臺灣博碩士論文加值系統

[Pd(imCnH2n+1)2Cl2] (n = 16) 與 [Pd(imCm(2-OH))2Cl2] (m = 16)為同時具有親水與疏水部份之兩性鈀(II)-咪唑 (Pd(II)-Imidazole) 錯合物分子。本研究由等溫壓力-面積曲線圖(π-A isotherm)觀察氣/液界面上的鈀(II)-咪唑分子之排列狀況，以布魯斯特角顯微鏡對分子薄膜因表面壓的改變所產生之變化做即時觀察，利用等溫壓力-面積循環曲線圖(π-A isocycle) 對薄膜的可逆性與穩定性進行鑑定。接著我們利用LB技術將分子薄膜轉移至固體基材，以低溫退火的方式將鈀(II)-咪唑錯合物中之鈀(II)金屬還原，在基材上製備出大小為奈米級的金屬顆粒。

在LB-film的拉膜技術中，拉膜的層數與膜分子轉移至基材上的轉移率可對膜厚做精準的控制，本實驗利用此拉膜技術的特性，試圖找出拉膜層數與轉移率對於奈米顆粒大小的關聯性，利用此關聯性對奈米顆粒的大小進行控制。

[Pd(imC16H33)2Cl2] and [Pd(imC16(2-OH))2Cl2] are both amphiphilic complexes. Molecular ordering of Pd(II)-imidazole complexes upon mechanical compression at the air/water interface is studied by surface pressure-area (π-A) isotherms and Brewster angle microscope (BAM). The repeatability of the isotherms and the stability of the Langmuir films are examined by successive compression–expansion cycles.

The monolayers at the air/water interface are transferred onto solid substrate using vertical dipping Langmuir-Blodgett (LB) technique. The LB films are comprised of monolayers or multilayers of Pd(II)-imidazole complexes, which are precisely controlled by the number of deposition cycles and the transfer ratio. It is found that after combustion of the LB films of [Pd(imC16(2-OH))2Cl2] at or below 350°C, fairly uniform and well dispersed Pd nanoparticles are formed on the solid substrate. The relationships between particle size and parameters including combustion temperature, combustion time, and the number of layers of LB films are explored.

中文摘要…………………………………………………ii
英文摘要…………………………………………………iii
總目錄……………………………………………………iv
第一章、序論……………………………………………1
1-1、前言 ………………………………………………1
1-2、研究目的 …………………………………………2
第二章 文獻回顧 ………………………………………3
2-1、奈米顆粒之製作方法與比較 ……………………3
2-2、LB轉移技術 ………………………………………3
第三章、實驗方法………………………………………8
3-1、藥品 ………………………………………………8
3-2、實驗儀器 …………………………………………9
3-3、實驗步驟 ………………………………………10
3-3-1、基材清洗………………………………………10
3-3-2、Pd(II)-Imidazole 錯合物分子溶液配置 …11
3-3-3、 Langmuir 單分子層製備觀察 ……………11
3-3-4、LB 薄膜之製作 ………………………………11
3-3-5、鈀-奈米顆粒的製作 …………………………12
3-4、分析方法 ………………………………………12
3-4-1、原子力顯微鏡 (AFM)…………………………12
3-4-2、熱重分析儀 (TGA)……………………………13
3-4-3、布魯斯特角顯微鏡……………………………14
第四章、結果與討論 …………………………………15
4-1薄膜分子可逆性、轉移方式之探討………………16
4-1-1、等溫壓力-面積曲線圖 (π-A isotherm)……16
4-1-2、等溫壓力-面積循環曲線圖 (π-A isocycle)16
4-1-3、布魯斯特角顯微鏡圖…………………………18
4-1-4、轉移率與堆疊方式之關係 ………………… 19
4-2、Pd-ImC16-2OH轉移至基材上之薄膜形貌與奈米顆粒 ………………………………………………………21
4-2-1、Pd-ImC16-2OH不同轉移率之表面形貌 ……21
4-2-2、Pd-ImC16-2OH層數與加熱時間，顆粒數量與顆粒大小之關係 ……………………………………………23
4-2-3、以10分鐘為單位，每層之燃燒時間與顆粒大小變化之關係 ………………………………………………24
4-2-4、以250°C連續燃燒2小時，層數與顆粒大小之關係 ………………………………………………………32
4-2-5、以350°C燃燒，層數與顆粒大小之關係 ……34
第五章、結論 …………………………………………44
第六章、參考文獻 ……………………………………45
附錄 ……………………………………………………50

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