臺灣博碩士論文加值系統

本論文主要利用溶膠凝膠方式製備前驅物，藉由靜電紡絲裝置進一步製備成有機-無機複合纖維，所製備之複合纖維再利用煅燒方式將其聚合物分解，進一步製備純金屬氧化物纖維，本論文分為兩個主題進行。
第一主題:
我們使用四丁氧基鋯和硝酸氧鋯兩種不同的鋯前驅物，藉由polyvinyl pyrrolidone(PVP) 輔助電紡成奈米複合纖維，再經由高溫煅燒去除有機物而成氧化鋯纖維。以四丁氧基鋯為前驅物只要少量的PVP就能電紡出約250奈米直徑勻稱的複合纖維，經由煅燒的氧化鋯纖維直徑約200奈米。以硝酸氧鋯為前驅物需要較多量的PVP才能電紡出約200~500奈米直徑勻稱的複合纖維，再經由煅燒的氧化鋯纖維直徑約100~400奈米，並使用SEM、TG-DTA、FT-IR分析比較兩者複合纖維之特性及差異。

第二主題:
我們使用硝酸氧鋯和硝酸鈰所製作的複合前驅物，藉由polyvinyl pyrrolidone(PVP) 輔助電紡成奈米複合纖維，再經由高溫煅燒去除有機物而成金屬複合氧化物纖維，電紡出約600 nm ~ 2 µm的複合纖維，經煅燒700℃~800℃後可得些許中空管纖維，並利用SEM、TG-DTA、FT-IR分析複合纖維之特性及型態。

We have successfully to fabricate the metal oxide fibers via electrospinning method. Precursor of the fiber is a sol-gel which is made use of electrospinning installation to make into composite fibers. These composite fibers were calcined on atmosphere to decompose organic polymer and furthermore to from metal oxide fibers. There are two topics in this thesis.
The first topic:
We use Zirconium butylate and Zirconyl(IV) nitrate hydrate are two different Zirconium precursor by polyvinyl pyrrolidone (PVP) assisted electrospinning into nano-composite fibers. and then calcined to remove organic matter form zirconia oxide fiber by high-temperature. A Zirconium butylate precursor as long as the small amount of PVP of about 250 nm in diameter electrospinning symmetrical composite fibers, Zirconia fibers by calcined about 200 nm in diameter. Zirconyl(IV) nitrate hydrate as precursor amount of PVP to need more electrospinning about 200 to 500 nm in diameter symmetrical composite fiber. and then through calcined zirconia oxide fiber diameter of about 100 to 400 nm, using SEM, TG-DTA, FT-IR analysis and comparison of the two composite fiber characteristics and differences.
The second topic:
We use Zirconyl(IV) nitrate hydrate and Cerium(Ⅲ) nitrate hexahydrate precursor compound produced by polyvinyl pyrrolidone (PVP) assisted electrospinning into nano-composite fibers, and then through calcination to remove organic matter from metal composite oxide fiber diameter of about 600 nm ~ 2 µm. calcined 700℃ ~ 800℃ can get a little hollow fiber, and the use of SEM, TG-DTA , FT-IR analysis of the characteristics and type of nano-composite fibers.

誌謝............................................................................i
摘要..........................................................................iii
Abstract ......................................................................iv
目錄...........................................................................vi
表目錄.........................................................................ix
圖目錄..........................................................................x
1-1纖維簡介.....................................................................1
1-2 靜電紡絲纖維的製備..........................................................1
1-3 靜電紡絲製備奈米纖維........................................................2
1-3-1靜電紡絲簡介...............................................................2
1-3-2影響纖維的參數.............................................................3
1-4研究動機與目的...............................................................5
第二章 理論基礎與文獻回顧.......................................................6
2-1 ZrO2的特性與應用............................................................6
2-2 Ce2Zr2O7化合物..............................................................6
2-3 靜電紡絲的設備介紹..........................................................8
2-4 靜電紡絲有機前驅理論........................................................9
2-6靜電紡絲陶瓷前驅物組成介紹..................................................15
第三章 實驗流程................................................................19
3-1實驗方法....................................................................19
3-2 實驗設備...................................................................20
3-3 實驗藥品...................................................................21
3-4 實驗步驟...................................................................22
3-4-1 有機化合物(zirconium butylate)溶膠凝膠合成製備纖維.......................22
3-4-2 無機化合物(Zirconyl(IV) nitrate hydrate)溶膠凝膠合成製備纖維.............22
3-4-3 Ce/Zr化合物複合借助聚合物PVP溶膠凝膠合成製備複合材料纖維.................22
3-5鑑定儀器原理及分析..........................................................23
3-5-1 X光粉末繞射儀(X-ray Powder Diffractometer，簡稱XRD)......................25
3-5-2 傅立葉轉換紅外線光譜儀...................................................27
3-5-3差熱熱重分析儀(TG - DTA)..................................................29
第四章 結果與討論..............................................................31
4-1 靜電紡絲ZrO2纖維..........................................................31
4-1-1有機金屬化合物(zirconium butylate)為前驅物................................31
4-1-2靜電紡絲及纖維SEM圖.......................................................33
4-1-3 TG –DTA分析.............................................................39
4-1-4 FT-IR分析................................................................40
4-2-1 製備前驅物sol-gel........................................................42
4-2-2 SEM分析..................................................................42
4-2-3 TG-DTA分析...............................................................46
4-2-4 XRD......................................................................47
4-2-5 FT-IR分析................................................................48
4-2-6 小結.....................................................................50
4-3 靜電紡絲Ce2O3-ZrO2纖維.....................................................51
4-3-1 製備無機金屬Ce/Zr化合物為前驅............................................51
4-3-2 SEM分析..................................................................51
4-3-3 TG-DTA分析...............................................................56
4-3-4 XRD分析..................................................................58
4-3-5 FT-IR光譜分析............................................................59
4-3-6 UV/Vis光譜分析...........................................................60
第五章 總結論..................................................................61
後期展望.......................................................................62
參考文獻.......................................................................63
簡 歷..........................................................................69


表目錄
表4-1醋酸添加30min後變化.......................................................32
表4-2 sol-gel調配參數..........................................................34
表4-3有機金屬化合物纖維化學成分分析............................................38
表4-4無機金屬化合物纖維化學成分分析............................................45
表4-5 Ce/Zr無機金屬化合物纖維化學成分分析......................................55


圖目錄
圖1-1熔融型靜電紡絲裝置圖.......................................................2
圖1-2 工作距離不足造成之形態影響 (a)纖維堆疊膠黏 (b)纖維溶劑未甩乾堆疊形成薄膜..5
圖2-1 靜電紡絲系統 (a)系統裝置簡要圖 (b)實際裝置圖..............................9
圖2-2原理圖 (a)液滴在內部產生內應力以及在注射器尾部形成重力、表面張力及靜電力 (b)噴甩後泰勒錐彎曲不穩定鞭甩遠視圖...............................................11
圖3-1實驗與儀器鑑定流程圖......................................................19
圖3-2靜電紡絲設備示意圖........................................................20
圖3-3電子槍設備圖..............................................................23
圖3-4 SEM構造圖................................................................24
圖3-5 X-ray繞射原理示意圖 .....................................................26
圖3-6繞射圖形半高寬圖 .........................................................27
圖3-7傅立葉轉換紅外線光譜儀示意圖..............................................29
圖4-1攪拌30 min後 圖左為SA-5、圖中為SA-10、圖右為SA-15.........................32
圖4-2 靜電紡絲不同聚合物濃度SEM圖(a) PZ-0 (b) PZ-1 (c) PZ-2 (d) PZ-3 (e) PZ-4 (f) PZ-5 (g) PZ-6..............................................................35
圖4-3 有機化合物纖維不同煅燒溫度結果(a)未煅燒前(b)煅燒400℃持溫5小時(c)煅燒500℃持溫5小時(d)煅燒1000℃持溫5小時................................................36
圖4-4有機金屬化合物纖維SEM圖...................................................37
圖4-5有機金屬化合物纖維EDS分析圖...............................................37
圖4-6有機化合物纖維DT-TGA......................................................39
圖4-7有機化合物纖維FT-IR (a) PVP(b) Zr/PVP composite fiber (c) 600℃持溫5h (d) 700℃持溫5h (e) 800℃持溫5h (f) 900℃持溫5h。4-1-2無機化合物(Zirconyl(IV) nitrate hydrate)前驅物.........................................................41
圖4-8無機化合物前驅配製流程圖..................................................42
圖4-9有機化合物纖維不同溫度煅燒圖(a)未煅燒前(b)煅燒600℃持溫5小時(c)煅燒700℃持溫5小時(d)煅燒900℃持溫5小時。...................................................43
圖4-10無機金屬化合物纖SEM圖....................................................44
圖4-11無機金屬化合物纖維EDS分析圖..............................................44
圖4-12無機化合物纖維TG-DTA.....................................................46
圖4-13無機化合物纖維XRD (a)未煅燒前(b) 600℃持溫5h (c) 700℃持溫5h (d) 800℃持溫5h (e) 900℃持溫5h (f) 1000℃持溫5h。..........................................47
圖4-14 無機化合物纖維FT-IR (a) PVP (b)無機化合物纖維(c) 600℃持溫5h (d) 700℃..49
圖4-15製備流程圖...............................................................51
圖4-16 PVP/CeZr化合物纖維 (a) 5000倍率 (b) 10000倍率...........................52
圖4-17經600℃煅燒後5小時之CeO3-ZrO2纖維 (a) 15000倍率 (b) 30000倍率............52
圖4-18經700℃煅燒後5小時之CeO3-ZrO2纖維 (a) 5000倍率 (b) 20000倍率.............52
圖4-19經800℃煅燒後5小時之CeO3-ZrO2纖維(a) 2000倍率 (b) 7000倍率...............53
圖4-20 Ce/Zr無機金屬化合物纖維SEM圖............................................54
圖4-21 Ce/Zr無機金屬化合物纖維EDS分析圖........................................54
圖4-22 PVP DT-TGA..............................................................56
圖4-23 Ce/Zr化合物纖維TG-TGA曲線圖.............................................57
圖4-24 Ce/Zr化合物纖維XRD圖(a) CeO3-ZrO2纖維(b)600℃ (c) 700℃(d) 800℃(e) 900℃(f) 1000℃ 煅燒5小時......................................................58
圖4-25 FT-IR光譜分析(a) PVP (b)未煅燒之CeZr/PVP化合物纖維......................59
圖4-26纖維煅燒各溫度點UV/Vis 光譜圖...........................................60

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