PDP纳米BaMgAl_（10）O_（17）：Eu～（2+）蓝色荧光粉的燃烧合成及其光谱特性
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摘要
在真空紫外光(VUV)激发下,BaMgAl10O17:Eu~(2+)(BAM)因具有量子效率和发光效率高以及色纯度好等优点而广泛应用于等离子平板显示(PDP)。
高温固相法是制备BAM荧光粉最常用的方法,但用这种方法合成的荧光粉尺寸较大(5~20μm)且形貌不规则,必须进一步通过长时间的球磨处理。但球磨会破坏晶形并增加晶体缺陷,从而导致荧光粉的发光强度下降。因此,开发制备BAM荧光粉的新工艺,对于降低BAM荧光粉的生产成本并提高其发光效率,均具有重要的意义。
溶液燃烧合成(solution combustion synthesis)技术是近年来倍受重视的一种制备超细甚至纳米氧化物粉末的新方法。本文采用溶液燃烧合成法制备了Eu2+离子激活的BAM蓝色纳米荧光粉,利用X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)和荧光光谱仪分别对不同工艺条件下获得的荧光粉的相结构、颗粒形貌和光谱特性进行了表征。
研究结果表明,工艺参数对BAM蓝色荧光粉颗粒形貌、粒径、发光性能和晶体结构有很大影响。当尿素与金属硝酸盐的摩尔比为2.0时,在600℃炉温下合成的产物为纯BAM相,平均颗粒尺寸为45nm;合成的BAM蓝色荧光粉的发光强度随Eu2+浓度增大而逐渐增大,且在Eu2+浓度x = 0.2时,其发光强度达到最大值。另外,添加量1.0 wt.%的H3BO3,可使合成的荧光粉的发光强度提高30%以上;而且,添加聚乙二醇(PEG)可改善BAM颗粒的形态和尺寸,当PEG的添加量为5.0 wt.%时,合成的BAM颗粒呈近球形且尺寸均一而细小(30nm)。
BaMgAl10O17:Eu2+ (BAM) has been widely used in plasma display panels (PDP) due to its merits such as good chromaticity, high quantum efficiency and luminescence efficiency under the excitation of vacuum ultraviolet (VUV) light.
The BAM have been mainly prepared by high temperature solid-state reaction process, the obtained phosphor contains irregularly shaped and aggregated particles (5~20μm). Therefore, a milling process for long time is required, but the process creates surface and crystal defects which reduce the brightness of the phosphor. Therefore, the development of new processes for preparing BAM has important significance,not only lowering production costs but also improving its luminous efficiency.
Recently, as a novel technology for the prepareation of oxidate powders with superfine or nanometer size, the solution combustion method has been gotten considerable attentions. In this paper, the technology was applied to prepare Eu2+ actived BAM blue phosphor. Phase structure, morphology and spectrum characteristic of the phosphor synthesized under different processing parameters were characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and spectrophotofluorometer.
The results indicate that the particle morphology, grain size, luminescent property and crystal structure of BAM phosphor is considerably influenced by processing parameters. When mol tatio of urea and metal nitrate is 2.0, the sample is BAM single phase with 600℃furnace temperature and its average grain size is about 45nm. The intensity of the fluorescence of BAM was increased obviously with increasing the Eu2+ doping concentration, and the optimum emission intensity was reached at x=0.2 . In addition, the content of H3BO3 is about 1.0%, which increased the relative emission intensity of the phosphor over 30%.Moreover, added PEG to improve BAM particle size and shape, when the content of PEG is 5.0%, the particles have nearly spherical shape, homogeneous and small size (30nm).
高温固相法是制备BAM荧光粉最常用的方法,但用这种方法合成的荧光粉尺寸较大(5~20μm)且形貌不规则,必须进一步通过长时间的球磨处理。但球磨会破坏晶形并增加晶体缺陷,从而导致荧光粉的发光强度下降。因此,开发制备BAM荧光粉的新工艺,对于降低BAM荧光粉的生产成本并提高其发光效率,均具有重要的意义。
溶液燃烧合成(solution combustion synthesis)技术是近年来倍受重视的一种制备超细甚至纳米氧化物粉末的新方法。本文采用溶液燃烧合成法制备了Eu2+离子激活的BAM蓝色纳米荧光粉,利用X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)和荧光光谱仪分别对不同工艺条件下获得的荧光粉的相结构、颗粒形貌和光谱特性进行了表征。
研究结果表明,工艺参数对BAM蓝色荧光粉颗粒形貌、粒径、发光性能和晶体结构有很大影响。当尿素与金属硝酸盐的摩尔比为2.0时,在600℃炉温下合成的产物为纯BAM相,平均颗粒尺寸为45nm;合成的BAM蓝色荧光粉的发光强度随Eu2+浓度增大而逐渐增大,且在Eu2+浓度x = 0.2时,其发光强度达到最大值。另外,添加量1.0 wt.%的H3BO3,可使合成的荧光粉的发光强度提高30%以上;而且,添加聚乙二醇(PEG)可改善BAM颗粒的形态和尺寸,当PEG的添加量为5.0 wt.%时,合成的BAM颗粒呈近球形且尺寸均一而细小(30nm)。
BaMgAl10O17:Eu2+ (BAM) has been widely used in plasma display panels (PDP) due to its merits such as good chromaticity, high quantum efficiency and luminescence efficiency under the excitation of vacuum ultraviolet (VUV) light.
The BAM have been mainly prepared by high temperature solid-state reaction process, the obtained phosphor contains irregularly shaped and aggregated particles (5~20μm). Therefore, a milling process for long time is required, but the process creates surface and crystal defects which reduce the brightness of the phosphor. Therefore, the development of new processes for preparing BAM has important significance,not only lowering production costs but also improving its luminous efficiency.
Recently, as a novel technology for the prepareation of oxidate powders with superfine or nanometer size, the solution combustion method has been gotten considerable attentions. In this paper, the technology was applied to prepare Eu2+ actived BAM blue phosphor. Phase structure, morphology and spectrum characteristic of the phosphor synthesized under different processing parameters were characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and spectrophotofluorometer.
The results indicate that the particle morphology, grain size, luminescent property and crystal structure of BAM phosphor is considerably influenced by processing parameters. When mol tatio of urea and metal nitrate is 2.0, the sample is BAM single phase with 600℃furnace temperature and its average grain size is about 45nm. The intensity of the fluorescence of BAM was increased obviously with increasing the Eu2+ doping concentration, and the optimum emission intensity was reached at x=0.2 . In addition, the content of H3BO3 is about 1.0%, which increased the relative emission intensity of the phosphor over 30%.Moreover, added PEG to improve BAM particle size and shape, when the content of PEG is 5.0%, the particles have nearly spherical shape, homogeneous and small size (30nm).
引文
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