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。     

铈和铽离子掺杂硼硅酸盐玻璃的发光性能

采用传统方法制备了Ce3 和Tb3 掺杂的硼硅酸盐玻璃样品.应用紫外可见分光光度计和荧光光谱仪测试了样品的透过、激发和发射光谱,并测量了Ce3 掺杂玻璃样品在X射线激发下的发射光谱.结果表明:基质玻璃具有很好的透光性能,截止波长约为300 nm,适于用作掺杂稀七离子的玻璃闪烁体的基质材料;与基质玻璃相比,Ce3 掺杂玻璃样品的截止波长发生红移;随着Ce3 离子含量的增加,样品的紫外截止波长向长波方向位移;随着基质玻璃光碱度的增加,Ce3 掺杂玻璃样品的激发峰和发射峰发生红移,Stokes位移增大;对于Ce3 和Tb3 共掺杂硼硅酸盐玻璃,存在Ce3 敏化Tb3 发光现象;在X射线激发下,Ce3 掺杂玻璃样品的发射光谱与荧光光谱相似,但发射峰发生红移.     

Dy3+/Tb3+单掺硼酸盐玻璃陶瓷的高效可见荧光发射

实验采用高温熔融-退火法分别合成了Tb³⁺掺杂和Dy³⁺掺杂的稀土硼酸盐玻璃陶瓷材料。XRD晶相分析表明,所制备的样品为非晶态玻璃陶瓷物质;SEM形貌分析表明,样品表面十分致密,无明显的结晶状物质;光谱特性试验结果表明,在紫外激发下,Tb³⁺和Dy³⁺单掺在这种新型硼酸盐玻璃陶瓷中分别发出了强烈的绿色和明亮的黄白光。该类材料在可见显示器件方面具有广阔的应用前景,可用于开发新型彩色光源、荧光显示器件、紫外传感器和可调谐可见光激光器。     

超声波辅助合成YOF:Tb~(3+)荧光粉及其荧光性能

以Tb4O7与Y2O3为主要原料,用超声波辅助合成前驱体,经高温煅烧后合成了稀土YOF:Tb3+绿色荧光粉。采用XRD、SEM和荧光分光光度计对样品的结构、形貌和荧光性能进行分析。样品XRD表明,产物为四方晶系YOF:Tb3+,结晶度较好。SEM表明合成的荧光粉为100mm~200nm左右的纳米颗粒。荧光分析显示,荧光粉的荧光性能受前驱体辅助合成方式及Tb3+掺杂浓度等各种因素影响。在230nm的紫外光激发下,40℃的低温超声波辅助下合成的前驱体经过煅烧后制得的荧光粉荧光性效果好。当Tb3+的摩尔掺杂浓度大于5%时,出现浓度淬灭现象。     

WLED用单基质硅酸盐荧光粉的制备及性能研究

采用溶液-燃烧法制备了Ca2MgSi2O7白光LED用荧光粉,探讨了溶液-燃烧法制备样品的工艺参数并分别对单掺Eu3+和三掺Eu3+,Ce3+,Tb3+在不同浓度下的荧光性能进行分析。通过同等条件下荧光光谱的对比分析发现单掺Eu3+离子,掺杂浓度为金属离子浓度的1%时荧光强度最强;三掺Eu3+,Ce3+,Tb3+的物质的量比为1∶1.5∶1时样品荧光强度最强。     

Tm~(3+)和Dy~(3+)共掺氟氧铝硼硅酸盐玻璃微晶化及白光发射性能

采用高温熔融-淬火/热处理方法在空气气氛中制备了Tm_2O_3和Dy_2O_3共掺氟氧铝硼硅酸盐玻璃及透明微晶玻璃。用转靶多晶X射线衍射仪、荧光分光光度计和热分析仪对玻璃样品进行了表征。结果表明:样品在640～660℃热处理4h和在640℃热处理4～16h可制得透明的含Ba_2LaF_7纳米晶玻璃。增大Tm-Dy共掺浓度并降低La_2O_3浓度时,Ba_2LaF_7析晶倾向降低。此外,热处理析出Ba_2LaF_7微晶相后,样品的Tm_2O_3和Dy_2O_3共掺浓度淬灭点由1%(摩尔分数,下同)提高到了2%。掺杂不同浓度Tm_2O_3和Dy_2O_3时,白光发光色度保持不变。     

Tb~(3+)、Gd~(3+)对硅酸盐发光玻璃发光性能的影响

对Nb3 + 激活的硅酸盐发光玻璃进行了研究 ,讨论了Tb3+ 和Gd3 + 对玻璃发光性能的影响。结果表明 :Tb3+ 激活的硅酸盐玻璃在紫外线和X 射线的激发下 ,产生蓝色荧光和较强的绿色荧光 ;随着Tb3+ 离子浓度的增加 ,Tb3 + 离子5D3 能级的能量向5D4 能级转移 ,绿色荧光得到增强 ;Gd3 + 离子通过无辐射能量共振方式对Tb3+ 离子的发光起到了敏化作用 ,加入Gd3+ 进一步提高了Tb3+ 激活硅酸盐玻璃的发光强度     

钕掺杂钡铝硅透明玻璃陶瓷的制备和表征

采用熔融-晶化技术制备了含纳米微晶的Nd3+:BaO-Al2O3-SiO2透明玻璃陶瓷,用差热分析仪、X射线衍射分析仪、扫描电子显微镜和紫外-可见-近红外分光光度计和Fourier变换荧光光谱仪对样品的成核-晶化温度、晶相组成、微观形貌、光透过率和光谱性能进行了测试和表征.结果表明,钕掺杂钡铝硅系透明玻璃陶瓷的最佳成核温度为690℃,最佳成核时间为4 h,观测到钕掺杂钡铝硅玻璃陶瓷在808 nm激发下于1068nm处存在较强发射峰.     

掺Tb~(3+)法拉第磁光玻璃研究新进展

Tb3+掺杂Faraday磁光玻璃是一种新型的功能材料,在光纤通信和传感领域有广阔的应用前景。介绍了磁光玻璃Faraday效应的基本原理和Tb3+离子的磁光性能,讨论了入射光波长、电子有效跃迁波长、基质玻璃、外界温度和Tb3+离子浓度对磁光效应的影响,以及Tb3+离子掺杂量对磁光玻璃形成能力和热稳定性的影响,提出了法拉第磁光玻璃研究新方向。     

Dy~(3+)/Y~(3+)掺杂GdPO_4玻璃陶瓷的制备及性能研究

以Na_2CO_3、Al_2O_3、SiO_2、NaF、GdF、DyF、YF、(HN_3)_2HPO_4为原料,利用熔融急冷法制备了GdPO_4玻璃陶瓷以及Y~(3+)、Dy~(3+)、Y~(3+)/Dy~(3+)掺杂的GdPO_4玻璃陶瓷,通过DSC、XRD、SEM、紫外可见光度计等研究了玻璃陶瓷的制备工艺、相成分、微观结构和透光性。结果表明:确定的热处理规程为570℃核化2h再670℃晶化2h,得到的玻璃陶瓷外观透明、成型良好,在玻璃基体中有明显的微晶。在GdPO_4中掺杂稀土有利于微晶从玻璃基体中析出,其中Dy~(3+)掺杂GdPO_4玻璃陶瓷中的微晶尺寸最大。所有的玻璃陶瓷在可见光区具有高透过性,Dy~(3+)掺杂的GdPO_4玻璃陶瓷的可见光区透光率低于其他样品。     

Preparation,optical, and thermal stability of Tb3+-doped glass ceramics containing Al4Ti2SiO12

The Tb³⁺-doped transparent glass ceramics containing Al₄Ti₂SiO₁₂ crystal are synthesized by the melt-solid-crystallization method. The optimal heat treatment conditions for the glass ceramic samples are determined to be 750°C, 1.5 h based on differential scanning calorimeter, X-ray diffractometer, scanning electron microscope, and light transmittance curve. The luminescence properties of the glass ceramics samples are characterized by a fluorescence spectrometer. The emission spectrum revealed that the dominant emission is green attributed to Tb³⁺, the optimal doping concentration is 0.3%. And the thermal quenching activation energy of 0.3% Tb³⁺-doped glass ceramics is 0.2554 eV, while the relative sensitivity is 1.50% K⁻¹ at 298 K and the absolute sensitivity is 2.27×10⁻² K⁻¹ at 418 K through variable temperature fluorescence spectroscopy test and a series of calculations. These findings demonstrate the excellent stability and temperature sensitivity of glass ceramics, thereby highlighting their potential for use in green lighting and temperature sensing applications.     

Crystallization and luminescence properties of Eu<Superscript>2+</Superscript> doped diopside glass ceramics

Eu²⁺ doped glass ceramics have been prepared and characterized. The crystallization and optical properties of the glass ceramics were studied by XRD, SEM, and fluorescence spectra. The precipitated crystalline phase in the glass ceramics was prismatic diopside (CaMgSi₂O₆) and plate-like cristobalite (β-SiO₂). As the heat treatment time increases, the content of crystals increases gradually. Fluorescence measurements showed that Eu²⁺ ions entered into the diopside crystalline phase and induced a much stronger emission in the glass ceramics than that in the corresponding glass. With increase of Eu²⁺ content, concentration quenching was observed.     

Fabrication and properties of transparent Tb:YAG fluorescent ceramics with different doping concentrations

Terbium doped yttrium aluminum garnet (Tb:YAG) transparent ceramics with different doping concentrations were fabricated by the solid-state reaction method using commercial Y₂O₃, α-Al₂O₃ and Tb₄O₇ powders as raw materials. Samples sintered at 1750 °C for 20 h were utilized to observe the optical transmittance, microstructure and fluorescence characteristics. It is found that all the Tb: YAG ceramics with different doping concentrations exhibit homogeneous structures with grain size distributions around 22–29 µm. For the 5 at% Tb:YAG transparent ceramics, the grain boundaries are clean with no secondary phases. The photoluminescence spectra show that Tb:YAG ceramics emit predominantly at 544 nm originated from the energy levels transition of ⁵D₄→⁷F₅ of Tb³⁺ ions, and the intensity of the emission peak reaches a maximum value when the Tb³⁺ concentration is 5 at%. The in-line transmittance of the 5 at% Tb:YAG ceramics is 73.4% at the wavelength of 544 nm, which needs to be further enhanced by optimizing the fabrication process. We think that Tb:YAG transparent ceramics may have potential applications in the high-power white LEDs.     

Modification of Optical Properties of SrAl_2O_4：Eu~（2＋）,Dy~（3＋） Phosphor by Terbium Doping

以尿素为燃料,采用快速燃烧法在650℃合成了Tb3＋掺杂的SrAl2O4：Eu2＋,Dy3＋新型长余辉光致发光材料。研究了Tb3＋掺杂对Eu2＋,Dy3＋共激活的铝酸盐长余辉发光材料的发光特性的影响。X射线衍射分析结果表明：当Tb3＋的掺杂量x=0.17%时,合成的样品结构为单相SrAl2O4单斜晶系。光致发光测试结果表明：样品的激发光谱为峰值位于345nm附近的连续宽带谱,发射光谱为峰值位于510nm左右的连续宽带谱。余辉衰减曲线结果表明：Tb3＋的适量掺杂可以提高铝酸锶的余辉性能。与SrAl2O4：Eu2＋,Dy3＋相比,掺杂Tb3＋有利于形成结晶度良好的固溶体,样品中的晶体细密紧凑,颗粒粒径约为100nm。     

Ag~+掺杂钛酸锶钡基玻璃陶瓷的显微结构和介电性能

采用熔融法制备了钛酸锶钡（barium strontium titanate,BST）基玻璃,然后将此玻璃样品在不同的温度下进行热处理得到BST基玻璃陶瓷,采用差热分析研究了BST基玻璃陶瓷析晶过程中的热力学特征,用扫描电子显微镜和X射线衍射分别分析了玻璃陶瓷的显微结构和相结构,并且系统研究了该玻璃陶瓷的介电特性以及耐击穿电场强度。结果表明：0.3%（质量分数）Ag＋掺杂时,BST基玻璃中BST相的析晶温度从885℃下降到840℃,有利于玻璃体中BST晶体的析出。另外,Ag＋的掺杂有利于提高BST基玻璃陶瓷的介电常数,同时能维持较低的介电损耗。此外,Ag＋掺杂能够提高BST基玻璃的耐击穿电场强度,其在800℃热处理后,可达96.3 kV/mm,高于未掺杂Ag＋的BST基玻璃的52.5kV/mm。     

Distribution of Nd3+ ions in oxyfluoride glass ceramics

It has been an open question whether Nd³⁺ ions are incorporated into the crystalline phase in oxyfluoride glass ceramics or not. Moreover, relative research has indicated that spectra characters display minor differences between before and after heat treatment in oxyfluoride glass compared to similar Er³⁺-, Yb³⁺-, Tm³⁺-, Eu³⁺-, etc.-doped materials. Here, we have studied the distribution of Nd³⁺ ions in oxyfluoride glass ceramics by X-ray diffraction quantitative analysis and found that almost none of the Nd³⁺ ions can be incorporated into the crystalline phase. In order to confirm the rationality of the process, the conventional mathematical calculation and energy-dispersive spectrometry line scanning are employed, which show good consistency. The distribution of Nd³⁺ ions in oxyfluoride glass ceramics reported here is significant for further optical investigations and applications of rare-earth doped oxyfluoride glass ceramics.     

Zn2+离子掺杂对负载TiO2薄膜光催化活性的影响

以钛酸丁酯和ZnSO₄·7H₂O为原料，采用溶胶-凝胶法在钛片、玻璃、釉面瓷砖、陶瓷、不锈钢和铝片六种载体上制备了Zn²⁺掺杂TiO₂薄膜，讨论了不同Zn²⁺掺杂浓度下不同载体表面上制备的TiO₂薄膜对甲基橙脱色率的影响。结果表明，Zn²⁺对TiO₂薄膜的掺杂效果与载体的类型密切相关，并且不同载体其Zn²⁺掺杂的最佳浓度也不同。Zn²⁺掺杂后，TiO₂薄膜光催化活性提高最大的是釉面瓷砖，其次是钛片、玻璃、陶瓷。不锈钢和铝片上TiO₂薄膜的光催化活性不但没有升高，反而降低了。     

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.     

The preparation of Yttrium Aluminosilicate (YAS) Glass Fiber with heavy doping of Tm3+ from Polycrystalline YAG ceramics

Yttrium aluminosilicate (YAS) glass core fibers with different doping concentration of Tm³⁺ were fabricated by a “Melt‐in‐Tube” method from YAG polycrystalline ceramics. The effect of Tm³⁺ concentration on the spectroscopy of YAG ceramics and laser performance of YAS fibers were discussed. A homemade linear all‐fiber laser based on the obtained 15% Tm³⁺‐doped YAS fiber shows an optimized slope efficiency of 12.8%. The YAS fibers have been proven to be practical to achieve extremely high Tm³⁺ doping concentration and are a promising option for the 2.0 μm laser.     

The charge state of titanium ions in Pd‐doped Ti:CMAS glass and glass‐ceramics

We have investigated the role of charge state of Ti in the electronic properties and structure of electrically conductive CMAS‐TiO₂‐Pd glass and glass‐ceramics by X‐ray photoelectron spectroscopy, electron paramagnetic resonance, positron annihilation lifetime spectroscopy, and fluorescence spectroscopy. These studies suggest the concentration of Ti³⁺ ions was, at most, ~0.1 wt% in glass‐ceramics devitrified in the reducing atmosphere of forming gas; no other glass or glass‐ceramic samples exhibited measurable levels of Ti³⁺. The observed fluorescence at liquid nitrogen temperature in parent glasses and glass‐ceramics obtained in air is explained by UV‐induced charge‐transfer processes involving Ti⁴⁺ ions and oxygen surroundings. The X‐ray photoelectron spectroscopy data are correlated with rutile, anorthite, diopside, and titanite crystalline phases identified in Pd‐free and Pd‐doped Ti:CMAS glass‐ceramics earlier.