基于氟化物微纳复合玻璃与透明陶瓷的设计与制备
文献类型：学位论文
| 作者 | 姜益光 |
| 文献子类 | 博士 |
| 导师 | 张龙 |
| 关键词 | CaF2/SrF2微纳复合玻璃 CaF2/SrF2 micro-composite glasses CaF2/SrF2透明陶瓷 CaF2/SrF2 transparent ceramics 单晶陶瓷化 ceramization of single crystals 可控溶胶-凝胶 controlled sol-gel method 液相烧结 liquid-phase sinter |
| 其他题名 | Design and preparation of fluoride based micro-composite glasses and transparent ceramics |
| 英文摘要 | CaF2/SrF2具有宽的透过范围、低的声子能量、低的非线性折射率和高的热导率等优点，有望成为下一代高功率激光增益介质。但是，CaF2/SrF2单晶存在低的机械性能、长的制备周期和难于大尺寸制备等局限严重限制了其应用。为了解决上述问题，本论文分别采用可控溶胶-凝胶技术、液相烧结技术和单晶陶瓷化技术，制备出了高光学质量稀土离子掺杂的CaF2/SrF2微纳复合玻璃和无气孔透明陶瓷。 创新点及重要成果如下： （1）通过反滴定法配合离心技术，制备了高分散、晶粒尺寸在~20 nm的Er3+:CaF2纳米粉体。基于传统溶胶-凝胶法的优缺点，借助物理方法直接在液态溶胶中引入微晶的理念发展了可控溶胶-凝胶技术，基于该技术得到了质量优异的Er3+:CaF2-SiO2微纳复合玻璃。 （2）通过熔融-淬火法，确定了氟磷（FP）前躯体玻璃的最佳组分和熔制工艺。基于在液相烧结上的技术积累，得到了高光学质量的Eu3+:CaF2微纳复合玻璃。并根据Eu3+的发光在结构方面具有高的灵敏度，系统研究了稀土离子在微纳复合玻璃中的局部空间格位环境。 （3）制备了高中红外透过率、低声子能量和大发射截面的Er3+:SrF2微纳复合玻璃，其有望成为红外固体激光器和放大器的候选材料。同时，拓展了微纳复合玻璃的种类，成功发展了Ce3+:YAG微纳复合玻璃。 （4）基于单晶陶瓷化技术得到了高光学质量的Nd3+,Y3+:CaF2（Nd:CYF）无气孔透明陶瓷，研究了样品形变率对Nd:CYF透明陶瓷性能的影响，摸索出了较优的工艺参数。相应的陶瓷样品具有高的透过率（Ta> 91％，3-mm，250-1200 nm）、小的散射损耗、高的断裂韧性（K1c~0.71 MPa.m1/2）、强的荧光发射、长的荧光寿命（τ= 348.72 μs）和大的半峰宽（FWHM~29.2 nm），且首次在Nd:CYF透明陶瓷中获得了35 mW的连续激光输出。 （5）基于单晶陶瓷化技术得到了高断裂韧性（1.28 MPa.m1/2）、高中远红外（~9 μm）透过率，低声子能量和高密度（ρ= 4.8466 g/cm3）的Nd3+,Gd3+:SrF2 (Nd:SGF)无气孔透明陶瓷，其有望应用于红外窗口、固体激光器、闪烁体和光子学领域。 （6）基于深度塑性形变得到了Nd:CYF和Nd:SGF无气孔透明陶瓷。系统研究了Nd:CYF和Nd:SGF透明陶瓷光学性能与形变率之间的关系以及光学性能下降的原因。探讨了Nd3+离子“再团簇”的机理，为陶瓷组分的设计和高质量Nd3+,B3+:MF2（B3+=缓冲离子，M2+=碱土金属离子）陶瓷的制备提供理论依据。; CaF2/SrF2 has the advantages of wide transmission range, low phonon energy, low nonlinear refractive index, and high thermal conductivity, and is expected to be the gain medium of the next-generation high-energy infrared laser. However, the low mechanical, long production cycle, and difficulty in large-scale preparation of the CaF2/SrF2 single crystal severely limit its application. In this paper, the optimum process parameters were determined and the RE3+:CaF2/SrF2 micro-composite glasses and free-pore transparent ceramics suitable were prepared. The innovations and significant results are as follows: (1) Highly dispersed Er3+:CaF2 nanopowders with a grain size of ~20 nm were prepared by counter-titration method with centrifugal. Based on the advantages and disadvantages of traditional sol-gels, the concept of direct introduction of microcrystals into liquid sols by physical methods was developed. High-quality Er3+:CaF2-SiO2 micro-composite glass was successfully prepared by the controllable sol-gel method. (2) The optimum composition and melting process of the FP precursor glass was determined by the melt quenching method. Eu3+:CaF2 micro-composite glass with high optical quality was prepared, and the occupation of rare-earth ions in micro-composite glass was studied. (3) An Er3+:SrF2 micro-composite glass with high infrared transmittance, low phonon energy, and large emission cross section was prepared, which is expected to be a candidate material for IR lasers and amplifiers. Expanded the types of micro-composite glass and successfully developed Ce3+:YAG micro-composite glass. (4) Transparent Nd:CYF pore-free ceramics with high optical quality was obtained by the single crystal ceramization. The effect of deformation rate on the properties of Nd:CYF ceramics were studied, and the optimum process parameters were determined. The corresponding ceramics have high transmittance (Ta> 91%, 3-mm, 250-1200 nm), small scattering loss, high fracture toughness (K1c = 0.71 MPa.m1/2), strong fluorescence emission, long fluorescence lifetime (τ = 348.72 μs), and large FWHM (29.2 nm). Meanwhile, a continuous laser output of 35 mW was achieved for the first time. (5) Nd:SGF transparent pore-free ceramics with high-fracture toughness (1.28 MPa.m1/2), high mid-far infrared (~9 μm) transmittance, low phonon energy, and high density (ρ=4.8466 g/cm3) were prepared by the single crystal ceramization , which are expected to be used in infrared windows, mid-far infrared lasers, scintillators and photonics materials. (6) Different deformation rates of Nd:CYF and Nd:SGF transparent ceramics were obtained through deep plastic deformation. The relationship between the optical properties and deformation of Nd3+,B3+-codoped MF2 (B = buffer ions; M = alkaline earth metal ions) transparent ceramics were systematically studied. Nd3+ ion re-clustering in ceramics was experimentally observed for the first time. The mechanism of re-clustering was studied. |
| 学科主题 | 材料学 |
| 源URL | [http://ir.siom.ac.cn/handle/181231/31031]  |
| 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 | 姜益光. 基于氟化物微纳复合玻璃与透明陶瓷的设计与制备[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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