Tb3+共摻雜與硼矽玻璃對於微波輔助燒結合成Sr2SiO4:Eu3+之發光特性及顯微結構之影響

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Tb3+共掺杂与硼矽玻璃对於微波辅助烧结合成Sr2SiO4:Eu3+之发光特性及显微结构之影响

Study of phosphor in glass of Sr2SiO4 doped with Eu3+ and co-doped with Tb3+

许嘉哲 , 硕士　　导师：施永辉　　共同指导教授：杨茹媛

繁体中文

萤光粉；光致发光；发光二极体；微波烧结法； phosphor ； photoluminescence ； LED ； microwave sintering method

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摘要 │ 参考文献 (58) │ 国际计量

摘要〈TOP〉

1996 年日亚化学Nakamura 等人成功开发出藍光发光二极体，随後搭配黄色萤光粉即掺铈之钇铝石榴石(cerium doped yttrium aluminum garnet,YAG:Ce)，成功开发出白光LED。然而，藍光LED晶片搭配YAG 虽发光效率佳，但有藍光转换效率不佳以及其白光演色性不高之问题。故探索热稳定性佳和高功率之矽酸锶萤光粉为本研究之重要目的。
本研究延续实验室杨育恺学长以微波烧结制备Sr2SiO4：Eu3+萤光粉 ，主要目的为开发新型矽酸盐萤光材料并研究其特性，在主体方面采用Orthorhombic结构之矽酸锶(Sr2SiO4：Eu3+)为基础，分别添加金属離子Eu3+当作活化剂发光中心及高纯度玻璃粉及低纯度玻璃粉为助熔剂，并分别探讨掺杂浓度及烧结温度对矽酸锶(Sr2SiO4：Eu3+)之微结构与光学性质之研究。主要的分析系使用扫描式电子显微镜(Scanning Electron Microscope, SEM)、X-光粉末绕射仪(X-ray Diffraction, XRD)、光致发光光谱仪(Photoluminescence Spectrum, PL)。其中活化剂Eu 用来取代主体晶格中Sr 的位置，其參數为(热处理条件、活化剂浓度、助熔剂添加量、持温时间) ，探讨其微结构与光学特性。
1.	以微波烧结制备之Sr2SiO4：Eu3+萤光粉，於低温烧结条件下(900 ℃ ) ，即可形成α- Sr2SiO4 正交晶体 (Orthorhombic)，此外，随着烧结温度的提升发光强度亦随之增加。根据本实验室杨育恺学长之研究发现当Sr2-xSiO4: xEu3+ 中x=0.1 时温度烧结条件(1200 ℃ )时其发光强度最大，推测此时活化剂浓度达最适浓度。另外，根据文献报导与实验室过去之研究，添加助熔剂玻璃粉亦能够提升萤光粉的发光强度，提升结晶性，降低烧结温度等优点并可利用Tb3+共掺杂调整发光波段，且随着玻璃粉纯度的不同及添加量的增加发光强度亦随之提升。
2.	由分析结果显示， 以上述发光强度最强之萤光粉，即添加於Sr2SiO4：Eu3+内，加入助熔剂：低纯度玻璃粉，由分析结果可得知其最佳之掺杂浓度为0.10wt%、烧结温度维持1200℃。由XRD分析中，可得知当掺杂量由0.05wt%增加至0.25wt%所制备之Sr2SiO4：Eu3+：低纯度玻璃粉皆为纯相。并可知道当掺杂度超过上述之最佳值时，会导致在Sr2SiO4：Eu3+低纯度玻璃粉有晶粒团聚现象，进而影响其发光强度，可推测为是因其掺杂浓度已超过饱和浓度而造成浓度淬灭，而导致其发光强度衰减。
3.	再以上述发光强度最强之萤光粉，即添加於Sr2SiO4：Eu3+内，加入助熔剂：高纯度玻璃粉，由分析结果可得知其最佳之掺杂浓度为0.10wt%、烧结温度维持1200℃。由XRD分析中，可得知当掺杂量由0.05wt%增加至0.25wt%所制备之Sr2SiO4：Eu3+高纯度玻璃粉皆为纯相。并可知道当掺杂度超过上述之最佳值时，会导致在Sr2SiO4：Eu3+高纯度玻璃粉有晶粒团聚现象，进而影响其发光强度，可推测为是因其掺杂浓度已超过饱和浓度而造成浓度淬灭，而导致其发光强度衰减。
4.	最後，经实验结果发现添加助熔剂：高纯度玻璃粉及低纯度玻璃粉之Sr2SiO4：Eu3+ 萤光粉，发光强度并无巨大差异，故以低纯度玻璃粉为助熔剂进行降低烧结温度实验，此举为降低萤光粉制作成本为出发点而设计，由实验发现将烧结温度降至1100℃时，由XRD分析中，可得知当掺杂量由0.05wt%增加至0.25wt%所制备之Sr2SiO4：Eu3+低纯度玻璃粉已有杂相产生。
5.	掺杂活化剂Tb3+：当烧结温度为1200℃，Sr2SiO4：Eu3+ 为纯相，掺杂浓度之最佳值为0.30wt%，可得知当掺杂量由0.025wt%增加至0.35wt%当激发波段於237nm，可得最强之放射波段550nm属於5D4-7F5之电子跃迁。CIE色度座标随着添加物Tb3+掺杂浓度增加而改变，由紫光慢慢偏向介於红光与绿光之间。

并列摘要〈TOP〉

In 1996, the white LEDs were fabricated with blue LED chips and yellow phosphors such as cerium doped yttrium aluminum garnet (YAG:Ce) by Nichia. Although the blue chip based white LEDs have high brightness and efficiency, they still have some problems such as low color rendor index and low reproducibility. The objects in this thesis are to find a phosphor with high thermal stability and high power density.
This study continues the Yu-kai Yang lab senior in microwave sintering of Sr2SiO4:Eu3+ phosphor, The main purpose of developing a new type of fluorescent material of silicate and study their characteristics. In the aspect of subject by Orthorhombic structure of the silicon strontium Sr2SiO4:Eu3+ based, respectively, with the addition of metal ions (Eu3+) as activating agent luminescence center and high purity glass powder and low purity glass powder as a flux in the, and doping concentration and sintering temperature on silicic acid strontium (Sr2SiO4:Eu3+) micro structure and optical properties of research are discussed. The main analysis using scanning electron microscopy (scanning electron microscope, SEM), X-ray powder diffraction X-ray diffraction (XRD), light induced luminescence spectrometer (increasing spectrum and PL). The activation agent EU used to replace the position of the host lattice in Sr, the parameters (thermal processing conditions, activation agent concentration), adding amount of flux, temperature and time) on the microstructure and optical properties.
1.	Prepared by microwave sintering of the Sr2SiO4:Eu3+ fluorescent powder, in under the condition of low temperature sintering (900 ℃) can be formed alpha Sr2SiO4 orthogonal crystal Orthorhombic. In addition, with sintering temperature ascension luminous intensity is also increased. According to the found of the laboratory fellow students Yang Yukai when Sr2-xSiO4: xEu3+=0.1 sintering temperature conditions (1200℃) the maximum luminous intensity, suggesting that this activation agent concentration was reached the optimal concentration degree. Also according to the reported in the literature and laboratory in the past research, add flux of glass powder can enhance the luminescent intensity of the phosphors, enhance the crystallization, the lower the sintering temperature and other advantages and using Tb3+ Co-doped adjust the luminous band, and with glass powder purity of different and Tim plus the amount of increase in the PL intensity also increased
2.	By the analysis results show that the luminescence intensity is the strongest of phosphors, is added in the Sr2SiO4:Eu3+, adding flux: low purity of glass powder. By analysis result can be that the optimal doping concentration maintains a 1200℃for 0.10wt%, sintering temperature. By the XRD analysis, it is found that when the doping amount is increased from 0.05wt% to 0.25wt%: low purity glass powder is pure phase. And know when the doping degree more than the optimum value, resulting in Sr2SiO4:Eu3+ low purity of glass powder is the aggregation of grains, thereby affecting the luminous intensity, presumably is due to the doping concentration has exceeded the saturation concentration caused by concentration quenching, which led to the luminescence intensity attenuation.
3.	Then the luminescence intensity is the strongest of phosphors, is added in the Sr2SiO4:Eu3+, adding flux: high purity glass powder, by the analysis results can be learned that the optimal doping concentration maintains a 1200 ℃ for 0.10wt%, sintering temperature. By XRD analysis, it is found that when the doping amount is increased from 0.05wt% to 0.25wt% high purity glass powder is pure phase. And know when the doping degree more than the optimum value, resulting in Sr2SiO4:Eu3+ high purity glass powder is the aggregation of grains, thereby affecting the luminous intensity, presumably is due to the doping concentration has exceeded the saturation concentration caused by concentration quenching, which led to the luminescence intensity attenuation.
4.	Finally, the experimental results, it is found that adding flux: high purity glass powder and low purity of glass powder Sr2SiO4:Eu3+ phosphor, luminescence intensity had no great difference, so to low purity of glass powder as fluxing agent to reduce the sintering temperature experiment, the move to reduce fluorescent powder made into this as a starting point and design, by experiment, it is found that the sintering temperature is reduced to 1100 ℃, by XRD analysis, that when doping amount by 0.05wt% increase to 0.25wt% of prepared Sr2SiO4:Eu3+ low purity glass powder has been mixed phase. 
5.	Doping activator Tb3+: when the sintering temperature is 1200℃, Sr2SiO4:Eu3+ for pure phase, the doping concentration of the best value for 0.30wt%, we can see that when the doping amount by 0.025wt% increased to 0.35 when the excitation band in 237nm, the strongest radiation at 550nm band belongs to the electronic transition of the 5D4-7F5. CIE chromaticity coordinates with additives increasing the Tb3+ doping concentration changed slowly by the purple bias between red and green.

参考文献 ( 58 ) 〈TOP〉

[2] 汤友圣，发光二极体之萤光材料及其封装特性分析，硕士论文，国立师范大学，光电科技研究所，台北，2008。
连结：
[4] Nakamura et al, United States Patent No. 5,578,839, November 26, 1996.
连结：
[5] Schubert, E. F., Light-Emitting Diodes, University Press, 2006.
连结：
[6] 郭子菱，吕绍旭，「白光LED技术发展演进近况」，光连双月刊，第72卷，2007，第34-37页。
连结：
[11] Schubert, F., Kim, J. K., “Solid-State Light Sources Getting Smart,” Science, Vol. 308, 2005, pp. 1274-1278.
连结：

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