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研究生：	江建志 Chiang, Chien-Chih
論文名稱：	鈰活化石榴石系列螢光粉體結構與特性 The Structure and Luminescent Properties of Ce3+-activated Garnet Series Phosphors
指導教授：	洪敏雄 Hon, Min-Hsiung
學位類別：	博士 Doctor
系所名稱：	工學院 - 材料科學及工程學系 Department of Materials Science and Engineering
論文出版年：	2009
畢業學年度：	97
語文別：	中文
論文頁數：	124
中文關鍵詞：	共價性、藍位移、紅位移、石榴石結構、螢光粉、白光發光二極體
外文關鍵詞：	covalency, phosphor, blue shift, garnet structure, red shift, WLED
相關次數：	點閱：69 下載：2
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目前用在白光發光二極體中，具有藍光激發而可發出黃色波段的螢光粉種類少且不易合成。本研究針對具石榴石結構材料對其結構與螢光性質深入探討，利用沉澱法製備釔鋁石榴石螢光粉體的前驅物，比較不同酸鹼值的沉澱環境下，所製備之前驅物之外觀與均勻性，在低溫得到純相YAG結構，並在不同溫度煆燒下，比較產物的發光效率。利用相同製程導入鋱鋁石榴石螢光粉體的合成，在1000℃下利用沈澱法合成純相的鋱鋁石榴石結構，利用三價不同離子半徑的稀土離子取代TAG晶格位置中的鋱離子，並藉由控制石榴石晶格中十二面體的平均離子半徑，將TAG:Ce螢光粉體的發光波段藍位移或紅位移，並在CIE色度座標圖上，將其座標與藍光色度座標相連獲得暖白至冷白的白色色光。滿足色溫可調的需求。另一方面藉由銦或鎵離子的少量添加，將TAG:Ce螢光粉體的吸收波段調整，搭配不同波長的藍光晶片混出所需的白光色溫。在釓鋁石榴石螢光粉體的合成中，由於釓鋁石榴石在結構上的特殊限制，為避免第二相pervoskite 結構生成，本研究利用小離子半徑的稀土金屬如Tb、Y、Lu、Er來取代Gd的十二面體位置或以In、Ga取代Al使GAG:Ce結構更穩定，利用Tb、Y、Lu與Ga、In取代GAG:Ce中的Gd與Al時，都使發光波長藍移。與TAG:Ce、YAG:Ce相較之下，GAG:Ce的低色溫適用於室內照明用之白光LED。隨著石榴石結構中佔據十二面體的平均陽離子半徑增加與平均陰電性下降，造成整體結構的共價性下降。Ce-O之間共價性高，電子運動距離大，發光強度隨之下降，且溫度增加時，整體晶體共價性低者下降幅度也增加。顯示石榴石系列的螢光粉體，螢光粉的發光性質對溫度的敏感性決定於整體結構的共價性。在較高的活化劑濃度，電子發生交叉緩解的機率增加使發光強度下降，此現象在高溫下更趨明顯。由組態座標發現，提高環境溫度，石榴石結構隨著整體陰電性的下降，Ce-O間共價性增加，非輻射傳遞的機率也隨之增加，造成發光效率下降，此時發射波長的偏移隨熱效應減小。

YAG:Ce phosphors were synthesized by different precipitating processes. Pure YAG:Ce powder can be obtained by using normal strike method as calcined at 850℃ for 1 hr. The property of YAG powder is affected by the cation homogeneity and the morphology of precursor powder. The product formed by normal strike precipitation method has the highest emission peak at 535 nm after excitation at 470 nm.
Ce3+-activated terbium aluminum garnet (Tb3Al5O12:Ce, TAG:Ce) powder as luminescent phosphor was synthesized by the co-precipitation method. The emission intensity of TAG:Ce has the near linear relationship with the calcinating temperature. TAG:Ce presents a broad band emission peak of Ce3+ at 552~562 nm as exciting at 470nm. The maximum concentration of Ce3+ used to replace Tb3+ is about 1 mol% for the highest emission intensity at 552 nm. The concentration quenching effect occurs when the Ce3+ concentration added is above 1 mol%. The color temperature of TAG:Ce is lower than that of YAG:Ce for warm white LED application. The behaviors of Y, Tb, and Gd garnet phosphor powders activated by cerium were studied. Emission spectra with continuous yellowish range from green-yellow to yellow-orange were produced by controlling the compositions of the solid solution.
An impure phase GdAlO3 usually remains in the product of GAG powder as synthesized. In this study, an attempt to prepare a stable GAG pure phase powder by substituting the dodecahedral sites of the garnet structure with the small cation ions of Tb3+, Y3+,Er3+ or Lu3+ was made. Pure garnet phase GAG powder was formed by calcining at 1500℃ for 2 h. It is found that increasing the Lu3+ content in the Gd3+ lattice of the dodecahedral site induces a slightly blue shift in the emission wavelength and increases the emission intensity of the phosphor. The color temperature of the pure GAG:Ce phosphor powder (~2900K) formed is lower than that of YAG:Ce and TAG:Ce phosphors.
Increasing the substitution concentration of large cations in the garnet phosphor, the emission intensity tends to decrease and the temperature sensitivity of phosphors tends to increase. The red shift of the emission wavelength depends on the electronegativity of the substituted cation at the dodecahedral site of the garnet structure. Using a quantum mechanically based configurational coordinate diagram, the thermal quenching behavior, emission spectra, Stokes shift, non-radiative transitions in different host environments and activator concentrations are discussed.

摘要	                                              Ⅰ
Abstract                                              III
總目錄	                                              V
表目錄	                                              X
圖目錄	                                              XI
中英文名詞對照	                                    XVIII
第一章 緒論	                                     1
1-1 前言	                                              1
1-2 研究動機與目的               	                   5
第二章 理論基礎	                                     6
2-1 螢光材料	                                     6
2-2 螢光材料發光機制分類	                            6
2-3 光放射之激發源種類	                            7
2-4 螢光體發光理論與影響因素	                   9
2-4-1 發光過程	                                     9
2-4-2 晶格場效應	                                     11
2-4-3 電子雲膨脹效應	                            13
2-4-4 濃度淬滅效應	                                     14
2-4-5 溫度淬滅效應	                                     15
2-5 螢光體發光機制模型	                            15
2-5-1 組態座標模型             	                   15
2-5-2 史托克位移	                                     16
2-5-3 溫度影響波形寬化行為	                            18
2-6 螢光材料設計	                                     19
2-6-1 主體材料晶格	                                     19
2-6-2 活化劑	                                     20
2-6-3 敏化劑	                                     20
2-6-4 淬滅劑	                                     20
2-7 稀土離子之發光特性	                            24
2-7-1  f-f軌域躍遷之稀土離子	                   24
2-7-2  f-d軌域躍遷之稀土離子 	                   25
2-8 螢光體螢光特性光譜	                            27
2-8-1 吸收光譜	                                     27
2-8-2 發光光譜及激發光譜	                            27
2-9 石榴石晶體結構及相關文獻回顧	                   29
2-10 石榴石晶體發光特性及相關文獻回顧	          34
第三章 實驗方法與步驟	                            36
3-1 實驗藥品	                                     36
3-2 石榴石結構中取代離子之離子半徑與陰電性	          37
3-3 實驗步驟	                                     38
3-4 分析方法與步驟	                                     40
3-4-1 X-ray晶體繞射	                            40
3-4-2 熱差及熱重分析	                            40
3-4-3 傅立葉式轉換紅外線光譜儀	                   40
3-4-4 光致發光光譜	                                     40
3-4-5 掃描式電子顯微鏡 	                            41
3-4-6 CIE色度座標	                                     41
第四章 實驗結果與討論	                            42
4-1 沉澱法合成YAG:Ce螢光粉體	                   42
4-1-1前驅物製備及EDX分析	                            43
4-1-2 沉澱所得產物之XRD分析	                            47
4-1-3 前驅物TEM分析	                            47
4-1-4 PL之分析	                                     50
4-1-5 Gd離子取代YAG晶格	                            51
4-1-5-1 XRD 分析	                                     51
4-1-5-2 PL分析	                                     51
4-1-6 小結	                                     54
4-2 鈰活化TAG螢光粉體	                            55
4-2-1 鈰活化TAG螢光粉體的製備	                   55
4-2-1-1 鈰活化TAG螢光粉體煆燒過程TG/DTA分析	          55
4-2-1-2  鈰活化TAG螢光粉體煆燒過程FTIR分析	          56
4-2-1-3 鈰活化TAG螢光粉體煆燒過程成相分析	          56
4-2-1-4 鈰活化TAG螢光粉體SEM分析	                   61
4-2-1-5 鈰活化鋱鋁石榴石的激發光譜及發射光譜	          61
4-2-2 稀土離子取代TAG晶格	                            64
4-2-2-1 稀土離子取代對TAG螢光粉體晶體結構之影響	 64
4-2-2-2 稀土離子的取代對TAG發光光譜之影響	          67
4-2-2-3  Ce含量對TAG的螢光性質影響	                   71
4-2-3  Ga與In離子取代TAG晶格	                   73
4-2-3-1  Ga與In離子的取代對TAG:Ce螢光粉體結構的影響	 73
4-2-3-2  Ga與In離子的取代對TAG:Ce螢光性質的影響	 76
4-2-4 小結	                                      78
4-3 鈰活化釓鋁石榴石(GAG:Ce)螢光粉體合成研究	          79
4-3-1-1 鈰活化GAG螢光粉體煆燒過程TG/DTA分析	          80
4-3-1-2 鈰活化GAG螢光粉體煆燒結過程成相分析	          80
4-3-1-3 鈰活化GAG螢光粉體煆燒後SEM分析	          82
4-3-1-4 鈰活化GAG螢光粉體激發與發光光譜分析	          86
4-3-2  稀土離子取代GAG晶格	                            88
4-3-2-1 稀土離子的取代對GAG螢光粉體晶體結構之影響	 88
4-3-2-2 稀土離子的取代對GAG螢光粉體螢光性質之影響	 89
4-3-3  Ga與In離子取代GAG晶格	                   92
4-3-3-1 Ga與In離子的取代對GAG螢光粉體晶體結構之影響 	 92
4-3-3-2 Ga與In離子的取代對GAG螢光粉體發光性質之影響     93
4-3-4 小結	                                      96
4-4  YAG:Ce、TAG:Ce、GAG:Ce光學與結構上的比較	          97
4-4-1  Ce在不同石榴石結構之光學特性影響	          97
4-4-2 石榴石螢光粉體的熱效應	                  102
第五章 總結論	                                    111
參考文獻	                                             113
表目錄	
Table1-1 Comparisons for different kinds of white LED.	 4
Table 2-1 Applications and devices of phosphors.	 8
Table 2-2 Cations that can be used to form phosphors.	 21
Table 2-3 Anions that are optically self -active activatied.	                                      21
Table 2-4 Anions that can be used to form phosphors.	 22
Table 2-5 Cations that can be used as activator centers 23
Table 2-6 Cations that can be used as quenchers.	 24
Table 4-1 Assignment of different IR analysis band in FTIR curve	                                               59
Table 4-2 5d positions of excitation bands of Ce activated garnet phosphors	                                      69
Table 4-3
Phases of the calcined product substituted at the desired concentration (10%, 20%, 30% of trivalent ions (Tb3+,Y3+,Lu3+ and Er3+) and temperature. "P" : GAP; "G" : GAG; The subscripts w and s describe the weak and strong peaks, respectively.	                             91
Table 4-4  5d positions of excitation bands of different Ga content in GAG:Ce phosphors	                    96
Table 4-5
The temperature dependence of chromaticity coordinates of garnet series phosphors on different activator concentrations.	                                     110
Table 4-6
The characteristic and application of the garnet series phosphors.	                                     110
 圖目錄	
Figure 1-1 Scheme of different kinds of method for white light generation.	                                       3
Figure 2-1 Scheme of configuration coordinate diagram to explain (a) radiative (b) nonradiative de-excitation.	  10
Figure 2-2 Scheme of d orbitals and ligand position. Open circle : ligands for octahedral symmetry. Filled circle : ligands for tetrahedral symmetry.	                    12
Figure 2-3 Scheme of energy level splitting of 3d1 electron in different symmetries.	                    12
Figure 2-4 Scheme of the split of d orbital for Nephelauxetic effect and crystal field effect.	  14
Figure 2-5 Scheme of concentration quenching by two mechanisms (a) energy migration of excitation along a chain of donors and quencher (b) cross relaxation between pairs of centers.	                                       16
Figure 2-6 Scheme of breathing model.	           17
Figure 2-7 Schemes of the vibration wave functions for the lowest vibration level and a high vibration level.	  18
Figure 2-8 The optical absorption and emission transition between the two parabolas which show the spectra broad band.	                                                19
Figure 2-9 Scheme of self-activated anion of VO3-.	  22
Figure 2-10 Ca5(FCl)(PO4)3:Mn2+(activator),Sb3+(sensitizer), where Mn2+ conc. are (A)0 (B)0.005 (C) 0.01 (D) 0.02 (E) 0.08 mol/mol Ca and the Sb3+ conc. is fixed at 0.01 mol/mol Ca.	                             23
Figure 2-11 Dieke diagram.                      	  26
Figure 2-12 Scheme of presentation of experiment, energy levels, spectra of (a) absorption (b) emission (c) excitation	                                      28
Figure 2-13 Phase diagram of Al2O3-Re2O3 system	 31
Figure 2-14 Unit cell of garnet	                   32 
Figure 3-1 Flowchart of experimental procedure.	 39
Fig. 4-1-1 shows the pH with time change of different metal ion precipitated by NH4HCO3 using reverse strike titration method	                                      45
Fig.4-1-2 The variation of the Al/Y ratio in the precursor changed with pH value using reverse strike titration method	                                               45
Fig. 4-1-3 shows the pH with mole change of different metal ion precipitated by NH4HCO3 using normal strike titration method	                                      46
Fig.4-1-4 The variation of the Al/Y ratio in the precursor changed with pH value using normal strike titration method	                                               46
Fig.4-1-5 XRD spectra of YAG:Ce precursor calcined at different temperatures for reverse strike titration method ( G:YAG O:YAP) at (A) 800℃,(B)850℃,(C)900℃(D):1000℃)	                                               48
Fig.4-1-6 XRD spectra of YAG:Ce precursor calcined at different temperatures for normal strike titration method at (A)800℃,(B)850℃,(C)900℃,(D)1000℃ )	          48
Fig.4-1-7 TEM images of YAG precursor obtained from reverse strike titration method (inset is precursor calcined at 900℃)	                                     49
Fig.4-1-8 TEM images of YAG precursor obtained from normal strike titration method (inset is precursor calcined at 900℃)	                                              49
Fig.4-1-9 shows the emission spectra of particles with different calcining temperature (a)900 (b)1100 (c)1300℃ dashed line : using normal strike titration method, solid line : using reverse strike titration method	          50
Fig.4-1-10 The XRD spectra of the Y2.97-xGdxAl5O12:Ce0.03 phosphors synthesized with different value of (a) x=0.1 (b) x=0.2 (c) x=0.3 (d) x=0.4 (e) x=0.5 (f) x =0.6 (g) x=0.7 (h) x=0.8 (i) x=0.9 (j) x=1	                   52
Fig.4-1-11 The shift of emission wavelength of the Y2.97-xGdxAl5O12:Ce0.03 phosphors synthesized with different value from x=0.1 to 1 	                            53
	Fig.4-1-12 The color coordination (x, y) and color temperature for (Y1-xGdx)3Al5O12:Ce0.01 phosphors synthesized with different value from x=0.1 to 1 in CIE diagram	                                              53
Fig.4-2-1 DTA/TG curves for the precursor of TAG:Ce0.03 phosphor	                                              57
Fig.4-2-2. Transmission FTIR spectra of TAG precursor calcined at different temperature(a) untreated (b) 200℃ (c) 500℃ (d) 800℃ 	                            58
Fig.4-2-3 XRD spectra of TAG:Ce (a) precursor and calcined at temperatures of (b)850℃,(c)900℃,(d) 950℃(e) 1000℃(f)
1100℃,(g) 1300℃ and (h) 1500℃ 	                   60
Fig.4-2-4 SEM morphologies of the (a) precursor and  calcined at temperatures of (b) 1100 (c) 1300 (d) 1500 ℃	                                               62
Fig.4-2-5 Excitation and emission spectra for TAG:Ce0.03 (Ex: 470nm, Em: 550nm)	                             63
Fig.4-2-6 The XRD spectra of (Tb1-xYx)3Al5O12:Ce phosphors with different concentrations of x (0<x≦1).	           65
Fig.4-2-7 The XRD spectra of (Tb1-yGdy)3Al5O12:Ce phosphors with different concentrations of y, respectively (0<y≦1).	                                               66
Fig.4-2-8 The emission wavelength and lattice parameter v.s. average ionic radii of the dodecahedral sites of garnet phosphors with different host ions (Y, Tb, Gd) and activator concentrations.	                             69
Fig.4-2-9 The color coordination (x, y) and color temperature for (T1-xYx)3Al5O12:Ce0.01 and (T1-yGdy)3Al5O12:Ce0.01 phosphors synthesized with different value from x and y = 0.1 to 1 in CIE diagram	           70
Fig.4-2-10 The photoluminescence intensity and the maximum emission band at different concentration of Ce3+ under 460nm excited	                                      72
Fig.4-2-11 The relative intensity drcreased with different concentrations of Ce3+ of different garnet series phosphors	                                               72
Fig.4-2-12 The XRD spectra of Tb3(Al1-xGax)5O12:Ce phosphors with different concentrations of x (x=10, 20, 30%)	                                               74
Fig.4-2-13 The XRD spectra of Tb3(Al1-xInx)5O12:Ce phosphors with different concentrations of x (a)10mol% (b)20mol% (c)30mol% (d)40mol% (e)50mol%	                    75
Fig.4-2-14 The PL spectra of Tb3(Al1-xGax)5O12:Ce phosphors with different concentrations of x (x=10, 20, 30%)	                                               77
Fig.4-2-15 The PL spectra of Tb3(Al1-xInx)5O12:Ce phosphors with different concentrations of x (x=10, 20, 30%)	                                               77
Fig. 4-2-16 5d positions of excitation bands of different Ga3+ content in TAG:Ce phosphors	                    78
Fig.4-3-1 DTA/TG curves for the precursor of GAG:Ce0.03 phosphor                                        	  81
Fig.4-3-2 Relative intensity of the X-ray diffraction peak of H-GAP (102), O-GAP (121) and GAG (420) as calcined at various temperatures.	                             83
Fig.4-3-3 XRD spectra of GAG:Ce (a) precursor and calcined at (b) 900 (c) 1000 (d) 1100 (e) 1200 (f) 1300 (g) 1400 (h) 1500 and (i) 1600 ℃. "H" : H-GAP , "P" : GAP , "G" :  GAG	                                               84
Fig.4-3-4 SEM morphologies of (a) precursor, and the products calcined at (b)900 (c)1100 (d)1300 (e)1400 (f)1500 (g)1600 ℃	                                      85
Fig.4-3-5 Excitation and emission spectra for GAG:Ce0.03 (Ex: 470nm, Em: 551nm)	                             87
Fig.4-3-6 XRD spectra of (Gd1-XRe’X)3Al5O12:Ce powder (Re =Er3+,Lu3+) calcined at 1500℃ for 2 h with different Re’3+ concentrations. "P" : GAP , "G" : GAG 
(a)Lu0.1(b) Lu0.2 (c) Lu0.3 (d) Er0.1 (e)Er0.2 (f) Er0.3	                                               90
Fig.4-3-7 The maximum emission band of GAG:Ce powders at different substituted concentrations of Lu3+ (solid line) and Ga3+ (dashed line) excited at 470nm.	           91
Fig.4-3-8 The XRD spectra of Ga3(Al1-xGax)5O12:Ce phosphors with different concentrations of x (a)10mol% (b)20mol% (c)30mol% (d)50mol% (e)75mol%	                    94
Fig.4-3-9 :XRD patterns of Gd3(Al1-xInx)5O12:Ce phosphors, (a) x=0.1 (b) x=0.2 (c) x=0.3 , (A)900 (B)1000 (C)1100 (D)1200 (E)1300(F)1400 (G)1500 ℃.	                    94
Fig.4-3-10 The PL spectra of Gd3(Al1-xGax)5O12:Ce phosphors with different concentrations of x (a)10mol% (b)20mol% (c)30mol% (d)50mol% (e)75mol%	                    95
Fig.4-3-11 The PL spectra of Gd3(Al1-xInx)5O12:Ce phosphors with different concentrations of x (x=10, 20, 30%)	                                                95
Fig.4-3-12 The energy schematic diagram of the YAG, TAG, pure GAG phosphor and the energy transfer process in Ce3+.	                                                98
Fig.4-3-13 High resolution TEM image of (a)YAG (b)TAG and (c) GAG grain stabled by 10% yttrium	                     99
Fig.4-3-14 Effect of normal stress gradients of YAG, TAG, and GAG stabled by 10% yttrium. (φ value : 0,  0.9087,  12.09,  15.89 )	                                      101
Fig.4-3-15 The color coordination (x, y) and color temperature for YAG : △, TAG : ● and pure GAG : ○ phosphor powders in CIE diagram.	                    101
Fig.4-4-1 The temperature dependence of PL intensity on different garnet series phosphors.	                    103
Fig.4-4-2 The temperature dependence of PL intensity of garnet series phosphors on different activator concentrations.	                                      105
Fig.4-4-3 The configurational coordinate diagram of phosphor at room temperature showing the difference of the Stokes shift with Ce activated YAG, TAG and GAG phosphors, respectively.	                                      106
Fig.4-4-4 The configurational coordinate diagram of phosphor at high temperature showing the energy difference of the Stokes shift and non-radiative transition with Ce activated YAG, TAG, and GAG phosphors.	           108
Fig.4-4-5 The temperature dependence of wavelength shift and intensity on different garnet series phosphors.(a)YAG:Ce (b)TAG:Ce (c)GAG:Ce	                             109
                                    

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