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研究生: 江宗穎
TZONG-YIING CHIANG
論文名稱: 聚丙烯腈系電紡不織布高溫氧化處理物性與 微細構造之研究
A Study on Effect of Oxidized Stabilization Process on The Physical Properties And The Microstructure of Polyacrylonitrile(PAN)-based Electrospinning Non-woven
指導教授: 蘇清淵
Ching-Iuan Su
口試委員: 李俊毅
Jiunn-Yih Lee
學位類別: 碩士
Master
系所名稱: 工程學院 - 材料科學與工程系
Department of 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: 127
中文關鍵詞: 氧化工程靜電紡絲奈米纖維環化指數限氧指數
外文關鍵詞: Limit Oxygen Index, Nanofibers, Oxidization, Electrospinning, Aromatization Index.
相關次數: 點閱:333下載:7
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  • 本研究採用聚丙烯腈為原料,利用靜電紡絲機製造奈米纖維布,以差式掃描熱量分析儀(DSC)與熱重量分析儀(TGA)熱分析結果,選取氧化條件參數,分別設定溫度為270、300與330℃三種,加熱時間為30、50、70 min與在有、無張力下進行氧化工程,探討不同的氧化條件,對聚丙烯腈系電紡布表觀與微細構造的影響。實驗結果得知,經氧化穩定加工後,電紡布隨氧化的溫度、時間與張力之增加,其強度與產率有逐漸下降的趨勢。織物重量損失率與收縮率隨著張力之增加,氧化溫度的提高,以及加熱時間的增長,亦隨之增大。氧化布之柔軟度隨氧化溫度的增高與時間的增長,而隨之降低,亦即挺硬度增大。且氧指數(LOI) 隨著氧化時間及溫度的提高而增加。氧化織物之顏色變化,在熱處理溫度300℃,加熱70分鐘時,呈現之黑色表觀,具有較穩定的結構,且環化指數值達62\%,經由SEM觀察,為均齊的非織物形態,當氧化溫度達到330℃,70 min時,氧化布產生脆化現象。綜合以上分析,氧化溫度在300℃,加熱時間為70min時,其環化已達氧化完全程度,且氧指數(LOI)值達43,顯示其為不燃纖維,而其他物性亦適合於後道加工之處理,此為本研究之最佳氧化處理條件。


    In this study we utilized an Electrospinner (ES) to produce precursor of PAN-based oxidized nanofibers non-woven fabrics from Polyacrylonitrile (PAN) fiber solution. The parameters of oxidized process used in this experiment chosen by the thermal analysis results of DSC and TGA were: oxidized temperature of 270, 300, and 330 ℃ and heating time of 30, 50, and 70 min, and three kinds of tension.
    The variation in yield rate, breaking strength, shrinkage and stiffness of PAN-based oxidized Electrospinning non-woven fabrics (ESNF) were examined in this article. The results indicated that the physical properties of ESNF were determined by oxidized conditions. In addition, the limit oxygen index (LOI) increased as these thermal conditions of temperature and time increased. As to the color-change of the oxidized ESNF, the black-colored ESNF showed the stabilized aromatic structure with higher Aromatization Index (AI).
    The experimental results showed that the optimum oxidized condition were 300℃ thermal temperature and 70 min heat time resulting in steady production and better properties of the PAN-based oxidized ESNF of 62\% AI and 43 LOI, ultimately yielding a good precursor of after-finishing process of carbonization.

    摘要I ABSTRACTII 誌謝III 目錄V 圖目錄VIII 表目錄XI 第一章、緒論1 1.1 前言1 1.2奈米纖維材料的定義及形態3 1.2.1奈米纖維材料的定義及形態3 1.2.2奈米纖維的製備方法與應用6 1.2.3傳統式纖維材料之熱處理加工方法與應用11 1.2.4奈米纖維之熱處理加工與應用13 1.3研究的動機與目的15 第二章、文獻回顧與原理16 2.1靜電紡絲工程與原理16 2.2氧化工程與原理19 2.2.1聚丙烯腈纖維受熱環化20 2.2.2氧對氧化工程的影響22 2.3聚丙烯腈纖維熱處理之發色原理25 2.3.1聚丙烯腈纖維受熱之變色基團26 2.3.2聚丙烯腈纖維受熱之變色機構27 第三章、實驗31 3.1實驗材料31 3.1.1 實驗原物料31 3.1.2 實驗藥劑與氣體31 3.2實驗設備與測試分析儀器32 3.2.1實驗設備32 3.2.2實驗測試分析儀器32 3.3實驗架構33 3.4實驗方法34 3.4.1聚丙烯腈系電紡不織布的準備工程34 3.4.2聚丙烯腈系電紡氧化布的備製35 3.4.3聚丙烯腈系電紡不織布熱性質分析37 3.4.4聚丙烯腈系電紡不織布氧化後微細構造分析38 3.4.5聚丙烯腈系電紡不織布氧化後之物性測試方法40 第四章、結果與討論42 4.1聚丙烯腈系電紡不織布熱性質分析42 4.1.1差式掃描熱量分析43 4.1.2差式掃描熱量與熱重量之綜合分析45 4.1.3氧化工程之溫度與時間的設定47 4.2聚丙烯腈系電紡不織布氧化後之物性探討48 4.2.1強力49 4.2.2收縮率54 4.2.3柔軟度64 4.2.4重量損失率69 4.2.5氧化產率74 4.2.6限氧指數79 4.3表觀顏色變化分析85 4.4 SEM觀察分析90 4.5廣角X-ray 繞射分析95 4.6最佳化熱處理條件分析103 第五章、結論106 參考文獻109

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