製備氧化鋅/鐵酸鋅層次級奈米結構與其本質催化性質之研究

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楊智傑(Jhih-jie Yang) 查詢紙本館藏

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材料科學與工程研究所

論文名稱

製備氧化鋅/鐵酸鋅層次級奈米結構與其本質催化性質之研究
(Fabrication of ZnO/ZnFe2O4 hierarchical nanostructures with improved intrinsic peroxidase-like activity)

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摘要(中)

近年來鐵酸鋅被發現具有類似過氧化酶催化活性 (peroxidase activity)，可將過氧化氫分解為氫氧自由基。過氧化氫通常會在有機物分解過程中產生，例如葡萄糖可被葡萄糖氧化酶 (GOx) 氧化為葡萄糖酸以及過氧化氫。由於鐵酸鋅有優異的本質過氧化酶活性，且於大多催化反應中具有良好的抗腐蝕能力以及結構穩定性，因此鐵酸鋅相當有潛力可應用於葡萄糖檢測及染料降解。由於鐵酸鋅的本質催化活性與其形貌及維結構有關，降低材料維度可有效地增加比表面積，因此能顯著的提升其催化性質。
本研究中共分兩大方向去提升鐵酸鋅催化活性。首先我們結合靜電紡絲技術與溶膠凝膠法製備氧化鋅/鐵酸鋅玉米穗棒狀奈米複合材料，鐵酸鋅奈米顆粒源自金屬鹽類前驅液中的Fe(OH)3晶核熱分解。由於鐵酸鋅奈米顆粒可提供額外的反應面積，故展現出優異的催化活性與葡萄糖檢測能力。
第二部分則是利用選擇性蝕刻方式製備氧化鋅/鐵酸鋅介孔複合奈米纖維。於SEM影像中顯示在經過化學蝕刻後的樣品表面出現許多微小孔洞，這些孔洞性質可藉由氮氣吸附-脫附儀分析，結果顯示蝕刻過後可將比表面積由30.1 m2/g 增加至38.3 m2/g，平均孔洞直徑由7.9 nm增加至12.2 nm，總孔洞體積由0.082 cm3/g增加至0.157 cm3/g。綜合SEM、XRD、BET及BJH量測結果顯示選擇性蝕刻能有效提升複合奈米纖維比表面積以及孔洞體積。由於蝕刻後的複合奈米纖維具有較大的比表面積，因此展現出較優異的催化活性。

摘要(英)

Recently, extensive research has shown that zinc ferrite possessed intrinsic peroxidase-like activity and it can catalyze H2O2 into hydroxyl radical. It is known that H2O2 is the main product of the glucose oxidase (GOx)-catalyzed reaction. Since it can be catalyzed by ZnFe2O4 to produce the color signal, the colorimetric detection of glucose can be realized. The peroxidase-like activity of zinc ferrite is strongly dependent on its morphology and microstructure. Thus, reducing the dimension of material can effectively enhance the catalytic ability.
This thesis contains two sections. First, we combined the electrospinning technique and sol gel method to fabricate ZnO/ZnFe2O4 composite nanocobs. The appearance of zinc ferrite NPs is due to the decomposed Fe(OH)3 nuclei in the metal salt precursor at annealing processes. Because zinc ferrite NPs can provide extra surface area, it possesses outstanding catalytic ability of glucose detection and degradation of dye.
Second, we utilized the selective etching method to fabricate mesoporous composite nanofiber. SEM images showed that a large number of mesopoles appeared at the surface after etching. The structural information of the etched sample were obtained by BET and BJH. The measurement results presented that the surface area, average pore diameter and total pore volume of the sample after etching were increased from 30.1 to 38.3 m2/g, 7.9 to 12.2 nm and 0.082 to 0.157 cm3/g, respectively. In summary, the result of SEM, XRD, BET and BJH indicated that the selective etching is an effective method to fabricate mesoporous nanofiber. Owing to the larger surface area, the sample after etching shows a better intrinsic peroxidase-like activity.

關鍵字(中)

★ 鐵酸鋅
★ 靜電紡絲
★ 選擇性蝕刻
★ 過氧化氫酶物質

關鍵字(英)

★ zinc ferrite
★ electrospinning
★ selective etching
★ peroxidase mimic

論文目次

摘要 i
Abstract ii
致謝 iii
目錄 v
圖目錄 viii
表目錄 xii
第一章緒論 1
1.1鐵酸鋅材料介紹 1
1.2製備鐵酸鋅奈米結構 2
1.2.1模板輔助法 (Template assisted method) 4
1.2.2靜電紡絲法 (Electrospinning) 5
1.3鐵酸鋅奈米纖維應用領域 6
1.3.1電磁波吸收材料 6
1.3.2 鋰電池陽極材料 7
1.3.3光催化 8
1.3.4葡萄糖感測 9
第二章分析儀器與實驗方法 10
2.1實驗藥品 10
2.2實驗流程 11
2.3實驗儀器 13
2.3.1靜電紡絲實驗機 (Nanofiber Electrospinning Unit) 13
2.3.2管型爐 (Tube Furnace) 14
2.3.3掃描式電子顯微鏡 (Scanning Electron Microscopy) 14
2.3.4 X光粉末繞射儀 (X-ray Diffraction) 14
2.3.5穿透式電子顯微鏡 (Transmission Electron Microscopy) 15
2.3.6氮氣等溫吸脫附儀 (N2 adsorption/desorption isotherm, ASAP2020) 15
2.3.7可見光/紫外光光譜儀 (UV/Visible Spectrometers) 16
第三章製備氧化鋅/鐵酸鋅玉米穗棒狀複合纖維應用於葡萄糖檢測及有機染料降解 17
3.1 研究動機 17
3.2 實驗步驟 20
3.2.1金屬鹽類前驅液配製 20
3.2.2靜電紡絲 20
3.2.3退火 21
3.2.4利用類過氧化酶活性降解有機染料 21
3.2.5葡萄糖檢測 22
3.3 實驗結果與討論 23
3.3.1靜電紡絲操作參數優化 23
3.3.3 XRD相鑑定分析 31
3.3.3 TEM微結構分析 32
3.3.4氧化鋅/鐵酸鋅玉米穗棒狀複合纖維成長機制探討 34
3.3.5鐵酸鋅/氧化鋅奈米纖維降解有機染料之特性 36
3.3.6葡萄糖感測性質量測 41
3.4結論 44
第四章利用選擇性蝕刻法製備氧化鋅/鐵酸鋅介孔奈米纖維應用於葡萄糖檢測及有機染料降解 45
4.1 研究動機 45
4.2實驗步驟 46
4.2.1利用選擇性蝕刻方式製備介孔奈米纖維 (M0.5/NaOH) 46
4.2.2利用類過氧化酶活性降解有機染料 46
4.2.3葡萄糖檢測 46
4.3實驗結果與討論 47
4.3.1 SEM表面形貌分析 47
4.3.2 XRD相鑑定分析 48
4.3.3 BET比表面積及BJH孔徑分析 49
4.3.4有機染料降解之特性 52
4.3.5葡萄糖感測性質量測 56
4.4結論 59
第五章總結 60
第六章未來研究 61
參考文獻 63

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指導教授

李勝偉(Sheng-wei Lee)

審核日期

2014-7-30

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