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研究生： 許凱智
Hsu, Kai-Chih
論文名稱： 奈米粒子沉積之還原氧化石墨烯的製備與應用
Preparation and applications of nanoparticles-deposited reduced graphene oxide
指導教授： 陳東煌
Chen, Dong-Hwang
學位類別： 博士
Doctor
系所名稱： 工學院 - 化學工程學系
Department of Chemical Engineering
論文出版年： 2015
畢業學年度： 103
語文別： 英文
論文頁數： 179
中文關鍵詞： 銀奈米粒子 、還原氧化石墨烯 、觸媒 、綠色合成 、共乘效應 、微波 、表面增強拉曼散射基材 、均勻性 、二氧化鈦奈米粒子 、再使用性 、靈敏度 、光催化
外文關鍵詞： Silver nanoparticles, Reduced graphene oxide, Catalyst, Green synthesis, Synergistic effect, Microwave, SERS substrate, Uniformity, Titanium dioxide nanoparticles, Reusable, Sensitivity, Photocatalysis.
相關次數： 點閱：147  下載：5 
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    • 近年來，石墨烯因其優異的物理、化學和電子特性，在各種應用中作為關鍵的材料或基材。此外，而其衍生物氧化石墨烯(GO）和還原氧化石墨烯（rGO），已經被廣泛地作為製造複合材料的起始材料，因為製造成本低廉並可大規模生產，豐富的含氧官能基也使其易進行官能化改質。
    本論文可分為四個主題: 1.銀/還原氧化石墨烯(Ag/rGO)奈米複合材料的綠色合成與其共乘催化效應。2.微波輔助綠色製程製備銀/還原氧化石墨烯(Ag/rGO)奈米複合材料作為高均勻性表面增強拉曼散射(SERS)基材。3.銀/二氧化鈦/還原氧化石墨烯(Ag/TiO2/rGO)奈米複合材料的製備與作為可再使用、高靈敏性與均勻性的表面增強拉曼散射(SERS)基材。4.二氧化鈦/還原氧化石墨烯(TiO2/rGO)複合材料的一步溶熱合成與作為可見光光觸媒。
    在第一個主題中，因為其高比表面積與還原氧化石墨烯的共乘效應，Ag/rGO奈米複合材料已被發展作為觸媒於催化硼氫化鈉還原對硝基苯酚為對胺基苯酚。使用精胺酸為還原劑，以便利快速的微波輔助綠色製程使銀奈米粒子與氧化石墨烯同時被還原。銀金屬在製備出的Ag/rGO奈米複合材料約佔51wt%，而沉積在還原氧化石墨烯的銀奈米粒子之平均粒徑約8.6 ± 3.5奈米。此外， Ag/rGO奈米複合材料作為觸媒於催化硼氫化鈉還原對硝基苯酚為對胺基苯酚的系統中具有傑出的催化活性和穩定性。其催化反應之擬一階動力式顯示其反應速率常數隨著反應環境溫度、觸媒量與對硝基苯酚初濃度增加而上升，說明還原氧化石墨烯藉由共乘效應(synergistic effect)可以提升觸媒的催化活性。藉由Ag/rGO奈米複合材料，硼氫化鈉還原對硝基苯酚為對胺基苯酚在液相與固相中的催化反應之機制亦被提出。
    在第二個主題中，因為還原氧化石墨烯的高比表面積與二維的網狀結構， Ag/rGO奈米複合材料被應用為SERS基材。使用精胺酸為還原劑，以便利快速的微波輔助綠色製程使銀奈米粒子均勻地成長並與氧化石墨烯同時被還原。藉由1次、4次與8次的微波次數，沉積在還原氧化石墨烯表面的銀奈米粒子的粒徑分別是10.3 ± 4.6、21.4 ± 10.5與41.1 ± 12.6奈米。Ag/rGO奈米複合材料的SERS特性可藉由使用常見的拉曼分子4-氨基苯硫酚(4-ATP)來測定。從結果可發現透過增加沉積在氧化石墨烯上的銀奈米粒子的尺寸與含量，4-ATP的拉曼訊號可以被顯著地提升。雖然還原氧化石墨烯的拉曼訊號也同時地被銀奈米粒子提升，進而限制了SERS偵測靈敏度的改善，4-ATP的偵測極限仍可達到10−10 M，其增強因子（EF）高達1.27 × 1010，且相對標準偏差(RSD)低於5%以下。這些結果證明了Ag/rGO奈米複合材料可作為高均勻性與靈敏度之表面增強拉曼散射(SERS)基材。
    在第三個主題中，為了解決在第二個主題中遇到的難題，透過使用TiO2作為中間層去消除還原氧化石墨烯D-band和G-band拉曼訊號的干擾，Ag/TiO2/rGO 奈米複合材料被作為一個更強力並具有高靈敏性與均勻性的SERS基材。4-ATP的偵測極限可從10−10 M降低到10−14 M，且同時RSD值仍可保持低於10%以下。結果可以說明使用TiO2作為中間層去抑制銀奈米粒子對於還原氧化石墨烯的SERS效應是有效的。此外，透過紫外光的照射與TiO2的光催化特性，4-ATP的拉曼訊號可以被消除，進而使此基材可以再使用，經過五次的再使用後，Ag/TiO2/rGO 奈米複合材料仍具有傑出的SERS表現，因此，本研究製備出的Ag/TiO2/rGO奈米複合材料可作為具有再使用、高靈敏性與均勻性的表面增強拉曼散射(SERS)基材。
    在第四個主題中，TiO2/rGO複合材料可透過一步溶熱法來合成，而TiO2奈米粒子可以均勻的沉積在還原氧化石墨烯的表面上。實驗結果證明TiO2/rGO複合材料具有比TiO2奈米粒子更好的光催化活性。TiO2與還原氧化石墨烯的結合不僅吸收光譜延伸至可見光的區域和使TiO2的能隙變小，也可促進TiO2照光後產生的電子轉移到還原氧化石墨烯上，進而使電子電洞分離。因此，本研究製備出的TiO2/rGO複合材料具有良好的光催化活性並可以被期待應用在有機汙染物的處理中。

    Recently, graphene has emerged as a key material or support for the various applications owing to its excellent physical, chemical and electronic properties. As the derivatives of graphene, graphene oxide (GO) and reduced graphene oxide (rGO) are widely used as starting materials for the fabrication of composites due to their low-cost property, large scale production and easy functionalization owing to the many reactive oxygenated functional groups.
    This dissertation includes four parts: 1. Green synthesis and synergistic catalytic effect of Ag/reduced graphene oxide nanocomposite; 2. Microwave-assisted green synthesis of Ag/reduced graphene oxide nanocomposite as a surface-enhanced Raman scattering substrate with high uniformity; 3. Fabrication of Ag/TiO2/reduced graphene oxide nanocomposite as a reusable surface-enhanced Raman scattering substrate with high sensitivity and uniformity; 4. One-step solvothermal synthesis of TiO2/reduced graphene oxide composite as a visible light photocatalyst.
    In the first part, a nanocomposite of silver nanoparticles and reduced graphene oxide (Ag/rGO) has been developed as a catalyst for the reduction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP) with sodium borohydride, owing to the larger specific surface area and synergistic effect of rGO. A facile and rapid microwave-assisted green route has been used for the formation of Ag nanoparticles and the reduction of graphene oxide simultaneously with L-arginine as the reducing agent. The resulting Ag/rGO nanocomposite contained about 51 wt% of Ag, and the Ag nanoparticles deposited on the surface of rGO had a mean diameter of 8.6 ± 3.5 nm. Also, the Ag/rGO nanocomposite exhibited excellent catalytic activity and stability toward the reduction of 4-NP to 4-AP with sodium borohydride. The reduction reaction obeyed the pseudo-first-order kinetics. The rate constants increased not only with the increase of temperature and catalyst amount but also with the increase of initial 4-NP concentration, revealing that the support rGO could enhance the catalytic activity via a synergistic effect. A mechanism for the catalytic reduction of 4-NP with NaBH4 by Ag/rGO nanocomposite via both the liquid-phase and solid-phase routes has been suggested.
    In the second part, Ag/rGO composites are applied as surface-enhanced Raman scattering (SERS) substrates owing to the large surface area and two-dimensional nanosheet structure of rGO. A facile and rapid microwave-assisted green route has been used for the uniform deposition of Ag nanoparticles and the reduction of graphene oxide simultaneously with L-arginine as the reducing agent. By increasing the cycle number of microwave irradiation from 1 and 4 to 8, the mean diameters of Ag nanoparticles deposited on the surface of rGO increased from 10.3 ± 4.6 and 21.4 ± 10.5 to 41.1 ± 12.6 nm. The SERS performance of Ag/rGO nanocomposite was examined using the common Raman reporter molecule 4-aminothiophenol (4-ATP). It was found that the Raman intensity of 4-ATP could be significantly enhanced by increasing the size and content of silver nanoparticles deposited on rGO. Although the Raman intensities of D-band and G-band of rGO were also enhanced simultaneously by the deposited Ag nanoparticles which limited the further improvement of SERS detection sensitivity, the detectable concentration of 4-ATP with Ag/rGO nanocomposite as the SERS substrate still could be lowered to be 10−10 M and the enhancement factor could be increased to 1.27 × 1010. Furthermore, it was also achievable to lower the relative standard deviation (RSD) values of the Raman intensities to below 5%. This revealed that the Ag/rGO nanocomposite obtained in this work could be used as a SERS substrate with high sensitivity and homogeneity.
    In the third part, to solve the problem we met in the second part, Ag/TiO2/rGO nanocomposite was developed as a more powerful SERS substrate with high sensitivity and uniformity by using TiO2 intermediate layer to diminish the interference from the Raman intensities of D-band and G-band of rGO. The detectable limit of 4-ATP could be further lowered from 10-10 M to 10-14 M. In the meanwhile, the RSD values remained below 10%. This revealed that the strategy using TiO2 intermediate layer to restrain the enhancement effect of Ag nanoparticles on the SERS intensity of rGO is indeed effective. Moreover, by UV irradiation in water, the photocatalytic property of TiO2 could eliminate the Raman signal of 4-ATP efficiently and made this substrate reusable. After reuse for 5 times, the excellent SERS performance of Ag/TiO2/rGO nanocomposite was retained. Accordingly, the Ag/TiO2/rGO nanocomposite developed in this work could be excellent candidates as a reusable SERS substrate with outstanding sensitivity and uniformity.
    In the fourth part, a composite of titanium dioxide nanoparticles and reduced graphene oxide (TiO2/rGO) have been prepared via a one-step solvothermal process of titanium(IV) butoxide and GO in the mixed solution of ethylene glycol and water. TiO2 nanoparticles could be deposited uniformly on the surface of rGO. The result revealed that TiO2/rGO composites possessed enhanced photocatalytic activities than pure TiO2 nanoparticles. The incorporation of rGO not only could extend the absorption to the visible light region and narrow the band gap of TiO2 nanoparticles, but also could facilitate the electron transfer from TiO2 nanoparticles to rGO and lead to the separation of the photogenerated electron-hole pairs. Hence, the resulting TiO2/rGO composites exhibited enhanced photocatalytic performance and were expected to be useful in the treatment of organic pollutants.

    中文摘要 i Abstract iv 誌謝 viii Contents x List of Figures xiii List of Tables xix Chapter 1 Introduction 1 1.1 Introduction of graphene and graphene oxide 1 1.1.1 Introduction of graphene 1 1.1.2 Introduction of graphene oxide 3 1.1.3 Syntheses of graphene and graphene oxide 7 1.2 Catalyst 12 1.3 Surface enhanced Raman scattering (SERS) 15 1.3.1 Introduction of Raman spectroscopy 15 1.3.2 Surface enhanced Raman scattering (SERS) 18 1.3.3 SERS applications 22 1.4 Photocatalyst 30 1.5 Reduced graphene oxide-based materials for catalysts, SERS and photocatalysts 33 1.6 Motivation 45 Chapter 2 Fundamental theory 47 2.1 Catalysis theory 47 2.2 SERS theory 53 2.2.1 Raman scattering 53 2.2.2 Surface enhanced Raman scattering 58 2.2.3 Surface plasmon resonance 63 2.2.4 Raman spectroscopy of graphene 66 2.3 Photocatalysis theory 68 Chapter 3 Green synthesis and synergistic catalytic effect of Ag/reduced graphene oxide nanocomposite 73 3.1 Introduction 73 3.2 Experimental 75 3.2.1 Materials 75 3.2.2 Preparation of GO 76 3.2.3 Microwave-assisted synthesis of Ag/rGO nanocomposite. 76 3.2.4 Characterization 77 3.2.5 Catalytic reduction of 4-nitrophenol 77 3.3 Results and discussion 78 3.4 Conclusions 94 Chapter 4 Microwave-assisted green synthesis of Ag/reduced graphene oxide nanocomposite as a surface-enhanced Raman scattering substrate with high uniformity 95 4.1 Introduction 95 4.2 Experimental 98 4.2.1 Materials 98 4.2.2 Microwave-assisted green synthesis of Ag/rGO nanocomposite. 98 4.2.3 Characterization 99 4.2.4 SERS property of Ag/rGO nanocomposite 100 4.3 Results and discussion 100 4.4 Conclusions 113 Chapter 5 Fabrication of Ag/TiO2/reduced graphene oxide nanocomposite as a reusable surface-enhanced Raman scattering substrate with high sensitivity and uniformity 114 5.1 Introduction 114 5.2 Experimental 117 5.2.1 Materials 117 5.2.2 Fabrication of Ag/TiO2/rGO nanocomposite 117 5.2.3 Characterization 118 5.2.4 SERS measurement of Ag/TiO2/rGO nanocomposite 119 5.3 Results and discussion 120 5.4 Conclusions 131 Chapter 6 One-step solvothermal synthesis of TiO2/reduced graphene oxide composite as a visible light photocatalyst 132 6.1 Introduction 132 6.2 Experimental 134 6.2.1 Materials 134 6.2.2 Preparation of TiO2/rGO composites. 135 6.2.3 Photocatalytic experiment 135 6.2.4 Characterization 136 6.3 Results and discussion 137 6.4 Conclusions 146 Chapter 7 Overall conclusions 147 References 149 Curriculum vitae 177

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