稀土掺杂钒酸盐、硼酸盐荧光粉的熔盐法制备及发光性能研究
发布时间：2019-02-25 21:08
【摘要】： 稀土钒酸盐、硼酸盐因其在紫外和真空紫外区有很好的透明性及较强的吸收并能将能量有效地传递给激活离子,因此被广泛地应用于光学、电学、磁学等领域。但是,此前该类材料主要采用高温固相法来生产,由于污染严重,投入过高,制备复杂,荧光粉粒径较大,形状难以控制等大大影响了该类荧光粉的商业应用,已经越来越不适应当前社会节能环保的需求。寻找污染程度低,造价低廉,产品发光性能优良的制备方法已经成为当前发光材料工业的主流。熔盐法(MSS)是近年来发展较快的一种新型粉体合成工艺,能耗较低,因此在荧光粉的生产领域受到广泛关注。如果将熔盐技术应用到上述材料的合成中,必将取得较好的经济价值和社会效益。 本文采用熔盐法,利用氯盐或硝酸盐作为熔盐合成出了发光性能优异、结晶性良好的稀土钒酸盐(YVO4:Eu3+、YVO4:Sm3+、YVO4:Dy3+、YVO4:Dy3+/Tm3+)及硼酸盐(YBO3:Eu3+、YBO3:Tb3+)荧光材料,合成粉体粒径均一,平均粒径在几百纳米左右。具体研究结果如下： 1、利用氯盐、硝酸盐作为熔盐体系,成功地合成了锆石结构的YVO4:Eu3+、YVO4:Sm3+、YVO4:Dy3+、YVO4:Dy3+/Tm3+荧光粉。合成的样品在紫外线照射下,均发射出掺杂稀土离子的特征发射,样品YVO4:Eu3+发射峰位对应于Eu3+的5D0→7Fn(n=0,1,2,3,4)跃迁。其中5D0→7F2跃迁发射峰为最强发射峰,粉体平均粒径为150 nm左右。在YVO4:Eu3+体系中通过Bi3+取代部分Y3+,实现了发射峰位强度的调控。 2、YVO4:Sm3+也能产生Sm3+的特征发射,但是与其它报道的掺Sm3+发光材料相比,熔盐法合成样品位于647 nm处Sm3+的4G5/2→6H9/2发射得到明显加强,从而使得样品发出明亮的红光,而不是通常的橙色光。当以硝酸盐作为熔盐体系时,最佳合成工艺参数为：掺杂浓度为1%；保温温度为500℃；保温时间为5个小时。 3、以硝酸钠作为熔盐成功地合成了YVO4:Dy3+黄色荧光材料；在此基础之上通过引入Tm3+合成了YVO4:Dy3+/Tm3+白色荧光材料,并通过调节Dy3+/Tm3+的掺杂浓度比例实现了对材料发光色度坐标的调控。 4、利用硝酸盐作为熔盐体系,成功地合成了六方结构的YBO3:Eu3+、YBO3:Tb3+荧光粉。荧光光谱(PL)分析结果表明,样品产生了稀土离子的特征发射,红色荧光粉YBO3:Eu3+发射峰对应于Eu3+的5D0→7F1,5D0→7F2跃迁,其中5D0→7F1跃迁略强于5D0→7F2；黄绿色荧光粉YBO3:Tb3+发射峰位对应于Tb3+的5D4→7Fn(n=3,4,5,6)跃迁。其中5D4→7F5跃迁的发射峰处于主导地位,其他的跃迁表现为相对弱的谱线。 本论文的研究工作为采用熔盐法合成稀土掺杂荧光材料,提供了一定的理论和工艺支持。
[Abstract]:Rare earth vanadates and borates are widely used in optical, electrical, magnetic and other fields because of their good transparency and strong absorption in the ultraviolet and vacuum ultraviolet regions and the efficient transfer of energy to active ions. However, because of the serious pollution, high investment, complex preparation, large particle size and difficult to control the shape of this kind of phosphor, the commercial application of this kind of phosphor has been greatly affected by the high temperature solid phase method. Has become increasingly unsuited to the current social demand for energy conservation and environmental protection. The preparation of low pollution, low cost and excellent luminescent properties has become the mainstream of the current luminescent materials industry. Molten salt method (MSS) is a new type of powder synthesis technology, which has been developed rapidly in recent years with low energy consumption, so it has been widely concerned in the field of phosphor production. If the molten salt technology is applied to the synthesis of the above-mentioned materials, better economic and social benefits will be obtained. In this paper, rare earth vanadate (YVO4:Eu3, YVO4:Sm3, YVO4:Dy3, YVO4:Dy3 / Tm3) and borate (YBO3:Eu3, YVO4:Dy3 / Tm3) with excellent luminescence and good crystallinity were synthesized by molten salt method using chloride or nitrate as molten salt. YBO3:Tb3) fluorescent material, the particle size is uniform, the average particle size is about several hundred nanometers. The results are as follows: 1. YVO4:Eu3, YVO4:Sm3, YVO4:Dy3, YVO4:Dy3 / Tm3 phosphors with zircon structure were successfully synthesized by using chloride and nitrate as molten salt system. Under UV irradiation, the synthesized samples all emit characteristic emission of doped rare earth ions, and the peak position of YVO4:Eu3 emission corresponds to the transition of 5D0 / 7Fn (n0, 1, 2, 3, 4) of Eu3. The emission peak of 5D0 / 7F2 transition is the strongest, and the average particle size of the powder is about 150 nm. In the YVO4:Eu3 system, partial Y3 was replaced by Bi3, and the intensity of emission peak was regulated. 2. The characteristic emission of Sm3 can also be produced by YVO4 / Sm3, but compared with other reported Sm3-doped luminescent materials, the emission of 4G5/2 / 6H9/2 of Sm3 at 647 nm is significantly enhanced by molten salt synthesis, which makes the sample emit bright red light. Not the usual orange light. When nitrate is used as molten salt system, the optimum synthetic parameters are as follows: doping concentration is 1%, holding temperature is 500 鈩，
本文编号：2430541
[Abstract]:Rare earth vanadates and borates are widely used in optical, electrical, magnetic and other fields because of their good transparency and strong absorption in the ultraviolet and vacuum ultraviolet regions and the efficient transfer of energy to active ions. However, because of the serious pollution, high investment, complex preparation, large particle size and difficult to control the shape of this kind of phosphor, the commercial application of this kind of phosphor has been greatly affected by the high temperature solid phase method. Has become increasingly unsuited to the current social demand for energy conservation and environmental protection. The preparation of low pollution, low cost and excellent luminescent properties has become the mainstream of the current luminescent materials industry. Molten salt method (MSS) is a new type of powder synthesis technology, which has been developed rapidly in recent years with low energy consumption, so it has been widely concerned in the field of phosphor production. If the molten salt technology is applied to the synthesis of the above-mentioned materials, better economic and social benefits will be obtained. In this paper, rare earth vanadate (YVO4:Eu3, YVO4:Sm3, YVO4:Dy3, YVO4:Dy3 / Tm3) and borate (YBO3:Eu3, YVO4:Dy3 / Tm3) with excellent luminescence and good crystallinity were synthesized by molten salt method using chloride or nitrate as molten salt. YBO3:Tb3) fluorescent material, the particle size is uniform, the average particle size is about several hundred nanometers. The results are as follows: 1. YVO4:Eu3, YVO4:Sm3, YVO4:Dy3, YVO4:Dy3 / Tm3 phosphors with zircon structure were successfully synthesized by using chloride and nitrate as molten salt system. Under UV irradiation, the synthesized samples all emit characteristic emission of doped rare earth ions, and the peak position of YVO4:Eu3 emission corresponds to the transition of 5D0 / 7Fn (n0, 1, 2, 3, 4) of Eu3. The emission peak of 5D0 / 7F2 transition is the strongest, and the average particle size of the powder is about 150 nm. In the YVO4:Eu3 system, partial Y3 was replaced by Bi3, and the intensity of emission peak was regulated. 2. The characteristic emission of Sm3 can also be produced by YVO4 / Sm3, but compared with other reported Sm3-doped luminescent materials, the emission of 4G5/2 / 6H9/2 of Sm3 at 647 nm is significantly enhanced by molten salt synthesis, which makes the sample emit bright red light. Not the usual orange light. When nitrate is used as molten salt system, the optimum synthetic parameters are as follows: doping concentration is 1%, holding temperature is 500 鈩，
本文编号：2430541
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