白光LED用BaMoO_4:Pr~(3+)体系红色荧光材料的制备及其光学性能研究
摘要
本论文通过一种简单方便的制备方法合成了高效的BaMoO4:Pr3+系列红色荧光粉,研究了掺杂碱金属、卤素等阴阳离子对其光学性能的影响。并在没添加任何表面活性剂的条件下,通过溶液化学法合成了BaMoO4:Pr3+/Na纳米晶构成的空心微球。同时,我们利用差热-热重(TG-DTA)、X-射线衍射(XRD)、X光电子能谱(XPS)、比表面吸附(BET)、扫描电子显微镜(SEM)、场发射扫描电子显微镜(FESEM)透射电子显微镜(TEM)、高分辨透射电子显微镜(HRTEM)及荧光光谱(PL)等测试手段对制备材料的结构、形貌及光学性能等方面进行了详细的表征,并得到如下结果:
通过简便的固相反应法,在900oC烧结条件下,成功地合成了Pr3+离子掺杂的BaMoO4红色荧光粉。所制备的发光材料粒径在3μm以下,对430～500 nm的光谱有很好的吸收,并能很强的发出主峰位于643 nm的红光,其发光强度约是商业红粉Y2O2S:Eu发光强度的5.6倍。并且该材料的物理化学性能稳定,发光效率较高。同时,该材料制作方法简便,原材料成本较低,完全适于工业化生产。该材料应用于白光LEDs将显著改善其显色性。
在制备BaMoO4:Pr3+的起始原料BaCO3, (NH4)6Mo7O24·4H2O和Pr6O11中加入碱金属卤化物,从而在材料中引入了碱金属离子和卤素离子,成功地制备了碱金属和卤素共掺杂的荧光材料。碱金属、卤素的掺杂可以起到平衡材料中电荷的作用。引入碱金属和卤素后,荧光材料的发光性能得到了显著提高,是掺杂前荧光材料发光强度的2.67倍。同时考察了样品的温度淬灭特性。实验表明:当测试温度达到150 oC时Ba0.96MoO4:0.02Pr3+,0.02KCl样品的发光强度仍保持在74%以上,满足市场上白光LEDs对荧光材料温度淬灭的应用指标。
另外,我们采用一种简便的溶液化学方法,在不添加任何表面活性剂的情况下,成功地合成了BaMoO4:Pr3+/Na+纳米晶空心微球。所制备的空心微球是由30-60 nm的BaMoO4:Pr3+/Na+纳米晶构成的,并且粒径均匀、在3-5μm之间。构成空心微球的纳米晶具有极高的结晶度,产生了非常优良的的红光特性。在样品中存在的少量Na+离子能够起到电荷补偿的作用,从而改善材料的光学性能。论文还对纳米晶空心微球BaMoO4:Pr3+/Na+的形成机理进行了深入的探讨,我们用奥斯特瓦熟化定律合理的解释了它的形成过程,并提出柠檬酸在纳米晶空心微球的形成过程中起到了关键的作用。同时,这种不添加表面活性剂的自组装方法也为设计构造其它新型的功能纳米装置提供了一种新的思路。
A highly efficient red phosphor, BaMoO4:Pr3+, has been fabricated by a convenient method and we researched the influence of optical properties by doping alkali metals and halide in the phosphor system BaMoO4:Pr3+. We also prepared BaMoO4:Pr3+/Na+ hollow microspheres composed of nanocrystals by a solution chemistry method without adding any templates. In addition,the structures, morphologies and optical properties of as-prepared products were thoroughly characterized by using TG-DTA, XRD, XPS, BET, SEM, FESEM, TEM, HRTEM), and PL, respectively. The main results are summarized as follows:
BaMoO4:Pr3+ phosphors were synthesized successfully by a convenient solid method via annealing at 900°C. The sizes of as-prepared particles are below 3μm and a strong red emission band centered at 643nm corresponding to the transition 3P0→3F2 of Pr3+ is observed under 430-500 nm excitation. The emission intensity of red phosphor BaMoO4: Pr3+ is 5.6 times compared with that of the commercial red phosphor Y2O2S:Eu3+. And the materials have the stable physical and chemical properties and high luminous efficiency. Furthermore, the material method is simple and the raw materials are low cost, fully suitable for industrial production. The color rendering will be improved significantly when the materials applied in white LEDs. The introduce of alkali metal and halide in the phosphor system BaMoO4:Pr3+ and the alkali metal and halide co-doped phosphors were prepared by adding appropriate amounts of alkali halide into the mixtures of BaCO3, (NH4)6Mo7O24·4H2O and Pr6O11.
The doping alkali metal and halide can play an important role in balancing the charge in the materials. The red emission intensity was enhanced significantly by doping alkali metal and halide in the BaMoO4:Pr3+ phosphor system and the emission intensity is 2.67 times compared with that of undoped alkali metal and halide samples. In addition, we checked the temperature dependence of the emission intensity of samples. Experimental results showed that the red emission intensity of Ba0.96MoO4:0.02Pr3+,0.02KCl remained about 74% at 150°C which met the temperature quenching indicators of phosphors for white LED application in the market.
In addition, we prepared BaMoO4:Pr3+/Na+ hollow microspheres composed of nanocrystals by a solution chemistry method without adding any templates. The average size of hollow mirospheres was 3-5μm and the hollow mirospheres composed by nanocrystals well-dispersed with a 30-60 nm size. The nanocrystals with extraordinarily high crystallinity produce excellent luminescence emission. The small amount of Na+ ions in BaMoO4:Pr3+ hollow mirospheres can play a role in charge balance and improve the optical properties of the materials. The paper discussed the growth mechanism of the hollow structured BaMoO4:Pr3+/Na+ microspheres. We explained the growth mechanism by Ostwald ripening and put forward that citric acid played a key role in the formation process of hollow microspheres composed of nanocrystals.Furthermore, the self-assembly concept may also be applicable to other compounds for design and fabrication of novel functional nanoarchitectures.
通过简便的固相反应法,在900oC烧结条件下,成功地合成了Pr3+离子掺杂的BaMoO4红色荧光粉。所制备的发光材料粒径在3μm以下,对430～500 nm的光谱有很好的吸收,并能很强的发出主峰位于643 nm的红光,其发光强度约是商业红粉Y2O2S:Eu发光强度的5.6倍。并且该材料的物理化学性能稳定,发光效率较高。同时,该材料制作方法简便,原材料成本较低,完全适于工业化生产。该材料应用于白光LEDs将显著改善其显色性。
在制备BaMoO4:Pr3+的起始原料BaCO3, (NH4)6Mo7O24·4H2O和Pr6O11中加入碱金属卤化物,从而在材料中引入了碱金属离子和卤素离子,成功地制备了碱金属和卤素共掺杂的荧光材料。碱金属、卤素的掺杂可以起到平衡材料中电荷的作用。引入碱金属和卤素后,荧光材料的发光性能得到了显著提高,是掺杂前荧光材料发光强度的2.67倍。同时考察了样品的温度淬灭特性。实验表明:当测试温度达到150 oC时Ba0.96MoO4:0.02Pr3+,0.02KCl样品的发光强度仍保持在74%以上,满足市场上白光LEDs对荧光材料温度淬灭的应用指标。
另外,我们采用一种简便的溶液化学方法,在不添加任何表面活性剂的情况下,成功地合成了BaMoO4:Pr3+/Na+纳米晶空心微球。所制备的空心微球是由30-60 nm的BaMoO4:Pr3+/Na+纳米晶构成的,并且粒径均匀、在3-5μm之间。构成空心微球的纳米晶具有极高的结晶度,产生了非常优良的的红光特性。在样品中存在的少量Na+离子能够起到电荷补偿的作用,从而改善材料的光学性能。论文还对纳米晶空心微球BaMoO4:Pr3+/Na+的形成机理进行了深入的探讨,我们用奥斯特瓦熟化定律合理的解释了它的形成过程,并提出柠檬酸在纳米晶空心微球的形成过程中起到了关键的作用。同时,这种不添加表面活性剂的自组装方法也为设计构造其它新型的功能纳米装置提供了一种新的思路。
A highly efficient red phosphor, BaMoO4:Pr3+, has been fabricated by a convenient method and we researched the influence of optical properties by doping alkali metals and halide in the phosphor system BaMoO4:Pr3+. We also prepared BaMoO4:Pr3+/Na+ hollow microspheres composed of nanocrystals by a solution chemistry method without adding any templates. In addition,the structures, morphologies and optical properties of as-prepared products were thoroughly characterized by using TG-DTA, XRD, XPS, BET, SEM, FESEM, TEM, HRTEM), and PL, respectively. The main results are summarized as follows:
BaMoO4:Pr3+ phosphors were synthesized successfully by a convenient solid method via annealing at 900°C. The sizes of as-prepared particles are below 3μm and a strong red emission band centered at 643nm corresponding to the transition 3P0→3F2 of Pr3+ is observed under 430-500 nm excitation. The emission intensity of red phosphor BaMoO4: Pr3+ is 5.6 times compared with that of the commercial red phosphor Y2O2S:Eu3+. And the materials have the stable physical and chemical properties and high luminous efficiency. Furthermore, the material method is simple and the raw materials are low cost, fully suitable for industrial production. The color rendering will be improved significantly when the materials applied in white LEDs. The introduce of alkali metal and halide in the phosphor system BaMoO4:Pr3+ and the alkali metal and halide co-doped phosphors were prepared by adding appropriate amounts of alkali halide into the mixtures of BaCO3, (NH4)6Mo7O24·4H2O and Pr6O11.
The doping alkali metal and halide can play an important role in balancing the charge in the materials. The red emission intensity was enhanced significantly by doping alkali metal and halide in the BaMoO4:Pr3+ phosphor system and the emission intensity is 2.67 times compared with that of undoped alkali metal and halide samples. In addition, we checked the temperature dependence of the emission intensity of samples. Experimental results showed that the red emission intensity of Ba0.96MoO4:0.02Pr3+,0.02KCl remained about 74% at 150°C which met the temperature quenching indicators of phosphors for white LED application in the market.
In addition, we prepared BaMoO4:Pr3+/Na+ hollow microspheres composed of nanocrystals by a solution chemistry method without adding any templates. The average size of hollow mirospheres was 3-5μm and the hollow mirospheres composed by nanocrystals well-dispersed with a 30-60 nm size. The nanocrystals with extraordinarily high crystallinity produce excellent luminescence emission. The small amount of Na+ ions in BaMoO4:Pr3+ hollow mirospheres can play a role in charge balance and improve the optical properties of the materials. The paper discussed the growth mechanism of the hollow structured BaMoO4:Pr3+/Na+ microspheres. We explained the growth mechanism by Ostwald ripening and put forward that citric acid played a key role in the formation process of hollow microspheres composed of nanocrystals.Furthermore, the self-assembly concept may also be applicable to other compounds for design and fabrication of novel functional nanoarchitectures.
引文
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