類及單位……………………………………………………..…………………1 1.1.2 影響輻射效應的因素……………………………………………………………………..1 1.1.3 輻射對高分子材料反應的機制..………………………...……………………………….4 1.1.4 輻射影響高分子材料機械和物理性質………………………………….……………….5 1.1.5 對排-聚苯乙烯(syndiotactic polystyrene, sPS)…………………………………………...6 1.2 高分子材料與溶劑的質傳行為 1.2.1 質傳的分類………………………………………………………………………………..7 1.2.2 影響質傳的因素……………………………………………….………………………….8 1.2.3 質傳模型……………………………………………………………….………………….9 1.2.4 溶劑引發結晶……………………………………………………………………………11 1.3 黏彈性高分子材料的奈米壓痕行為…………………………………………..…………….12 1.4 本文研究動機與目的………………………………………….……………………………..15 附圖…………………………………………………………………………..……………………..17 第二章 加馬輻射影響高分子光學性質及色心消失動力學研究 2.1節 真空、空氣和氧中照射加馬射線對高分子光學性質的影響 2.1.1 簡介………………………………………………………………….…………………….18 2.1.2 實驗步驟……………………………………………………………………………….….19 2.1.2.1 材料………………………………………………………………..………………….19 2.1.2.2 試片製備…………………………………..………………………………………….20 2.1.2.3 加馬照射…………………………………………………………….………………..20 2.1.2.4 紫外-可見光譜儀量測……………………………………………………...……...…20 2.1.2.5 霍氏轉換紅外光譜儀量測……………………………………………………….…..21 2.1.3 結果與討論……………………………………………………………….……………….21 2.1.3.1 聚碳酸酯(PC)………………………………………………………...…….…………22 2.1.3.2 聚甲基丙烯酸甲酯(PMMA)………………………………………..………………..23 2.1.3.3 對排-聚苯乙烯(sPS)………………………………………………………………….24 2.1.2.4 氧的效應……………………………………………………………….……………..25 2.1.4 結論…………………………………………………………………………………..……26 附表…………………………………………………………...………………………………….28 附圖……..………………………………………………………………………………………..30 2.2節 受加馬照射之非晶態對排-聚苯乙烯於退火過程色心消失之動力學分析 2.2.1 簡介…………………………………………………………………………...…..……….50 2.2.2 實驗步驟……………………………………………………………………………….….51 2.2.2.1 材料………………………………………………………………..………………….51 2.2.2.2 試片製備…………………………………………………………..………………….51 2.2.2.3 加馬照射…………………………………………………………….………………..52 2.2.2.4 熱性質量測……………………………………………………..…………………….52 2.2.2.5 紫外-可見光譜儀量測………………………………………………………………..52 2.2.2.6 電子順磁共振儀量測…………………………………………………………..…….52 2.2.2.7 紅外光譜儀量測………………………………………………………………..…….53 2.2.3 結果與討論……………………………………………………………………….……….53 2.2.3.1 DSC量測分析…………………………………………………………………………53 2.2.3.2 UV-Vis光譜分析……………………………………………………………….……..54 2.2.3.3 試片厚度之影響…………………………………………………………..………….55 2.2.3.4 色心消失動力學模型…………………………………………………….…………..56 2.2.3.5 UV-Vis光譜儀量測分析…………………………………………………………...…57 2.2.3.6 單色儀臨場量測分析……………………………………………………………...…59 2.2.3.7 自由基消失動力學…………………………………………………………………...60 2.2.3.8 電子自旋共振(EPR)譜分析……………………………………………………….…62 2.2.3.9 FT-IR光譜分析…………………………………………………………………..……63 2.2.4 結論…………………………………………………………………………………..……64 附表………………………………………………………………………...…………………….66 附圖……..………………………………………………………………………………………..70 第三章 加馬輻射影響對排-聚苯乙烯結晶熔融行為及動力學研究 3.1節 受加馬輻射之對排-聚苯乙烯等溫結晶熔融行為分析 3.1.1 簡介………………………………………………………………….…………………….94 3.1.2 實驗步驟……………………………………………………………………………….….96 3.1.2.1 材料………………………………………………………………..………………….96 3.1.2.2 試片製備…………………………………..………………………………………….96 3.1.2.3 加馬照射…………………………………………………………….………………..96 3.1.2.4 等溫結晶量測……………………………………………………...……………....…96 3.1.2.5 紅外光譜量測…………………………………………………………………….…..97 3.1.2.6 X-ray繞射儀量測…………………………………..………………………..………97 3.1.2.7 偏極光顯微鏡觀察………………………………………………………………….97 3.1.3 結果與討論……………………………………………………………….……………….97 3.1.4 結論………………………………………………………………………………..……101 附表…………………………………………………………...……………………………..….103 附圖……..………………………………………………………………………………………105 3.2節 受加馬輻射照射之對排-聚苯乙烯非等溫結晶動力學分析 3.2.1 簡介…………………………………………………………………………...………….114 3.2.2 實驗步驟……………………………………………………………...………………….116 3.2.2.1 材料…………………………………………………………………....…………….116 3.2.2.2 試片製備…………………………………………………………..…..…………….116 3.2.2.3 加馬照射…………………………………………………………….………………116 3.2.2.4 非等溫結晶量測…………………………………………………………………….116 3.2.2.5 X-ray繞射儀量測………………………………………………………………..…..117 3.2.3 結果與討論……………………………………………………………………….…..….117 3.2.3.1 修改之Avrami方程式及Ozawa方法………………………………………………117 3.2.3.2 非等溫結晶放熱峰及相對結晶度計算……………………………...……….…….119 3.2.3.3 於真空中受加馬照射之對排-聚苯乙烯非等溫結晶行為………..………….…….120 3.2.3.4 於空氣中受加馬照射之對排-聚苯乙烯非等溫結晶行為…………………..……..121 3.2.3.5 於氧氣中受加馬照射之對排-聚苯乙烯非等溫結晶行為…………………………122 3.2.3.6 非等溫結晶的活化能…………………………………………………..………...…123 3.2.3.7 非等溫結晶結構分析………………………………………………..……………...125 3.2.4 結論………………………………………………………………………...………….…125 附表………………………………………………………………………...………...…………127 附圖……..………………………………………………………………………………………135 第四章 溶劑在高分子材料及有機質中的質傳分析及其模型之建立 4.1節 丙酮於外施壓縮應力之聚碳酸酯的質傳行為及厚度效應 4.1.1 簡介………………………………………………………………….………………...…146 4.1.2 實驗步驟…………………………………………………………………………………147 4.1.2.1 材料………………………………………………………………..……...…………147 4.1.2.2 試片製備…………………………………..………………………………...………147 4.1.2.3 外施壓縮應力………………………………………….……………………………147 4.1.2.4 質傳量測……………………………………………………...…………..……....…148 4.1.2.5 光學顯微鏡觀察表面形態……………..…………………………………...………148 4.1.3 結果與討論……………………………………………………………….………...……148 4.1.3.1 壓縮應力對質傳之效應……………………………………………….……………148 4.1.3.2 厚度對質傳之效應……………………………...……….………………………….151 4.1.3.3 壓縮應力對平衡溶脹比(equilibrium-swelling ratio)之效應………..…………...…152 4.1.3.4 厚度對平衡溶脹比之效應…………………………………………………...……..152 4.1.3.5 時效(aging)處理對平衡溶脹比之效應………………………………..……………153 4.1.3.6 FT-IR光譜分析…………………………………………………..…………...…...…153 4.1.3.7 表面形態分析………………………………………………………..……………...154 4.1.4 結論…………………………………………………………………………..…………..156 附表…………………………………………………………...……………………………..….157 附圖……..………………………………………………………………………………………160 4.2節 豆子吸收水之質傳模型的建立及實驗驗證 4.2.1 簡介…………………………………………………………………………...………….173 4.2.2 質傳模型………………………………...……………………………………………….174 4.2.2.1 水吸收(water absorption)模型……………………...………………....…………….174 4.2.2.2 種皮潤濕(testa wetting)理論………………..………………………………...…….177 4.2.3 實驗步驟…………………………………………………………………………………178 4.2.3.1 材料………………………………………………………………..……...…………178 4.2.3.2 加馬照射…………………………………………….………………………………179 4.2.3.3 質傳量測………………………………………….…………………………………179 4.2.3.4 熟度測試………………………………...…………..………………………........…179 4.2.4 結果與討論……………………………………………………………………….…..….179 4.2.4.1 綠豆吸收水之質傳………………………………………………….………………180 4.2.4.2 紅豆吸收水之質傳……………………………...…………………………….…….182 4.2.4.3 黃豆與黑豆吸收水之質傳………..…………………………………………..…….183 4.2.4.4 文獻分析（加州小白豆及黃豆）…………………………………………...……..184 4.2.4.5 種皮對水吸收的效應……………………………………………………….………184 4.2.5 結論………………………………………………………………………...………….…185 附表………………………………………………………………………...………...…………186 附圖……..………………………………………………………………………………………189 第五章 高分子機械性質-奈米壓痕理論模型之建立及量測 5.1節黏彈性材料之奈米壓痕負載-位移關係 5.1.1 簡介…………………………………………………………………...………………….198 5.1.2 理論模型建立………………………….………………………………………….….….199 5.1.3 實驗步驟…………………………………………………………………………………203 5.1.3.1 材料………………………………………………………………..………………...203 5.1.3.2 試片製備…………………………………..………………………………...………204 5.1.3.3 奈米壓痕量測……………………………….…………………………...………….204 5.1.3.4 固定負載、卸載速率量測…………………………………………...…………....…204 5.1.3.5 潛變量測…………………………………………………………………….………205 5.1.4 結果與討論……………………………………………………………….………...……205 5.1.5 結論……………………………………………………………………………..…..……208 附表…………………………………………………………...……………………………..….210 附圖……..………………………………………………………………………………………211 5.2節 丙酮溶劑引發聚碳酸酯結晶之形態及奈米壓痕量測 5.2.1 簡介…………………………………………………………………………...………….219 5.2.2 實驗步驟……………………………………………………………...………………….220 5.2.2.1 材料…………………………………………………………………....…………….220 5.2.2.2 試片製備…………………………………………………………..…..…………….220 5.2.2.3 溶劑吸收…………………………………………………………….………………220 5.2.2.4 密度量測…………………………………………………………………………….220 5.2.2.5 熱性質量測……………………………………………………………………...…..220 5.2.2.6 X-ray繞射儀量測……………………………………………………………………221 5.2.2.7 光學顯微鏡觀察結晶及劈裂面形態……………………………………………...221 5.2.2.8 奈米壓痕量測……………………………………………………………………….221 5.2.3 結果與討論……………………………………………………………………….…..….222 5.2.4 結論………………………………………………………………………...………….…225 附表………………………………………………………………………...………...…………227 附圖……..………………………………………………………………………………………229 第六章 總結與未來展望 6-1總結……………………………………………………………………………………………235 6-2未來展望………………………………………………………………………………………236 附錄A 豆子吸收水之質傳模型求解…………………………………………………………….238 附錄B 黏彈性材料之柏格斯模型(Burgers model)……………………………………………...249 附錄C 聚甲基丙烯酸甲酯(PMMA)與氘化甲醇(CH3OD)裂縫癒合系統研究………………...262 參考文獻………………………………………………………………………………..…………281

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