Eu掺杂YAG微晶玻璃的制备及光谱性能

采用熔融法制备了Eu掺杂的YAG微晶玻璃.通过XRD和FESEM,研究了纯相YAG晶体的析出和Eu掺杂前后YAG晶体的微结构变化,通过荧光光谱和CIE色坐标研究微晶玻璃的发光性能.结果表明:在1050℃热处理开始析出了纯相YAG晶体,晶粒尺寸20~60 nm.在短波和长波紫外光激发下都能同时得到Eu3+和Eu2+的特征发射峰,但长波紫外激发下的发光强度是短波激发下的数十倍.随着Eu掺杂浓度的增加,Eu2+发光强度明显增强, Eu3+发光强度先增强后降低.通过改变激发波长和Eu掺杂浓度,最后得到微晶玻璃样品的CIE色坐标为(0.3326, 0.3005),接近白光坐标.因此通过单掺杂Eu可以得到白光发光的YAG微晶玻璃.     

Tb~(3+)掺杂氟硅酸盐微晶玻璃的制备及性能研究

结合当前对光学材料发展的需求,制备了Tb3+掺杂的氟硅酸盐微晶玻璃,并研究了其晶化工艺和发光性能。通过DSC分析,确定了母体玻璃的析晶温度652℃。通过研究样品不同保温时间下的晶化热处理工艺制备出含CaF2纳米晶的透明微晶玻璃,且保温时间为24 h时获得最佳晶粒尺寸。探讨了365 nm激发下Tb3+掺杂氟硅酸盐微晶玻璃的光谱性能,发现在Tb3+掺杂微晶玻璃样品能发出强烈的绿色荧光(545 nm)。随着热处理时间增加,其荧光发射强度呈现增高的趋势,在热处理24 h时发射光谱强度最强。     

利用正交法优化掺杂La2O3微晶玻璃的热处理制度

实验在前期研究工作基础上选择了稀土氧化物La2O3,采取外加法对Li2O-Al2O3-SiO2(LAS)系统微晶玻璃进行掺杂,为了寻找掺杂La2O3后LAS系统微晶玻璃的最佳热处理制度,采用正交试验设计,对试样在不同温度下进行了热处理,并对晶化后各试样进行了各项性能测试并对测试结果进行了分析,结果表明:热处理制度对微晶玻璃的各项性能影响显著,其中又以晶化温度的影响最大;综合各项性能后,得到合适热处理制度为590℃/1 h→790℃/2 h,此时,试样的力学性能和热膨胀性能最好,其抗折强度为141 MPa,热膨胀系数为1.26×10-7℃-1(20～400℃).     

Ce:YAG微晶玻璃制备及光谱性能

在Y2O3-Al2O3-SiO2-Li2O-K2O-Na2O基质玻璃中掺入Ce,经过不同温度热处理,制备出白光LED用Ce∶Y3Al5O12(Ce∶YAG)微晶玻璃.利用X射线衍射仪、X射线光电子能谱仪、场发射扫描电子显微镜、荧光光度计等方法对微晶玻璃的晶相、所掺杂Ce的价态、微观形貌以及光谱性能进行了研究.结果表明:...     

Er3+和Yb3+共掺锗硅酸盐玻璃的上转换发光性能

采用熔融-淬火法制备了基体为30SiO2-20GeO2-15Al2O3-5B2O3-30CaF2的Er3+和Yb3+共掺锗硅酸盐玻璃.采用X射线衍射仪、荧光光谱仪和热分析仪对样品进行了表征.结果表明:Er2O3含量从0.5％(摩尔分数,下同)增加到2.0％时,玻璃转变温度Tg和Tx-Tg(Tx为第一析晶温度)数值均有明显下降.Yb2O3含量从1.5％增加到4.5％时,玻璃上转换红光发光强度数量级由103提高到105,对其中1个样品在740℃热处理12h后发现,微晶化处理并未对Er的上转换发光产生有益影响.     

Y2O3对高分子网络凝胶法制备Li2O-Al2O3-SiO2系微晶玻璃性能的影响

以丙烯酰胺、N,N'-亚甲基双丙烯酰胺、碳酸锂、硝酸铝和正硅酸乙酯为原料,采用高分子网络凝胶法成功地制备出多组分氧化物Li2O-Al2O3-SiO2(LAS)微晶玻璃超微粉末,并掺杂了稀土氧化物Y2O3.将粉体压制烧结得到微晶玻璃块体.用IR,XRD,SEM等测试手段研究了掺杂对微晶玻璃组织与性能的影响,测定了微晶玻璃的热膨胀系数.实验表明:Y2O3使微晶玻璃的相变温度降低到900℃;掺杂后微晶玻璃的粒径减小;高分子网络凝胶法制备的Li2O-Al2O3-SiO2(LAS)微晶玻璃热膨胀系数达到10-7数量级,掺Y2O3使Li2O-Al2O3-SiO2(LAS)微晶玻璃的热膨胀系数提高.     

热处理制度对Li20-Al2O3-SiO2系微晶玻璃晶化过程和性能的影响

采用熔融法获得了以 TiO2+ZrO2 和 P2O5 为复合晶核剂的 LiO-Al2 O3-SiO2 系统基础玻璃,通过差热分析和正交实验的方法确定了使该玻璃微晶化的热处理制度,获得了不同热处理制度下 Li2O-Al2O3-SiO2 系统低膨胀微晶玻璃.利用 X 射线衍射分析和扫描电子显微镜对晶化样品的物相和微观结构进行了研究;讨论了热处理制度对玻璃的晶化过程及热膨胀系数的影响.研究结果表明:不同热处理温度下的微晶玻璃均可以得到具有细小等轴晶粒的组织结构,材料的热膨胀系数较低;析晶初始温度下首先析出的晶相为β-石英固溶体,随晶化温度升高β-石英固溶体转变为β-锂辉石固溶体,晶化温度进一步升高,β-锂辉石固溶体结晶完全,材料的热膨胀系数更低.     

用天然锂辉石制备透明微晶玻璃的研究

作者建议利用新疆天然锂辉石作为制备透明微晶玻璃的原料。 制备了Li_2O-MgO-Al_2O_3-SiO_2系母体玻璃,含有TiO_2、ZrO_2、P_2O_5作为成核剂;当采用天然锂辉石时,玻璃较易熔化。母体玻璃热处理后获得性能优良的透明微晶玻璃。用差热分析法、X-射线衍射法、透射电镜法考察了该材料的显微结构,讨论了天然锂辉石内所含杂质造成的影响。     

Tb3+掺杂钼酸盐玻璃陶瓷的制备及发光性能表征

采用熔融-晶化法制备了Tb3+掺杂的CaMoO4为主晶相的透明钼酸盐玻璃陶瓷。利用DSC、XRD、SEM确定了该体系玻璃样品的最佳热处理制度：715℃保温2.5 h;随着热处理时间的增加,玻璃陶瓷中的晶粒尺寸逐渐变大;利用UV-Vis-NIR得到样品玻璃陶瓷在可见光区的透过率可达80%;并利用荧光光谱讨论了在相同热处理条件下,不同Tb3+掺杂浓度对玻璃陶瓷样品发光性能的影响,研究表明Tb3+掺杂浓度为7.0mol%时样品的荧光强度最大。     

无色透明微晶玻璃

本发明介绍一种含有β—石英固溶体的透明微晶玻璃。这种材料一般为无色并在20～300℃温度范围内其热膨胀系数低于15×10-7/℃。将含有SiO_2,Al_2O_3,P_2O_5,Li_2O,MgO,ZnO和少量晶核剂的玻璃热处理后,能析出细粒的β—石英或β—锂辉石固溶体。这种细粒晶体以及它的均匀析出,使得所形成的玻璃一晶体混合物,即微晶玻璃的大多数性质与母体玻璃不同。     

Influence of Yb and Si on the fabrication of Yb:YAG transparent ceramics using spherical Y2O3 powders

Yb:YAG (yttrium aluminum garnet) transparent ceramics were fabricated by the solid-state method using monodispersed spherical Y₂O₃ powders as well as commercial Al₂O₃ and Yb₂O₃ powders. Pure YAG phase was obtained at low temperature due to homogeneous mixing of powders. Under the same sintering conditions, the Yb:YAG ceramics with different doping contents of Yb³⁺ had similar morphologies and densification rates. After being sintered at 1700 °C in vacuum, the ceramic samples had high transparencies. The Yb:YAG ceramics doped with 0.5 wt% SiO₂ formed Y–Si–O liquid phase and nonstoichiometric point defects that enhanced sintering. Compared with Nd doping, Yb doping hardly affected the YAG grain growth, sintering densification or optical transmittance, probably because Yb³⁺ easily entered the YAG lattice and had a high segregation coefficient.     

Fabrication and microstructure development of Yb:YAG transparent ceramics from co-precipitated powders without additives

Sintering additives are generally considered to be important for improving densification in fabrication of transparent ceramics. However, the sintering aids as impurities doped in the laser materials would decrease the laser output power and produce additional heat during laser operation. In this work, Yb:YAG ceramics were vacuum-sintered without additives at different temperatures for various soaking time through using ball-milled powders synthesized by co-precipitation route. The densification behavior and grain growth kinetics of Yb:YAG ceramics were systematically investigated through densification curves and microstructural characterizations. It was determined that the densification in the 1500°C-1600°C temperature range was controlled by a grain-boundary diffusion. It is revealed that the volume diffusion is the main mechanism controlling the grain growth between 1600°C and 1750°C. Although SiO₂ additives can promote densification during low-temperature sintering, the optical transmittance of Yb:YAG ceramic with no additives, sintered at 1800°C for 15 hours, reaches a maximum of 83.4% at 1064 nm, very close to the measured transmittance value of Yb:YAG single crystal. The optical attenuation loss was measured at 1064 nm in Yb:YAG transparent ceramic, to be 0.0035 cm⁻¹, a value close to that observed for single crystals.     

锂铝硅透明微晶玻璃着色研究

引入Cr2O3、CoO、NiO、MnO2等过渡金属氧化物对低膨胀锂铝硅透明微晶玻璃进行着色研究,结果表明,微晶玻璃与其母体玻璃相比,颜色有明显的不同,主波长向长波方向移动。研究还发现,在从核化阶段到晶化阶段的过程中颜色变化最为明显,而在核化阶段和晶化阶段颜色没有发生明显的变化。同时运用配位场理论和光散射原理来解释这种颜色变化的原因。     

钇铝石榴石(YAG)激光透明陶瓷研究进展

钇铝石榴石(YAG)激光透明陶瓷由于具有单晶、玻璃激光材料无可比拟的优势而成为研究热点,并得到迅速发展,高性能的稀土元素掺杂YAG透明激光陶瓷被相继报导.本文综述了近年来国内外关于YAG激光透明陶瓷的最新研究成果.主要包括YAG微细粉体合成、烧结添加刺及多晶YAG透明陶瓷的致密化烧结技术,并对比了YAG透明陶瓷相对于Y...     

Optical properties of Er,Yb co-doped YAG transparent ceramics

The transparent polycrystalline erbium and ytterbium co-doped yttrium aluminum garnet (Er,Yb:YAG) ceramics with various Yb contents from 5% to 25% were prepared by the solid-state reaction and the vacuum-sintering technique. The in-line transmittances of the mirror-polished ceramics exceed 80% from the visible band to the infrared band. The samples are very compact with few pores. The average grain size of the Er,Yb:YAG ceramic is about 15 μm. The upconversion luminescence spectra, infrared luminescence spectra and luminescence decay curves of the ceramics were observed and discussed. For 1%Er doped YAG ceramic, the best ion ratio of Yb³⁺ and Er³⁺ is around 15:1.     

Enhanced Thermostability,Thermo‐Optics,and Thermomechanical Properties of Barium Gallo‐Germanium Oxyfluoride Glasses and Glass‐Ceramics

Serial substitutions of BaF₂ for BaO in BaO–Ga₂O₃–GeO₂ glasses were performed, and the effects of the substitutions on the glass properties were investigated. The glass transition temperature, density, refractive index, thermo‐optics coefficient, and figure of merit for thermal shock decreased with the replacement of oxygen by fluorine. On the other hand, the glass‐forming ability increased. Fluorine substitution removed the absorption band of hydroxyl near 2.9 μm. Raman scattering spectroscopy was used to characterize the fluorogermanate glasses. The crystallization process of the glass‐ceramics under different heat‐treatment conditions was also investigated using differential scanning calorimetry, X‐ray diffraction, scanning electron microscopy, and atomic force microscopy. The thermal and mechanical properties were improved by controlling the crystal size of the near‐ and middle‐infrared transparent glass‐ceramics.     

A novel route to fabricate Yb:YAG ceramic fiber and its optical performance

Transparent laser ceramics are the attractive gain medium for solid-state lasers. However, they have not been applied to the fiber lasers due to the difficulty of forming green fibers by traditional methods. In this study, a novel route combined aqueous gelcasting with capillary glass tube was designed to prepare Yb:YAG transparent ceramic fiber with a diameter of 1.0 mm and 43.0 mm in length for the first time. The slurry with high solid loading and low viscosity was smartly inhaled into the capillary glass tube to conquer the difficulty of casting. The green fibers without cracks and deformation had highly dense microstructure. The in-line transmittance of highly doped 15.0 at.% Yb:YAG transparent ceramic disc prepared from the same preparation conditions of Yb:YAG ceramic fiber was 80.0 % at 1064 nm. This study provides a novel route to prepare transparent ceramic fiber differing from extrusion processing, promoting the development of fiber laser.     

溶胶-凝胶燃烧法合成Er3+:YAG纳米粉体

以氧化铒、氧化钇、硝酸铝及柠檬酸作为起始原料,采用溶胶-凝胶燃烧法制备50%Er3 (摩尔分数)掺杂的Y3Al5O12(YAG)纳米粉体.通过热重-差热分析仪,X射线衍射仪、红外光谱仪和透射电镜研究Er3 :YAG粉体的相变过程、结构和形貌.结果表明:烧结温度小于900℃时,前驱体粉末直接转变为纯YAG晶相,不形成任何中间相.随着烧结温度的增加,晶粒尺寸增大.在900℃烧结的粉体尺寸约为70～150nm,有利于制备性能优异的Er3 :YAG陶瓷.     

Thermal Properties of Transparent Yb‐Doped YAG Ceramics at Elevated Temperatures

This work presents the thermal properties of ytterbium‐doped yttrium aluminium garnet (Yb:YAG) transparent ceramics at elevated temperatures in dependence on the dopant concentration and on temperature. Transparent polycrystalline Yb:YAG ceramics were prepared by solid‐state reaction of oxide powders sintered under high vacuum. The dopant amount varied from 0 to 20 at.% of Yb. Thermal diffusivity of the sintered samples was measured by the laser and xenon flash methods at temperatures ranging from room temperature to 900°C. Both the thermal diffusivity and thermal conductivity values decreased with increasing dopant content, and until 500°C a decrease was observed also with increasing temperature. When available, the measured values were compared to data published in literature, and were found to be in good agreement. Based on the measured values, empirical relations in the form of shifted power laws are proposed for the temperature dependence of thermal diffusivity.