用于白光LED稀土Eu掺杂SiAlON基荧光粉的发光性能

doi:10.15541/jim20220169

无机材料学报 ›› 2023, Vol. 38 ›› Issue (1): 97-104.DOI: 10.15541/jim20220169

用于白光LED稀土Eu掺杂SiAlON基荧光粉的发光性能

陆晨辉(), 葛万银(), 宋盼盼, 张盼锋, 徐美美, 张伟

陕西科技大学材料科学与工程学院, 西安 710021

收稿日期:2022-03-02 修回日期:2022-05-09 出版日期:2022-08-26 网络出版日期:2022-08-26
通讯作者: 葛万银, 教授. E-mail: gewanyin@sust.edu.cn
作者简介:陆晨辉(1996-), 男, 硕士研究生. E-mail: 1429653804@qq.com
基金资助:
国家自然科学基金(52073165);中国科学院无机功能材料与器件重点实验室开放课题(KLIFMD202202)

Luminescence Property of Eu Doped SiAlON Phosphors for White LEDs

LU Chenhui(), GE Wanyin(), SONG Panpan, ZHANG Panfeng, XU Meimei, ZHANG Wei

School of Materials Science & Engineering, Shaanxi University of Science and Technology, Xi’an 710021, China

Received:2022-03-02 Revised:2022-05-09 Published:2022-08-26 Online:2022-08-26
Contact: GE Wanyin, professor. E-mail: gewanyin@sust.edu.cn
About author:LU Chenhui (1996-), male, Master candidate. E-mail: 1429653804@qq.com
Supported by:
National Natural Science Foundation of China(52073165);Key Laboratory of Inorganic Function Material and Device, Chinese Academy of Sciences(KLIFMD202202)

摘要/Abstract

摘要：

SiAlON基荧光粉因其优异的化学和物理稳定性, 成为近年来发光领域的一个研究热点, 尤其在LED等领域, 受到研究者的热切关注。稀土掺杂SiAlON基荧光粉体有望成为新一代照明光源。由于缺乏青色光发射, 往往会造成显色性能不足。本研究通过传统高温固相法合成了β-Si5AlON7:Eu荧光粉, 采用X射线衍射仪(XRD)、扫描电镜(SEM)、X射线光电子能谱(XPS)等研究了其结构、形貌、元素和价态。通过光谱仪表征了样品的激发光谱以及发射光谱的波长范围并测试了热猝灭性能, 发现激发波长覆盖紫外至蓝色光区域, 并且发射光谱显示出典型的Eu2+跃迁的宽谱。在300 ℃下, 样品的发射光强度依然可达到室温强度的40%左右, 热激活活化能(Ea)达到了3.7 eV, 相比较商用YAG:Ce3+(YAG)荧光粉, 热稳定性有一定的提升。在与蓝色芯片复合后成功制备了高显色（显色指数Ra=87）的白色发光LED, 对应的色温也达到了暖白光范围(CCT=4501 K)。本研究实现了SiAlON基青色发射, 获得了热稳定性较为优异的荧光粉, 在发光的可持续性能上也比商用YAG有明显优势。

关键词: SiAlON, 白光LED, 稀土, 离子掺杂, 荧光材料

Abstract:

SiAlON-based phosphor has become a research hotspot due to its excellent chemical and physical stability. Especially in the LEDs field, it has received extensive attention in recent years. Rare earth doped SiAlON phosphor is expected to become a new generation of lighting source. However, due to the lack of cyan light emission, the color rendering performance of white-LED (wLED) is often insufficient. In this research, β-Si₅AlON₇:Eu phosphors were synthesized by the traditional high-temperature solid-state route. The structure, morphology, elements and valence states were examined. The wavelength range of excitation spectrum and emission spectrum of Si₅AlON₇:Eu, as well as the thermal quenching performance were studied. It is found that the excitation wavelength range covered the ultraviolet to blue region, and the emission spectrum is a typical broad feature of Eu²⁺ transition. At 300 ℃, the emitted light intensity of the sample can still reach about 40% that of the room temperature, while the thermal activation energy (E_a) reaches 3.7 eV. Compared with the commercial YAG:Ce³⁺ (YAG) phosphor, the thermal stability of Si₅AlON₇:Eu is improved. The wLED with high color rendering of R_a=87 is realized after compounding with the blue chip, and the corresponding color temperature reaches the warm white light range (CCT=4501 K). In this study, SiAlON-based cyan emission is realized, and the phosphor with excellent thermal stability is obtained. Compared with commercial YAG, it also has obvious advantages in the sustainability of luminescence.

Key words: SiAlON, white LED, rare earth, ions doping, fluorescent material

中图分类号:

TQ174

陆晨辉, 葛万银, 宋盼盼, 张盼锋, 徐美美, 张伟. 用于白光LED稀土Eu掺杂SiAlON基荧光粉的发光性能[J]. 无机材料学报, 2023, 38(1): 97-104.

LU Chenhui, GE Wanyin, SONG Panpan, ZHANG Panfeng, XU Meimei, ZHANG Wei. Luminescence Property of Eu Doped SiAlON Phosphors for White LEDs[J]. Journal of Inorganic Materials, 2023, 38(1): 97-104.

图/表 7

图1 β-Si5AlON7:Eu的XRD图谱、结构示意图和合成路线示意图

Fig. 1 XRD pattern, structure diagram and synthetic route of β-Si5AlON7:Eu (a) XRD pattern; (b) Structure diagram; (c) Synthetic route of β-Si5AlON7:Eu Colorful figures are available on website

图2 不同放大倍数下β-Si5AlON7:Eu的SEM形貌照片

Fig. 2 SEM images of β-Si5AlON7:Eu under different magnifications

图3 β-Si5AlON7:Eu 的XPS总图谱及各元素的XPS拟合图

Fig. 3 Total XPS spectrum of β-Si5AlON7:Eu and the XPS fitting spectra of each element (a) XPS total spectrum; (b) Si2p; (c) Al2p; (d) O1s; (e) N1s; (f) Eu3d

图4 β-Si5AlON7:Eu的激发和发射光谱图以及稀土离子Eu2+的能级跃迁情况

Fig. 4 Excitation and emission spectra of β-Si5AlON7:Eu and energy level transition of rare earth ion Eu2+ (a) Excitation and emission spectra; (b) Energy level transition of rare earth ion Eu2+

图5 β-Si5AlON7:Eu与YAG:Ce3+两种粉体在不同测试温度下光致发光强度的变化情况以及热激活活化能拟合图谱

Fig. 5 Variation of photoluminescence intensity and thermal activation energy fitting patterns of β-Si5AlON7:Eu and YAG:Ce3+ powders at different test temperatures (a, b) β-Si5AlON7:Eu; (c, d) YAG:Ce3+

图6 不同电流下用β-Si5AlON7:Eu复合而成的白光LED的EL光谱变化情况和LED的EL色谱范围及实物照片

Fig. 6 Changes of EL spectra of white LEDs compounded with β-Si5AlON7:Eu under different currents, EL chromatographic range of LEDs and pictures of real objects (a) EL spectra changes; (b) EL chromatographic range and real pictures

图7 β-Si5AlON7:Eu和YAG:Ce3+的时间-强度图谱和红外温度变化图

Fig. 7 Time-intensity spectra and IR temperature variations of β-Si5AlON7:Eu and YAG:Ce3+ (a, b) Time-intensity spectra; (c) Infrared camera photos

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用于白光LED稀土Eu掺杂SiAlON基荧光粉的发光性能

Luminescence Property of Eu Doped SiAlON Phosphors for White LEDs

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