氧化鐵奈米粒子之合成鑑定與磁性質｜國立清華大學博碩士論文庫

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研究生：	吳宗峰 Tsung-Feng Wu
論文名稱：	氧化鐵奈米粒子之合成鑑定與磁性質 Iron Oxide Nanoparticles: Synthesis, Characterization, and Magnetic Property
指導教授：	賴志煌 Chih-Huang Lai
口試委員:
學位類別：	碩士 Master
系所名稱：	工學院 - 材料科學工程學系 Materials Science and Engineering
論文出版年：	2005
畢業學年度：	93
語文別：	中文
論文頁數：	111
中文關鍵詞：	奈米粒子、氧化鐵
相關次數：	點閱：2 下載：0
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磁性奈米粒子逐漸受到許多注意，且廣為科學界所研究。其最主要被利用做為許多應用的功能性材料，例如：磁性媒體儲存、磁核共振顯影劑、藥物釋放、及催化劑等。氧化鐵奈米粒子具有無毒性、生物可相容性、化學穩定性、以及製作成本便宜等優點，因此值得我們投入研究。傳統上，氧化鐵奈米粒子主要為利用還原等化學劑量比的兩價與三價的鐵離子水溶液的反應來製備；但近年來，許多合成奈米粒子的製程被開發，而這些製作方式皆涉及了高溫的有機溶劑反應，因此可以獲得具有高品質，高結晶性的單分散相奈米粒子。

在本論文中，我們使用非水相合成法作為製作氧化鐵奈米粒子的方式。藉由穿透式電子顯微鏡、X-ray結晶繞射儀，以及化學分析電子能譜儀等鑑定了我們所合成的氧化鐵奈米粒子為Fe3O4的結構。此外，藉由改變一些實驗參數，所合成的氧化鐵奈米粒子的形式亦可達到改變；同時我們也導入不同的配位基於合成的過程中。藉由磁性量測，如；超導量子干涉儀，我們發現氧化鐵奈米粒子的磁性表現與其所具有的形狀或配位基有關。

Magnetic nanoparticles draw great attention from the field of technology and science due to their extensively application as advanced functional materials on magnetic storage, MRI contrast agent, drug delivery, and catalysis. Iron oxide nanoparticles have many merits such as non-toxicity, chemistry stable, and low-cost; hence, we have to pay our effort on the investigation of these nanoparticles. Traditionally, iron oxide nanoparticles have been synthesized by aqueous solution method, which involved the reduction reaction of ferrous and ferric ions. However, in recent, more and more method have been developed for nanoparticles synthesis. These strategies for nanoparticles synthesis all involved the high temperature reaction that is easy to obtain monodisperse and high-quality nanoparticles.

In this thesis, we applied a non-aqueous system to synthesis iron oxide nanoparticles. From many characterizations such as TEM, XRD, and XPS, we confirm these iron oxide nanoparticles to magnetite (Fe3O4) phase that is the most interesting iron oxide species due to its half-metal property. Besides, by tuning growth factors, the shape of nanocrystals can be changed from spherical to cubelike. Other surfactants are also involved in our synthesis system. The magnetic properties of these nanoparticles are dependent on many factors such as shape and surfactant ligand. Hence, SQUID measurement is conducted to observe zero-field-cooling and field-cooling processes that are mentioned to discuss the magnetic nanoparticles behavior in the low temperature.

Contents

Abstract…………………………………………………………………. I
Acknowledgement……………………………………………………... III
Contents……………………………………………………………...… IV
List of Figures………………………………………………………….VII
List of Tables……………………………………………………...…… XI

Chapter 1 Introduction ……………………………………... 1
1 Motivation ……………………………………………………… 1

Chapter 2 Background …………………………………..….. 3
1 Overview of Synthetic Magnetic Nanopartciles ….…………….. 3
1.1 Overture ……………………………………………………... 3
1.2 Mechanism of Nucleation and Growth ………..…………….. 4
1.3 Stabilization of Nanoparticles ………………………...…...... 7
1.4 Synthesis and advances of Magnetic Nanoparticles ………… 9
2 Characteristics of Magnetic Nanoparticles ……………………. 27
2.1 Magnetic Anisotropy …………………………………….... 28
2.2 Magnetic Domain ………………………………………….. 31
2.3 Superparamagnetism Phenomenon ………………………… 33
2.4 Low-Temperature Ordering ……………………………….. 35
3 Introduction to the Iron Oxides ……………………………….. 37
4 Applications of Magnetic Nanoparticles ……………………… 42
4.1 Requirements for Biomedical Application ………………… 43
4.1.1 Hyperthermia Treatment …………………………………. 44
4.1.2 Targeted drug delivery …………………………………… 44
4.1.3 Magnetic Resonance Imaging …………………………….45
4.1.4 Biosensors …………………………………………………47
4.2 Requirements for Magnetic Recording Media ……………...48

Chapter 3 Experimental Design and Analysis Technique... 49
1 Experimental Procedures ……………………………………… 49
2 Experimental Design ………………………………………….. 50
2.1 The Apparatus of Experiment ……………………………… 51
2.2 Reagent List ………………………………………………... 51
2.3 Procedures of Experiment …………………………………..52
3 Experimental and Analysis Equipment ……………………….. 52
3.1 Transmission Electron Microscopy ……….……………….. 52
3.2 X-Ray Photoelectron Spectroscopy ………………………... 54
3.3 Thermal Gravimetric Analysis ……….…………………….. 56
3.4 Superconducting Quantum Interference Device …………… 56
3.5 Fourier Transform Infrared Spectroscopy …………………. 58
3.6 Vibrating Sample Magnetometer ………………………........59
3.7 X-Ray Diffraction ………………………………………….. 60

Chapter 4 Results and Discussion ………………………….63
1 Synthesis and Characterization of Iron Oxide Nanoparticles ….63
1.1 Introduction …………………………………………………63
1.2 Synthesis by Oleic Acid and Oleylamine as Surfactant……..64
1.2.1 Effect of the Solvent with Different Boiling Point.....……64
1.2.2 Effect of the Concentration of Surfactant..……………….67
1.2.3 Kinetics of Growth Stage..………………………………69
1.2.4 Cubelike Iron Oxide Nanoparticles ...……………………74
1.3 Synthesis by Involving Other Surfactants…………………...78
1.3.1 Introduction …………………………………………….. 78
1.3.2 Oleic Acid and Trioctylphosphine Oxide as Surfactant … 79
1.3.3 Oleylamine and Trioctylphosphine Oxide as Surfactant…81
1.3.4 TOP and TOPO as Surfactant…………….........................82
1.3.5 Summary ………………………………………………... 83
1.4 Characterization ……………………………………………. 84
1.4.1 X-Ray Diffraction Analysis …………………………….. 84
1.4.2 X-Ray Photoemission Spectrum Analysis ……………… 87
2 Magnetic Property ……………………………………………...88
2.1 Introduction …………………………………………………88
2.2 Vibration Sample Magnetometer Measurement …………….89
2.2.1 Hysteresis Loops at Room Temperature …………………87
2.2.2 Langevin fitting ………………………………………….93
2.3 SQUID measurement………………………….……………95
2.3.1 ZFC/FC Measurement …………………………………...95
2.3.2 Low Temperature Hysteresis Loops ……………………..99

                                

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