吳乃立Wu, Nae-Lih臺灣大學:化學工程學研究所王德成Wang, De-ChengDe-ChengWang2010-06-302018-06-282010-06-302018-06-282008U0001-1407200813042000http://ntur.lib.ntu.edu.tw//handle/246246/186897次微米粒子螢光材料BaMgAl10O17:Eu2+, Mn2+可直接由商業化的螢光粉經過濕式球磨的方式製備而得；亦可以均勻相沈澱法去合成製備。本研究論文包括了粒子形態改變的觀察、結晶程度的變化、發光強度的分析及粒徑大小與其分佈的量測。商業化螢光粉的粒子大小會隨著球磨時間增加而減小。在經過3小時的球磨時間後，粒徑的分佈十分集中，粒徑大小大約可達170 nm。而在球磨過後，發光強度非常明顯地降低。其中以回火的處理方式，可以有效地幫助改善發光強度。以水熱法將Mn2+摻雜進去球磨過後的商業化螢光粉BaMgAl10O17:Eu2+。此法也被試著拿來製備次微米粒子的BaMgAl10O17:Eu2+, Mn2+。然而不幸地，因為在原本的粉體中就只有相當少的間隔空隙可讓Mn2+進入，因此水熱法是不可行的辦法。在均勻相沈澱程序上，有塞子的錐形瓶及高壓釜是被拿來使用的兩個反應器。其中以高壓釜為反應器的均勻相沈澱法，可以控制螢光粉的粒徑大小，它會隨著反應溫度提高而減小，在反應溫度為95 °C，粒徑大小大約為100 nm。而在經過1400 °C的燒結後，粉體會有最佳的結晶相。但發光強度卻是與粒徑大小成正比的。BaMgAl10O17:Eu2+, Mn2+ phosphor particles with submicron size were directly prepared by wet ball milling from the commodity and synthesized by homogeneous precipitation process. Morphology, crystallinity, photoluminescence (PL) intensity, particle size and size distribution were investigated. The particle size of the commercial phosphor was reduced with increasing milling time. The particle size distribution was very sharp and the size of particle was about 170 nm after 3 hrs of milling time. It also was found that the crystallinity and the PL intensity of the phosphor were decreased obviously after ball milling. Post-annealing treatment was helpful to improve the PL intensity finitely. Dope Mn2+ into the milled commercial phosphor BaMgAl10O17:Eu2+ by using hydrothermal method was also tried to prepare the submicron phosphor particles of BaMgAl10O17:Eu2+, Mn2+. Unfortunately, it was not a practicable method due to few vacant sites in the original phosphor.wo reactors, the flask with a stopper and the autoclave, were used in homogeneous precipitation process. The particle size of the phosphor BaMgAl10O17:Eu2+, Mn2+ could be controlled by using this method with the autoclave. It was decreased with increase in aging temperature. The size of particle was about 100 nm at 95 °C of aging temperature. The best crystallinity of the phosphor was observed after 1400 °C calcination. But the PL intensity was proportional to the particle size.摘要 Ibstract IIable of Contents IIIist of Figures VIist of Tables XIIIhapter 1 Introduction 1.1 Background 1.2 Motivations and Objectives 1hapter 2 Literature Review 4.1 Introduction of Solid Luminescent Material 4.1.1 Principle and Mechanism of Luminescence 6.1.2 Fluorescence and Phosphorescence 8.1.3 Franck-Condon Principle 9.1.4 Stokes’ Shift 11.2 Introduction of BaMgAl10O17:Eu2+, Mn2+ 13.2.1 Composites of Phosphor 13.2.2 Imperfections in Ceramics 16.2.3 Energy Transfer 22.3 Methods of Phosphor Synthesis 28.3.1 Solid State Reaction 28.3.2 Sol-gel Method 30.3.3 Hydrothermal Method 31.3.4 Homogeneous Precipitation Method 32hapter 3 Experimental 35.1 Chemical Reagents and Experimental Instruments 35.1.1 Chemical Reagents 35.1.2 Experimental Instruments 37.2 Preparation of Submicron Phosphor 37.2.1 Ball Milling Method 37.2.2 Hydrothermal Method 38.2.3 Homogeneous Precipitation Method 38.3 Thin Film 44.3.1 Spin Coating 44.4 Analysis and Characterization 47.4.1 Analytical Instruments 47.4.2 Phase Identification 47.4.3 Microstructure Characterizations 50.4.4 Measurement of Chemical State 50.4.5 Measurement of X-ray Absorption Spectroscopy 50.4.6 Measurement of Zeta Potential and Particle Size 51.4.7 Measurement of Photoluminescence 53hapter 4 Results and Discussion 55.1 Preparation of Submicron Phosphor Particles by Wet Ball Milling Method 55.1.1 Introduction 55.1.2 Characterization of the Phosphor with Ball Milling 55.2 Improvement of PL Intensity for the Milled Phosphor 66.2.1 Introduction 66.2.2 Characterization of the Milled Phosphor with Post-annealing 66.2.3 Characterization of the Phosphor Milled with Alcohol 76.3 Preparation of Submicron Phosphor Particles by Hydrothermal Method 80.3.1 Introduction 80.3.2 Characterization of the Phosphor with Some Processes 80.4 Preparation of Phosphor Thin Film by Spin Coating Method 87.5 Preparation of Submicron Phosphor Particles by Homogeneous Precipitation Method 90.5.1 Introduction 90.5.2 Characterization of the Synthesized Phosphor with a Flask Reactor 91.5.3 Characterization of the Synthesized Phosphor with an autoclave Reactor 107hapter 5 Conclusions 115eferences 1187416398 bytesapplication/pdfen-USBaMgAl10O17:Eu2+, Mn2+球磨均勻相沈澱ball millinghomogeneous precipitationthesishttp://ntur.lib.ntu.edu.tw/bitstream/246246/186897/1/ntu-97-R95524060-1.pdf