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研究生：	方盈倩 Fang, Ying-Chien
論文名稱：	開發照明用螢光體與螢光特性分析 Development of Phosphors for Lighting and Analysis of Their Luminescent Properties
指導教授：	朱聖緣 Chu, Sheng-Yuan
學位類別：	博士 Doctor
系所名稱：	電機資訊學院 - 電機工程學系 Department of Electrical Engineering
論文出版年：	2011
畢業學年度：	100
語文別：	英文
論文頁數：	108
中文關鍵詞：	螢光粉、發光二極體、鉬酸鹽、氮氧化物、熱穩定性、封裝、能量轉移
外文關鍵詞：	phosphor, LEDs, molybdate, oxynitride, thermal stability, energy transfer, remote
相關次數：	點閱：121 下載：0
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為了提升目前常用之白光LED元件 (blue LED+YAG: Ce3+)之演色性，開發適合綠色與紅色螢光粉是必要的。本研究分為三個部份，第一部分，本研究發現Sm3+藉由能量轉移方式可以增強Eu3+紅光表現，但會減弱螢光粉體之熱穩定。因此探討增感劑離子Sm3+ 對Eu3+摻雜-紅光鉬酸鹽類螢光粉之熱淬滅行為影響可能原因也許是由於Sm3+共摻雜後使得較低CTS能階出現使得熱穩定性減弱或是由於彼此間4f能階差異小，熱使電子在彼此能階中以非輻射方式來回跳躍傳遞，減弱發光特性。
第二部分為開發常壓製程之氮氧化物螢光粉。首先探討Si-N含量對發光與熱穩定之影響。當Si-N含量增加時,提供具有較高共價性環境，使得Eu2+發光產生紅位移現象，同時其激發光譜也變得更寬廣(UV-blue range)，亦提升螢光粉體之熱穩定性(其熱淬滅溫度大於175oC)。另一方面，利用矽酸鹽為前驅物進行二階段合成方式製備氮氧化物綠色螢光粉體，此方式提供一個容易反應路徑，可提升氮氧化物螢光粉之結晶性、發光與熱穩定之特性。
第三部分，將二階段合成之氮氧化物螢光粉在高溫高濕(85oC與濕度85%)環境下進行可靠性評估，發現此氮氧化物螢光粉具有不錯的熱穩定性與濕度穩定性，適合應用於固態照明。同時將含二價銪離子之鋇氮氧化物與鍶氮氧化物藍、綠光螢光粉搭配商用紅色螢光粉與商用藍光LED結合製作成白光LED。發現使用兩種以上之螢光粉之白光LED具有較高演色性(大於75)。同時探討不同封裝方式對白光LED之電穩定性之影響。藉由遠距封裝方式可以提升演色性，亦改善LED電穩定性，使得LED元件在較高電流驅動下可以盡量維持其顏色一致性。同時白光LED元件亦進行85oC與濕度85%之環境測試，其結果顯示本研究之白光LED元件兼具可靠性與實際應用性。

To enhance the CRI of white-LEDs, developing green- and red- phosphors are necessary. This thesis is composed of three parts. Part (1), the red emission intensity of Eu3+ dopants in molybdate-based red phosphor is enhanced by Sm3+ ion co-doping. The reasons of weaken the thermal stability of Eu3+-activated phosphors may be the lower energy of the CTS band, and thermal quenching between 4f levels. Thus, the trade-off between increasing emission intensity and thermal stability of Eu3+ and Sm3+ co-doping in other phosphors should be considered whether the CTS band shifts to higher or lower energy after Sm3+ co-doping and a small energy different in 4f energy levels. Part (2), oxynitride phosphors are prepared using a convenient solid-state reaction Si–N content effect on the luminescence and thermal stability of these phosphors are reported. This incorporation of Si–N effect drastically changes the bonds of phosphor materials from being ionic-rich to being covalent-rich. Improved properties method of oxynitride phosphors is two-step synthesis method, which are investigated by using differential thermal analysis (DTA) spectra and luminescence measurements. Oxynitride green phosphors exhibit excellent thermal stability and color stability. The thermal quenching temperature (T50) of Eu2+ doped oxynitride phosphor is above 150 oC. Results show that oxynitride green phosphors have a broad excitation band, good thermal stability, and good humidity stability, making them suitable for use in solid-state lighting.
Part (3), Using 2pc- or 3pc-WLEDs, the color rendering index is higher than 75, and is better than that of conventional 1pc-WLEDs (blue-chip+ YAG: Ce3+). In addition, remote phosphor packaging type is very important and efficient method to improve electric stability of pc-WLEDs under various driven-current. Fabrication of 3pc-WLEDs with remote type on a blue LED chip has the real application capability.

Table of Contents
Abstract	I
Chinese Abstract	II
List of Journal Paper Publications	III
Acknowledgment	IV
Table of Contents	V
List of Figures	IX
List of Tables	XIV
Chapter 1: General Introduction	1
1.1 Introduction to phosphor converted-White Light-LEDs [1-3]	1
1.2 Aims of the research	3
1.3 Background and Motivation [4-6]	3
1.4 Dissertation organization of this Thesis	5
Chapter 2: Theory [1, 3, 7-9]	6
2.1 Introduction to Luminescence [3]	6
2.1.1 Classification of Optical Processes	7
2.1.2 Emission Rate and Luminescent Efficiency	11
2.2 Fundamentals of Luminescence [3]	13
2.2.1 Excitation	13
2.2.2 Emission	16
2.2.3 Nonradiative Transitions	21
2.2.4 Energy Transfer	22
2.3 Luminescent Centers	25
2.3.1 Trivalent Rare Earth Ions	26
2.3.2 Divalent Rare Earth Ions	27
Chapter 3: Experimental Procedures	29
3.1 Introduction	29
3.2 Synthesis of materials	29
3.2.1 Solid-state reaction method	29
3.2.2 Synthesis of Molybdate based phosphors (CaLa2(MoO4)4: Sm3+, Eu3+)	30
3.2.3 Synthesis of Oxynitride phosphors (MAl2-xSixO4-xNx: Eu2+, M=Ca, Sr, Ba)	30
3.3 Structure measurement: XRD, XPS, and FTIR analyses	31
3.4 Activation energy of crystallization measurement: TGA and DTA analyses	31
3.5 Optical properties measurement	31
3.6 Humidity test	32
3.7 Electroluminescence properties of WLEDs	33
Chapter 4: Molybdate based red phosphor−Energy Transfer and Thermal Quenching Behaviors of CaLa2(MoO4)4: Sm3+, Eu3+ Red Phosphors	34
4.1 Introduction	34
4.2 Results and Discussion	36
4.2.1 XRD analysis of CaLa2(MoO4)4: 0.04Sm3+, xEu3+ (CLM: 0.04Sm3+, xEu3+)	36
4.2.2 Absorption and photoluminescence spectra of CLM: Sm3+, Eu3+ phosphors	37
4.2.3 Energy transfer from Sm3+ to Eu3+ in CLM: Sm3+, Eu3+ phosphors	40
4.2.4 Effect of co-doped Sm3+ on the thermal quenching behavior of CLM: Sm3+, Eu3+	46
4.3 Summary	49
Chapter 5: Oxynitride based phosphors－Effect of Si-N Incorporation on MEuAl2–xSixO4–xNx (M=Ca, Sr, Ba) Phosphors: Luminescence, Thermal Stability, and Its Application	50
5.1 Introduction	50
5.2 Results and discussion	52
5.2.1 Ca0.96Eu0.04Al2-xSixO4-xNx phosphors: XRD and XPS analysis	52
5.2.2 Photoluminescence spectra of Ca0.96Eu0.04Al2-xSixO4-xNx phosphors	54
5.2.3 Effect of Si-N content on Ca0.96Eu0.04Al2-xSixO4-xNx phosphors: luminescence and thermal quenching behaviors	55
5.2.4 Evaluation of Ca0.96Eu0.04Si2O2N2 for modifying solar cell response spectra	61
5.2.5 Sr0.96Eu0.04Al2-xSixO4-xNx and Ba0.96Eu0.04Al2-xSixO4-xNx phosphors: Structure and luminescence analysis	63
5.3 Summary	68
Chapter 6: Improvement the luminescence properties of SrSi2O2N2: Eu2+oxynitride phosphor using two-step synthesis method	69
6.1 Introduction	70
6.2 Results and discussion	71
6.2.1 Photoluminescence and activation energy of crystallization analysis for SrSi2O2N2: Eu2+	71
6.2.2 XRD and FTIR analysis of SrSi2O2N2: 0.02Eu2+	74
6.2.3 Electron-phonon coupling and thermal quenching behaviors	76
6.2.4 SrSi2O2N2: 0.02Eu2+ phosphors: Quantum efficiency and its applications	79
6.3 Summary	80
Chapter 7: Fabrication of pc-WLEDs	82
7.1 Introduction	82
7.2 Results and discussion	83
7.2.1 Reliability of oxynitride phosphors: Temperature and Humidity Test	83
7.2.2 Phosphor -converted LED: 450 nm-Blue chip+ RG phosphors	86
7.2.3 Improvement of Electric Stability for WLEDs	92
7.3 Summary	96
Chapter 8: Conclusion and Future work	97
8.1 CaLa2(MoO4)4: Sm3+, Eu3+ red phosphors	97
8.2 Oxynitride phosphors	98
8.3 Fabrication of pc-WLEDs	99
8.4 Future work	99
References	100


 
List of Figures

Figure 1.1: Optical processes of the incident light interacting with an optical medium.	2
Figure 1.2: Principle of color conversion in pc-LEDs.	2
Figure 2.1: Optical processes of the incident light interacting with an optical medium.	8
Figure 2.2: Absorption between two levels of an atom.	9
Figure 2.3: A configurational coordinate model illustrating the luminescence process (ABS = absorption).	11
Figure 2.4: An optically active center, OL6, containing a doping ion O that is coordinated to six ligand ions L.	15
Figure 2.5: Schematic image of the crystal field splitting of Ce3+.	16
Figure 2.6: Configurational coordinate diagram showing the emission and relaxation processes.	17
Figure 2.7: Donor-killer energy migration mechanism for concentration quenching of luminescence. The excitation energy is transferred to a killer center (black) along a chain of donors (grey).	20
Figure 2.8: Quenching of higher levels of emission (5D3-7FJ) by the cross-relaxation mechanism in Tb3+-doped phosphors.	21
Figure 2.9: Sequential steps for a nonradiative energy transfer process.	23
Figure 2.10: The emission spectra of the phosphor Ca5(PO4)3 (FCl) activated with a fixed concentration of Sb3+ (1%) and co-activated with two different concentrations of Mn2+ (2% , and 8 %) (reproduced with permission from Nakazawa, 1998).	23
Figure 2.11: An energy-level diagram for trivalent lanthanide rare earth ions in lanthanum chloride (after Dieke, 1968).	28
Figure 4.1: XRD patterns of CaLa2(MoO4)4: 0.04Sm3+, xEu3+ with Eu3+ content of (a) x=0.01, (b) x=0.03, (c) x=0.1, and (d) x=0.3.	37
Figure 4.2: Absorption spectra of CLM, CLM: 0.1Eu3+ and CLM: 0.04Sm3+, 0.1Eu3+. The inset shows the excitation spectrum of CLM: 0.04Sm3+, 0.1Eu3+ (λem= 615 nm).	38
Figure 4.3: (a) Emission spectra of CLM: 0.04Sm3+, CLM: 0.04Sm3+, 0.01Eu3+, and CLM: 0.01Eu3+ (λex= 403 nm). The inset shows the integrated emission intensity of CLM: Sm3+ with various Sm3+ content. (b) Emission spectra of CLM: 0.04Sm3+, xEu3+ and commercial Y2O2S: Eu3+ (λex= 403 nm). The inset shows CIE chromaticity coordinates of CLM: 0.04Sm3+, xEu3+ with various Eu3+ content.	42
Figure 4.4: Energy level diagrams of Sm3+ and Eu3+ showing the energy transfer process from Sm3+ to Eu3+.	43
Figure 4.5: Decay curves of Sm3+ emission for CLM: 0.04Sm3+, 0.1Eu3+ phosphor. The inset shows a plot of the experiment data of CLM: 0.04Sm3+, 0.1Eu3+ according to Eq. (4-4).	45
Figure 4.6: (a) Temperature-dependent relative PL intensity of CLM: 0.1Eu3+ and CLM: 0.04Sm3+, 0.1Eu3+ phosphors measured at 25–200 °C (λex= 403 nm). The inset shows the fitted activation energy for the thermal quenching process. (b) Configurational coordinate diagram that shows the thermal quenching pathway for CLM: Sm3+, Eu3+ phosphor.	48
Figure 5.1: (a) XRD patterns of Ca0.96Eu0.04Al2O4 and Ca0.96Eu0.04Si2O2N2; (b) XPS spectra (O 1s) of Ca0.96Eu0.04Al2-xSixO4-xNx with x=0 and x=2. The inset shows the XPS (Si 2p) spectrum of the x=2 sample.	53
Figure 5.2: Photoluminescence spectra of Ca0.96Eu0.04Al2-xSixO4-xNx phosphors with various levels of Si-N content (x=0~2): (a) PLE spectra (b) PL spectra under an excitation of 340nm.	54
Figure 5.3: Splitting of energy levels of Eu2+ in Eu2+-activated phosphors.	56
Figure 5.4: CIE chromaticity coordinates of Ca0.96Eu0.04Al2-xSixO4-xNx phosphors with various levels of Si－N content (x=0－2). The inset shows a pc-LED image (Ca0.96Eu0.04Si2O2N2 + 450 nm LED) driven by 2.5 V at room temperature.	58
Figure 5.5: (a) Temperature-dependent relative integral PL intensity of Ca0.96Eu0.04Al2-xSixO4-xNx phosphors with various levels of Si－N content (x): x=0 and 0.5 under 340 nm excitation; x=1.5 and 2 under 395 nm excitation. (b) Temperature-dependent normalized PL intensity of Ca0.96Eu0.04Si2O2N2 phosphors under 395 nm excitation. The inset shows a configurational coordinate diagram of Eu2+.	59
Figure 5.6: (a) AM1.5 sun light spectrum, (b) Spectral response of a-Si, GaAs, and GaAsAl solar cells, (c) PLE/ PL spectra of Ca0.96Eu0.04Si2O2N2. The inset shows a schematic diagram of phosphor-conversion modified solar cell device, (d) Luminescence efficiency of Ca0.96Eu0.04Si2O2N2 under 290~ 480 nm excitation.	62
Figure 5.7: (a) XRD patterns of Sr0.96Eu0.04Al2O4 and Sr0.96Eu0.04Si2O2N2; (b) XRD patterns of Ba0.96Eu0.04Al2O4 and Ba0.96Eu0.04Si2O2N2..	63
Figure 5.8: XPS spectra (O 1s) of M0.96Eu0.04Al2-xSixO4-xNx with x=0 and x=2: (a) M= Sr and (b) M= Ba.	64
Figure 5.9: Photoluminescence spectra of Sr0.96Eu0.04Al2-xSixO4-xNx phosphors with various levels of Si-N content (x=0 and 2): (a) PLE spectra (b) PL spectra (λex=395nm).	66
Figure 5.10: Photoluminescence spectra of Ba0.96Eu0.04Al2-xSixO4-xNx phosphors with various levels of Si-N content (x=0 and 2): (a) PLE spectra (b) PL spectra (λex=395nm)	66
Figure 5.11: Temperature-dependent relative integral PL intensity of M0.96Eu0.04Al2-xSixO4-xNx (x=0 and 2) phosphors (λex=395nm): (a) M= Sr, (b) M= Ba.	67
Figure 6.1: (a) PLE and PL spectra of Sr2SiO4: Eu2+ and SrSi2O2N2: Eu2+ obtained using two synthesis processes.  (b) TGA and DTA curves of starting powder SrSi2O2N2: 0.02Eu2+ (sample I) with a heating rate of 10 °C/min. (c) Plot of the DTA curve of SrSi2O2N2: Eu2+ obtained using two synthesis processes according to Eq. (6-1).	73
Figure 6.2: (a) XRD patterns of SrSi2O2N2: 0.02Eu2+ (samples I and II). (b) FTIR spectra of SrSi2O2N2: 0.02Eu2+ (samples I and II).	75
Figure 6.3: (a) Temperature dependence of the relative integral PL intensity of Sr2SiO4: 0.02Eu2+ under 340 nm excitation and SrSi2O2N2: 0.02Eu2+ (samples I and II) under 395 nm excitation. (b) Temperature dependence of FWHM for emission sites of Sr2SiO4: 0.02Eu2+ [(Eu(1) and Eu(2)]. (c) Temperature dependence of FWHM for SrSi2O2N2: 0.02Eu2+ (samples I and II).	77
Figure 6.4: (a) Quantum efficiency of SrSi2O2N2: 0.02Eu2+ (sample II) under 290 ~ 480 nm excitation. (b) Spectra of GaAsAl solar cells and AM 1.5 sunlight spectrum compared with PLE/ PL spectra of SrSi2O2N2: 0.02Eu2+.	81
Figure 7.1: Relative conductivity of MSi2O2N2: Eu2+ (M=Ca, Sr, Ba) and commercial green oxynitride phosphors as function of time.	84
Figure 7.2: PL degradation behavior (λex= 395 nm) of MSi2O2N2: Eu2+ (M=Ca, Sr, Ba) and commercial green oxynitride phosphors as function of time under 85 oC and 85% humidity treatment: (a) without silicon gel and (b) with silicon gel.	85
Figure 7.3: PL degradation behavior (λex= 450 nm) of MSi2O2N2: Eu2+ (M=Ca, Sr, Ba) and commercial green oxynitride phosphors as function of time under 85 oC and 85% humidity treatment: (a) without silicon gel and (b) with silicon gel.	85
Figure 7.4: SrSi2O2N2: Eu2+ and commercial red oxynitride phosphors in conjunction with 450nm-chip (2pc-WLEDs): (a) EL spectrum. The inset shows the photo of LED package driven by 20 mA at room temperature; (b) Luminous efficiency and CRI of 2pc-WLEDs driven by various current (mA); (c) CIE chromaticity coordinates of 2pc-WLEDs driven by various current (mA).	88
Figure 7.5: CIE chromaticity coordinates of 2pc-WLEDs driven by 300 mA with various thickness of phosphor.	89
Figure 7.6: BaSi2O2N2: Eu2+, SrSi2O2N2: Eu2+ and commercial red oxynitride phosphors in conjunction with 450nm-chip (3pc-WLEDs): (a) EL spectrum. The inset shows the photo of LED package driven by 20 mA at room temperature; (b) Luminous efficiency and CRI of 3pc-WLEDs driven by various current (mA); (c) CIE chromaticity coordinates of 3pc-WLEDs driven by various current (mA).	91
Figure 7.7: Two packaging types of pc-WLEDs (a) without remote type and (b) with remote type.	92
Figure 7.8: Comparing the without remote type and remote type of 2pc-WLEDs driven by various current (mA): (a) Luminous efficiency, (b) △CIE shift, and (c) CRI.	94
Figure 7.9: Comparing the without remote type and remote type of 3pc-WLEDs driven by various current (mA): (a) Luminous efficiency, (b) △CIE shift, and (c) CRI.	95
Figure 7.10: Time dependence of Luminous efficiency of 3pc-WLEDs with different packaging type under 85 oC and 85% humidity treatment driven by (a) 20mA and (b) 350 mA.	96
 
List of Tables

Table 2.1: Classification of Luminescence.	7
Table 2.2: Electronic Configurations and Ground State of Lanthanide Ions.	27
Table 4.1: Donor-acceptor distance and energy transfer efficiency for CaLa2(MoO4)4: 0.04Sm3+, xEu3+ (λex= 403 nm).	45
Table 5.1: Electronegativity, covalent character, and ionic character of Ca0.96Eu0.04Al2-xSixO4-xNx	56
Table 6.1: Electron-lattice coupling parameters of phosphors.	79


                                    

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