节能灯用蓝粉BaMgAl_(10)O_(17)：Eu~(2+)，Mn~(2+)和绿粉（Ce，Tb）MgAl_(11)O_(19)的改性研究
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摘要
三基色节能灯具有寿命长、显色指数优良、色温可调、节约电能、无辐射污染等特点,因而在倡导绿色照明的行动下得到大力推广。节能灯用三基色荧光粉在紫外激发下均具有优异的光学特性,目前,商业化的三基色荧光粉主要有：红粉Y2O3:Eu2+、蓝粉BaMgAl10O17:Eu2+/BaMgAl10O17:Eu2+, Mn2+(BAM)和绿粉(Ce,Tb)MgAl11O19(CMAT)。然而随着三基色节能灯的广泛使用,三基色粉中蓝粉和绿粉的问题也日益凸现出来。蓝粉BAM由于自身结构的限制,在制灯和日常使用中存在明显的热劣化和辐照劣化现象,严重影响节能灯的显色性及使用寿命；工业中绿粉CMAT的合成采用高温固相法,虽然合成工艺、设备简单,但烧结出的荧光粉因团聚严重而必须经过球磨,破坏荧光粉晶形、亮度下降。本论文针对蓝粉BAM和绿粉CMAT在实际应用中的问题做相关改性研究,包括以下内容：
1、将BaMgAl10O17:Eu2+,Mn2+的热劣化和辐照劣化现象进行对比研究,通过对发射光谱、吸收光谱、热释光谱和ICP数据的分析发现了热劣化和辐照劣化的异同点。
2、沿用高温固相法,研究不同助熔剂对(Ce,Tb)MgAl11O19绿色荧光粉发光性能的影响。发现添加了复合助熔剂后,(Ce,Tb)MgAl11O19绿色荧光粉发光性能有所改善。
热处理和紫外辐照处理都能使BaMgAl10O17:Eu2+,Mn2+发生劣化,但热劣化主要涉及到Eu2+的氧化及其格位偏移,紫外辐照劣化则与上述过程无关,而是主要源自于高能辐照使Eu2+处于更不稳定的状态；调节H3BO3+AlF3+NH4F复合助熔剂比例可制备出分散性好、形貌规则、亮度高的(Ce,Tb)MgAl11O19绿色荧光粉。
Tricolor compact fluorescent lamp is widely used at the call of "Green Lighting" because of the characteristics such as long service life, excellent color index, color temperature adjustable, energy saving, no radiation pollution, and so on. Tricolor phosphors for compact fluorescent lamp exhibit excellent photoluminescence excited by ultraviolet. At present, the commercial tricolor phosphors are red Y2O3:Eu2+, blue BaMgAl10O17:Eu2+/BaMgAl10O17:Eu2+, Mn2+(BAM) and green (Ce,Tb)MgAl11O19(CMAT). However, the problems of ricolor phosphors become obvious with the tricolor compact fluorescent lamp widely used. The thermal and the ultraviolet radiation degradation appears in lamp-making and daily use due to BAM phosphor's structure limitation, effecting the color and service life of compact fluorescent lamp seriously. The CMAT phosphor powders were prepared by conventional high-temperature solid state reaction in industrial production. But the phosphors sintering to agglomeration seriously and must to be through ball milling in order to get uniform size phosphor although the simple synthesis process and equipment. Milling process reduces the brightness of phosphors due to the damages of surface structure. In this paper, some experimental work was done for improving the photo luminescent properties of BaMgAl10O17:Eu2+,Mn2+and (Ce,Tb)MgAl11O19phosphors. The main works were contained as below:
1. The thermal and the ultraviolet radiation degradation mechanisms of BaMgAl10O17:Eu2+, Mn2+phosphor are investigated in a comparative way. The difference between the thermal and the ultraviolet radiation degradation mechanisms have been found through emission spectra, absorption spectra, thermoluminescence spectra and ICP analysis data.
2. The effect of flux on (Ce,Tb)MgAl11O19phosphor through high-temperature solid state reaction is studied. The photoluminescence of (Ce,Tb)MgAl11O19phosphor was improved due to the addition of complex flux.
Thermal and ultraviolet radiation treatments can both seriously damage the luminous efficiency of BaMgAl10O17:Eu2+,Mn2+. It is revealed that the thermal degradation is involved in the oxidation and migration of Eu2+ions. The ultraviolet radiation makes the Eu2+in metastable state, which weakens the direct absorption of Eu2+and thus reduces the relative luminescence intensity of BaMgAl10O17:Eu2+,Mn2+. The H3BO3+AIF3+NH4F flux ratio was optimized to prepare the (Ce,Tb)MgAl11O19phosphor powders with fine dispersion, regular morphology, high brightness.
1、将BaMgAl10O17:Eu2+,Mn2+的热劣化和辐照劣化现象进行对比研究,通过对发射光谱、吸收光谱、热释光谱和ICP数据的分析发现了热劣化和辐照劣化的异同点。
2、沿用高温固相法,研究不同助熔剂对(Ce,Tb)MgAl11O19绿色荧光粉发光性能的影响。发现添加了复合助熔剂后,(Ce,Tb)MgAl11O19绿色荧光粉发光性能有所改善。
热处理和紫外辐照处理都能使BaMgAl10O17:Eu2+,Mn2+发生劣化,但热劣化主要涉及到Eu2+的氧化及其格位偏移,紫外辐照劣化则与上述过程无关,而是主要源自于高能辐照使Eu2+处于更不稳定的状态；调节H3BO3+AlF3+NH4F复合助熔剂比例可制备出分散性好、形貌规则、亮度高的(Ce,Tb)MgAl11O19绿色荧光粉。
Tricolor compact fluorescent lamp is widely used at the call of "Green Lighting" because of the characteristics such as long service life, excellent color index, color temperature adjustable, energy saving, no radiation pollution, and so on. Tricolor phosphors for compact fluorescent lamp exhibit excellent photoluminescence excited by ultraviolet. At present, the commercial tricolor phosphors are red Y2O3:Eu2+, blue BaMgAl10O17:Eu2+/BaMgAl10O17:Eu2+, Mn2+(BAM) and green (Ce,Tb)MgAl11O19(CMAT). However, the problems of ricolor phosphors become obvious with the tricolor compact fluorescent lamp widely used. The thermal and the ultraviolet radiation degradation appears in lamp-making and daily use due to BAM phosphor's structure limitation, effecting the color and service life of compact fluorescent lamp seriously. The CMAT phosphor powders were prepared by conventional high-temperature solid state reaction in industrial production. But the phosphors sintering to agglomeration seriously and must to be through ball milling in order to get uniform size phosphor although the simple synthesis process and equipment. Milling process reduces the brightness of phosphors due to the damages of surface structure. In this paper, some experimental work was done for improving the photo luminescent properties of BaMgAl10O17:Eu2+,Mn2+and (Ce,Tb)MgAl11O19phosphors. The main works were contained as below:
1. The thermal and the ultraviolet radiation degradation mechanisms of BaMgAl10O17:Eu2+, Mn2+phosphor are investigated in a comparative way. The difference between the thermal and the ultraviolet radiation degradation mechanisms have been found through emission spectra, absorption spectra, thermoluminescence spectra and ICP analysis data.
2. The effect of flux on (Ce,Tb)MgAl11O19phosphor through high-temperature solid state reaction is studied. The photoluminescence of (Ce,Tb)MgAl11O19phosphor was improved due to the addition of complex flux.
Thermal and ultraviolet radiation treatments can both seriously damage the luminous efficiency of BaMgAl10O17:Eu2+,Mn2+. It is revealed that the thermal degradation is involved in the oxidation and migration of Eu2+ions. The ultraviolet radiation makes the Eu2+in metastable state, which weakens the direct absorption of Eu2+and thus reduces the relative luminescence intensity of BaMgAl10O17:Eu2+,Mn2+. The H3BO3+AIF3+NH4F flux ratio was optimized to prepare the (Ce,Tb)MgAl11O19phosphor powders with fine dispersion, regular morphology, high brightness.
引文
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