Yb3+掺杂石英粉末及玻璃的制备和性能研究
文献类型：学位论文
| 作者 | 尹圣楠 |
| 文献子类 | 硕士 |
| 导师 | 陈丹平 |
| 关键词 | 四氯化硅水解法 Hydrolysis of silicon tetrachloride 多孔玻璃粉烧结法 nanoporous silica glass powder sintering technique Yb3+ Yb3+ 凝胶老化 gel aging 光谱性能 Spectral performance |
| 其他题名 | The study of preparation and properties of Yb3+-doped silica power and glass |
| 英文摘要 | 对于稀土掺杂光纤激光器而言，纤芯预制棒的制备一直都是核心技术。为了克服传统工艺改进的化学气相沉积法的缺点，本课题旨在研究四氯化硅水解法和多孔玻璃粉烧结法制备掺镱石英粉末及玻璃，并探究这两种制备工艺的制备原理及产物的性能差异。 本论文主要包五个部分：文献综述、实验方法及理论计算、凝胶老化对水解法制备镱铝共掺石英玻璃原料粉晶化和光谱性能的影响、Yb3+掺杂石英粉末及玻璃的性能研究、结论。具体内容如下： 论文首先在文献综述部分阐述了掺镱石英玻璃的研究背景、组成及光谱性能，总结了国内外Yb3+掺杂石英玻璃光纤预制棒的制备技术。并综述了Yb3+掺杂石英大模场光子晶体光纤激光器的国内外研究进展。 本文第二章介绍了四氯化硅水解法和多孔玻璃粉烧结法制备镱铝共掺石英粉末及玻璃的制备过程、粉末及玻璃性能的测试方法、以及Yb3+离子掺杂石英玻璃的光谱参数计算的理论依据。 本文第三章系统研究了四氯化硅水解法制备镱铝共掺石英玻璃原料粉在1100℃处理后的析晶性能。通过改变老化处理的温度和时间，探讨老化处理效应的机理。实验证实老化处理过程中，Al3+和Yb3+通过扩散与凝胶中的断键连接，致使凝胶组分均一化，结构得到固定，有效地抑制了石英玻璃原料粉的析晶行为，同时也提高了其高温稳定性。老化处理后，Yb3+在石英玻璃结构中的分散性得到增加，有效提高了Yb3+的荧光强度和荧光寿命。高压釜不仅能缩短老化处理时间，并且可以进一步提高样品的荧光强度和荧光寿命。 本文第四章主要对四氯化硅水解法和多孔玻璃粉烧结法制备所得镱铝共掺石英粉末及玻璃进行性能表征，比较了这两种方法制备所得稀土掺杂石英粉末及玻璃的性能和各工艺的优缺点。证明了多孔玻璃粉烧结法制备的多孔粉末比水解法制备的硅酸凝胶更易于分散Yb3+离子，但却容易吸收水分和空气中的杂质。四氯化硅水解法制备的玻璃样品的羟基含量为1.794ppm，荧光寿命为1.32ms，最大的吸收截面为2.16pm2(975nm)，最大受激发射截面为0.62pm2(1030nm)。而多孔玻璃粉烧结法制备的玻璃样品的羟基含量为4.879ppm。荧光寿命为1.25ms，最大的吸收截面为2.25pm2(975nm)，最大受激发射截面为0.57pm2(1030nm)。 论文最后总结了全文的实验结果，并指出了实验中存在的不足和需要进一步研究之处。; The preparation of fiber core has always been the core technology for rare earth doped fiber lasers. In order to overcome the shortcomings of Modified Chemical Vapor Deposition, this work aims to study the preparation of ytterbium-doped quartz powder and glass by hydrolysis of silicon tetrachloride and nanoporous silica glass powder sintering technique, and explore the principles of these two methods and the performance differences of products. Thesis consists of five sections: a literature summarizations; experimental methods and theoretical calculation; influence of gel aging on the crystallization and spectroscopic properties of Yb-Al co-doped SiO2 powder; study on properties of Yb3+-doped silica powder and glass; conclusion. Firstly, the research background，the composition and spectral properties of ytterbium - doped quartz glass are introduced in the literature summarizations. The preparation methods of Yb3+-doped quartz glass fiber preforms at home and abroad are summarized. Then the research progress of Yb3+-doped quartz large mode field photonic crystal fiber lasers is reviewed. In the second chapter, the preparation process of ytterbium-aluminum co-doped quartz powder and glass prepared by hydrolysis of silicon tetrachloride and nanoporous silica glass powder sintering technique are introduced, as well as the test method of powder and glass properties, and the theoretical basis of spectral parameters for Yb3+-doped quartz glass In the third chapter, the crystallization performance of ytterbium-aluminum co-doped silica powder prepared by hydrolysis of silicon tetrachloride at 1100℃ is studied. The mechanism of aging treatment effect is also discussed by changing the temperature and time of aging treatment. Experiment results confirms that Yb3+ and Al3+ ions are linked to the broken keys of the gel by diffusion during aging treatment. So, composition of the gel is homogenized and the structure becomes stable. It inhibits the crystallization and improves the high-temperature stability of co-doped silica powder. Besides, the dispersion of Yb3+ in glass structure is increased effectively, so the fluorescence intensities and the fluorescence lifetimes of Yb3+ ions are enhanced. The autoclave treatment can not only shorten the aging time, but the fluorescence intensities and the fluorescence lifetimes of the samples can be further improved. In the fourth chapter, the properties of the ytterbium-aluminum co-doped silica powder and glass prepared by hydrolysis of silicon tetrachloride and nanoporous silica glass powder sintering technique are studied. The properties of the rare earth doped silica powder and glass prepared by the two methods and the advantages and disadvantages of the two methods are compared. It confirms that the porous powder prepared by nanoporous silica glass powder sintering technique is easier to disperse Yb3+ ions than silicic acid gel prepared by hydrolysis of silicon tetrachloride, but it is easy to absorb moisture and impurities in air. The hydroxyl content in our glass prepared by hydrolysis of silicon tetrachloride is calculated to be 1.794ppm. The corresponding fluorescence lifetime at 1020nm is 1.32ms. The maximum absorption cross section (σabs) at 975nm is 2.16pm2, and the emission cross section (σemi) near 1030nm is 0.62pm2. Then the hydroxyl content in our glass prepared by nanoporous silica glass powder sintering technique is calculated to be 4.879ppm. The corresponding fluorescence lifetime at 1020nm is 1.25ms. Then the maximum absorption cross section (σabs) at 975nm is 2.25pm2, and the emission cross section (σemi) near 1030nm is 0.57pm2. In the fourth chapter, the performance of the obtained ytterbium-aluminum co-doped quartz powder and glass prepared by the hydrolysis method of silicon tetrachloride and the sintering method of porous glass powder were studied. In the last section, conclusions are outlined, and further research is suggested. |
| 学科主题 | 材料学 |
| 源URL | [http://ir.siom.ac.cn/handle/181231/30950]  |
| 专题 | 中国科学院上海光学精密机械研究所 |
| 作者单位 | 中国科学院上海光学精密机械研究所 |
| 推荐引用方式 GB/T 7714 | 尹圣楠. Yb3+掺杂石英粉末及玻璃的制备和性能研究[D]. |
入库方式： OAI收割
来源：上海光学精密机械研究所
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