YAG:Ce~（3+）荧光粉的制备及发光性能
摘要
白光LED具有能耗低、亮度高、工作电压低、使用寿命长等特点,广泛应用于照明、指示及显示领域。白光LED是由蓝光LED芯片((In,Ga)N)和颜色转换层(YAG:Ce3+荧光粉均匀分散在环氧树脂等基质中)两部分组成的。基于互补的两种发射光混合形成适于照明应用的白色光源的原理,(In,Ga)N蓝色LEDs发出的部分蓝光被颜色转换层吸收而发出黄光与剩余蓝光混合形成白色光源。稀土铈离子掺杂钇铝石榴石荧光粉(YAG:Ce3+)具有很高的发光效率和化学稳定性,所以被广泛应用于真空紫外、等离子平板显示、固体激光器以及白光LED等应用技术领域。论文中全面介绍了飞YAG:Ce3+发光材料的发展概况、发光机理以及常用的制备技术,同时还提出了一种制备YAG:Ce3+发光材料的新的简单方法——直接蒸发烧结法(简称：DESM)。
本文分别采用溶剂热法和直接蒸发烧结法(DESM)制备YAG:Ce3+荧光粉。研究了这两种制备方法的后处理温度对YAG:Ce3+荧光粉结晶性能、表面形貌、发光性能等的影响。同时还对YAG:Ce3+荧光粉发光性能的温度依赖性、荧光寿命、量子效率等有更深入的研究,弥补了现有文献资料对YAG:Ce3+荧光粉低温发光性能研究数据的不足。总结如下：
溶剂热法合成YAG:Ce3+荧光粉的成相烧结温度大约在900℃,1000℃时得到YAG纯相,粉体颗粒形貌是不规则的球形,颗粒尺寸大约35 nm。样品的光致发光光谱显示出YAG:Ce3+荧光粉的激发光谱中有两个很强的激发峰,分别为340 nm和460nm。发射光谱是一个很宽的发射带(500-700nm),峰值波长为540 nm。
与溶剂热法制备YAG:Ce3+荧光粉相比,DESM法更有优势。首先,DESM法的合成路径更简单,反应物不需要离心、水洗、醇洗等处理过程。如此,便避免了由于这些处理过程可能带来的产物流失或者引入新的杂质元素等问题。其次,DESM法的烧成温度更低。从XRD分析结果可知,溶剂热法烧成的YAG:Ce3+荧光粉的纯相形成温度为1000℃左右,且颗粒形貌不是很规则的球形。而DESM法制备YAG:Ce3+荧光粉的纯相形成温度仅为850℃,而且颗粒形貌是很规则的球形,颗粒平均尺寸为30 nm。量子效率方面,同是纯相的YAG:Ce3+荧光粉,DESM法制备的样品量子效率比溶剂热法合成的产品高9个百分点左右。另外,溶剂热法需要在高压釜内进行,而DESM法在大气环境中即可进行反应,且不需要昂贵的高温(>1000℃)烧结炉,因此DESM法更安全,成本更低。
YAG:Ce3+荧光粉发光的温度依赖性研究结果显示,其发光性能会受烧结温度和环境温度影响。随着烧结温度的提高,YAG:Ce3+荧光粉的杂相含量降低、结晶性能提高；表面形貌逐步趋于圆球形；发光强度逐渐增强；量子效率有效提高。从低温光谱可知,在较低环境温度下,可以明显看到发射峰是由两个峰值很接近的发射峰组成的,分别对应Ce3+的两个能级发射,即5d1→2F5/2和5d1→2F7/2。而且随着温度的升高,发射峰变宽,两个发射峰的重叠部分逐渐增加,变成一个发射宽峰。其发光强度呈指数形式衰减,而且衰减时间会随着环境温度的增加而降低。
文章最后,我们对YAG:Ce3+荧光粉的发展前景及今后的研究趋势进行了展望。
White LEDs are typically used as illuminators and indicators and used in displays due to low energy consumption, high brightness levels, low operating voltages and longer lifetimes. The white LED is composed of a blue LED chip ((In.Ga)N) and a color conversion layer of YAG:Ce3+ phosphors dispersed in a medium such as epoxy resin. It is based on the principle of integrating two complementary luminescence emissions to generate white light suitable for lighting applications. Part of the blue light from the (In.Ga)N LED is absorbed by the color conversion layer and is converted into yellow light. The combination of blue and yellow gives a bright white light source. Ce3+-doped YAG phosphors have been recognized as the most excellent phosphors satisfactorily applied in vacuum ultraviolet. plasma display panels, solid-stated lasers, and white LED commercial market, because of the high luminescent efficiency and chemical stability. In this article, the development of YAG:Ce3+ photoluminescent materials and photoluminescent mechanism and common preparation methods are introduced. Furthermore, a novel simple method which is called Direct Evaporation Sintering Method (DESM) is proposed for preparing YAG:Ce3+phosphors.
In this paper, YAG:CeJ3+ phosphors have prepared by solvothermal method and DESM, respectively. We study the effect of sintering temperature on crystallization properties, surface morphology and luminescent properties of YAG:Ce3+ phosphors. Meanwhile, we pay attention to the behavior of temperature-dependence of luminescence, fluorescence decay lifetimes and quantum efficiency (QE) of prepared YAG:Ce3+ phosphors. which make up the insufficient data of lower temperature luminescent properties of YAG:CeJ-phosphors in the existing literatures. Such as follows:
For solvothermal method, the formation temperature of YAG phase is about 900℃, while the pure YAG phase can be obtained at 1000℃. The morphology of the particles can be described as irregular ellipse spherical and the average particle size is about 35 nm. As shown in PL spectra of YAG:Ce3+ phosphors, The excitation spectra are consist of two broad Ce3+ absorption bands peaked at 340 nm and 460 nm. And the emission spectra show a broad emission band with a maximum at 540 nm and located in the range from 500 nm to 700 nm.
Compared with the solvothermal method (STM), DESM has some advantages. Firstly, DESM is very simple; reaction product does not need to fast speed centrifugation. water or alcohol washes. So, the problems of products loss and new impurities which are caused by these processes can be avoided. Secondly, the sintering temperature of DESM is lower. According to the XRD results, the pure YAG phase can be generated at 1000℃by STM. and the morphology of the samples is irregularly spherical. While the pure YAG phase can be formed at 850℃by DESM, and the surface morphology of the YAG:Ce3+ phosphors can be described as spherical, and the average particle size is about 30 nm. For the quantum efficiency (QE) of prepared YAG:Ce3+ phosphors, the QE of DESM is 9% higher than STM. Furthermore, the high-pressure reaction kettle is needed for STM, while DESM does not need it. All reaction processes are carried out in open systems, and no need expensive high temperature (>1000℃) sintering furnace, so the DESM is more secure, low-cost.
The behavior of temperature-dependence luminescent properties of YAG:Ce3+ phosphors between 6 K and 325 K shows that the luminescent properties are influenced by sintering temperature and environment temperature. As the sintering temperature rising, the impurity phase is gradually disappeared and the crystallinity is increased; surface morphology will become more spherical; luminescent intensity and quantum efficiency are also effectively improved. From the low temperature spectra of YAG:Ce3+ phosphors, we can clearly observe the well-known double band structure of the Ce3+ emission at low environment temperature, that is attributed to the emissions of Ce3+, viz.5d1→2F5/2 and 5d1→2F7/2. And with the rising of temperature, the two emission bands broaden and start to overlap, resulted in one broad emission band. Meanwhile.the intensity of luminescence is exponential decay, and decrease with the environment temperature rising.
Finally, the prospect and the development trend for the YAG:Ce3+ phosphors are also proposed.
本文分别采用溶剂热法和直接蒸发烧结法(DESM)制备YAG:Ce3+荧光粉。研究了这两种制备方法的后处理温度对YAG:Ce3+荧光粉结晶性能、表面形貌、发光性能等的影响。同时还对YAG:Ce3+荧光粉发光性能的温度依赖性、荧光寿命、量子效率等有更深入的研究,弥补了现有文献资料对YAG:Ce3+荧光粉低温发光性能研究数据的不足。总结如下：
溶剂热法合成YAG:Ce3+荧光粉的成相烧结温度大约在900℃,1000℃时得到YAG纯相,粉体颗粒形貌是不规则的球形,颗粒尺寸大约35 nm。样品的光致发光光谱显示出YAG:Ce3+荧光粉的激发光谱中有两个很强的激发峰,分别为340 nm和460nm。发射光谱是一个很宽的发射带(500-700nm),峰值波长为540 nm。
与溶剂热法制备YAG:Ce3+荧光粉相比,DESM法更有优势。首先,DESM法的合成路径更简单,反应物不需要离心、水洗、醇洗等处理过程。如此,便避免了由于这些处理过程可能带来的产物流失或者引入新的杂质元素等问题。其次,DESM法的烧成温度更低。从XRD分析结果可知,溶剂热法烧成的YAG:Ce3+荧光粉的纯相形成温度为1000℃左右,且颗粒形貌不是很规则的球形。而DESM法制备YAG:Ce3+荧光粉的纯相形成温度仅为850℃,而且颗粒形貌是很规则的球形,颗粒平均尺寸为30 nm。量子效率方面,同是纯相的YAG:Ce3+荧光粉,DESM法制备的样品量子效率比溶剂热法合成的产品高9个百分点左右。另外,溶剂热法需要在高压釜内进行,而DESM法在大气环境中即可进行反应,且不需要昂贵的高温(>1000℃)烧结炉,因此DESM法更安全,成本更低。
YAG:Ce3+荧光粉发光的温度依赖性研究结果显示,其发光性能会受烧结温度和环境温度影响。随着烧结温度的提高,YAG:Ce3+荧光粉的杂相含量降低、结晶性能提高；表面形貌逐步趋于圆球形；发光强度逐渐增强；量子效率有效提高。从低温光谱可知,在较低环境温度下,可以明显看到发射峰是由两个峰值很接近的发射峰组成的,分别对应Ce3+的两个能级发射,即5d1→2F5/2和5d1→2F7/2。而且随着温度的升高,发射峰变宽,两个发射峰的重叠部分逐渐增加,变成一个发射宽峰。其发光强度呈指数形式衰减,而且衰减时间会随着环境温度的增加而降低。
文章最后,我们对YAG:Ce3+荧光粉的发展前景及今后的研究趋势进行了展望。
White LEDs are typically used as illuminators and indicators and used in displays due to low energy consumption, high brightness levels, low operating voltages and longer lifetimes. The white LED is composed of a blue LED chip ((In.Ga)N) and a color conversion layer of YAG:Ce3+ phosphors dispersed in a medium such as epoxy resin. It is based on the principle of integrating two complementary luminescence emissions to generate white light suitable for lighting applications. Part of the blue light from the (In.Ga)N LED is absorbed by the color conversion layer and is converted into yellow light. The combination of blue and yellow gives a bright white light source. Ce3+-doped YAG phosphors have been recognized as the most excellent phosphors satisfactorily applied in vacuum ultraviolet. plasma display panels, solid-stated lasers, and white LED commercial market, because of the high luminescent efficiency and chemical stability. In this article, the development of YAG:Ce3+ photoluminescent materials and photoluminescent mechanism and common preparation methods are introduced. Furthermore, a novel simple method which is called Direct Evaporation Sintering Method (DESM) is proposed for preparing YAG:Ce3+phosphors.
In this paper, YAG:CeJ3+ phosphors have prepared by solvothermal method and DESM, respectively. We study the effect of sintering temperature on crystallization properties, surface morphology and luminescent properties of YAG:Ce3+ phosphors. Meanwhile, we pay attention to the behavior of temperature-dependence of luminescence, fluorescence decay lifetimes and quantum efficiency (QE) of prepared YAG:Ce3+ phosphors. which make up the insufficient data of lower temperature luminescent properties of YAG:CeJ-phosphors in the existing literatures. Such as follows:
For solvothermal method, the formation temperature of YAG phase is about 900℃, while the pure YAG phase can be obtained at 1000℃. The morphology of the particles can be described as irregular ellipse spherical and the average particle size is about 35 nm. As shown in PL spectra of YAG:Ce3+ phosphors, The excitation spectra are consist of two broad Ce3+ absorption bands peaked at 340 nm and 460 nm. And the emission spectra show a broad emission band with a maximum at 540 nm and located in the range from 500 nm to 700 nm.
Compared with the solvothermal method (STM), DESM has some advantages. Firstly, DESM is very simple; reaction product does not need to fast speed centrifugation. water or alcohol washes. So, the problems of products loss and new impurities which are caused by these processes can be avoided. Secondly, the sintering temperature of DESM is lower. According to the XRD results, the pure YAG phase can be generated at 1000℃by STM. and the morphology of the samples is irregularly spherical. While the pure YAG phase can be formed at 850℃by DESM, and the surface morphology of the YAG:Ce3+ phosphors can be described as spherical, and the average particle size is about 30 nm. For the quantum efficiency (QE) of prepared YAG:Ce3+ phosphors, the QE of DESM is 9% higher than STM. Furthermore, the high-pressure reaction kettle is needed for STM, while DESM does not need it. All reaction processes are carried out in open systems, and no need expensive high temperature (>1000℃) sintering furnace, so the DESM is more secure, low-cost.
The behavior of temperature-dependence luminescent properties of YAG:Ce3+ phosphors between 6 K and 325 K shows that the luminescent properties are influenced by sintering temperature and environment temperature. As the sintering temperature rising, the impurity phase is gradually disappeared and the crystallinity is increased; surface morphology will become more spherical; luminescent intensity and quantum efficiency are also effectively improved. From the low temperature spectra of YAG:Ce3+ phosphors, we can clearly observe the well-known double band structure of the Ce3+ emission at low environment temperature, that is attributed to the emissions of Ce3+, viz.5d1→2F5/2 and 5d1→2F7/2. And with the rising of temperature, the two emission bands broaden and start to overlap, resulted in one broad emission band. Meanwhile.the intensity of luminescence is exponential decay, and decrease with the environment temperature rising.
Finally, the prospect and the development trend for the YAG:Ce3+ phosphors are also proposed.
引文
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