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研究生： 楊紫琳
Yang, Zih-Lin
論文名稱： 合成具尺寸可調之硒化鎘奈米粒子並探討其於光學與電化學上的性質
Synthesis of Size-Tunable CdSe Nanocrystals and Their Optical and Electrochemical Properties
指導教授： 黃暄益
Huang, Hsuan-Yi
口試委員: 吳文偉
Wu, Wen-Wei
洪崧富
Hung, Sung-Fu
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： 2021
畢業學年度： 109
語文別： 英文
論文頁數： 68
中文關鍵詞： 能隙調控 、硒化鎘 、阻抗測量 、奈米粒子 、螢光
外文關鍵詞： band gap tuning, cadmium selenide, impedance measurements, nanocrystals, photoluminescence
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    • 因量子效應展現在光學、電學、磁學等等的性質上使得多數文獻聚焦於量子點上，較少人研究當合成的粒徑超過材料本身的波爾半徑時，是否仍會觀察到類似量子效應的現象。在水溶液下利用前驅物硝酸鎘、硒代硫酸鈉和酸液鹽酸分別在15、45和70度下攪拌一小時製備15、24和32奈米非圓形硒化鎘奈米粒子。改選用氯化鎘和硝酸作為反應物、調整反應物濃度並延長反應時間至4小時可以合成44奈米的硒化鎘奈米粒子。粉末式X射線繞射與選區繞射分析可確定材料為閃鋅礦結構硒化鎘；藉由掃描式電子顯微鏡的成像得知粒子成長過程中從一開始的聚集與不均勻經過一段時間後變得分散與均勻。1544奈米硒化鎘奈米粒子的吸收波帶位置隨著粒徑的增加從520紅位移至571奈米而漫反射光譜決定出的能隙從2.03電子伏特降低至1.68電子伏特，這些光學上的結果說明了當粒子粒徑超過硒化鎘本身的波爾半徑時能隙仍可以被調控。有趣的是，在合成的過程中加入界面活性劑十六烷基三甲基氯化銨分子可以促使硒化鎘奈米粒子放光。在螢光光譜觀察到粒徑從15增加至44奈米時，放光波帶位置從544紅位移至583奈米。由光學技術得到的能隙能量結合Mott‒Schottky分析可以決定材料不同粒徑下的導帶與價帶位置。由電化學阻抗與活性面積分析發現尺寸效應亦反應在電子轉移與電雙層電容值上。

    Quantum dots have attracted scientists attention due to the quantum effect, however, few people know the properties when the particle sizes over the Bohr radius of the material. By preparing an aqueous mixture of Cd(NO3)2, HCl, and Na2SeSO3 at 15, 45, and 70 ºC for 1 h, 15, 24, and 32 nm CdSe nanocrystals with some polyhedral shapes have been synthesized. Adjusting the reagent concentrations, use of CdCl2 and HNO3, and extending the reaction time to 4 h enables the formation of 44 nm CdSe nanocrystals. Powder X-ray diffraction (PXRD) analysis shows that the nanocrystals have a zinc blende crystal structure. Scanning electron microscopy (SEM) observation shows that the initial aggregated and heterogeneous particles eventually become dispersed and uniform. Their absorption bands red-shift progressively from 520 to 571 nm with increasing particle sizes. Diffuse reflectance spectra yield optical band gaps decreasing continuously from 2.03 eV for the 15 nm CdSe particles to 1.68 eV for the 44 nm particles. These optical results clearly demonstrate that their band gaps are still tunable with sizes well beyond the Bohr radius of CdSe. Interestingly, the non-emissive CdSe nanocrystals show an emission band red-shifted progressively from 544 to 583 nm with increasing particle sizes from 15 to 44 nm if CTAC surfactant is added during particle synthesis. Mott‒Schottky plots and the related calculations have determined their valence band and conduction band positions. Differences in the rate of charge transfer and the double layer capacitance of the size-tunable CdSe nanoparticles were also found.

    論文摘要 I ABSTRACT II ACKNOWLEDGEMENT IV TABLE OF CONTENTS V LIST OF FIGURES VIII LIST OF SCHEMES XVI LIST OF TABLES XVII Chapter 1 Introduction 1 1.1 Size-dependent properties of nanocrystals 1 1.1.1 Size-dependent optical properties of Cu2O and Cu3Se2 nanocrystals 1 1.1.2 Size-dependent electrochemical properties of nanomaterials 6 1.2 Methods for enhancing the fluorescence intensity of CdSe nanocrystals 9 1.3 Synthesis of CdSe nanocrystals in organic phase 11 1.4 Synthesis of CdSe nanocrystals in aqueous phase 13 Chapter 2 Facile Synthesis of Size-Tunable CdSe Nanocrystals Showing Size-Dependent Optical and Electrochemical Properties 16 2.1 Chemicals 17 2.2 Instrumentation 17 2.3 Preparation of sodium selenosulfate solution 18 2.4 Synthesis of CdSe nanocrystals using different Cd precursors and acids 19 2.5 Synthesis of CdSe nanocrystals by tuning acid concentration 20 2.6 Synthesis of size-tunable CdSe nanocrystals 21 2.7 Enhanced photoluminescence of CdSe nanocrystals in the presence of cetyltrimethylammonium chloride 23 2.8 Adding CTAC to as-prepared CdSe nanoparticles to check photoluminescence 25 2.9 Electrochemical measurements 25 2.9.1 Electrochemical impedance spectroscopy analysis 27 2.9.2 Electrochemical active surface area analysis 29 2.9.3 Mott–Schottky analysis 29 Chapter 3 Results and Discussion 31 3.1 Effect of Na2SeSO3 solution pH 31 3.2 Effect of HCl concentration 32 3.3 Selection of cadmium precursor and acid 34 3.4 X-ray diffraction patterns and EM images 36 3.5 Growth process of CdSe nanocrystals with different sizes 40 3.6 Size-dependent optical properties of CdSe nanocrystals 45 3.6.1 Light absorption 45 3.6.2 Photoluminescence (PL) analysis 48 3.6.3 The morphology, size, and crystallinity of CdSe nanoparticles in the presence of CTAC molecules 50 3.7 Size-dependent electrochemical properties of CdSe nanocrystals 54 3.7.1 Determination of conduction and valence band positions 54 3.7.2 Electrochemical impedance spectroscopy (EIS) measurements 56 3.7.3 Electrochemically active surface area (ECSA) measurements using cyclic voltammetry 58 Chapter 4 Conclusions 61 Chapter 5 References 62

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