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完整後設資料紀錄
DC 欄位 | 值 | 語言 |
---|---|---|
dc.contributor.advisor | 呂宗昕 | |
dc.contributor.author | Shih-Yen Chen | en |
dc.contributor.author | 陳師彥 | zh_TW |
dc.date.accessioned | 2021-06-13T04:49:14Z | - |
dc.date.available | 2010-07-18 | |
dc.date.copyright | 2006-07-18 | |
dc.date.issued | 2006 | |
dc.date.submitted | 2006-07-16 | |
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dc.identifier.uri | http://tdr.lib.ntu.edu.tw/jspui/handle/123456789/33592 | - |
dc.description.abstract | 本論文的第一部份成功地以新穎的逆微乳膠法合成出摻雜銪、镝離子的鋁酸鍶螢光體。採用本製程,最大的特色在於奈米尺度的微胞反應器的生成時,可以有效的減少原子與原子間反應時的擴散距離,進而增加前驅物的反應性,來降低合成溫度。在本實驗中,不但有效地將鋁酸鍶的合成溫度降低到900度左右,同時也將螢光粉體粉體的粒徑縮小至奈米尺度。在螢光特性上,可以清楚的觀察到隨著粉體結晶性的提升,螢光強度有明顯增加的趨勢外,同時也可以發現當螢光體降低到奈米尺度的範圍時,激發與放射峰的位置會產生藍移的現象。而在餘暉方面,也可以觀察到隨著煅燒的溫度提升,餘暉衰減速度有明顯下降的趨勢。
本論文的第二部分在研究以異己酸鋅當作鋅的前驅物,並採用微波法來進行合成奈米級硫化鋅摻雜錳離子螢光體。在本製程當中,不但可以有效的在硫化鋅表面形成異己酸根的鍵結,並藉由此鍵結鈍化表面的缺陷,進而提高螢光強度。本實驗使用FTIR及XPS等測量儀器,來證明表面鍵結的型態是由在同一個酸根中的兩個對稱氧原子同時鍵結再同一個鋅原子上。上述所提的陰離子團,除了表面鈍化作用外,同時也使得螢光體表面帶有相同電性的電荷,藉由此電荷的排斥效應可以改善奈米粉體的聚集現象。並藉由ESR的顯微結構結果發現,在本次實驗當中硫化鋅晶格中所摻雜的錳離子彼此間具有良好的分散性。螢光特性上,本次製備的奈米級硫化鋅摻雜錳離子螢光體,在585 nm左右(4T1->6A1的電子躍遷),產生一個非常明亮的黃橘色放射峰,再次證明所摻雜的錳離子有效的進入晶格當中並取代鋅原子的位置。 本論文的第三個部份,在探討上述實驗中,微波能量的改變對於奈米級硫化鋅摻雜錳離子螢光體的物理特性影響。由實驗結果可以發現,經由不同的微波能量下所合成的螢光體,其粉體尺寸有著些許的差異性,而由於量子效應的關係,造成硫化鋅的能隙跟著程度上的變化,並進一步反應在放光的位置上。同時也可以清楚的發現,在微波能量為300W的條件下,具有最強的放射能力,經由ICP的量測後,可以發現是由於錳離子進入晶格的數量最多的原因所造成。藉由本實驗的結果,可以得知在微波能量為300W的條件下,本製成具有最適合的反應環境。 | zh_TW |
dc.description.abstract | In the first part of this thesis, synthesis of Eu2+, Dy3+ -activated strontium aluminate nanosized phosphors via a novel reverse microemulsion process is reported. This new synthesis technique not only reduced the synthesis temperature of SrAl2O4:Eu2+, Dy3+ phosphors to as low as 900oC, but also reduced the phosphor particle size to nanometer scale. In the microemulsion process, nanometered-micellees trapped the constituent cations, leading to a reduction of the interdiffusion length and an enhancement of the reactivity of the precursors. The photoluminescence intensity of prepared phosphors was found to substantially depend on their crystallinity and the results also indicated that the main peaks of nanosized SrAl2O4:Eu2+, Dy3+ phosphors in the excitation and emission spectrum shifted to shorter wavelengths. The decay time of prepared phosphors was greatly increased when synthesized at elevated temperature.
In the second part of this thesis, synthesis of highly luminescent ZnS: Mn2+ nano-particles via a microwave irradiation technique using zinc 2-ethylhexanoate as a novel zinc precursor is reported. This process was revealed as an efficient technique for producing in-situ capping of 2-ethylhexanoic acid on the ZnS: Mn2+ nano-particle surface, resulting in high luminescence intensity due to effective surface passivation. The chemical interaction of the carboxylic acid group with the ZnS: Mn2+ nano-particle was investigated using Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS). The obtained results indicated that 2-ethylhexanoic acid is chemisorbed as a carboxylate onto the surface of ZnS: Mn2+ nano-particles and the two oxygen atoms in the carboxylate are coordinated symmetrically to the Zn atoms, leading to the formation of the covalent Zn-O bond. The anion bound onto the nano-particle surface prevents particle agglomeration due to electrostatic repulsion between two adjacent particles. Electron spin resonance (ESR) study showed a hyperfine sextet indicating well separated Mn2+ states without agglomeration. The prepared ZnS: Mn2+ nano-particles showed bright yellow-orange luminescence at about 585 nm, characteristic of 4T1 (excited)-> 6A1 (ground) transition of Mn2+ ion at Td symmetry in ZnS crystals. In the last part of this thesis, the effect of microwave irradiation power on the physical properties of ZnS: Mn2+ nanophosphors is investigated. A series of ZnS: Mn2+ nanoparticles is synthesized changing the microwave power (from 150 W-500 W) to study its effect on the physical properties of the ZnS:Mn2+ nanoparticles, when all other synthesis conditions are kept fixed. From the obtained experimental results, it is observed that with changing power, there is also some effect in the particle size, leading to change the band gap of the prepared nano-phosphors. In the photoluminescence spectra, the blue shift phenomena is also revealed due to the quantum size effect and the sample synthesized with microwave power of 300 W showed highest luminescence intensity because of more manganese ions going inside the host lattice. From this experiment, the synthesis condition with microwave power at 300W is proven to be the optimum condition for synthesizing the nano ZnS: Mn2+ phosphors in this process. | en |
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dc.description.tableofcontents | 誌謝
摘要 Abstract Table of Contents……………………………………………………….…..…Ⅰ List of Figures………………………………………………………………….Ⅳ List of Tables…………………………………………………………………..Ⅸ Chapter 1 Introduction........................................................................................1 1.1 Phosphor Materials………………………………………………………1 1.1.1 Classification of Luminescence…………………………………….. 1 1.1.2 Mechanism of Luminescence and Afterglow…………………………...2 1.1.3 Application of Phosphors………………………………………………... 3 1.2 Luminescence Theory……………………………………………………. 4 1.2.1 The Configuration Coordinate Diagram…………………………... 4 1.2.2 Nonradiative Transition…………………………………………………. 5 1.2.3 Energy Transfer between the Luminescent Centers……………….. 5 1.2.4 Crystal-Field Theory and Stark Splits……………………………... 7 1.2.5 The Concentration Quenching Phenomenon……………………… 8 1.2.6 Quantum Yield……………………………………………………... 9 1.2.7 The Rare Earth Ions……………………………………………… 10 1.2.8 Eu2+ Activator……………………………………………………. …….. 11 1.2.9 The Transition Metal Ions(d5)……………………………………............11 1.2.10 Mn2+ Activator…………………………………………………...12 1.2.11 The Influence of Host Lattice on Eu2+ emission: The Proot’s Model………………………………………………..………….. 12 1.3 Introduction to Microemulsion Method…................................................ 14 1.4 Introduction to Microwave Method……………………………….......... 16 1.5 Crystal Structure of SrAl2O4 and ZnS…………………………………... 18 1.6 Research Objective……………………………………………………………. 20 Chapter 2 Investigation on Photoluminescence Properties of SrAl2O4:Eu2+,Dy3+ Phosphor Prepared via Microemulsion Method………………………………………………………………………... 33 2.1 Introduction…………………………………………………………….. 33 2.2 Experimental……………………………………………………………. 34 2.2.1 Synthesis of SrAl2O4:Eu2+,Dy3+ Phosphor via Mmicroemulsion Method……………………………………………………………… 34 2.2.2 Analysis Technique………………………………………………….. 35 2.3 Investigation on SrAl2O4:Eu2+,Dy3+ Phosphor via Microemulsion Method………………………………………………………………….. 36 2.3.1 Preparation of SrAl2O4:Eu2+,Dy3+ Phosphor via Microemulsion Method…………………………………………………………….... 36 2.3.2 The microstructural analysis of SrAl2O4: Eu2+, Dy3+ phosphors…... 37 2.3.3 The photoluminescence analyses of SrAl2O4: Eu2+, Dy3+ phosphor…………………………………………………………… 38 2.3.4 The decay curve analyses of SrAl2O4: Eu2+, Dy3+ phosphors………. 39 2.4 Summary………………………………………………………………... 40 Chapter 3 Investigation on Luminescence Properties of ZnS:Mn2+ Phosphor Prepared via Microwave Route………………………………………………. 53 3.1 Introduction…………………………………………………………….. 53 3.2 Experimental............................................................................................. 55 3.2.1 Synthesis of ZnS:Mn2+ Phosphor via Microwave Method…………… 55 3.2.2 Synthesis of ZnS:Mn2+ Phosphor via Different Microwave Power Source................................................................................................. 56 3.2.3 Analysis Technique………………………………………………….. 57 3.3 Investigation on Luminescence Properties of Nano-Sized ZnS:Mn2+ Phosphor……………………………………………………………....... 58 3.3.1 Preparation of Nano-Sized ZnS:Mn2+ Phosphor via Microwave Route………………………………………………………………... 58 3.3.2 Effects of Microwave Power Source on Crystal Structure and Luminescence Properties…………………………………................ 67 3.4 Summary………………………………………………………………... 73 Chapter 4 Conclusion………………………………………………………… 92 Reference……………………………………………………………………... 94 List of Figures Figure 1.1 kinds of phosphor devices according to the sources used to excite the phosphors Phosphor devices……………………………….. 22 Figure 1.2 Schematic diagram of radiative transitions between the conduction band (Ec), the valence band (Ev) and excition (EE), donor (ED) and acceptor (EA) levels in a semiconductor…….… 22 Figure 1.3 (a) Diagram of the configurational coordinate model plotted by the energy E versus the metal-ligand distance R and (b) three cases of nonradiative transitions………………………………………………………. 23 Figure 1.4 A sketch map for the concentration quenching………………… 24 Figure 1.5 Effect of crystal field on the energy state splitting……………... 24 Figure 1.6 Concentration quenching phenomenon………………………… 25 Figure 1.7 Energy levels of 4fn configurations of trivalent lanthanide ions.. 26 Figure 1.8 The energy levels of the d5 configuration as a function of the octahedral crystal field. The abscis is the ground state level (6S – 6A1). Only the sextet and the quartets are given. Doublets are omitted for clarity……………………………………………… 27 Figure 1.9 Absorption spectrum of MnF2…………………………………. 28 Figure 1.10 Partial phase diagram of the cyclohexane, Triton X-114 and 1.0 M AlCl3 ternary system at 38oC………………………………. 28 Figure 1.11 Composition in the film of the interface between the oil and aqueous phase………………………………………………… 29 Figure 1.12 A schematic representation of the reverse micelle…………….. 29 Figure 1.13 Schematic illustration suggested changes in solution behavior of surfactant organization with the HLB of surfactant in 1: 1 volume mixture of water and oil containing a finite amount of surfactant………………………………………………………. 30 Figure 1.14 The sketch map of dipole molecules which try to align with an oscillating electric field………………………………………....31 Figure 1.15 The sketch map of charge particles in a solution will follow the applied electric field…………………………………………… 31 Figure 1.16 Schematic views of the monoclinic phase of SrAl2O4 along the a- and c-directions……………………………………………….... 32 Figure 1.17 A unit cell for the zinc blende crystal structure……………..…. 32 Figure 2.1 Experimental procedure of the reverse microemulsion process for the formation of SAO: Eu2+,Dy3+ phosphors……..……………. 43 Figure 2.2 The ternary phase diagram composes of the water phase, the oil phase, and the composite surfactant phase……………………. 44 Figure 2.3 XRD pattern of SrAl2O4:Eu2+,Dy3+ phosphors prepared via reverse microemulsion method at 800~1400℃ in reducing atmosphere (5% H2-N2) for 3 h………………..………...……. 45 Figure 2.4 SEM image of SrAl2O4:Eu2+,Dy3+ phosphors prepared via reverse microemulsion method at (a) 900℃, (b) 1000℃, (c) 1200℃ (d) 1400℃ for 3 h in reducing atmosphere……………….……... 46 Figure 2.5 TEM image of SrAl2O4:Eu2+,Dy3+ phosphors prepared via reverse microemulsion method at (a) 900℃, (b) 1000℃ for 3 h in reducing atmosphere……………………………………..…… 47 Figure 2.6 Particle size evaluated from electron microscopy images in Figure 2.4 and Figure 2.5.Crystallite size calculated by scherrer equation in Figure 2.3…………………………………………. 48 Figure 2.7 Excitaion spectrum of SrAl2O4:Eu2+,Dy3+ phosphors prepared via reverse microemulsion route monitored the emission at 524nm…………………………………………………………. . 49 Figure 2.8 Emission spectrum of emulsion-derived SrAl2O4:Eu2+,Dy3+ phosphors calcined at 900-1200oC for 3 h in the reducing atmosphere under the excitation of 360 nm radiation……..…... 50 Figure 2.9 Decay time of emulsion-derived SrAl2O4:Eu2+,Dy3+ phosphors with various temperature...………………………………..…... 51 Figure 2.10 Fitting curve of emulsion-derived SrAl2O4:Eu2+,Dy3+ phosphors calcined at 1400 oC for 3 h in reducing atmosphere…………… 52 Figure 3.1 The synthesizing process of the nano ZnS: Mn2+ phosphors….. 76 Figure 3.2 The synthesizing process of the nano ZnS: Mn2+ phosphors with different power supplied……………………………………….. 77 Figure 3.3 Transmission electron micrograph (TEM) with corresponding electron diffraction pattern, (b) Particle size analysis data and (c) Powder X-ray diffraction pattern of 2-ethylhexanoic acid coated ZnS:Mn2+ nano-particles prepared using 200W microwave power........................................................................................... 78 Figure 3.4 FTIR spectra of (a) 2-ethylhexanoic acid and (b) 2-ethylhexanoic acid coated ZnS:Mn2+ nano-particles prepared using 200W microwave powe.......................................................................... 79 Figure 3.5 The sketch of the interaction between the carboxylate head and the metal atom…………………………………………………. 80 Figure 3.6 XPS spectra for C 1s (a) and O 1s (b) levels in 2-ethylhexanoic acid coated ZnS:Mn2+ nano-particles prepared using 200W microwave power........................................................................ 81 Figure 3.7 XPS spectra for Zn 2p levels in 2-ethylhexanoic acid coated ZnS:Mn2+ nano-particles prepared using 200W microwave power. Inset shows the deconvulation of each peak of the Zn 2p doublet......................................................................................... 82 Figure 3.8 Optical Transmission spectrum of 2-ethylhexanoic acid coated ZnS:Mn2+ nano-particles prepared using 200W microwave power. Inset shows the (αhν)2 vs. hν plot for determining the bandgap of the sample.................................................................................... 83 Figure 3.9 PL excitation spectrum of 2-ethylhexanoic acid coated ZnS:Mn2+ nano-particles prepared using 200W microwave power. Inset shows the fine structure in the spectrum at the wave-length region 400-550 nm................................................................................. 84 Figure 3.10 PL emission spectrum of 2-ethylhexanoic acid coated ZnS:Mn2+ nano-particles prepared using 200W microwave power. Inset shows the bright yellow-orange luminescence coming from the sample......................................................................................... 85 Figure 3.11 ESR spectrum of 2-ethylhexanoic acid coated ZnS:Mn2+ nanoparticles prepared using 200W microwave power............... 86 Figure 3.12 Transmission electron micrograph (TEM) with corresponding electron diffraction pattern with power condition at 300W......... 87 Figure 3.13 XRD pattern of 2-ethylhexanoic acid coated ZnS:Mn2+ nano-particles prepared using different microwave power.......... 87 Figure 3.14 Absorption spectrum of 2-ethylhexanoic acid coated ZnS:Mn2+ nano-particles prepared using different microwave powe…...… 88 Figure 3.15 EPR spectra of 2-ethylhexanoic acid coated ZnS:Mn2+ nano-particles prepared using different microwave power….… 89 Figure 3.16 Luminescence spectrum of 2-ethylhexanoic acid coated ZnS:Mn2+ nano-particles prepared using different microwave power. It depicts the emission spectrum under the excitation of 325 nm radiation……………………………………………………...… 90 Figure 3.17 Comparisons of molar ratio of manganese to zinc and sulfur to zinc with different power conditions………………………….. 91 List of Tables Table 1.1 The influence of different host lattice structures on emission wavelength…………………………………………………………. 21 Table 2.1 Decay time constants calculated by a curve fitting technology from strontium aluminate crystals with various temperatures…...……... 42 Table 3.1 Assignments of vibrational mode for 2-ethylhexanoic acid……….....75 Table 3.2 Comparisons of crystallite size calculated by Debey Scherrer equation and particle size calculated from bandgap approximation...75 Table 3.3 Compositions of ZnS:Mn2+ prepared at different power source measured by iductively coupled plasma atomic emission spectrometer……………………………………………………..... 75 | |
dc.language.iso | en | |
dc.title | 奈米鋁酸鍶與硫化鋅螢光材料製備及光學與結構之特性研究 | zh_TW |
dc.title | Luminescent and Structural Analysis of Nanosized Strontium Aluminate and Zinc Sulfide Phosphors | en |
dc.type | Thesis | |
dc.date.schoolyear | 94-2 | |
dc.description.degree | 碩士 | |
dc.contributor.oralexamcommittee | 吳紀聖,林麗瓊 | |
dc.subject.keyword | 奈米,鋁酸鍶,硫化鋅,螢光材料, | zh_TW |
dc.subject.keyword | nano-phosphors,strontiu,aluminate,zinc sulfide, | en |
dc.relation.page | 101 | |
dc.rights.note | 有償授權 | |
dc.date.accepted | 2006-07-17 | |
dc.contributor.author-college | 工學院 | zh_TW |
dc.contributor.author-dept | 化學工程學研究所 | zh_TW |
顯示於系所單位: | 化學工程學系 |
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