臺灣博碩士論文加值系統

本實驗以噴霧熱裂解法合成中空二氧化鈰顆粒球，並以初濕含浸法將奈米銀顆粒沉積於二氧化鈰表面。所合成的樣品首先以X光繞射儀 (X-ray Diffraction, XRD)、穿透式電子顯微鏡 (Transmission electron microscopy, TEM)、顯微拉曼光譜儀 (Micro-Raman Spectrometer)，以及X光吸收光譜(X-rays Absorption Spectroscopy，XAS) 分析其成分、形貌、結構與價態變化。由TEM觀察可以得知，噴霧裂解所製成之中空CeO2球直徑約為200奈米至2微米，殼層厚度約為30奈米。所沉積的銀均勻的分佈在球表面上，銀顆粒大小約為5至50奈米，非形成一個連續的殼層；銀顆粒的間距及覆蓋率可由前驅物濃度進行控制。X光吸收光譜與拉曼光譜的測量分析指出，當銀奈米顆粒沉積於中空CeO2球表面時，Ce3+與氧空缺含量皆增加，並且發現有電荷轉移之現象。接著以VSM (Vibrating Sample Magnetometer) 進行室溫下的磁性量測，發現所合成的中空CeO2-Ag具有室溫鐵磁特性 (Room Temperature Ferromagnetism, RTFM)，且經過磁性強度與所沉積的銀數量有關。最後，拉曼光譜量測結果顯示中空CeO2-Ag複合材料能大幅提升表面增強拉曼光譜偵測 (Surface-Enhanced Raman Scattering, SERS)的靈敏度，0.002g的中空CeO2-Ag可偵測到R6G的最低濃度為10-12 M，增強因子(enhance factor)達1011。本實驗成功製備了一種具有室溫鐵磁性及良好SERS效果的多功能複合材料。

In this study, hollow CeO2-Ag composite ((H)CeO2-Ag) was prepared by two-step process. Hollow CeO2 spheres were synthesized by Spray Pyrolysis process at first, and then Ag nanoparticles were deposited on sphere surface by incipient wetness method. X-ray Diffraction (XRD), Transmission electron microscopy (TEM), X-rays Absorption Spectroscopy (XAS) and Raman were utilized to investigate the morphology, structure and valence state of cations. VSM (Vibrating Sample Magnetometer) and Raman spectrometer was utilized to measure magnetic behavior at room temperature and Surface-Enhanced Raman Scattering (SERS), respectively. Microstructural investigations demonstrated that the radius of hollow CeO2 sphere ranges from 200 nm to 2 µm with the shell thickness of sphere was about 30 nm. Silver nanoparticles which of size vary from 5 to 50 nm randomly distributed on the surface of sphere. Both of the size of silver nanoparticles and the coverage of silver nanoparticles on CeO2 sphere can be tuned by adjusting the concentration of precursor. XAS analysis predicted that defects were introduced after depositing silver nanoparticles. Moreover, charge transfer between silver and CeO2 was observed. All (H)CeO2-Ag composites were ferromagnetic at RT. Notably, the sensitivity and enhance factor of SERS was significantly improved. This study successfully synthesis a multifunction- material contain SESR effect and RTFM.

目錄
中文摘要 I
Abstract III
致謝 IV
目錄 V
圖目錄 VII
第一章 緒論 1
前言 1
研究動機 2
第二章 文獻回顧 7
2.1材料性質與應用介紹 7
2.1.1二氧化鈰介紹 7
2.1.2銀的介紹[38] 13
2.2拉曼光譜 15
2.2.1拉曼光譜的歷史 15
2.2.2拉曼光譜的原理 15
2.2.3表面增強拉曼光譜簡介 17
2.2.4表面增強拉曼光譜原理 18
第三章 實驗方法 21
3.1 實驗藥品 21
3.2 實驗流程 21
3.2.1 中空二氧化鈰製備 21
3.2.2 奈米銀顆粒沉積 22
3.2.3 表面增強拉曼光譜樣品製備 23
3.3 性質分析 24
3.3.1 X光繞射分析 24
3.3.2 穿透式電子顯微鏡 26
3.3.3 拉曼光譜分析 26
3.3.4 X光吸收光譜分析[98] 27
3.3.5 振動樣品磁力量測 29
第四章 結果與討論 31
4.1 CeO2中空球與表面奈米Ag顆粒微結構分析及之介面交互作用 31
4.1.1 XRD分析 31
4.1.2 TEM分析 32
4.1.3 XANES分析 34
4.1.4 Raman光譜分析 38
4.2 (H)CeO2-Ag物理性質分析 40
4.2.1 VSM磁性研究 40
4.2.2表面增強拉曼光譜之研究 41
第五章 結論 45
參考文獻 46

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