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研究生： 丘珉瑞
Chiu, Ming Jui
論文名稱： 利用色胺酸作為螢光溫度計 定量金奈米粒子之光熱轉換效率
Quantifying the photothermal efficiency of gold nanoparticles using tryptophan as an in situ fluorescent thermometer
指導教授： 朱立岡
Chu, Li Kang
口試委員: 陳仁焜
陳益佳
朱立岡
學位類別： 碩士
Master
系所名稱： 理學院 - 化學系
Department of Chemistry
論文出版年： 2015
畢業學年度： 103
語文別： 中文
論文頁數： 75
中文關鍵詞： 金奈米粒子 、光熱效應 、色胺酸 、螢光
相關次數： 點閱：4  下載：0 
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    • 金奈米粒子具有表面電漿共振的光學性質，隨著不同的粒徑、形狀與環境介電常數，其共振吸收波長可由可見光波段位移到紅外光的波段，且在吸收光能後，得以熱的形式將能量釋出，即具有光熱轉換的特性。在過去十幾年中，金奈米粒子被視為奈米熱源的最佳材料，並廣泛應用於生物醫療領域，尤其在癌症熱治療。然而在金奈米粒子的光熱效應的定量研究，並未有一致的結論。本篇論文利用色胺酸的螢光強度變化與溫度所具有相依性，建立一套光致熱效螢光調變偵測系統。有別於以往利用熱電偶測量法的實驗技術，吾人以光譜技術觀察金奈米粒子其光致熱的過程，並以熱傳導模型分析加熱體積內的熱散失過程及定量各粒徑金奈米粒子的光熱轉換效率。
    實驗中藉由調變532 nm連續光源雷射能量(45.8-67.6 mJ cm-2)激發六種不同粒徑(22-86 nm)的金奈米粒子，並以色胺酸螢光作為在原位的(in situ)分子溫度計，偵測金奈米粒子光熱效應造成的溫度變化。當環境溫度上升1 oC，色胺酸螢光強度衰減2.05 %，溫度偵測極限為0.2 oC。在激發樣品時，激發光束(0.83 mm)完全包覆偵測光束(0.81 mm)，確保擷取到的色胺酸螢光強度變化皆為金奈米粒子熱效應所影響。在溶液樣品在532 nm的消光度一致的前提下，隨著金奈米粒子的粒徑越大，其光熱效應造成環境的溫度變化逐漸變小。根據溫度梯度所建立的熱傳導模型能適當地描述整體熱散失的過程，並得到各粒徑金奈米粒子的絕對光熱轉換效率，而相對於22 nm的金奈米粒子之光熱轉換效率隨粒徑變化的趨勢也與米氏理論相符。
    吾人所建立的光致熱效應螢光調變偵測系統有別於以往使用熱電偶測量法，色胺酸螢光強度變化能即時反映金奈米粒子光熱效應造成的環境溫度變化，使訊號得到更佳的訊雜比以及實驗再現性。此外，色胺酸的螢光強度與溫度的相依性，亦可應用上於生物的熱影像的研究。

    The photothermal efficiencies, denoting the efficiency of transducing incident light to heat, of gold nanoparticles of different diameters (Ø = 22–86 nm) were quantified upon exposure at 532 nm. The fluorescence of tryptophan at 300–450 nm upon 280 nm excitation serves as an in situ fluorescent thermometer to illustrate the evolution of the average temperature change in the heating volume of the nanoparticle solution. The fluorescence intensity decreases as the temperature increases, having a linear gradient of 2.05% fluorescence decrease per degree Celsius increment from 20 to 45 oC. The presence of gold nanoparticles at the nM level does not perturb the temperature-dependent fluorescence of tryptophan in terms of fluorescence contour and temperature response. The heating volume was defined by overlapping the collimated 532 nm laser (Ø = 0.83 mm) for exciting the nanoparticles and the 280 nm continuous-wave beam (Ø = 0.81 mm) for exciting tryptophan in a 2 mm × 2 mm square tube, and the fluorescence was collected perpendicularly to the collinear alignment. This method has satisfactory reproducibility and a sufficient temperature detectivity of 0.2 oC. The profiles of the average temperature evolution of the mixtures containing nanoparticles and tryptophan were derived from the evolution of fluorescence and analyzed using collective energy balancing. The relative photothermal efficiencies for different sizes of gold nanoparticles with respect to the 22 nm nanoparticle agree with those predicted using Mie theory. The employment of tryptophan as a fluorescent thermometer not only provides an in situ tool to monitor the photothermal effect of nanostructures but is also applicable to thermal imaging in biological applications.

    第一章 緒論 1 1.1 前言 1 1.2 文獻回顧與實驗動機 1 1.2.1 金奈米粒子光熱效應的分析與應用 1 1.2.2 實驗動機與目的 2 第二章 金奈米粒子與色胺酸的性質 5 2.1 金奈米粒子的光學性質及其原理 5 2.1.1 米氏理論 5 2.1.2 侷域性表面電漿共振 (Localized Surface Plasmon Resonance，LSPR) ……………………………………………………………………7 2.1.3 光熱效應 8 2.2 色胺酸的螢光性質 9 2.2.1 色胺酸光學性質 9 2.2.2 色胺酸螢光強度與溫度的相依性 10 第三章 實驗儀器原理、實驗系統架設及實驗樣品製備 18 3.1 實驗光譜原理介紹 18 3.1.1 穩態紫外/可見光吸收光譜 18 3.1.2 螢光光譜 19 3.1.3 電子顯微鏡 21 3.1.4 光致熱效應螢光調變偵測系統 22 3.2 光致熱效應螢光偵測系統架設 23 3.3 樣品製備 25 3.3.1 奈米晶種的合成 25 3.3.2 不同粒徑的金奈米粒子製備 26 3.3.3 色胺酸濃度最佳化 27 3.3.4 實驗樣品製備 27 3.3.5 實驗藥品 28 3.4 儀器參數設定 29 3.4.1 靜態紫外/可見光吸收光譜儀 29 3.4.2 螢光分光光譜儀 29 3.4.3 光致熱效應螢光調變偵測系統 29 第四章 實驗結果與討論 41 4.1 金奈米粒子形貌與粒徑之鑑定 41 4.1.1 金奈米粒子的穩態紫外/可見光光譜 41 4.1.2 電子顯微影像 41 4.2 含金奈米粒子樣品中色胺酸螢光對溫度的相依性 42 4.3 數據處理 43 4.3.1 背景值校正 43 4.3.2 螢光訊號轉換為溫度訊號之程序 44 4.4 金奈米粒子光熱效應分析 44 4.4.1 金奈米粒子光熱效應之環境熱傳導模型 45 4.4.2 光熱轉換效率與粒徑之相依性 50 第五章 結論 66 第六章 參考文獻 68   圖目錄 第二章 圖 2 1金奈米粒子的消光效率、散射效率以及吸收效率的計算結果。 12 圖 2 2 金奈米粒子的吸收/消光比例與粒徑關係圖。 13 圖 2 3 侷限性表面電漿共振示意圖45。 14 圖 2 4 金奈米粒子經光激發後，各瞬態事件所對應的時域圖57。 15 圖 2 5 色胺酸的結構。 16 圖 2 6 規一化的色胺酸紫外/可見光吸收光譜與螢光放光光譜。 16 圖 2 7 色胺酸的能量緩解機制圖66。 17 第三章 圖 3 1 紫外/可見光吸收光譜電子躍遷示意圖74。 30 圖 3 2 比爾定律吸收光路徑的示意圖。 31 圖 3 3 (a) 自組裝式紫外/可見光吸收光譜儀。(b) 光譜儀內部構造圖1。 32 圖 3 4 Jablonski 圖61。 33 圖 3 5 光致熱效應螢光調變偵測系統架設圖。 34 圖 3 6 激發光源與偵測光源在空間中相對位置示意圖。 34 圖 3 7 測量280 nm光束直徑之儀器架設圖。 35 圖 3 8 (a) 在距離針孔不同位置下，280 nm光束截面積的直徑掃描圖。(b) 280 nm光束直徑與針孔距離關係圖。 36 圖 3 9 在距離樣品槽不同位置下，532 nm光束截面積的直徑掃描圖。 37 圖 3 10 金奈米粒子合成過程溶液顏色變化。 38 圖 3 11 金奈米粒子溶液顏色隨粒徑的變化。 38 圖 3 12 (a)不同濃度的色胺酸螢光光譜。(b)色胺酸濃度與螢光強度關係圖。 39 圖 3 13 CTAB濃度對雷射散射光的影響。 40 第四章 圖 4 1 金奈米粒子樣品的紫外/可見光光譜。 51 圖 4 2 金奈米粒子的TEM與SEM圖。 52 圖 4 3 色胺酸在不同粒徑的金奈米粒子溶液中及水溶液中的規一化螢光光譜。 53 圖 4 4 含有色胺酸與未含有色胺酸的金奈米粒子溶液以280 nm激發之螢光光譜。 54 圖 4 5 不同粒徑之金奈米粒子溶液在不同溫度下的螢光光譜。 55 圖 4 6 各粒徑金奈米粒子溶液相對螢光強度隨溫度變化的檢量線圖。 56 圖 4 7 光電倍增管所獲得的電壓訊號轉換成溫度變化之程序。 57 圖 4 8 532 nm連續雷射激發樣品時，2 mm×2 mm的石英樣品槽側面圖，下方為加熱體積內熱傳導的示意圖。 58 圖 4 9 (a) 各粒徑金奈米粒子溶液以三種不同雷射能量激發後的溫度變化。(b) 各粒徑金奈米粒子溶液之雷射能量規一化的溫度變化。 59 圖 4 10 各粒徑金奈米粒子溶液之雷射能量規一化的平均波形。 60 圖 4 11 各粒徑金奈米粒子溶液經由熱傳導模型適解的結果。 61 圖 4 12 不同粒徑金奈米粒子相對於22 nm的光熱轉換效率(η_rel)。 62 第五章 圖 5 1 光致熱效應螢光調變偵測系統的實驗概念圖。 67 表目錄 表 1 1 金奈米粒子的應用 4 表 4 1 各粒徑下， 及相對光熱轉換效率 63 附錄目錄 附錄 4 1 熱傳導動力學方程式推導 64

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