Ce, Pr:YLuAG原料合成、晶体生长及LED应用

doi:10.15541/jim20150160

无机材料学报 ›› 2015, Vol. 30 ›› Issue (11): 1183-1188.DOI: 10.15541/jim20150160

Ce, Pr:YLuAG原料合成、晶体生长及LED应用

牛雪姣¹, 徐家跃¹, 周鼎¹, 王树贤², 张怀金²

(1. 上海应用技术学院材料科学与工程学院, 晶体生长研究所, 上海 201418; 2. 山东大学晶体材料研究所, 济南 250100)

收稿日期:2015-04-03 修回日期:2015-04-25 出版日期:2015-11-20 网络出版日期:2015-10-20
作者简介:牛雪姣(1989–), 女, 硕士研究生. E-mail: niuxuejiao102@163.com
基金资助:
国家自然科学基金(51472263);上海市基础研究重点项目(11JC1412400)

Synthesis and Growth of Ce,Pr:YLuAG Crystal for LED Application

NIU Xue-jiao¹, XU Jia-Yue¹, ZHOU Ding¹,WANG Shu-Xian², ZHANG Huai-Jin²

(1. Institute of Crystal Growth, School of Materials Science and Engineering, Shanghai Institute of Technology, Shanghai 201418, China; 2. Institute of Crystal Materials, Shandong University, Jinan250100, China)

Received:2015-04-03 Revised:2015-04-25 Published:2015-11-20 Online:2015-10-20
About author:NIU Xue-jiao. E-mail: niuxuejiao102@163.com
Supported by:
National Natural Science Foundation of China (51472263);Key Project of Basic Research in Shanghai(11JC1412400)

摘要/Abstract

摘要：

采用共沉淀法合成了Ce,Pr:YLuAG粉末, 在1450℃下煅烧可获得石榴石结构纯相。经过压制成型、固相烧结等工艺制备了多晶料棒, TEM显示二次烧结获得的料棒具有良好的结晶性。采用光学浮区法生长了Ce,Pr:YLuAG晶体。晶体通体透明, 呈浅黄色, 肩部有少量裂纹。透过率达到81.8%, 接近于理论值84.2%。晶体在460 nm波长激发下呈现530 nm发射带和610 nm发射峰, 分别对应Ce³⁺和Pr³⁺的特征发射, 表明Ce³⁺可以向Pr³⁺进行能量转移; 在487 nm激发下晶体仅出现Pr³⁺离子的特征发射峰。Ce,Pr:YLuAG晶体色坐标为(0.474,0.495), 比商用Ce:YAG荧光粉更靠近红光区域, 可以弥补现有荧光粉不足, 更适合制造白光LED。

关键词: 光学浮区法, 晶体生长, 掺杂, YLuAG晶体

Abstract:

Ce,Pr:YLuAG pure phase powder was synthesized by co-precipitation method and calcined at 1450℃, which had a garnet structure. The feed rod was prepared by press forming and solid state sintering. TEM showed that the sintered rod had good crystallinity and density. Ce,Pr:YLuAG single crystal was grown by the floating zone method. The as-grown crystal was transparent with a pale yellow color, and small cracks were observed in the shoulder. The transmittance of the crystal is 81.8%, which is close to the theoretical value 84.2%. Under 460 nm excitation, Ce,Pr:YLuAG crystal shows the emission band of Ce³⁺ at 530 nm and peak of Pr³⁺at 610 nm, which shows that Ce³⁺ can transfer the energy to Pr³⁺. However, only Pr³⁺ emission peak appears when it is excitated at 487 nm. The color coordinate is located at (0.474, 0.495) which shifts to red zone compared with commercial Ce:YAG yellow phosphor. As a result, Ce,Pr:YLuAG crystal is more suitable to fabricate white LED.

Key words: floating zone method, crystal growth, doping, YLuAG crystal

中图分类号:

O799

牛雪姣, 徐家跃, 周鼎, 王树贤, 张怀金. Ce, Pr:YLuAG原料合成、晶体生长及LED应用[J]. 无机材料学报, 2015, 30(11): 1183-1188.

NIU Xue-jiao, XU Jia-Yue, ZHOU Ding,WANG Shu-Xian, ZHANG Huai-Jin. Synthesis and Growth of Ce,Pr:YLuAG Crystal for LED Application[J]. Journal of Inorganic Materials, 2015, 30(11): 1183-1188.

图/表 10

图1 不同温度煅烧的Ce,Pr:YLuAG原料的XRD图谱(插图为原料棒)

Fig. 1 XRD patterns of Ce,Pr:YLuAG feed calcined at different temperatures (the inset showing a feed rod)

图2 烧结后Ce,Pr:YLuAG料棒粉末的TEM照片

Fig. 2 TEM images of sintered Ce,Pr:YLuAG feed powders

表1 Ce,Pr:YLuAG晶体的生长参数

Table 1 Growth parameters for Ce,Pr:YLuAG crystal

Diameter of feed rod	4-5 mm
Length of feed rod	60-70 mm
Power of halogen lamp	3 kW
Rotation speed	15-20 r/min
Growth speed	5-7 mm/h
Atmosphere	O₂
Heating rate	200℃/h
Cooling rate	300℃/h

图3 Ce,Pr:YLuAG晶体照片

Fig. 3 Picture of as-grown Ce,Pr:YLuAG crystal

图4 Ce,Pr:YLuAG晶体粉末的X射线衍射图谱

Fig. 4 Powder XRD pattern of Ce,Pr:YLuAG crystal

图5 Ce,Pr:YLuAG晶体的X射线摇摆曲线

Fig. 5 X-ray rocking curve of Ce,Pr:YLuAG crystal

图6 Ce,Pr:YLuAG晶体的透过光谱

Fig. 6 Transmission spectrum of Ce,Pr:YLuAG crystal

图7 Ce,Pr:YLuAG混晶的激发(a,b)和发射光谱(c,d)

Fig. 7 Excitation (a,b) and emission (c,d) spectra of Ce,Pr: YLuAG single crystal

图8 Ce,Pr:YLuAG晶体及市售Ce:YAG荧光粉的色坐标

Fig. 8 CIE coordinates of Ce,Pr:YLuAG crystal and commercial Ce:YAG phosphor

图9 Ce,Pr:YLuAG晶体的衰减曲线

Fig. 9 Decay curves of Ce,Pr:YLuAG crystal

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Ce, Pr:YLuAG原料合成、晶体生长及LED应用

Synthesis and Growth of Ce,Pr:YLuAG Crystal for LED Application

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