臺灣博碩士論文加值系統

本研究採用化學沉澱法合成氧化銅奈米結構，其製備過程容易，不需添加劑，在常溫常壓下即可大量製造(產率約75 %)。利用前驅物間的化學反應，控制反應溫度和時間，可得到不同形貌。在室溫下(23.5 ± 1.5 ℃)，生成時間約2-5分鐘，就能形成長度約數十微米、直徑約25-50奈米的氫氧化銅奈米線，將放置時間延長 (從一天到九天)，生成物會由氫氧化銅(Cu(OH)2)轉變成氧化銅(CuO)，形貌由奈米線(Nanowires)轉變為奈米片狀結構(Nanoslabs)，寬度約1-1.5微米。若改變靜置溫度(從室溫提升至50 ℃)，奈米線轉變成奈米片狀結構的過程將從9天縮短至4小時，且為相同的氧化銅結構。利用Brunauer-Emmett-Teller方法偵測奈米線和奈米片狀結構之比表面積，分別為35.38 m2/g及15.75 m2/g。此外，變更前驅添加順序以及提升氨水濃度，能得到奈米束及海膽狀形貌的氫氧化銅結構，主要是定向性成長導致。接著測試氫氧化銅奈米線以及氧化銅奈米片狀結構的熱穩定性，發現加熱至400 ℃，依然保持原本形貌，當溫度升至600 ℃，形成塊狀結構，而在800 ℃皆轉變為氧化亞銅組成的塊狀結構，且由X-ray粉末繞射儀可知為立方體結構，其比表面積，隨溫度增加至800 ℃，分別遞減至0.42 m2/g和0.13 m2/g。氧化銅結構能有效提升葡萄糖感測之電化學性能，相較於不同形貌結構，其中以氧化銅奈米線的表現較出色，其偵測範圍為0.05-1 mM，靈敏度則是229.6 µAcm-2mM-1，具有良好的準確度且能大量製造，因此有助於無葡萄糖氧化酵素酶電化學感測商業化發展。

The preparations of the metal oxide nanostructures have been studied, on account of their unique size, dimension and chemicophysical properties. Here, we report the formation of copper-based nanostructures using chemical precipitation. The chemical precipitation method can produce copper hydroxide (Cu(OH)2) nanowires and cupric oxide (CuO) nanoslabs without surfactants as well as a high yield (approximately 75 %). Through changing reaction temperature and aging of synthisis process, we can produce different morphologies of nanostructures. The originally generated copper-based nanostructures using chemical precipitation at room temperature (about 23.5 ± 1.5 ℃) was copper hydroxide (Cu(OH)2) nanowires with approximately 50 nm in diameter and several micrometers in length. However, the transformation of Cu(OH)2 nanowires into CuO nanoslabs was observed when the samples aged at room temperature from 24 (started) to 216 hours (fully finished). Additionally, if reaction temperature increased to 50 oC, we found that time of transformation was shorten to 4hours and got the same nanoslab structures. Through Brunauer-Emmett-Teller method, the specific surface area of Cu(OH)2 nanowires and CuO nanoslabs were 35.38 and 15.75 m2/g, respectively. We also produced nano bondle and urchin-like copper hydroxide nanostructures when we changed add-ordring of percusors and increased concentration of ammonia. The as-grown Cu-based nanostructures are sensitive to thermal treatments (400-800 oC). Therefore, the specific surface areas of the heat-treated nanowires significantly reduced from 35.4 to 0.4 m2/g and nanoslabs also reduced from 19.6 to 0.1 m2/g. Nanowires and nanoslabs remained their structures below 400 ℃ and transformed into block structures above 600 ℃. The X-ray diffraction spectrum demonstrated the composition of block stucture about temperature of heat treament at 800 ℃ is cuprous oxide. Additionally, the CuO nanowires show better electrochemical property than other nanostructures. In the amperometric detection of glucose, the CuO nanowires modified copper electrode exhibited a range between 0.05-1 mM with sensitivity of 229.6 µAcm-2mM-1. The CuO nanowires have good accuracy and high precision for the quantification of glucose concentration so that it could be applied to commerical non-enzymatic glucose sensors.

中文摘要………………………………………………………………………………….…....i
英文摘要………………………………………………………………...……………..…....iii
致謝 .…………………………………………………………………………...……….….. iv
目錄 ………………………………………………………………………………….……....v
表目錄……………………………………………………………………………….....…..vii
圖目錄……………………………………………………………………………….…….viii

第一章 緒論………………………………………………………………………………….1
第一節 前言…………………………………………………………………….…1
一 奈米銅氧化物介紹………………………………………………………..….1
第二章 文獻探討與回顧…………………………………………………………………...5
第一節 奈米銅氧化物之合成方法………………………………………….……5
一 水熱法…………………………………………………………………….…..5
二 化學沉澱法………………………………………………………………..….9
三 電化學法………………...………………………………….……………….12
四 熱氧化法…………………………………………….………………...…….13
第二節 奈米銅氧化物之成長機制………………………………………...……16
一 定向性吸附………………………………….………………………..……16
二 奧斯瓦爾德熟化……………………………….……………………..……17
三 自組裝………………………………………...…..………………………..18
第三節 葡萄糖感測器之發展…………………………………………………...21
第四節 研究目的與動機………………………………………...……………....23
第三章 實驗方法
第一節 以化學沉澱法合成氧化銅奈米結構….………………………...….…24
一 實驗材料…………………………………………………………..………...24
二 反應系統……………………………………………………...……………..24
三 實驗步驟………………………………………………………………..…...26
四 儀器鑑定……………………………………………………………..……...27
第二節 氧化銅奈米線/奈米片應用於無葡萄糖氧化酵素酶電化學感測......…28
一 實驗材料…………………………………..………………………..……….28
二 工作電極製作……………………………………..…………………..…….28
三 電化學量測……………………………………………..………..………….29
第四章 結果與討論………………………………………………..……………………...30
第一節 合成氫氧化銅奈米線和氧化銅奈米片……………………………..….30
一 時間效應的探討…………………………………………………..………….30
二 溫度效應的探討…………………………………………………………..….34
三 前驅物添加順序的探討………………………………………………...……35
四 濃度效應的探討……………………………………………………..……….38
第二節 奈米線及奈米片熱穩定性的探討……………………………………...40
一 奈米線熱穩定效應之探討…………………………………………………...40
二 奈米片熱穩定效應之探討……………………………………….......………43
第三節 氧化銅奈米線/奈米片應用於無葡萄糖氧化酵素酶電化學感測…..…47
一 氧化銅奈米線應用於無葡萄糖氧化酵素酶電化學感測之探討………...…47
二 氧化銅奈米片應用於無葡萄糖氧化酵素酶電化學感測之探討…………...52
第五章、結論………………………………………………………………………………….57
第六章、參考文獻…………………………………………………………………………….58

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