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草酸沉淀法制备细颗粒红色荧光粉Y2O3∶Eu3+的发光特性
Luminescent Properties of Small-sized Red Phosphor Y2O3∶Eu3+ Synthesized by Oxalic Acid Precipitation Method
【摘要】 对草酸作为沉淀剂制备的细颗粒红色荧光粉Y2 O3 ∶Eu3 + 进行结构和发光特性研究 ,结果表明 :其一次粒径为 2 0~ 30nm ,团聚尺寸D50 =0 .5 3μm。该荧光粉最大激发峰位于 2 5 2 .2nm ,较微米级荧光粉 2 33nm红移了 19.2nm ;最大的发射峰位于 6 12nm ,与微米级的相比几乎没有差别。Eu3 + 离子的掺入构成了发光中心 ,其最佳掺杂的质量分数为 9% ,荧光粉发光的猝灭浓度由微米级的 6 %提高到 9%。由于纳米晶存在表面缺陷和悬挂键 ,其亮度约为微米晶的 70 %左右 ,随着团聚尺寸的增加、煅烧温度的提高和助熔剂的加入 ,荧光粉的发光强度增大。包膜能部分消除表面缺陷和悬挂键 ,提高发光亮度。荧光粉的色坐标为x =0 .6 4 79,y =0 .344 2。
【Abstract】 Y2O3∶Eu3+ is a red phosphor with good property. It is usually synthesized by high temperature solid state method. The particle size of the phosphor prepared by this method is lager ,so it must be milled when used. The oxalic acid precipitation method was developed to synthesize non-grinded and small-size red phosphor in our experiment. Firstly, the mixture of Y2O3 and Eu2O3 was dissolved in nitric acid in certain proportion. Secondly, the prepared oxalic acid solution was placed in a reactor and at the same time a little surfactant was added in it. When the reaction temperature was controlled to be certain value, the nitric acid solution of Y, Eu was added. Afterwards the precipitation formed and then washed, filtrated, dried and calcined to become white Y2O3∶Eu3+ power. The Luminescent properties of the phosphor were mainly studied . The result shows that the particle diameter is 20~30 nm . The agglomerate size is D50 =0.53 μm. The particle is fine and the granularity distribution displays a narrow and normal distribution. The maximum excitation spectrum of the phosphor peaks at λ=252.2 nm, red shift 19.2 nm compared with micro-Y2O3∶Eu3+. The maximum emission spectrum peaks at λ=612 nm under 254 nm excitation. Compared with the ordinary power of Y2O3∶Eu3+ , the emission spectrum of the phosphor appears unchangeable. The luminescent intensity increases with growing of agglomerate size. The addition of Eu3+ can constitute luminescent centers when Y2O3 as basic particle and Eu3+as activator in Y2O3∶Eu3+ . The less the amount of the added Eu3+ is, the lower the luminescent brightness of the phosphor is. The critical concentration of Eu3+ increases from 6% for micro-Y2O3∶Eu3+ to 9% for nano-Y2O3∶Eu3+. The phosphor shows a relative luminescent brightness about 70% of that of the micro-Y2O3∶Eu3+, because of the existence of hanging-bonds and defects on the surface of nano-Y2O3∶Eu3+ particles. The phosphor particle was increased and the defects on the surface of the phosphor was decreased at high temperature, so luminescent brightness of the phosphors was increased. Adding assist melting agent can decrease sintering temperature and increase D50 of the phosphor,and the brightness of the phosphor increased, too. Coating-process on phosphor can dispel defact and increase brightness. The luminescent chromatic coordinate parameters of the phosphor are x=0.647 9, y=0.344 2 ,which accords with the phosphor.
【Key words】 oxalic acid precipitation; small-sized; phosphor; Y2O3∶Eu3+; luminescence;
- 【文献出处】 发光学报 ,Chinese Journal of Luminescence , 编辑部邮箱 ,2004年04期
- 【分类号】O482.31
- 【被引频次】24
- 【下载频次】403