Gd，Eu共掺杂LaPO_4的合成及发光性能研究
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摘要
稀土元素因其独特的4f电子层结构,有着优异的光学性能,在纳米发光材料领域具有很光明的应用前景。发展制备稀土纳米荧光材料的新方法,实现在纳米尺度上原子的可控排列;探索微观形貌与荧光性能的关联性;以及在实际应用上提高发光材料的稳定性和发光亮度对开展稀土发光材料的深度利用和精细研究方面具有独特的意义。
本文采用化学沉淀法和水热法,以Eu2O_3、La(NO_3)_3·6H_2O、Gd(NO_3)_3和H3PO_4为原料,氨水控制pH,合成了Gd~(3+)和Eu~(3+)共掺杂的LaPO_4纳米材料,结合XRD、DTA、SEM和荧光测试等手段,对荧光粉的物相、形貌和发光性能进行了表征,分析了pH值、热处理温度、掺杂离子浓度、表面活性剂对产物性能的影响。
实验结果表明:室温、强酸性溶液中,化学沉淀法合成的粉体为束状的六方相LaPO_4,长度在300-700nm之间;碱性时仍为六方相,但长径比减小,形貌类似枝杈;中性时没有明显衍射峰,变为米粒状的团簇结构。荧光性能显示pH=9时发光强度最好,(~5D_0→~7F_1)和(~5D_0→~7F_2)跃迁强度相当,Eu~(3+)为橙-红发射,不在反演中心格位。粉体经过热处理之后,物相和荧光性能都发生了变化。单斜相逐渐取代六方相,1000℃变为完全的单斜相,发光强度也最高,同时粉体的团聚也变得严重,形成了许多大的块状颗粒。比较不同离子浓度时粉体的荧光性能发现,离子在高浓度时发生了浓度猝灭,确定了最佳离子浓度为Gd~(3+)(2.5%mol),Eu~(3+)(5%mol),Gd~(3+)→Eu~(3+)的能量传递方式为共振能量传递。
控制pH=9,用水热的方法,在不同温度下合成了LaPO_4 :Gd~(3+),Eu~(3+)纳米粉。100℃时得到六方相,不太均一的长棒状结构的LaPO_4;200℃时变为粗短的柱状结构,晶型也变为单斜相。与1000℃煅烧样品相比,晶化程度还不够高,可能是温度不够高,水热釜密封不够好,或者时间不够长所致。因为结晶性能差,发射强度也比较弱。表面活性剂PEG2000的加入,使得晶粒有从棒状生长向颗粒生长的趋势,主要是由于大分子的空间位阻效应抑制了晶粒的各向异性生长。水热条件下晶体的生长可用“生长基元”理论来解释。生长基元通过在某些界面上的叠合来控制生长速率,决定晶体的最终形貌。
Due to the unique 4f electronic shell, lanthanide elements show outstanding optical properties, which make them have bright applications prospect in nanophosphors field. Establishing new synthetic strategies of these materials to make the atomic arrangement controllable in the nano-scale; understanding the relations between morphology and luminescent properties and raising the stability and intensity of materials practically are crucial to deep processing and detailed study of rare earth phosphors.
In this article, chemical precipitation method and hydrothermal method are used to synthesize LaPO_4 :Eu~(3+),Gd~(3+), with Eu2O_3、La(NO_3)3·6H_2O、Gd(NO_3)3 and H3PO_4 as raw materials and ammonia as pH regulator. The phase, morphology and luminescent properties of products are investigated by XRD、DTA、SEM and spectrofluorometers; the effect of pH values, thermal treatment temperature, doped concentration of ions and surfactant on the luminescent properties are studied.
The experimental results show that the products are fasciculated hexagonal LaPO_4 synthesized by chemical precipitation method under acidic condition at room temperature, which have a length of 300-700nm; the phase is still hexagonal with a decreased length-diameter ratio under basic condition but the morphology is branch-like; when pH=7, the grain-like cluster products have no obvious diffraction peaks. Photoluminescence analysis shows that the products have the greatest luminescent properties when pH=7, and the transition intensities of (5D0→7F1) and (5D0→7F2) are equal, indicating a non-centro-symmetrical environment for Eu~(3+) with orange-red emission. The phase、morphology and luminescent properties are changeable after the thermal treatment. Monoclinic powders replace hexagonal ones gradually, and products have a totally monoclinic phase and greatest intensity after calcinations at 1000℃. Meanwhile powders gather into large massive particles. The best concentration of doped ions is confirmed by contrasting photoluminescence intensity of powders with different ion concentrations, the best values of Gd~(3+) and Eu~(3+) are 2.5%mol and 5%mol respectively. Concentration quenching occurs with increasing concentration. The energy transfer mode between Gd~(3+) and Eu~(3+) is resonance transfer dominated by electric multipole interaction.
In the second part, LaPO_4 :Eu~(3+),Gd~(3+) phosphors(pH=9) are synthesized by hydrothermal method at different temperatures. The obtained LaPO_4 is hexagonal phase and inhomogenous linear structure after 100℃. When the temperature is 200℃, the phase turns to monoclinic, and the morphology turns to smooth columnar. Compared with ones calcined at 1000℃, products synthesized by hydrothermal method have a low degree of crystallization and a low luminescence intensity, which caused by low temperature, bad sealed autoclave, or not long time. Products have a growth trend from linear ones to particles with the addition of PEG2000. This is because Steric Hindrance Effect of macromolecule suppresses the anisotropy growth.“Growth unit”theory is used to explain the growth of crystal under hydrothermal condition. The“unit”control the rate of reaction ions by aggregating on some interfaces to determine the final morphology of crystals.
本文采用化学沉淀法和水热法,以Eu2O_3、La(NO_3)_3·6H_2O、Gd(NO_3)_3和H3PO_4为原料,氨水控制pH,合成了Gd~(3+)和Eu~(3+)共掺杂的LaPO_4纳米材料,结合XRD、DTA、SEM和荧光测试等手段,对荧光粉的物相、形貌和发光性能进行了表征,分析了pH值、热处理温度、掺杂离子浓度、表面活性剂对产物性能的影响。
实验结果表明:室温、强酸性溶液中,化学沉淀法合成的粉体为束状的六方相LaPO_4,长度在300-700nm之间;碱性时仍为六方相,但长径比减小,形貌类似枝杈;中性时没有明显衍射峰,变为米粒状的团簇结构。荧光性能显示pH=9时发光强度最好,(~5D_0→~7F_1)和(~5D_0→~7F_2)跃迁强度相当,Eu~(3+)为橙-红发射,不在反演中心格位。粉体经过热处理之后,物相和荧光性能都发生了变化。单斜相逐渐取代六方相,1000℃变为完全的单斜相,发光强度也最高,同时粉体的团聚也变得严重,形成了许多大的块状颗粒。比较不同离子浓度时粉体的荧光性能发现,离子在高浓度时发生了浓度猝灭,确定了最佳离子浓度为Gd~(3+)(2.5%mol),Eu~(3+)(5%mol),Gd~(3+)→Eu~(3+)的能量传递方式为共振能量传递。
控制pH=9,用水热的方法,在不同温度下合成了LaPO_4 :Gd~(3+),Eu~(3+)纳米粉。100℃时得到六方相,不太均一的长棒状结构的LaPO_4;200℃时变为粗短的柱状结构,晶型也变为单斜相。与1000℃煅烧样品相比,晶化程度还不够高,可能是温度不够高,水热釜密封不够好,或者时间不够长所致。因为结晶性能差,发射强度也比较弱。表面活性剂PEG2000的加入,使得晶粒有从棒状生长向颗粒生长的趋势,主要是由于大分子的空间位阻效应抑制了晶粒的各向异性生长。水热条件下晶体的生长可用“生长基元”理论来解释。生长基元通过在某些界面上的叠合来控制生长速率,决定晶体的最终形貌。
Due to the unique 4f electronic shell, lanthanide elements show outstanding optical properties, which make them have bright applications prospect in nanophosphors field. Establishing new synthetic strategies of these materials to make the atomic arrangement controllable in the nano-scale; understanding the relations between morphology and luminescent properties and raising the stability and intensity of materials practically are crucial to deep processing and detailed study of rare earth phosphors.
In this article, chemical precipitation method and hydrothermal method are used to synthesize LaPO_4 :Eu~(3+),Gd~(3+), with Eu2O_3、La(NO_3)3·6H_2O、Gd(NO_3)3 and H3PO_4 as raw materials and ammonia as pH regulator. The phase, morphology and luminescent properties of products are investigated by XRD、DTA、SEM and spectrofluorometers; the effect of pH values, thermal treatment temperature, doped concentration of ions and surfactant on the luminescent properties are studied.
The experimental results show that the products are fasciculated hexagonal LaPO_4 synthesized by chemical precipitation method under acidic condition at room temperature, which have a length of 300-700nm; the phase is still hexagonal with a decreased length-diameter ratio under basic condition but the morphology is branch-like; when pH=7, the grain-like cluster products have no obvious diffraction peaks. Photoluminescence analysis shows that the products have the greatest luminescent properties when pH=7, and the transition intensities of (5D0→7F1) and (5D0→7F2) are equal, indicating a non-centro-symmetrical environment for Eu~(3+) with orange-red emission. The phase、morphology and luminescent properties are changeable after the thermal treatment. Monoclinic powders replace hexagonal ones gradually, and products have a totally monoclinic phase and greatest intensity after calcinations at 1000℃. Meanwhile powders gather into large massive particles. The best concentration of doped ions is confirmed by contrasting photoluminescence intensity of powders with different ion concentrations, the best values of Gd~(3+) and Eu~(3+) are 2.5%mol and 5%mol respectively. Concentration quenching occurs with increasing concentration. The energy transfer mode between Gd~(3+) and Eu~(3+) is resonance transfer dominated by electric multipole interaction.
In the second part, LaPO_4 :Eu~(3+),Gd~(3+) phosphors(pH=9) are synthesized by hydrothermal method at different temperatures. The obtained LaPO_4 is hexagonal phase and inhomogenous linear structure after 100℃. When the temperature is 200℃, the phase turns to monoclinic, and the morphology turns to smooth columnar. Compared with ones calcined at 1000℃, products synthesized by hydrothermal method have a low degree of crystallization and a low luminescence intensity, which caused by low temperature, bad sealed autoclave, or not long time. Products have a growth trend from linear ones to particles with the addition of PEG2000. This is because Steric Hindrance Effect of macromolecule suppresses the anisotropy growth.“Growth unit”theory is used to explain the growth of crystal under hydrothermal condition. The“unit”control the rate of reaction ions by aggregating on some interfaces to determine the final morphology of crystals.
引文
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