利用噴霧熱裂解法製備分析Ce3+和Mn2+添加非晶CaAl2O4螢光粉

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研究生：	Ayu Marsha Alviani Ayu Marsha Alviani
論文名稱：	利用噴霧熱裂解法製備分析Ce3+和Mn2+添加非晶CaAl2O4螢光粉 Preparation and characterization of glassy Ce3+and Mn2+ -doped CaAl2O4 powder using spray pyrolysis
指導教授：	施劭儒 Shao-Ju Shih
口試委員:	Yee-Wen Yen Yee-Wen Yen Chin-Yang Yu Chin-Yang Yu Chen-Hao Wang Chen-Hao Wang
學位類別：	碩士 Master
系所名稱：	工程學院 - 材料科學與工程系 Department of Materials Science and Engineering
論文出版年：	2018
畢業學年度：	106
語文別：	英文
論文頁數：	104
中文關鍵詞：	鋁酸鈣、Ce3+/Mn2+ 、發光、非晶、螢光粉
外文關鍵詞：	Calcium aluminate, Ce3+/Mn2+, luminescence
相關次數：	點閱：243 下載：12
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無機發光材料(亦可稱為螢光粉)已被廣泛應用於諸多研究之中，例如安全標籤、緊急信號、固態照明以及發光二極體中(LED)。而在現代，用於安全標籤的螢光粉，可以在流通貨幣、護照或是其他重要文件中皆可發現它的身影。而在美國、英國、德國以及日本等國家，磷光油墨已被利用於郵票的印刷中。此外，Shih團隊中於非晶矽酸鋁二鈣磷光體材料之研究提及此一材料具有良好的活化劑顆粒分佈。因此，對於目前應用以及非晶相的優勢相比，玻璃螢光粉將於本研究中進一步探討。

在本研究中，使用鋁酸鈣做為本研究的主體材料，因其具有發光時間長、化學穩定性佳、毒性低、成本低以及量子效率高等特性，此外於文獻中，透過將敏化劑能夠有效提高活化劑的發光強度，如Wang團隊成功地合成Ce3+/Mn2+摻雜鋁酸鈣螢光粉，以提高其磷光性質。而在Teixera團隊中，採用兩種不同的方法製備出Ce3+/Mn2+摻雜矽酸鋁二鈣螢光粉，透過激發以產生綠光與藍光。因此，於本研究合成非晶Ce3+/Mn2+摻雜鋁酸鈣螢光粉，以95%N2/ 5%H2混合氣體持溫800℃的退火條件下將Ce4+還原為Ce3+，以即將Mn4+還原為Mn2+。藉由X光繞射儀(XRD)來確認本實驗中Ce3+/Mn2+摻雜鋁酸鈣螢光粉之相組成，並透過場發式電子顯微鏡(SEM)測定材料的表面形貌，最後使用光致發光光譜(PL)以273nm為分析波長進行檢驗。由實驗結果顯示，0.5%Ce3+/1%Mn2+摻雜鋁酸鈣螢光粉具有較強的發光強度。

Inorganic luminescent materials (also known as phosphors), have been extensively studied in numerous application such as security label, emergency signalling, solid state, and laser light-emitting diodes (LEDs). Nowadays, phosphor for security labels can be found in money, passport, and other important paper. In several countries such as US, Great Britain, Germany and Japan, phosphorescent ink have been used in printing of all kind of postage stamps. In addition, Shih et al determined that amorphous gehlenite phosphor material have a good activator particle distribution. Therefore, as compared to the application and amorphous phase superiority, glassy phosphor will be further investigated in this study. In this research calcium aluminate (CaAl2O4) is used because it has special characteristics such as long after glow time, good chemical stability, low toxicity, low cost, and high quantum efficiency in the visible region. In some research, the activator are mixed to enhance the photoluminescence properties. For example, Wang successfully synthesized CaAl2O4 doped Ce3+, Mn2+ to produce long lasting phosphorescence. Ce3+, Mn2+ -doped Ca2Al2SiO7 were done to emit two colors, which are green and blue, using two different methodologies by Teixera. Hence, in this study, Ce3+, Mn2+ doped with CaAl2O4 were synthesized with amorphous phase. Annealing temperature at 800oC in 95%N2/ 5%H2 condition was used to reduce Ce4+ to Ce3+ and Mn4+ to Mn2+. The obtained phosphor CaAl2O4:Ce3+, Mn2+ phase was characterized by X-ray diffraction technique (XRD). The surface morphology was determined by scanning electron microscopy (SEM). Also photoluminescence spectra (PL), characterization were done with excitation at 273 nm. The maximum composition to increase the intensity of the blue-green light is 0.5%Ce3+ and 1%Mn2+ in CaAl2O4.

CONTENT
摘要    iv
ABSTRACT    v
ACKNOWLEDGEMENTS    vi
CONTENT    vii
LIST OF TABLES    x
LIST OF FIGURES    xi
CHAPTER 1 INTRODUCTION    1
1    Background    1
2    Objective    2
CHAPTER 2 LITERATURE REVIEW    3
1.    Luminescence material    3
1.1    Afterglow duration    3
1.2    Light source mechanism    5
2    Luminescence mechanism    9
3    Luminescent security label application    13
4    CaAl2O4 characteristics    14
5    Activator characteristics    16
5.1    Cerium    16
5.2    Manganese    16
6    Spray pyrolysis method    19
CHAPTER 3 EXPERIMENTAL METHOD    22
1    Chemicals    22
2    Experimental procedure    22
3    Material preparation    23
3.1    Adjusting annealing temperature    23
3.2    Adjusting atmospheric gases condition    25
3.3    Variation of cerium and manganese composition    28
4    Materials characterization    30
4.1    X-ray diffraction    30
4.2    Scanning electron microscope    30
4.3    Spectrofluorometer    30
CHAPTER 4 RESULTS    32
1    Adjusting temperature    32
1.1    Phases analysis    32
1.2    Morphology analysis    33
1.3    Photoluminescence analysis    36
2    Adjusting atmospheric gases    37
2.1    Phases analysis    38
2.2    Morphology analysis    39
2.3    Photoluminescence analysis    41
3    Variation of cerium    42
3.1    Phases analysis    42
3.2    Morphology analysis    44
3.3    Photoluminescence analysis    49
4    Variation of manganese    51
4.1    Phases analysis    52
4.2    Morphology analysis    54
4.3    Photoluminescence analysis    57
CHAPTER 5 DISCUSSION    61
1    Adjusting the temperature    61
1.1    Crystallization of as received Ce3+ and Mn2+-doped CaAl2O4 powder…........................................................................................................61
1.2    Morphological analysis    62
1.3    Photoluminescence analysis    63
2    Adjusting atmospheric gases    65
2.1    Crystallization of as received Ce3+ and Mn2+-doped CaAl2O4 powder    .........................................................................................................65
2.2    Morphological analysis    67
2.3    Photoluminescence analysis    67
3    Variation of Ce composition    69
3.1    Crystallization of as received Ce3+ and Mn2+-doped CaAl2O4 powder............................................................................................................69
3.2    Morphological analysis    69
3.3    Photoluminescence analysis    70
4    Variation of Mn composition    72
4.1    Crystallization of as received Ce3+ and Mn2+-doped CaAl2O4 powder    .........................................................................................................73
4.2    Morphological analysis    73
4.3    Photoluminescence analysis    74
CHAPTER  6 CONCLUSIONS    77
CHAPTER 7 FUTURE WORKS    78
REFERENCES    79


                                

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