亚超细Y2O2S:Er3+,Yb3+荧光粉的制备及其上转换发光特性

采用高温固相法,通过引入添加剂Bi2O3制备了亚超细(约为500 nm)的上转换荧光粉Y2O2S:Er3+,Yb3+.采用X射线衍射、扫描电子显微镜、能谱、吸收光谱和荧光光谱研究了Bi2O3掺杂对Y2O2S:Er3+,Yb3+荧光粉晶体生长和和上转换发光特性的影响(在980 nm和1550nm波长下激发).结果表明:加入Bi2O3添加剂,由于低温烧结过程中产生液相影响晶体生长,制备出亚超细荧光粉.该荧光粉在980 nm和1550nm波长激发下发光强度有所降低,但仍产生较强上转换发光.     

Er,Yb:(LaGd)_2O_3纳米粉体的制备与发光性质

以碳酸氢铵为沉淀剂,采用共沉淀法制备了Er,Yb:(La Gd)2O3纳米粉体。经1 000℃煅烧2 h得到的粉体颗粒呈规则球形,平均粒径约为90 nm,团聚低,分布均匀。研究了Er3+,Yb3+的掺杂量对样品发光强度的影响。结果表明:掺杂Er3+和Yb3+的摩尔分数分别为4%和5%时,所得样品的发光性能最优。样品的激发和发射光谱显示:在379 nm处激发峰最强,对应Er3+的4I15/2→4G11/2能级跃迁;最强发射峰位于562 nm处,对应于4S3/2/2H11/2→4I15/2能级跃迁。样品的上转换光谱表明:样品在548和662 nm有较强的发射峰,对应Er3+的4S3/2/2H11/2→4I15/2跃迁和4F9/2→4I15/2跃迁。并讨论了发光跃迁机制。     

Er~(3+)-Yb~(3+)共掺杂ZrO_2-TiO_2粉末的上转换发光性质

通过共沉淀方法制备了Er3+和Yb3+共掺的ZrO2-TiO2上转换发光材料。用X射线衍射(XRD)对合成的物相结构进行了检测,并对样品在980 nm激光激发下的上转换发光性质进行了研究。观察到了位于528、550和662 nm附近的绿色和红色发光,分别对应于Er3+离子的2H11/2,4S2/3→4I15/2and4F9/2→4I15/2跃迁。样品的红光和绿光强度随着ZrO2和TiO2配比的变化而变化。随着烧结温度的升高,样品整体发光强度增加。讨论了上转换发光可能的机理:激发态吸收(ESA)和能量传递上转换(ET)过程。     

金属离子掺杂对TiO_2:Yb~(3+)/Er~(3+)上转换材料发光性能的调控研究

稀土文章采用水热法合成掺杂不同金属离子的Ti O2:Yb3+/Er3+上转换发光材料。系统的探讨了不同的金属离子对Ti O2:Yb3+/Er3+发光材料发光性能、形貌以及晶型的影响。具体到通过荧光光谱数据分析离子价态、离子半径等对红、绿光性能的影响;通过SEM数据分析掺杂不同金属离子对应样品形貌的变化;通过XRD数据分析掺杂不同金属离子对应样品的晶型的变化。结果表明离子价态以及离子半径都会改变Ti O2:Yb3+/Er3+材料的发光性能,但与Ti O2:Yb3+/Er3+材料发光性能之间不存在线性关系;掺杂不同金属离子不会改变样品的形貌;掺杂不同金属离子得到了纯相的Ti O2:Yb3+/Er3+样品,且不改变样品的晶型。     

In∶Yb∶Er∶LiNbO_3晶体的生长和光谱性能

采用提拉法生长了掺0.25%(摩尔分数,下同)Yb2O3,0.25%Er2O3和(0.5%、1.0%、1.5%)In2O3的3种同成分In∶Yb∶Er∶LiNbO3晶体。通过晶体的红外光谱,解释了In3+,Yb3+和Er3+在晶体中的占位,由于Yb3+和Er3+离子的掺入,在In∶Yb∶Er∶LiNbO3晶体中In3+既占据Li位又部分占据Nb位,使2%In∶Yb∶Er∶LiNbO3晶体达到阈值浓度。采用980nm二极管激光器测试了In∶Yb∶Er∶LiNbO3晶体上转换发射光谱。结果表明:晶体的绿光上转换发射中心波段位于525、550nm处,分别相应于Er3+的2 H11/2→4 I15/2跃迁和4 S3/2→4 I15/2跃迁;上转换红光发射中心波段在660nm处,对应Er3+的4 F9/2→4 I15/2辐射跃迁。In3+能提高Yb∶Er∶LiNbO3晶体的抗光损伤能力,改变Er3+和Yb3+的局部环境及Yb3+对Er3+的敏化作用,使得In∶Yb∶Er∶LiNbO3晶体发光性能改变。     

基于Er3+/Yb3+掺杂的上转换玻璃陶瓷材料的制备和性能

采用熔融-晶化法在ZnO-Al2 O3-SiO2系玻璃陶瓷的基础上,用GeO2取代部分SiO2成功制备出Er3+/Yb3+共掺ZnO-Al2 O3-GeO2-SiO2系玻璃陶瓷,并通过对样品的硬度及上转换荧光测试分析确定了GeO2的最佳取代量为7.5wt％.研究发现在980 nm波长光的激发下,样品产生了绿色(524 nm、546 nm)和红色(659 nm)上转换发光,且当Er3+/Yb3+掺杂比为2.5:6.5时样品上转换荧光强度最强.     

La2O2S:Yb,Er的制备及其上转换发光性能

采用共沉淀法制备了氧化物La2O3:Yb,Er,高温硫熔法煅烧后得到硫氧化物La2O2S:Yb,Er颗粒,采用XRD和SEM对其晶体结构和微观形貌进行表征,利用荧光光谱仪测试其上转换发光性能. 结果表明,共沉淀温度40℃、草酸过量5%、草酸浓度2.34%、pH值5.53~6.45、热处理温度800℃时可得理想La2O3:Yb,Er. 在1250℃下煅烧3 h得到单一均相La2O2S六方晶体,颗粒呈不规则多边形,尺寸约1 mm. 在980 nm激光激发下,样品呈绿色和红色上转换发光.     

Y2O2S:Yb,Ho上转换发光材料的制备及性能

利用硫熔法制备了不同浓度的Yb和Ho掺杂的Y2O2S:Yb,Ho上转换发光材料。采用X线衍射仪、扫描电镜和荧光光谱仪对粉体的相组成、形貌和上转换发光性能进行表征。结果表明:不同浓度的Yb和Ho掺杂后没有改变Y2O2S的晶体结构;颗粒形貌较为规则,多呈现多面体状,分散性较好,颗粒表面很光滑;在980nm激光激发下,Y2O2S:Yb,Ho呈现出以绿光发射为主的上转换荧光,Yb的最佳掺杂量为8%(摩尔分数),Ho的最佳掺杂量为2%(摩尔分数),Ho3+和Yb3+掺杂浓度可显著影响不同颜色发射峰的强度;对激活离子Ho3+来说,同类离子之间发生能量传递和交叉弛豫行为,导致上转换荧光强度发生猝灭;对敏化离子Yb3+来说,Yb3+吸收能量,以热的形式释放出来,产生杂质猝灭。     

同一上转换机理下Yb3+掺杂浓度对发光强度比值的影响

通过固相反应法制备了Ho3+/Yb3+共掺杂ZrO2-ZnO粉末和Er3+/Yb3+共掺杂不同基质材料的样品,在980nm激发下测量了各样品的绿色和红色上转换发光,分析了各波段的上转换发光机理.在同一上转换机理下,当Yb3+的掺杂浓度增加时,绿光对红光的上转换强度比值呈现出一定规律的变化趋势.这是由于Yb3+的掺杂浓度会影响样品的测试温度,从而改变样品的上转换发光特性.     

柠檬酸凝胶法制备Er,Tm∶Yb3Al5O12纳米粉体及发光性能

以柠檬酸为燃烧剂,采用柠檬酸凝胶法制备了Er,Tm∶Yb3Al5O12(Er,Tm:YbAG)纳米粉体,其最佳的制备工艺条件:Er3+和Tm3+掺杂的摩尔分数分别为2%和1%,柠檬酸与金属硝酸盐原子总数的摩尔比为1.7∶1,煅烧温度和时间分别为950℃和2h。制备的粉体颗粒为规则球形,粒径均匀、分散性好,平均粒径约为45nm。研究了样品的发光性能,结果表明:2%Er,1%Tm∶YbAG样品的发光性能最好,在1 587、1 658和1 711nm处有较强发射峰,分别对应Er3+的4 I13/2→4 I15/2跃迁和Tm3+的3 F4→3 H6跃迁。样品的上转换光谱表明,上转换荧光峰包括了蓝光、绿光和红光。     

Phase equilibrium in binary La2O3-Dy2O3 and ternary CeO2-La2O3-Dy2O3 systems

Cerium oxide doped with oxides of rare earth elements is a multifunctional material, a wide range of uses which is associated with its unique physicochemical properties. Phase diagrams of multicomponent systems are the physicochemical basis for the creation of new materials with improved characteristics.In this work, phase equilibria in ternary CeO₂–La₂O₃–Dy₂O₃ and binary La₂O₃–Dy₂O₃ systems in the whole concentration range were studied. No new phases have been identified in these systems. An isothermal section of the phase diagram of the CeO₂–La₂O₃–Dy₂O₃ system at a temperature of 1500 °С is constructed. No new phases have been detected in the system. It was found that in the studied ternary system solid solutions are formed on the basis of (F) modification of CeO₂ with structure of fluorite type, monoclinic (B), cubic (C) and hexagonal (A) modifications of Ln₂O₃.In the La₂O₃–Dy₂O₃ binary system (1500–1100 °С) three types of solid solutions are formed: based on hexagonal modification A-La₂O₃, monoclinic modification B-Dy₂O₃ and cubic modification C-Dy₂O₃ separated by two-phase fields (A+B) and (B+C), respectively. The boundaries of the regions of homogeneity of solid solutions based on A-La₂O₃ are determined by compositions containing 35–40, 20–25, 15–20 mol% Dy₂O₃ at 1500, 1250, 1100 °C, respectively. From the obtained data it follows that the solubility of Dy₂O₃ in the hexagonal modification of lanthanum oxide is 39 mol% at 1500 °C, 23 mol. % at 1250 °C and 16 mol% at 1100 °C. The limits of existence of solid solutions based on monoclinic B-modification are determined by compositions containing 30–35, 65–60 (1250 °С), 35–40, 55–60 (1100 °С) 40–45, 70–75 (1500 °C) mol% Dy₂O₃.In the studied system, with a decrease in temperature from 1500° to 1100°C, there is a decrease in the solubility of La₂O₃ in the crystal lattice of cubic solid solutions of C-type from 16 to 10 mol%.     

钕-铝系稀土色料的研制

通过钕-铝系列色料合成实验,分析不同配比及不同矿化剂等对色料呈色效果的影响,确定最佳工艺方法。对实验结果进行XRD及色度分析,确定其主晶相为钕酸铝,试样的明度均在70以上,色彩鲜艳亮丽。     

Polycrystalline In2O3 and In2O3/Y2O3 photoanodes

Single crystal In₂O₃ shows promise as a photoanode for the decomposition of water. Because of various difficulties in the preparation of the single crystal material, two simple techniques were developed for the preparation of polycrystalline In₂O₃ anodes. One method involves the thermal decomposition of the nitrate while the other utilizes the chemical vapour deposition technique. Voltammograms and photoresponse spectra of these anodes are compared to the single crystal material. Among other observations, it is noted that the quantum efficiencies of the thermally decomposed films are comparable to the single crystal material. It is also shown that the on-set potential can be shifted to more negative values by forming the mixed oxide In₂O₃/Y₂O₃.     

Na2O-Al2O3-Fe2O3系烧结过程中铝、铁的反应行为

以Al2O3, Fe2O3和Na2CO3为原料,对Na2O-Al2O3-Fe2O3系烧结过程中的反应行为进行了详细研究. 基于溶出率与时间、温度的关系,证明Na2O×Al2O3和Na2O×Fe2O3的生成反应动力学都服从Zhuralev-Lesokin-Tempelman模型,表观活化能分别为186.59和80.92 kJ/mol,表明Na2O×Fe2O3比Na2O×Al2O3在动力学上更易形成;Al2O3易与Na2O×Fe2O3反应形成Na2O×Al2O3和Fe2O3,在1273 K烧结30 min,所得熟料Al2O3溶出率达98.51%;Fe2O3对Na2O×Al2O3的形成有双重作用,在1273 K下可加速Na2O×Al2O3的形成,超过1323 K,促使Na2O×Al2O3分解成Na2O和b-Al2O3,且随着温度升高或时间延长,分解程度增高,从而导致熟料中Al2O3溶出率显著降低.     

Properties of RO-Y2O3-Al2O3-SiO2 glasses

The coefficient of linear expansion, glass-transition temperature, temperature at the orset of deformation (strain point), density. Young modulus, microhardness, crystallizability, and contact angle are studied as a function of the composition in RO–Y₂O₃–Al₂O₃–SiO₂ (R=Ca and/or Mg) glass systems. The composition ranges for glasses (with strain point >900°C and coefficient of linear expansion of (32–45)×10^–7°C^–1) that can be used for soldering silicon-nitride ceramics were established.Translated from Steklo i Keramika, No. 12, pp. 5–7, December, 1996     

Cr2O3-Al2O3-ZrO2高铬制品

介绍了Cr2O3-Al2O3-ZrO2制品的组成及各组成的作用、烧成气氛、制品的显微结构特征和性能指标.着重论述了影响制品性能的烧成工艺和以电熔、烧结两种Cr2O3颗粒生产的Cr2O3-Al2O3-ZrO2制品的显微结构差异,表明在还原气氛下烧成的Cr2O3-Al2O3-ZrO2制品性能优良,而采用电熔Cr2O3料生产的Cr2O3-Al2O3-ZrO2制品性能优于使用烧结Cr2O3料生产的.     

Fe2O3-MnO-Cr2O3-La2O3系统紫色颜料的制备及表征

采用溶胶均匀共沉淀法于低温下合成了含少量稀土氧化物La2O3的紫色颜料，并采用颜色测定、SEM、XRD等手段对颜料的颜色、检度及结晶构造等进行了表征。     

CaO-SiO2-Al2O3-Fe2O3-SO3多元体系高温相变研究

实验采用石灰石、砂岩、粉煤灰和低品位铝矾土等工业原料,制备C3S相和C4A3S-相共存的水泥熟料;利用DSC-TG、高温XRD、岩相等方法对CaO-SiO2-Al2O3-Fe2O3-SO3多元体系烧制过程中高温相变进行分析,获得C4A3S-相和C3S相的变化规律,为利用废渣制备低碳排放的水泥熟料提供了理论支持.     

含Y2O3的锂铝硅系统微晶玻璃

The rare earth oxide Y2O3 was added to the system Li2O—Al2O3—SiO2 glass—ceramics and the effects of Y2O3 on the properties of melting, crystallizing, microstruoture as well as thermal expansion coefficient of the glass was studied by DTA, SEM and XRD. The results indicate that, adding YZO3 to Li2O—Al2O3—SiO2 systems glass could increase the viscosity of glass melt, in6rease the melting temperature and the crystallization temperature of glass,increase the volume fraction of crystals while the crystal types are not changed, and the coefficient of thermal expansion of glass-ceramics decreases with the increasing of Y2O3 content.     

Separation of Phases by Spinodal Decomposition in the Systems Al2O3−Cr2O3 and Al2O3−Cr2O3−Fe2O3

Separation of phases was investigated in the hexagonal (rhombohedral) systems Al₂O₃−Cr₂O₃ and Al₂O₃−Cr₂O₃−Fe₂O₃. The binary system shows a miscibility gap with a T_c of 950°C; the miscibility gap for the ternary system was determined for a constant Cr₂O₃ content of 16.6 mol%. Dark field transmission electron microscopy of solid solutions annealed within the miscibility gap showed dark and light lamellas ∼50 to 200 Å thick. X-ray diffraction results for the solid solutions in the ternary system indicated that, in the early stages of annealing, broadening occurred only on (hkl) reflections where l≠0. There was no major change in the X-ray diffraction patterns of the annealed solid solutions in the binary system. Electron diffraction results indicated, however, that phase separation in both systems proceeded in the [001] direction. Solid solutions in the binary system separated very slowly; the separation could be enhanced hydrothermally. The mechanism of the separation of phases in both systems is spinodal and proceeds as follows: solid solution→intermediate modulated phase→equilibrium phases.