白光LEDs用掺稀土磷酸盐、焦磷酸盐发光材料的制备及性能研究
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摘要
由于稀土元素的独特电子层结构,稀土离子激活的发光材料往往具有优异的光学性能,而以磷酸盐、焦磷酸盐为基质的发光材料通常具有较好的化学稳定性和热稳定性,因此以磷酸盐、焦磷酸盐为基质的发光材料已成为白光发光二极管(light-emitting diodes, LEDs)用荧光粉的研究热点之一。基于此,本文主要进行了以下几个方面的工作：
1、采用高温固相法合成了新型Ba16Cao.4P207：Eu2+荧光粉,并对其发光性能和能量转移机理进行了研究。光致发光的激发和发射光谱表明,掺杂Eu2+占据了两个不同的晶体学格位；而且随着Eu2+浓度的增加,占据两个不同格位的Eu2+之间发生了能量转移。利用时间分辨光谱研究了供体(Eu2+(1))和受体(Eu2+(2))的发光衰减行为。
2、采用高温固相反应法合成了Eu2+、 Mn2+共掺的新型Ba16Cao4P207：Eu2+,Mn2+荧光粉,并对掺Eu2+、Mn2+的Ba1.6Ca0.4P207的光致发光性能进行了研究。Ba1.6Cao.4P207：0.04Eu2+的发射光谱在400nm和470nm处有两个明显的宽带发射峰。激发光谱为从250nm到400nm的宽带激发。从单掺Mn2+的样品中观测到在565nm处有一个黄色光的宽发射带,并且其强度可通过共掺Eu2+而增强。证明了从Eu2+到Mn2+发生了高效的能量传递。
3、采用高温固相法合成了Ba1.6Cao.4P207:Ce3+,Tb3+荧光粉,研究了其发光性能和Ce3+、Tb3+离子间的能量传递机理。其中,Ba1.6Ca0.4P2O7：Ce3+荧光粉在280nm紫外光激发下,在370nm处有个发射峰,同时在370nm的较长波长处有一个肩峰。从Ba1.6Ca0.4P2O7：Tb3+荧光粉的发射光谱图上可以观测到由Tb3+的5D4-7FJ跃迁引起的特征发射谱线。在紫外光激发下,由于发生了Ce3+到Tb3+的能量传递,所以增强了Tb3+的绿光发射,其能量转移效率可从光谱数据分析得知。
4、采用高温固相反应法合成了Ba3P4013：Eu2+荧光粉,在高温空气气氛中,掺杂的Eu3+几乎都还原成了Eu2+,这种不寻常的还原可以通过电荷补偿机制来解释。光致发光发射光谱和发光衰减动力学研究结果表明,掺杂的Eu2+占据了Ba2+的两个不同的格位,激发光谱为宽带,这与紫外芯片的发射光谱相一致。因此,Ba3P4O13：Eu2+可以作为白光LEDs用荧光粉。
5、采用高温固相反应法合成了Sr3P401.3：Eu2+荧光粉,并对样品的光致发光性能进行了研究,用不同波长的紫外光激发荧光粉得到的发射峰的位置和形状基本相同,其发射峰值波长为408nm,且体系中Eu2+的最佳掺杂浓度为x=0.08。
6、采用高温固相反应法合成了Ca3Mg3(PO4)4：Eu2+荧光粉,并对样品的光致发光性能进行了研究,其发射峰值波长为450nm,最佳掺杂浓度为x=0.08。激发光谱覆盖范围宽,与近紫外芯片的发射匹配,是一种潜在的可以用于白光LEDs的蓝色荧光粉。
Due to the unique electronic shell structure of rare earth elements, the luminescent materials activated by rare earth ions usually have excellent optical properties. Moreover, the luminescent materials based on phosphates and pyrophosphates have good chemical stability and thermal stability. Therefore, the investigation on phosphates and pyrophosphates phosphors for LEDs has attracted more attention recently. In this thesis, I synthesized a series of phosphates and pyrophosphates phosphors and investigated their optical properties:
1. Eu2+doped Ba1.6Cao.4P207phosphors were prepared by high temperature solid state reaction method. The photoluminescence (PL) properties and energy transfer of Ba1.6Ca0.4P207:Eu2+phosphors were investigated. The PL excitation and emission spectra reveal that the doped Eu2+ions occupy two different crystallographic sites. The concentration dependence of PL emission spectra indicates that energy transfer between two different Eu2+ions takes place. Decay kinetics of donor (Eu2+(1)) and acceptor (Eu2+(2)) ions luminescence have also been analyzed. The possible energy transfer mechanism and the temperature dependence of the Eu2+luminescence decay kinetics have also been investigated in detail.
2. Eu2+and Mn2+doped phosphors in the novel system Ba1.6Ca0.4P207were synthesized through high temperature solid state reaction. The PL property of Eu2+Mn2+in Ba1.6Cao.4P207were reported and discussed. The emission spectrum of Ba1.6Ca0.4P2O7:0.04Eu2+consists of two distinct broad bands peaking at about400and470nm, and the excitation spectra exhibit broad band in the range of250to400nm. A broad yellow emission band is observed around565nm in Mn2+single doped sample, and the intensity can be enhanced by co-doping Eu2+ions. It also reveals that the energy transfer from Eu2+to Mn2+occurs in this host lattice.
3. Ba1.6Cao.4P207:Ce3+, Tb3+phosphor was synthesized by the method of high temperature solid state reaction, the emission and excitation spectra and energy transfer of Ce3+and Tb3+in Ba1.6Cao.4P207were also investigated. Under excitation at280nm the emission spectrum of Bai.6Cao.4P207:Ce3+consists of a peak at370nm and a shoulder at the longer wavelength side. The emission spectra of Ba1.6Cao.4P207:Tb3+shows the well-known emission lines due to5D4-7FJ transitions of Tb3+. The green emissions of Tb3+ions are enhanced upon UV excitation through energy transfer from Ce3+to Tb3+ions. The efficiency of such an energy transfer is estimated based on spectroscopic data.
4. Ba3P4O13:Eu2+phosphor was synthesized by the method of high temperature solid-state reaction. The doped Eu3+ions can almost be reduced to Eu2+ions in air atmosphere at high temperature. Besides, the kind of abnormal reduction can be explained by charge compensation mechanism. The fact of the doped Eu2+ions occupy two different Ba2+sites is confirm by PL emission spectrum and luminescence decay kinetics. The PL excitation spectrum shows a broad band which matches well with the emission of near UV chip. Ba3P4O13:Eu2+is a promising phosphor for near UV chip excited white LEDs.
5. Eu2+doped Sr3P4O13phosphors were prepared by high temperature solid state reaction method, the emission and excitation spectra of Eu2+in Sr3P4O13were also investigated. Excited the phosphors by ultraviolet light with different wavelength, the position and appearance of the emission peak are almost the same. The emission spectrum situates at about408nm. The optimum concentration of Eu2+is x=0.08.
6. Ca3Mg3(PO4)4:Eu2+phosphors were synthesized by the method of high temperature solid state reaction. The PL properties of Eu2+in Ca3Mg3(PO4)4were reported and discussed. It is concluded that the wavelength of the emission peak is450nm and the optimum concentration is x=0.08. The wide range of the excitation spectrum matches well with the emission of near UV chip. Therefore, Ca3Mg3(PO4)4:Eu2+phosphor is a promising blue phosphor for white LEDs.
1、采用高温固相法合成了新型Ba16Cao.4P207：Eu2+荧光粉,并对其发光性能和能量转移机理进行了研究。光致发光的激发和发射光谱表明,掺杂Eu2+占据了两个不同的晶体学格位；而且随着Eu2+浓度的增加,占据两个不同格位的Eu2+之间发生了能量转移。利用时间分辨光谱研究了供体(Eu2+(1))和受体(Eu2+(2))的发光衰减行为。
2、采用高温固相反应法合成了Eu2+、 Mn2+共掺的新型Ba16Cao4P207：Eu2+,Mn2+荧光粉,并对掺Eu2+、Mn2+的Ba1.6Ca0.4P207的光致发光性能进行了研究。Ba1.6Cao.4P207：0.04Eu2+的发射光谱在400nm和470nm处有两个明显的宽带发射峰。激发光谱为从250nm到400nm的宽带激发。从单掺Mn2+的样品中观测到在565nm处有一个黄色光的宽发射带,并且其强度可通过共掺Eu2+而增强。证明了从Eu2+到Mn2+发生了高效的能量传递。
3、采用高温固相法合成了Ba1.6Cao.4P207:Ce3+,Tb3+荧光粉,研究了其发光性能和Ce3+、Tb3+离子间的能量传递机理。其中,Ba1.6Ca0.4P2O7：Ce3+荧光粉在280nm紫外光激发下,在370nm处有个发射峰,同时在370nm的较长波长处有一个肩峰。从Ba1.6Ca0.4P2O7：Tb3+荧光粉的发射光谱图上可以观测到由Tb3+的5D4-7FJ跃迁引起的特征发射谱线。在紫外光激发下,由于发生了Ce3+到Tb3+的能量传递,所以增强了Tb3+的绿光发射,其能量转移效率可从光谱数据分析得知。
4、采用高温固相反应法合成了Ba3P4013：Eu2+荧光粉,在高温空气气氛中,掺杂的Eu3+几乎都还原成了Eu2+,这种不寻常的还原可以通过电荷补偿机制来解释。光致发光发射光谱和发光衰减动力学研究结果表明,掺杂的Eu2+占据了Ba2+的两个不同的格位,激发光谱为宽带,这与紫外芯片的发射光谱相一致。因此,Ba3P4O13：Eu2+可以作为白光LEDs用荧光粉。
5、采用高温固相反应法合成了Sr3P401.3：Eu2+荧光粉,并对样品的光致发光性能进行了研究,用不同波长的紫外光激发荧光粉得到的发射峰的位置和形状基本相同,其发射峰值波长为408nm,且体系中Eu2+的最佳掺杂浓度为x=0.08。
6、采用高温固相反应法合成了Ca3Mg3(PO4)4：Eu2+荧光粉,并对样品的光致发光性能进行了研究,其发射峰值波长为450nm,最佳掺杂浓度为x=0.08。激发光谱覆盖范围宽,与近紫外芯片的发射匹配,是一种潜在的可以用于白光LEDs的蓝色荧光粉。
Due to the unique electronic shell structure of rare earth elements, the luminescent materials activated by rare earth ions usually have excellent optical properties. Moreover, the luminescent materials based on phosphates and pyrophosphates have good chemical stability and thermal stability. Therefore, the investigation on phosphates and pyrophosphates phosphors for LEDs has attracted more attention recently. In this thesis, I synthesized a series of phosphates and pyrophosphates phosphors and investigated their optical properties:
1. Eu2+doped Ba1.6Cao.4P207phosphors were prepared by high temperature solid state reaction method. The photoluminescence (PL) properties and energy transfer of Ba1.6Ca0.4P207:Eu2+phosphors were investigated. The PL excitation and emission spectra reveal that the doped Eu2+ions occupy two different crystallographic sites. The concentration dependence of PL emission spectra indicates that energy transfer between two different Eu2+ions takes place. Decay kinetics of donor (Eu2+(1)) and acceptor (Eu2+(2)) ions luminescence have also been analyzed. The possible energy transfer mechanism and the temperature dependence of the Eu2+luminescence decay kinetics have also been investigated in detail.
2. Eu2+and Mn2+doped phosphors in the novel system Ba1.6Ca0.4P207were synthesized through high temperature solid state reaction. The PL property of Eu2+Mn2+in Ba1.6Cao.4P207were reported and discussed. The emission spectrum of Ba1.6Ca0.4P2O7:0.04Eu2+consists of two distinct broad bands peaking at about400and470nm, and the excitation spectra exhibit broad band in the range of250to400nm. A broad yellow emission band is observed around565nm in Mn2+single doped sample, and the intensity can be enhanced by co-doping Eu2+ions. It also reveals that the energy transfer from Eu2+to Mn2+occurs in this host lattice.
3. Ba1.6Cao.4P207:Ce3+, Tb3+phosphor was synthesized by the method of high temperature solid state reaction, the emission and excitation spectra and energy transfer of Ce3+and Tb3+in Ba1.6Cao.4P207were also investigated. Under excitation at280nm the emission spectrum of Bai.6Cao.4P207:Ce3+consists of a peak at370nm and a shoulder at the longer wavelength side. The emission spectra of Ba1.6Cao.4P207:Tb3+shows the well-known emission lines due to5D4-7FJ transitions of Tb3+. The green emissions of Tb3+ions are enhanced upon UV excitation through energy transfer from Ce3+to Tb3+ions. The efficiency of such an energy transfer is estimated based on spectroscopic data.
4. Ba3P4O13:Eu2+phosphor was synthesized by the method of high temperature solid-state reaction. The doped Eu3+ions can almost be reduced to Eu2+ions in air atmosphere at high temperature. Besides, the kind of abnormal reduction can be explained by charge compensation mechanism. The fact of the doped Eu2+ions occupy two different Ba2+sites is confirm by PL emission spectrum and luminescence decay kinetics. The PL excitation spectrum shows a broad band which matches well with the emission of near UV chip. Ba3P4O13:Eu2+is a promising phosphor for near UV chip excited white LEDs.
5. Eu2+doped Sr3P4O13phosphors were prepared by high temperature solid state reaction method, the emission and excitation spectra of Eu2+in Sr3P4O13were also investigated. Excited the phosphors by ultraviolet light with different wavelength, the position and appearance of the emission peak are almost the same. The emission spectrum situates at about408nm. The optimum concentration of Eu2+is x=0.08.
6. Ca3Mg3(PO4)4:Eu2+phosphors were synthesized by the method of high temperature solid state reaction. The PL properties of Eu2+in Ca3Mg3(PO4)4were reported and discussed. It is concluded that the wavelength of the emission peak is450nm and the optimum concentration is x=0.08. The wide range of the excitation spectrum matches well with the emission of near UV chip. Therefore, Ca3Mg3(PO4)4:Eu2+phosphor is a promising blue phosphor for white LEDs.
引文
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