利用共沉淀法制备超细YAG粉体及其表征

钇铝石榴石(YAG)具有稳定的化学性能,在作为化工新型材料使用中得到了广泛应用。本文通过利用共沉淀法制备超细YAG粉体。通过研究可以得到,前驱体在1100℃下煅烧1h后,生成了纯的YAG晶体。合成的YAG颗粒比较分散、细小,其粒度大小相当均一,粉体颗粒粒径在200～350nm之间,其颗粒近似球形,颗粒之间有部分烧结现象出现。     

YAG:Er~(3+)纳米粉体的合成及上转换发光的研究

以稀土氧化物、硝酸铝为原料,采用溶胶-凝胶法合成了铒掺杂的钇铝石榴石(Y3Al5O12,YAG)纳米晶粉体.用X射线衍射(XRD)及傅里叶红外光谱(FTIR )确定前驱体和不同温度处理的粉末的相组成,同时表明在1200 ℃形成了结晶完全的YAG相.该粉体在波长为980 nm的半导体激光器激发下发射出中心波长为666 nm的红色上转换荧光及525 nm、556 nm的绿色上转换荧光,分别对应于Er3+离子的4F9/2 → 4I15/2,2H11/2 → 4I15/2,4S3/2 → 4I15/2跃迁.其中666 nm的上转换荧光为双光子过程,激发态吸收和能量转移是主要的上转换机制.     

共沉淀法合成钇铝石榴石纳米粉体及透明陶瓷的制备

以硝酸铝[Al(NO3)3·H2O]和硝酸钇[Y(NO3)3·6H2O]为原料、以碳酸氢铵[NH4HCO3]为沉淀剂,硫酸铵[(NH4)2SO4]为分散剂,用共沉淀法合成钇铝石榴石(yttrium aluminum garnet,YAG)纳米粉体.用X射线衍射仪、红外光谱仪、热分析仪和场发射扫描电镜等测试手段对YAG前驱体和煅烧后的粉体进行表征.结果表明:前驱体经过1 000℃煅烧5h后已完全转变成纯立方相YAG,所得的粉体分散性好、无团聚、形状近似球形、平均颗粒尺寸约为100 nm.以该YAG粉体为原料,正硅酸乙酯[Si(OC2H5)4,TEOS]为添加剂,用真空烧结技术在1 700～1 800℃煅烧20h制备YAG透明陶瓷.YAG陶瓷样品的平均晶粒尺寸为10 μm,存在少量气孔相和杂质相.为了提高YAG陶瓷的透过率,需要进一步优化陶瓷的制备工艺.     

共沉淀法制备掺钕钇铝石榴石透明陶瓷:滴加方式的影响

用共沉淀法正滴和反滴工艺制备了掺钕钇铝石榴石(Nd:YAG)粉体.测试了粉体的相组成、显微形貌,粒度分布.结果表明:经1100℃煅烧后,正滴工艺得到粉体主相为YAG(Y3Al5O12),但有少量的YAM(Y4Al2O9),反滴工艺则得到纯的YAG.晶粒尺寸分别为24.7 nm和26.6 nm,平均粒径分别为1.26μm...     

丙二酸溶胶-凝胶法合成亚微米级YAG:Ce,Gd黄色荧光粉

以丙二酸为络合剂,通过溶胶-凝胶法合成了亚微米级YAG:Ce,Gd黄色荧光粉.采用TG/DSC、XRD研究干凝胶热分解和YAG晶相形成的过程;通过荧光光谱分析了Gd~(3+)的掺杂对荧光粉的发光强度的影响规律;通过SEM观察粉体的微观形貌.结果表明:经1200 ℃煅烧3 h得到的荧光粉,粉体粒径为0.3～1 μm,颗粒规则接近球形;随着Gd~(3+)掺杂量的增加,荧光粉的发射光谱由525 nm红移到550 nm.     

高分子网络凝胶法制备纳米YAG粉体

以硝酸铝和硝酸钇为原料,采用高分子网络凝胶法制备纳米YAG粉体,对网络凝胶机理和胶体的煅烧过程进行了研究。研究表明干凝胶在900℃煅烧即可全部转变为YAG纯相,没有YAM、YAP等中间相生成。所制备的粉体粒度尺寸大小为20nm左右,颗粒呈球形,有轻微团聚。     

铈掺杂钇铝石榴石纤维的电纺丝制备及光学性能

采用静电纺丝技术制备了铈掺杂钇铝石榴石(cerium doped yttrium aluminium garnet,YAG:Ce)纳米纤维,利用扫描电镜观测了电纺丝纤维的微结构与形貌,利用荧光光谱仪表征了YAG:Ce电纺丝纤维的荧光性能。结果表明:在还原气氛下热处理制备YAG:Ce电纺丝纳米纤维时,在纳米纤维表面出现了一层直径为50～100 nm的球形凸起物。相比于空气气氛中,在还原气氛中热处理制备YAG:Ce纳米纤维的荧光发射强度显著增强。并且随着Ce~3+掺杂含量增加,YAG:Ce电纺丝纤维的荧光发射带发生红移。     

共沉淀法制备YAG:Ce~(3+)纳米荧光粉

以Al(NO_3)_3·9H_2O、Y (NO_3)_3·6H_2O和Ce (NO_3)_3·5H_2O为原料、NH_4HCO_3为沉淀剂、十二烷基苯磺酸(C_(18)H_(30)SO_3)为分散剂,采用改进的共沉淀法合成YAG:Ce~(3+)纳米荧光粉体。实验结果表明:前驱体经过800℃煅烧2 h后已完全转变成纯立方相YAG:Ce~(3+)纳米荧光粉体,900℃煅烧2 h后的粉体分散性好、颗粒尺寸分布均匀、形状近似球形,平均粒径约为70 nm。在450 nm激发下荧光粉的最强发射峰为545 nm,在约180℃条件下的亮度为30℃条件下的88. 5%左右,具有优异的高温热稳定性能。     

溶剂热法合成YAG晶粒的形成过程

钇铝石榴石(Y3Al5O12,YAG)透明陶瓷因其优异的光学性能和制备工艺方面的优势而成为极具潜力的激光材料。性能优良的YAG微粉有利于制备高性能YAG陶瓷。利用铝和钇的硝酸盐为起始原料制备反应前驱物,用乙醇作溶剂,在280℃保温4h下合成了球形YAG晶粒。在溶剂热反应过程中,溶剂中反应前驱物通过溶解、脱水、析晶及生长的过程直接形成YAG晶粒,无中间相形成,晶粒平均尺寸约为80nm,且尺寸分布均匀,晶粒间基本无团聚。     

碳酸盐共沉淀法制备掺镱钇铝石榴石透明陶瓷的工艺

以质量分数为99．999％的Yb2O3,Y2O3和Al2O3为原料,碳酸氢铵作为共沉淀剂,采用碳酸盐共沉淀法在1200℃制备出掺镱钇铝石榴石(Yb：YAG)陶瓷超细粉体。1700℃真空烧结后得到透光度良好的Yb：YAG多晶陶瓷。对Yb：YAG粉体样品进行X射线衍射分析、热重-差热分析和扫描电镜分析。结果表明：所合成的YAG超细粉仍为立方晶系晶体结构,晶格常数为a=12．01A。Yb：YAG粉体样品颗粒度小、粒径均匀、流动性好,粒径在100～150nm之间。对烧结后的Yb：YAG陶瓷样品进行的形貌和红外光谱分析表明：陶瓷断面气孔率低,多晶晶粒尺寸在1～2μm之间。     

Synthesis, growth mechanism and photoluminescence of monodispersed cubic shape Ce doped YAG nanophosphor

In the present work, a novel method for the synthesis of monodispersed cubic shape Ce-doped yttrium aluminum garnet (YAG:Ce) nanophosphors is reported. Single phase Ce doped YAG nanoparticles are prepared by solvothermal processing, followed by annealing treatment. Morphological investigation by scanning electron microscopy (SEM) showed the formation of monodispersed 500 nm cubic shape Ce-doped YAG phosphor. The crystalline Ce-doped YAG showed broad emission peaks in the range of 480-640 nm with maximum intensity at 524 nm. The emission intensity increased with increase in calcination temperatures while reduced with increase in Ce³⁺ ions concentration. Detailed study was carried out to understand the formation of monodispersed cubic shape Ce doped YAG nanoparticles. It was found that the solvent, surfactant and impurity (counter ions of cerium and aluminum salt) has significant effect on the crystal growth.     

One‐Pot Synthesis of Submicrometer‐Sized Ce:YAG Spherical Particles by Solvothermal Process Using Alcohol Solvents

A rapid synthesis method for preparing homogeneous and submicrometer‐sized cerium‐doped yttrium aluminum garnet (Ce:YAG) particles was proposed in this work. Instead of precipitating the YAG amorphous precursor prior to the solvothermal process, cerium, yttrium, and aluminum nitrates were dissolved in alcoholic solvents to form transparent and clear solutions that were directly transferred into the stainless autoclave to undergo the solvothermal reaction. Four different alcohol solvents, that is, ethanol, 2‐propanol, 2‐butanol, and tert‐butanol, were used as the reaction medium. The crystallization mechanisms in correlation with the alcohol solvent properties, such as the supercritical point and the dielectric constant, were discussed. The interaction between the alcohol solvent and the precursor salts were also investigated. Well‐dispersed and spherical Ce:YAG particles in size ranging from 200 to 350 nm were obtained in one pot via solvothermal reaction at 285°C from 5 to 8 h.     

共沉淀法合成YAG：Ce纳米粉体

通过在NH4HCO3溶液中滴加Ce（NO3）3、A1（NO3）3和Y（NO3）3的混合溶液,共沉淀生成YAG：Ce的碳酸盐前驱体,对YAG前驱体在不同温度下进行灼烧,并采用IR、XRD和TEM等测试手段对粉体进行表征。结果表明,在1100℃下煅烧YAG前驱体,得到无YAP、YAM中间相的出现纯YAG晶相,所得粉体晶粒直径为20～50nm,具有较好的分散性。同时,荧光测试表明Ce：YAG粉体具有良好的发光性能。     

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.     

Synthesis and Characterization of Ce3+:YAG Phosphors by Heterogeneous Precipitation Using Different Alumina Sources

Ce³⁺-doped yttrium aluminum garnet (Ce:YAG) phosphor powders were synthesized by heterogeneous precipitation process using three different aluminum sources: α-phase, θ-phase, and boehmite (AlOOH). Mixtures of yttrium and cerium nitrate solutions containing various aluminum sources were precipitated by ammonia solution in normal and reverse strike methods. The influence of pH was studied in the normal strike method by maintaining the solutions at pH 7, 9, and 11 during precipitation. Dried precipitates were double calcined at 1300°C/16 h and 1300–1500°C/24 h, at a ramping rate of 10°C/min, with an intermittent wet ball milling in water. Structural evolution of the resultant phosphors was studied by powder XRD. In the normal strike method, a highly pure YAG phase was formed by α- alumina (pH 7, 11) and θ-alumina (pH 11) while boehmite source ended up with mixed phases of YAlO₃ (YAP) and Y₄Al₂O₉ (YAM) along with YAG phase at all pH values of precipitation. However, in the reverse strike process, the θ-phase of alumina gave an extremely pure Ce:YAG phase at a relatively lower calcination temperature (1400°C/24 h) compared with the α-phase and also showed more intense emission of yellowish-green light under blue (λ=469 nm) excitation. Scanning electron microscopy revealed 1–2 μm sized particles with least agglomeration in the reverse strike method.     

Comment on an article by Gonzaga et al. J Am Ceram Soc. 2020;103:6280-6288

I argue that the authors’ interpretation of X-ray photoelectron spectroscopy (XPS) Ce3d spectra of their materials is untenable because it largely neglects the electronic structure of cerium ions and spin-orbit interaction of the Ce3d subshell. I conclude that at %Ce³⁺ values the authors derived from their Ce3d spectra offer an inaccurate account of the cerium chemistry of their materials.     

溶胶凝胶法制备的Y3Al5O12:Tb3+,Ce3+的光学性能及能量传递研究

用溶胶凝胶法制备了一系列不同掺杂浓度的Y3Al5O1 2(YAG):Tb3+,Ce3+荧光粉,对其物相、光学性能和能量传递进行了研究.多晶粉末X-射线衍射结果表明,所有样品均为YAG晶相,没有其它杂相.当样品在Tb3+的特征激发峰273 nm激发时,除了Tb3+的特征发射外,还观察到位于467 nm的YAG基质的电荷迁...     

Optical performances of mono‐dispersed spherical YAG:Ce3+ nano‐phosphor achieved by one‐pot synthesis

Mono‐dispersed spherical YAG:Ce³⁺ nano‐phosphors were successfully synthesized by a one‐pot glycol‐thermal process using aluminum isopropoxide, yttrium, and cerium acetate hydrates as the precursor, (1,4)‐butanediol as the solvent, ethidenediamine as the additive agent that can both control the morphology and improve the optical performances of the as‐achieved products. The as‐prepared YAG:Ce³⁺ nano‐phosphors displayed mono‐dispersed spheres of about 150 nm and an improved optical performance with a quantum yield (QY) of 41% and good photostability, indicating that they have a considerable potential to be applied in solid‐state lighting or used as coatings in other optical electronic devices.     

The effect of Lu3+ doping upon YAG:Ce phosphor ceramics for high-power white LEDs

Intense green emission is extremely significant to the color rendering index (CRI) of white LEDs. Various green-emitting YLuAG:Ce phosphor ceramics were successfully prepared by vacuum sintering. The effects of Lu³⁺ doping on structure and luminescence property were investigated in detail. In comparison with YAG:Ce, YLuAG:Ce ceramics own smaller grain size, better luminescence performance and higher thermal stability. The photoluminescence (PL) intensity of YLuAG:Ce ceramics increases by 23.6 % due to the “light scattering enhanced effect”. Furthermore, the Ce³⁺ emission is obviously blue-shifting from 533 nm to 519 nm, and the intensity of YLuAG:Ce ceramics reduces only about 8.9 % at 250 °C, showing better thermal stability (vs 11.1 % of YAG:Ce). The LE of LED packaged by YLuAG:Ce ceramic is up to 148.88 lm/W when the doping Lu³⁺ y is 2.1. The above results show that tailored YLuAG:Ce phosphor ceramic is a potential green-emitting color converter for high-power LEDs (hp-LEDs).