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研究生:顏敬容
研究生(外文):Ching-Jung Yen
論文名稱:固態離子選擇電極陣列試片製程及其應用於水耕栽培中營養離子感測之研究
論文名稱(外文):Fabrication of a Solid-Contact Ion-Selective Electrode Array on a Chip and Its Application to Nutrient Ion Sensing in Hydroponics
指導教授:陳林祈
指導教授(外文):Lin-Chi Chen
口試日期:2017-06-26
學位類別:碩士
校院名稱:國立臺灣大學
系所名稱:生物產業機電工程學研究所
學門:工程學門
學類:機械工程學類
論文種類:學術論文
論文出版年:2017
畢業學年度:105
語文別:中文
論文頁數:101
中文關鍵詞:固態式多元素網印參考電極網印離子選擇電極陣列離子電子傳導層聚(34-乙烯二氧基噻吩)養液水耕
外文關鍵詞:All-solid-stateMulti-elementScreen-printed reference electrodeScreen-printed ion-selective electrodeArrayIon-to-electron transducerPoly(34-ethylenedioxythiophene)Nutrient solutionHydroponics
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本研究主要針對多元素固態離子選擇電極陣列之製程進行探討,並致力於水耕養液中硝酸根(NO3-)、銨根(NH4+)、鉀(K+)、鈣(Ca2+)等巨量元素離子濃度變化之監測。此電極陣列以四元素離子選擇電極與一平面式Ag/AgCl參考電極組成;為減少成本及微小化製作,以網版印刷的方式將銀漿及碳膠依序覆蓋至聚對苯二甲酸乙二酯 (polyethylene terephthalate, PET)上作為導電層與基版。然而,對於電位式感測器而言,參考電極的電位穩定性是不可或缺的條件,因此,本研究首先探討四種不同製程之固態式網印參考電極,分別針對有無薄膜及保存方式兩方面進行實驗,分析其性能並觀察其是否適用於本系統。然而缺少內溶液之固態式離子選擇電極會造成內部離子與電子之間的傳遞出現障礙,量測期間待測溶液中之水分子亦可能滲入至電極內部中,導致感測時電極發生電位訊號不穩定的情形,因此需要導入一層離子電子傳導層材料。因此,本研究針對三種導電高分子及無機材料進行探討,分別為聚(3,4-乙烯二氧基噻吩) (poly(3,4-ethylenedioxythiophene), PEDOT)、聚苯胺 (polyaniline, PANI) 及石墨烯 (graphene)。首先對以各材料修飾與未修飾任何材料之電極進行電容、電阻及靈敏度等性能之分析,並使用電化學方法、接觸角量測儀測試電極之穩定性及親疏水性,比較其關聯性,另外,為觀察電極內部是否確實有水層產生,本研究使用共軛焦顯微鏡進行驗證。最後,將網印參考電極與以PEDOT修飾之四元素離子選擇電極整合成一試片(長25 mm,寬20 mm),評估電極陣列之性能。實驗結果顯示,硝酸根離子選擇電極靈敏度為58.64 mV/decade (R2=0.9868),鉀離子選擇電極靈敏度為59.27 mV/decade (R2=0.9985),銨根離子選擇電極靈敏度為54.13 mV/decade (R2=0.9801),鈣離子選擇電極靈敏度為31.13 mV/decade (R2=0.9981)。此外,為評估四元素離子選擇電極於養液當中之測試情形,本實驗針對植物工廠水耕萵苣養液之比例進行分析,並配置各目標元素於變化50 %、75 %、100 %、125 %及150 %之樣品,量測四元素試片於混合溶液並改變微量濃度之情況下各離子濃度變化情形。實驗結果顯示以四元素離子選擇電極試片所測試之濃度與樣品配置濃度理論值均呈現高度相關性,其中,硝酸根、鉀、銨根及鈣離子選擇電極所測試之濃度與樣品配置濃度理論值之相關係數R分別為0.9891、0.9942、0.9804及0.8904。
致謝 i
中文摘要 ii
Abstract iv
目錄 vi
圖目錄 x
表目錄 xii
符號說明 xiii
第一章 緒論 1
1.1 前言 1
1.2 研究動機 2
1.3 研究目的 3
1.4 研究架構 5
第二章 文獻探討 7
2.1 固態式參考電極 7
2.2 離子選擇電極 8
2.2.1 感測原理 8
2.2.2離子載體與選擇性 9
2.2.3 離子電子傳導層 12
2.2.4 離子電子傳導層常遇到之問題 15
2.2.5 固態離子選擇電極發展與陣列 16
2.3 植物生理 18
2.4養液元素量測方法 20
第三章 研究方法 22
3.1 實驗儀器與藥品 22
3.1.1 實驗儀器與設備 22
3.1.2 實驗藥品 23
3.2 全固態式網印參考電極之開發製作 25
3.2.1 參考電極之薄膜製備 26
3.3全固態式網印離子選擇電極之開發製作 27
3.3.1 網版印刷電極的製作 27
3.3.2 離子電子傳導層製備 27
3.3.3 離子選擇薄膜製備 28
3.4電化學性能分析 30
3.4.1 開環電位法量測 30
3.4.2 計時電位法 30
3.4.3 循環伏安法 30
3.4.4 電化學交流阻抗法 30
3.5 表面性質與結構分析 31
3.5.1 接觸角量測儀 31
3.5.2 共軛焦顯微鏡 31
3.5.3 掃描式電子顯微鏡 32
3.6 高效液相層析法 32
第四章 結果與討論 33
4.1 固態式參考電極之討論 33
4.1.1 電荷轉移阻抗分析 33
4.1.2 網印參考電極之穩定度測試 36
4.1.3不同濃度及溶液下對網印參考電極之影響 39
4.2 離子電子傳導層材料之討論 41
4.2.1 電容分析 41
4.2.2 電荷轉移阻抗分析 43
4.2.3 材料疏水性與水層測試 45
4.2.4 X射線光電子能譜儀測試 53
4.2.5離子選擇電極之穩定性測試 55
4.2.6離子選擇電極之靈敏度測試 58
4.2.7 離子選擇電極之再現性測試 60
4.2.8 離子電子傳導層材料之綜合比較 64
4.3 離子選擇試片之性能測試 67
4.3.1 靈敏度及偵測極限 67
4.3.2 響應時間測試 71
4.4 植物工廠水耕養液之測試評估 75
第五章 結論與未來展望 80
5.1綜合討論 80
5.2 結論 83
5.3 未來展望 85
第六章 參考文獻 86
附錄 94
附錄一、各離子電子傳導層之SEM表面影像 94
附錄二、各離子電子傳導層之SEM縱切面影像 98
附錄三、硝酸根離子選擇電極邊緣之共軛焦顯微鏡影像 100
姚傑文。2013。平面式離子選擇電極研究與水耕養液巨量元素感測應用。碩士論文。台北:臺灣大學生物產業機電工程學系。
張家豪。2015。全固態式陰離子網印選擇電極製備與養液元素感測應用之研究。碩士論文。台北:臺灣大學生物產業機電工程學系。
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