Eu~（3+）-Sr~（2+）共掺杂纳米二氧化硅发光材料的制备及其发光性能研究
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摘要
由于稀土离子有独特的电子层结构,使得稀土离子掺杂的发光材料具有其他发光材料所不能有的很多优异性能。论文选用原料丰富、价格较便宜的铕作为纳米二氧化硅材料的激活剂,使得材料能够发光。在制备Eu~(3+)掺杂纳米二氧化硅发光材料的过程中,添加了Sr~(2+),研究发现Eu~(3+)-Sr~(2+)共掺杂纳米二氧化硅材料不仅改善了原材料的光学性能,并产生新的发光中心,这对开辟更实用便宜的新型发光材料具有突破性。
论文采用溶胶-凝胶方法,以正硅酸乙酯为硅源,无水乙醇为溶剂,制备了未掺杂纳米二氧化硅粉体材料、稀土离子Eu~(3+)单掺杂、Sr~(2+)单掺杂以及Eu~(3+)-Sr~(2+)共掺杂的纳米二氧化硅发光材料。利用XRD、SEM、DSC-TG、FTIR、PL等现代材料测试技术对Eu~(3+)-Sr~(2+)共掺杂纳米二氧化硅发光材料的结构、物相、形貌、发光性能进行了表征和分析。研究了发光性能的主要影响因素,探讨发光机理。
在制备Eu~(3+)-Sr~(2+)共掺杂纳米二氧化硅发光材料的前期阶段,采用正交试验法分析了影响凝胶时间的主要因素,即醇硅比、水硅比、陈化温度、反应时间和pH值。研究结果表明:陈化温度和醇硅比是影响溶胶凝胶时间的主要因素,凝胶化时间较合理的反应条件为:醇硅比=6:1,水硅比=6:1,陈化温度=50℃,pH=2,反应时间=8小时。
XRD和SEM表征结果表明,Eu~(3+)-Sr~(2+)共掺杂的纳米二氧化硅发光材料为无定形态,颗粒分布较均匀,但有少量团聚现象出现。
对未掺杂纳米二氧化硅材料的发光性能进行研究发现,在不同波长的光激发下,样品可以发射出345nm、360nm紫外和670nm左右的可见光,这些光的发射可能与材料制备过程中形成的氧空位、非桥氧中心等缺陷有关。
研究了稀土离子Eu~(3+)单掺杂纳米二氧化硅发光材料的发光性能,发射光谱中存在5个发射峰,分别位于365nm、580-590nm、616nm、660nm、710nm。其中365nm处发射峰的强度最大,位于不可见光区;在可见光区范围内616nm处的谱线的强度最大,其颜色为红色,是Eu~(3+)的特征谱。Eu~(3+)离子掺杂纳米二氧化硅发光材料中可见光区的580-590nm、616nm、660nm、710nm这些发光峰分别是由5D0-7FJ(J=0,1,2,3,4)能级跃迁引起。考察了Eu~(3+)离子掺杂的不同浓度对材料发光性能的影响,随着Eu~(3+)离子掺杂浓度的提高,发射光的强度先增强后减弱;当掺杂浓度为0.5%时,发射光的强度较强。
Sr~(2+)单掺杂纳米二氧化硅材料的发射光谱出现了位于343nm和670-690nm的发射峰。将其激发光谱和发射光谱与未掺杂纳米二氧化硅材料的激发光谱和发射光谱进行比较,可以发现光谱极其相似;Sr~(2+)的加入并未引起纳米二氧化硅材料发光峰的位置改变,只是发光峰强度增强,仅起到了加强作用。
Eu~(3+)-Sr~(2+)共掺杂纳米二氧化硅发光材料的发射光谱中主要存在有4个发射峰,分别位于409nm、470nm、580-590nm、616nm处。研究表明,不仅Sr~(2+)离子的加入对材料的发光性能有很大的影响,并且加入的量不同对其影响不同。与只掺杂Eu~(3+)离子的纳米二氧化硅发光材料相比较,Sr~(2+)掺杂浓度≤0.5%时发射峰位置几乎未发生变化,只是发光强度有不同程度的增强;但是在0.5%nm处的属于Eu~(2+)的特征发射峰,说明随着Sr~(2+)的加入使材料中一部分的Eu~(3+)离子转换成了Eu~(2+)。考察了不同温度对材料发光性能的影响,随着温度的升高,发射峰位置没有改变,只是强度发生了变化,409nm处的发射峰强度随之减弱,616nm处的发射峰强度随之增强。
Because of the special electron shell structure, the rare earth- doped luminescence materials has been provide with outstanding luminescence properties than the other type luminescence materials.The abundant and cheap Eu~(3+) was selected as the activated dose of nano-silica material, and the materials were luminous. In the process of preparation of Eu~(3+) doped nano-silica, a definite amount of Sr~(2+) was added . The results showed that Eu~(3+)-Sr~(2+) co-doped nano-silica were not only improved the luminescence properties of raw materials, and also produced new luminescence centers. It was very useful to making cheaper and more practical luminescent materials.
In this paper with TEOS as precursor, ethanol as solvent, nothing doped , rare earth Eu~(3+) single-doped, Sr~(2+) single-doped and Eu~(3+)-Sr~(2+) co-doped nano-silica luminescence materials were prepared by sol - gel method. Using XRD, SEM, DSC-TG, FTIR, PL, and other modern test technology on Eu~(3+)-Sr~(2+) doped nano-silica luminescence materials, we characterized and analyzed the structure, phase, morphology, luminescence properties of materials. The affecting factors on the luminescence properties were studied, and its luminescence mechanism were also analyzed.
In the pre-stage of preparation the Eu~(3+)-Sr~(2+) co-doped nano-silica luminescence materials, the main factors affecting gelation time were analyzed by orthogonal test ,they were alcohol- silicon ratio, silicon-water ratio, aging temperature, reaction time and pH . The results showed that the aging temperature and alcohol-silicon ratio were the important factor affecting the gelation time . Discuss the conditions ,when alcohol-silicon ratio=6:1, silicon-water ratio = 6:1 ,aging temperature=50℃, pH =2, the reaction time is 8 hours, the gelation time is reasonable.
The XRD and SEM results showed that Eu~(3+)-Sr~(2+) co-doped nano-silica luminescence materials was amorphous.Its particle were very uniform, but has a small amount of agglomeration phenomenon.
When the nothing doped of nano-silica materials was irradiated by different wavelength light , the sample can emit ultraviolet radiation band with two peak at 345nm, 360nm and one visible light at 670nm.These emission may be related to oxygen vacancy defects, non-bridging oxygen center defects formed in the material preparation processes .
The luminescence properties of Eu~(3+) single-doped silicon was studied. In the emission spectra exist five emission peaks are located at 365nm ,580-590nm, 616nm, 660nm, 710nm. 365nm emission peak where the intensity of the largest is not visible; in the visible spectral range of 616nm was greatest strength, its color is red, is the characteristic spectrum of Eu~(3+). In the visible region 580-590nm, 616nm, 660nm, 710nm emission peak of Eu~(3+) doped silica luminescence materials, were induced by the 5D0-7FJ (J = 0,1,2,3,4) of Eu~(3+) energy transition . The influence of Eu~(3+) ions doped concentration to the luminescence properties was studied . With the Eu~(3+) ion doping concentration increased , the intensity of emission first increased and then decreased; when the doping concentration of 0.5%, the intensity of emission was strongest .
The luminescence properties of Sr~(2+) single-doped silicon was studied. In the emission spectra exist two emission peaks appeared at 343nm and 670-690nm . The similar spectrum can be found when compared its excitation and emission spectra with undoped nano-silica material .The addition of Sr~(2+) did not change the luminescence peak position , only made emission peak intense.It played the role only to strengthen .
In the emission spectra of the Eu~(3+)-Sr~(2+) co-doped silicon luminescent materials there were four main emission peaks.They are located at 409nm, 470nm ,580-590nm, 616nm. It was found that not only the addition of Sr~(2+) ions on the luminescent properties have significant influence, but also the different amount added to their have different effects.And compared it with Eu~(3+) ion doped nano-silica luminescent materials, when Sr~(2+) doping concentration of≤0.5%,the emission peak is almost not changed, but there are different levels of luminous intensity increased; when 0.5%ng concentration≤1.0%, there appeared 409nm emission peaks which is the department characteristic Eu~(2+) emission peaks. The phenomenon indicating that Sr2 + doped the material converted part of the Eu~(3+) ions into Eu~(2+). The influence of different temperature on the luminescence properties was studied. With the temperature changed, the emission peak position has not changed, but the intensity has changed. The intensity of 409nm emission peak weakened, but 616nm has enhanced in emission intensity.
论文采用溶胶-凝胶方法,以正硅酸乙酯为硅源,无水乙醇为溶剂,制备了未掺杂纳米二氧化硅粉体材料、稀土离子Eu~(3+)单掺杂、Sr~(2+)单掺杂以及Eu~(3+)-Sr~(2+)共掺杂的纳米二氧化硅发光材料。利用XRD、SEM、DSC-TG、FTIR、PL等现代材料测试技术对Eu~(3+)-Sr~(2+)共掺杂纳米二氧化硅发光材料的结构、物相、形貌、发光性能进行了表征和分析。研究了发光性能的主要影响因素,探讨发光机理。
在制备Eu~(3+)-Sr~(2+)共掺杂纳米二氧化硅发光材料的前期阶段,采用正交试验法分析了影响凝胶时间的主要因素,即醇硅比、水硅比、陈化温度、反应时间和pH值。研究结果表明:陈化温度和醇硅比是影响溶胶凝胶时间的主要因素,凝胶化时间较合理的反应条件为:醇硅比=6:1,水硅比=6:1,陈化温度=50℃,pH=2,反应时间=8小时。
XRD和SEM表征结果表明,Eu~(3+)-Sr~(2+)共掺杂的纳米二氧化硅发光材料为无定形态,颗粒分布较均匀,但有少量团聚现象出现。
对未掺杂纳米二氧化硅材料的发光性能进行研究发现,在不同波长的光激发下,样品可以发射出345nm、360nm紫外和670nm左右的可见光,这些光的发射可能与材料制备过程中形成的氧空位、非桥氧中心等缺陷有关。
研究了稀土离子Eu~(3+)单掺杂纳米二氧化硅发光材料的发光性能,发射光谱中存在5个发射峰,分别位于365nm、580-590nm、616nm、660nm、710nm。其中365nm处发射峰的强度最大,位于不可见光区;在可见光区范围内616nm处的谱线的强度最大,其颜色为红色,是Eu~(3+)的特征谱。Eu~(3+)离子掺杂纳米二氧化硅发光材料中可见光区的580-590nm、616nm、660nm、710nm这些发光峰分别是由5D0-7FJ(J=0,1,2,3,4)能级跃迁引起。考察了Eu~(3+)离子掺杂的不同浓度对材料发光性能的影响,随着Eu~(3+)离子掺杂浓度的提高,发射光的强度先增强后减弱;当掺杂浓度为0.5%时,发射光的强度较强。
Sr~(2+)单掺杂纳米二氧化硅材料的发射光谱出现了位于343nm和670-690nm的发射峰。将其激发光谱和发射光谱与未掺杂纳米二氧化硅材料的激发光谱和发射光谱进行比较,可以发现光谱极其相似;Sr~(2+)的加入并未引起纳米二氧化硅材料发光峰的位置改变,只是发光峰强度增强,仅起到了加强作用。
Eu~(3+)-Sr~(2+)共掺杂纳米二氧化硅发光材料的发射光谱中主要存在有4个发射峰,分别位于409nm、470nm、580-590nm、616nm处。研究表明,不仅Sr~(2+)离子的加入对材料的发光性能有很大的影响,并且加入的量不同对其影响不同。与只掺杂Eu~(3+)离子的纳米二氧化硅发光材料相比较,Sr~(2+)掺杂浓度≤0.5%时发射峰位置几乎未发生变化,只是发光强度有不同程度的增强;但是在0.5%
Because of the special electron shell structure, the rare earth- doped luminescence materials has been provide with outstanding luminescence properties than the other type luminescence materials.The abundant and cheap Eu~(3+) was selected as the activated dose of nano-silica material, and the materials were luminous. In the process of preparation of Eu~(3+) doped nano-silica, a definite amount of Sr~(2+) was added . The results showed that Eu~(3+)-Sr~(2+) co-doped nano-silica were not only improved the luminescence properties of raw materials, and also produced new luminescence centers. It was very useful to making cheaper and more practical luminescent materials.
In this paper with TEOS as precursor, ethanol as solvent, nothing doped , rare earth Eu~(3+) single-doped, Sr~(2+) single-doped and Eu~(3+)-Sr~(2+) co-doped nano-silica luminescence materials were prepared by sol - gel method. Using XRD, SEM, DSC-TG, FTIR, PL, and other modern test technology on Eu~(3+)-Sr~(2+) doped nano-silica luminescence materials, we characterized and analyzed the structure, phase, morphology, luminescence properties of materials. The affecting factors on the luminescence properties were studied, and its luminescence mechanism were also analyzed.
In the pre-stage of preparation the Eu~(3+)-Sr~(2+) co-doped nano-silica luminescence materials, the main factors affecting gelation time were analyzed by orthogonal test ,they were alcohol- silicon ratio, silicon-water ratio, aging temperature, reaction time and pH . The results showed that the aging temperature and alcohol-silicon ratio were the important factor affecting the gelation time . Discuss the conditions ,when alcohol-silicon ratio=6:1, silicon-water ratio = 6:1 ,aging temperature=50℃, pH =2, the reaction time is 8 hours, the gelation time is reasonable.
The XRD and SEM results showed that Eu~(3+)-Sr~(2+) co-doped nano-silica luminescence materials was amorphous.Its particle were very uniform, but has a small amount of agglomeration phenomenon.
When the nothing doped of nano-silica materials was irradiated by different wavelength light , the sample can emit ultraviolet radiation band with two peak at 345nm, 360nm and one visible light at 670nm.These emission may be related to oxygen vacancy defects, non-bridging oxygen center defects formed in the material preparation processes .
The luminescence properties of Eu~(3+) single-doped silicon was studied. In the emission spectra exist five emission peaks are located at 365nm ,580-590nm, 616nm, 660nm, 710nm. 365nm emission peak where the intensity of the largest is not visible; in the visible spectral range of 616nm was greatest strength, its color is red, is the characteristic spectrum of Eu~(3+). In the visible region 580-590nm, 616nm, 660nm, 710nm emission peak of Eu~(3+) doped silica luminescence materials, were induced by the 5D0-7FJ (J = 0,1,2,3,4) of Eu~(3+) energy transition . The influence of Eu~(3+) ions doped concentration to the luminescence properties was studied . With the Eu~(3+) ion doping concentration increased , the intensity of emission first increased and then decreased; when the doping concentration of 0.5%, the intensity of emission was strongest .
The luminescence properties of Sr~(2+) single-doped silicon was studied. In the emission spectra exist two emission peaks appeared at 343nm and 670-690nm . The similar spectrum can be found when compared its excitation and emission spectra with undoped nano-silica material .The addition of Sr~(2+) did not change the luminescence peak position , only made emission peak intense.It played the role only to strengthen .
In the emission spectra of the Eu~(3+)-Sr~(2+) co-doped silicon luminescent materials there were four main emission peaks.They are located at 409nm, 470nm ,580-590nm, 616nm. It was found that not only the addition of Sr~(2+) ions on the luminescent properties have significant influence, but also the different amount added to their have different effects.And compared it with Eu~(3+) ion doped nano-silica luminescent materials, when Sr~(2+) doping concentration of≤0.5%,the emission peak is almost not changed, but there are different levels of luminous intensity increased; when 0.5%
引文
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