臺灣博碩士論文加值系統

本研究以噴墨印刷技術製備迴圈式奈米銀電極於可撓式聚醯亞胺(polyimide, PI)薄膜上，以金屬-有機骨架衍生之半導體型氣敏材料氧化鋅、氧化銅，並摻入銀至1：1氧化鋅/氧化銅作為感測層，成功製備氣體感測元件，探討在室溫下對有機揮發氣體之感測能力，搭配UV-LED燈來改善半導體氣體感測器需應用於高溫下的限制。
首先以簡易多元醇還原法來製備奈米銀顆粒，硝酸銀為銀來源、乙二醇作為還原劑、聚乙烯聚乙烯吡咯烷酮作為保護劑。SEM、TEM鑑定銀顆粒表面形貌，得知其粒徑為60-80 nm，由XRD鑑定確認球形奈米銀顆粒為面心立方的金屬銀。將奈米銀顆粒配製成5 wt%銀墨水，填充至墨水匣後，在聚醯亞胺薄膜上印製銀電極。以四種材料分別為氧化鋅、氧化銅、氧化鋅/氧化銅複合及銀摻雜氧化鋅/氧化銅作為氣體感測層，塗覆於銀電極上，即為氣體感測元件。
將感測元件至於自製氣體感測室中，以10 W UV LED燈照射，通入不同濃度(0-400 ppm)之有機揮發性氣體進行測試，感測元件連接萬用電表(Keithley 2400)，連接電腦讀取紀錄電流值。在室溫條件下感測三種氣體丙酮、甲醇及乙醇，以50 ppm丙酮為例，四種材料：氧化鋅(N-type)、氧化銅(P-type)、氧化鋅/氧化銅 (P-N junction)和銀摻雜氧化鋅/氧化銅的響應值分別為為37.7、28.3、63.2與95.9，響應時間(Tres)分別為4秒、34秒、5秒與3秒、恢復時間(Trec)為6秒、12秒、7秒和5秒，且感測的瞬間電流值隨丙酮氣體濃度增加而有明顯變化，為有效的丙酮氣體感測器。以UV LED燈輔助，可有效取代傳統金屬氧化物半導體氣體感測器需在高工作溫度下操作之限制。摻入貴金屬銀，能夠提升感測能力，在室溫下對低濃度ppm級之有機揮發性氣體有良好的感測能力。

In this study, inkjet printing technology was used to prepare a looped electrode composed of silver nanoparticles on flexible polyimide (PI) films. Pure ZnO and CuO were synthesized by hydrothermal method. ZnO, CuO and Ag doped ZnO/CuO were used as sensing layer and coated onto sliver electrode. To improve the traditional semiconductor gas sensor needs to be applied the high temperature environment, the gas sensing was tested under room temperature with UV LED.
Silver particles was synthesized by a simple polyol reduction method. The silver nanoparticle was formulated into 5 wt% silver ink, and the ink was filled in a commercially available EPSON T50 printer ink cartridge. The silver loop type electrode is printed on the polyimide film and then coated with a layer of gas sensitive material, wherein the sensing layer is ZnO (N-type), CuO (P-type), the formation of heterogeneous interface (P-N Junction) of ZnO mixed with CuO (ZnO/CuO), and silver doped ZnO/CuO to complete the preparation of sensors. The sensors are placed in a homemade gas sensing chamber, and the sensing test is carried out under reducing gas atmosphere (0-400 ppm) at room temperature with a low wattage UV-LED (10 W) lamp irradiated. The sensors was connected to a source meter (Keithley 2400), and the current value was read at different reducing gas concentrations. After the computer software was recorded, the sensing performance of the gas sensor at room temperature was investigated.
The gas sensing results revealed that the Ag doped Zno/CuO based gas sensor has superior gas sensing properties like, high response(95.9), good stability, and fast response (3 s) and recovery (5 s) time towards 50 ppm acetone gas at room temperature compared to pure ZnO(37.7/4 s/6 s), CuO(28.3/34 s/12 s)and ZnO/CuO(63.2/5 s/7 s) based sensors. The sensed instantaneous current value significantly changed with increasing acetone gas concentration, and was an effective acetone gas sensor. The sensors with UV-LED can effectively improve the limitations of conventional metal oxide semiconductor gas sensors operating at high operating temperature, and Ag doped ZnO/CuO gas sensor have good sensing ability for the acetone gas with low ppm concentration at room temperature.

摘要 i
Abstract iii
致謝 v
總目錄 vi
表目錄 ix
圖目錄 x
第一章 緒論 1
第二章 基本原理與文獻回顧 4
2-1 銀的物理性質 4
2-1-1 銀的晶體結構與特性 4
2-1-2 奈米銀顆粒合成之簡介 6
2-1-3 多元醇製備奈米銀粒子之簡介 7
2-1-4 奈米銀墨水之製備 8
2-2 可撓曲式印刷電路板 10
2-2-1 聚醯亞胺（Polyimide, PI） 10
2-2-2 聚醯亞胺的特性與應用 11
2-3 噴墨印刷製程電子元件 12
2-3-1噴墨印刷技術 12
2-3-2 壓電式噴墨技術 15
2-3-3 噴墨印刷技術之文獻 16
2-4 氣體感測器 17
2-4-1 金屬半導體型氣體感測器 18
2-5 氣體感測簡介 20
2-5-1金屬有機骨架材料簡介 20
2-5-2金屬有機骨架材料種類與合成 21
2-5-3感測層-氧化鋅 23
2-5-4感測層-氧化銅 25
2-5-5金屬氧化物半導體(MOS)感測機制 25
2-6 氣體感測器之應用 29
2-6-1工業上應用 29
2-6-2醫學上應用 30
第三章 實驗 31
3-1實驗藥品 31
3-2分析儀器及器材 32
3-2-1商用噴墨印表機 34
3-2-2四點探針 35
3-2-3 多功能電源電錶 36
3-2-4 掃描式電子顯微鏡 36
3-2-5 X光繞射儀（X-ray Diffractometer, XRD） 37
3-2-6 熱重損失分析儀 37
3-3 實驗流程 38
3-3-1 銀奈米顆粒製備 38
3-3-2 墨水製備 39
3-3-3 迴圈式電極圖形 40
3-3-4 利用噴墨印刷技術製備銀電極 41
3-3-5 ZnO感測層製備 41
3-3-6 CuO感測層製備 42
3-3-7 銀摻雜ZnO/CuO感測層製備 42
3-3-8 氣體感測分析 43
第四章 結果與討論 46
4-1奈米銀電極之性質分析 46
4-1-1銀顆粒之表面型態 46
4-1-2銀奈米顆粒晶體結構 49
4-2噴墨印刷法列印迴圈式奈米銀電極之鑑定 50
4-2-1可撓曲式奈米銀電極之圖形 50
4-2-2不同列印次數之奈米銀電極表面形貌 51
4-2-3奈米銀電極電性分析 53
4-3感測層氧化鋅之性質分析 54
4-3-1氧化鋅表面形貌之鑑定 54
4-3-2氧化鋅之晶體結構 57
4-3-3氧化鋅之紫外光鑑定 58
4-4感測層氧化銅之性質分析 59
4-4-1氧化銅表面形貌之鑑定 59
4-4-2氧化銅之晶體結構 61
4-4-3氧化銅之紫外光鑑定 62
4-5感測層銀摻雜1：1氧化銅/氧化鋅之性質分析 63
4-5-1銀摻雜氧化銅/氧化鋅表面形貌之鑑定 63
4-5-2銀摻雜氧化銅/氧化鋅之晶體結構 65
4-6氣體感測試驗 66
4-6-1氣體感測試驗-甲醇 67
4-6-2氣體感測試驗-乙醇 71
4-6-3氣體感測試驗-丙酮 75
4-6-4氣體靈敏度 79
4-6-5耐久性測試 81
第五章 結論 82
第六章 未來展望 84
參考文獻 85

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