掺铕铽钨酸锶荧光粉的制备与发光性质分析

通过化学共沉淀法制备了Sr0.95WO4∶xEu3+∶(0.05-x)Tb3+荧光粉.采用X射线粉末衍射仪、扫描电子显微镜和荧光光谱仪对样品材料的结构、形貌和发光性能进行了表征.分别讨论了在不同反应温度下及稀土离子Eu3+和Tb3+共掺比例变化对荧光粉的发光性能和形貌的影响.结果表明:所得SrWO4∶xEu3+∶(0.05-x)Tb3样品是由无规则棒组成的发光材料,它们在800℃时,发光性能最好;样品在223 nm紫外光的激发下,在543 nm和614 nm处,呈现出两个主要发光中心,分别归属于5D4→7F5和5D0→7F2跃迁,说明稀土离子Eu3+和Tb3具有良好的发光性能,同时随着Eu3和Tb3+掺杂比例的改变,荧光体的发光色度也在不断改变.     

超声辅助共沉淀法合成CaMoO4:Eu3+红色荧光粉及其发光性能研究

采用超声辅助共沉淀法合成了以Eu3+为激活离子的CaMoO4荧光粉.通过X-射线衍射、扫描电镜(SEM)、荧光分光光度计对样品进行了表征和分析,研究了溶剂浓度、表面活性剂种类、表面活性剂添加量、超声时间等反应参数对CaMoO4:Eu3+发光性能的影响.结果表明:制备的样品为球形纯相四方晶系CaMoO4晶体,在CaMoO4:Eu3+中存在MoO2-4到Eu3+的能量传递.以50;丙酮溶液作为溶剂、PEG添加量为9 mL、Eu3+掺杂浓度为10;、超声时间为10 min时,制备的样品在393 nm光激发下,CaMoO4:Eu3+的最强峰所在位置是616 nm,实现了有效的红光发射,样品在紫外灯下呈现出明亮的红色.     

Eu3+对Ba3La(PO4)3∶Dy3+白光荧光粉发光性能的影响及发光机理的研究

采用高温固相法制备了Ba3La1-x-y(PO4)3∶ xDy3+,yEu3+白光荧光粉,并通过XRD和荧光光谱性能分析手段对样品的物相组成、发光性能和发光机理进行了研究.结果表明:由于Eu3+的掺杂影响了Ba3La(PO4)3∶ Dy3+荧光粉的晶体场环境,在Dy3+的6F9/2能级与Eu3+的5D0能级间发生交叉弛豫,并通过能量共振转移,Dy3向Eu3+传递能量,Ba3La1-x-y(PO4)3∶xDy3+,yEu3+荧光粉在350 nm紫外光激发下同时出现了Dy3+和Eu3+的特征发射,发射光谱中增加了红光成分,改善了色温.实验得出Dy3+和Eu3+掺杂浓度分别为0.08和0.06时,荧光粉的发射光最接近于理想白光.     

Dy3+,Eu3+共掺杂NaLa(WO4)2白色荧光粉的发光性能研究

利用共沉淀法合成了Dy3+、Eu3+共掺杂的NaLa(WO4)2荧光粉,通过扫描电子显微镜、X射线衍射仪、荧光分析仪对荧光粉的性能进行了分析测试.结果表明,在393 nm波长激发下,添加0.188 g的PVP作为表面活性剂,同时控制金属离子浓度在0.06 mol/L时NaLa(WO4)2荧光粉与其他浓度样品比较有较好的发光性能样品呈多孔状,孔大且分布较为均匀,因此调控Dy3+和Eu3+物质的量之比可以对NaLa(WO4)2:Dy3+,Eu3+荧光粉的色坐标进行有效的调节,当Dy3+/Eu3+的掺杂比为1:1时NaLa(WO4)2荧光粉的色坐标为(0.327,0.341)接近标准白光色坐标(0.33,0.33),是有望用于暖白光LED的候选材料.     

FeYO3/Y2O3:1;Eu3+,1;Tb3+粉体的制备及其磁性研究

以FeCl2和KOH为原料采用水热法制备Fe3 O4粉体,然后以氧化钇、氧化铕和氧化铽为原料制备Eu3+,Tb3+共掺杂的Y2 O3荧光粉体,并通过XRD对粉体的物相结构进行分析;然后以三聚氰胺以及所制备的Fe3 O4和Y2 O3:Eu3+,Tb3+粉体为原料,采用微波烧结法在Ar气氛下制备FeYO3/Y2 O3:1;Eu3+,1;Tb3+粉体,并对其磁学性能进行了研究.研究结果表明:当Fe3 O4,Y2 O3:1;Eu3+,1;Tb3+和三聚氰胺比例为1:3:4时,所制备的FeYO3/Y2 O3:1;Eu3+,1;Tb3+粉体的磁力饱和强度为12.299 emu·g-1,磁力最强.     

白光LED用铽铕共掺镓酸锌微晶玻璃的制备、结构与发光性能研究

采用溶胶-凝胶法制备了Tb3+/Eu3+共掺ZnGa2O4微晶玻璃,研究了热处理温度对材料显微结构的影响以及不同稀土离子掺杂材料的发光性能.结果表明干凝胶样品在800～900℃温度热处理后可得到透明的含尖晶石结构ZnGaO4微晶玻璃,在1000℃热处理时由于SiO2非晶基体晶化析出三方Zn2SiO4与六方SiO2晶相导致样品失透.在微晶玻璃中具有ZnGa2O4纳米晶到Tb3+与Eu3+的能量传递.在900℃热处理Tb3+/Eu3+∶ZnGa2O4微晶玻璃样品中,Tb3+与Eu3+分别发射绿光和红光,并与ZnGa2O4纳米晶发射的蓝光组合成近白光发射.     

Tb3+-Eu3+共掺杂2ZnO·2.2B2O3·3H2O的制备和发光性能

采用水热法合成了Tb3+和Eu3+共掺的2ZnO.2.2B2O3.3H2O红色荧光粉。通过固定Eu3+的掺杂浓度为3%(物质的量比:Eu∶Zn=3%),改变Tb3+的掺杂浓度(2%～15%),研究Tb3+掺杂浓度对红色荧光粉晶相结构和光学性能的影响。用X射线衍射和荧光光谱仪对样品的结构和发光性能进行表征,结果表明:随着Tb3+掺杂浓度的升高,样品由晶态向无定形的玻璃态转变;Eu3+的发光强度也逐渐增强;Tb3+与Eu3+之间存在能量传递的过程,且当采用不同的激发波长(220 nm和393 nm)激发时,其能量传递的过程也不一样。     

白光LED用绿色荧光粉Ba3(PO4)2∶Tb3+的发光性能研究

本文采用高温固相法制备出一种绿色荧光粉Ba3(PO4)2∶Tb3+,并通过X射线粉末衍射仪(XRD)和荧光分光光度计对所得荧光粉的结构和光谱性能进行了表征.结果 表明:Ba3(PO4)2体系中掺杂稀土离子Tb3+并没有引起结构的变化;荧光粉Ba3(PO4)2∶Tb3+的激发光谱的主峰位于485 nm,发射光谱的主峰位于548 nm、560 nm和647 rnm;荧光粉Ba3(PO4)2∶Tb3+中Tb3的最佳掺杂浓度为20mol;.由此可见,荧光粉Ba3(PO4)2∶Tb3是可被蓝光LED有效激发的绿色荧光粉.     

单一基质Na2Ca3Si2O8∶Tb3+,Eu3+荧光粉发光性质和能量传递的研究

通过传统的高温固相法成功的制得了一系列紫外激发的硅酸盐荧光粉Na2 Ca3 Si2O8∶Tb3+,Eu3+.X射线衍射(XRD)研究表明所制得的荧光粉为纯相.在Na2Ca3Si2O8∶Tb3+,yEu3+荧光粉体系中,随着Eu3+的掺杂浓度增大,发射光谱中Tb3的特征峰发光强度降低而Eu3+的不断升高,并且荧光寿命不断减小,说明了Tb3+和Eu3之间能量传递方式是交换相互作用,能量传递效率(ET)达到了15.8;.此外,通过CIE色坐标观察到,随着Eu3+浓度的增加,样品从绿色变成黄色,最终变成红色.由于它多彩的颜色变化,所以它是一种用于制作多彩LED的良好材料.     

Eu3+,Tb3+共掺杂的NaGd(WO4)2颜色可调荧光粉的水热合成及发光性质研究

在不添加任何模板剂的情况下,采用温和水热法,制备了一系列NaGd0.96-x(WO4)2:0.04Tb3+,xEu3+(x=0,0.005,0.01,0.02,0.04,0.06,0.08,0.10,0.12,0.14,0.16,0.18)荧光粉.采用X射线粉末衍射仪(XRD)、扫描电子显微镜(SEM)以及荧光分光光度计分别对所得样品的物相结构、形貌粒度及发光性能进行分析表征.结果表明:所合成的样品为NaGd(WO4)2的纯相,属四方晶系白钨矿结构.其形貌为规整的四方盘形,尺寸均一、分散性良好.系列样品均能被近紫外光有效激发,通过改变NaGd(WO4)2中Eu3+/Tb3+的掺杂浓度,实现了对荧光粉发光颜色由绿色到红色的全色调控.     

The structures of three trimethylarsine-boron trihalide adducts: (CH3)3AsBCl3, (CH3)3AsBBr3, and (CH3)3AsBI3

An X-ray structure analysis of three trimethylarsine-boron trihalide adducts has been undertaken. Crystals of (CH₃)₃AsBCl₃ and (CH₃)₃AsBBr₃ are monoclinic with space groupP2₁/m (No. 11) withZ=2 while those of (CH₃)₃AsBI₃ are orthorhombic with space groupPnma (No. 62) withZ=4. For (CH₃)₃AsBCl₃,a=6.497(3) Å,b=10.735(3) Å,c=7.070(2) Å,=111.8(3)°,V=458.4(3) ų,R=0.0343. For (CH₃)₃AsBBr₃,a=6.672(4) Å,b=11.135(7) Å,c=7.199(4) Å,=111.5(1)°,V=497.7(5) ų,R=0.0434. For (CH₃)₃ÅsBI₃,a=13.113(7) Å,b=11.733(5) Å,c=7.387(3) Å,V=1136.5(5) ų,R=0.0329. The As-B bond lengths are 2.065(6), 2.04(1), and 2.03(1) Å, respectively, for the chloride, bromide, and iodide. These and other structural parameters are discussed with reference to previous predictions based on vibrational spectra and previous structural studies on the trimethyl-phosphine and trimethylamine adducts.     

Crystal and molecular structures of three trimethylamine-boron halide adducts: (CH3)3NBCl3, (CH3)3NBBr3, and (CH3)3NBI3

X-ray diffraction data from single crystals of the trimethylamine complexes of the three boron halides, BCl₃, BBr₃, and BI₃, lead to aP2₁/m monoclinic cell containing two molecules for each complex. The unit cell dimensions area = 6·68(1),b = 10·247(3),c = 6·502(6) Å, =116·2(1)° (chloro);a = 6·86(1),b = 10·612(4),c = 6·737(6) Å, = 115·8(1)° (bromo);a = 6·92(2),b = 10·86(1),c = 7·147(6) Å, = 93·9(1)° (iodo). The structures were solved by three-dimensional sharpened Patterson functions and show only the chloro and bromo compounds to be isomorphous. Refinement of 662,718 and 954 observed reflexions for the chloro, bromo and iodo complexes, respectively, using anisotropic thermal parameters yielded conventionalR factors of 0·045, 0·087 and 0·054.The molecules are shown to possess a B—N dative bond, a staggered conformation, and effective 3m (C _3v) symmetry. Average C—N bond lengths are 1·52(1) Å for all three complexes. Boronhalogen bond lengths average 1·864(4), 2·04(2) and 2·28(2) Å, while B—N bond distances are 1·609(6), 1·60(2) and 1·58(3) Å, respectively, for the chloro through iodo compounds. Bond angles are approximately tetrahedral with the C—N—C angle decreasing by several degrees in the Cl Br I series.Based in part on a dissertation submitted by Patty H. Clippard to the Rackham School of Graduate Studies of the University of Michigan, January 1969 in partial fulfillment of the requirements of the Ph.D. Degree.     

Second harmonic generation properties of Ca3(O3C3N3)2 ‐Sr3(O3C3N3)2 solid solutions

Solid solutions of the second harmonic generation (SHG) materials Ca₃(O₃C₃N₃)₂ (CCY) and Sr₃(O₃C₃N₃)₂ (SCY) were prepared via exothermic solid state metathesis reactions from appropriate amounts of the corresponding metal chlorides and potassium cyanate at 525 °C. The change in SHG intensity caused by the successive cation substitution is reported. Differential thermal analyses are used to explore the SCY–K(OCN) phase diagram as a medium for the growth of SCY crystals.     

Growth and characteristic of Sr3Tb(BO3)3 crystal

A new borate single crystal of Sr₃Tb(BO₃)₃ with dimension Ф20×25 mm² has been grown by the Czochralski method. The grown crystal was characterized by DTA–TGA, FTIR and X-ray powder diffraction analysis. The results showed the crystal with [BO₃]^3? is congruently melting at 1351.35 °C which belongs to hexagonal structure. The hardness of Sr₃Tb(BO₃)₃ crystal is 422.5 VDH, and is equal to 5.0 moh. The thermal expansion coefficients were determined to be 2.08×10^?5/°C along (1 0 0) direction and 7.43×10^?6/°C along (0 0 1) direction and the transmission spectrum was measured in 320–1800 nm at room temperature. The magnetic properties of the single crystal were studied which showed its paramagnetism and magnetic anisotropy. The specific Faraday rotation of single crystal was measured at room temperature in 532, 633, and 1064 nm wavelength. The Verdet constants and magneto-optical figures of merit were investigated. The primary emphasis is laid to explore a new magneto-optical material, all the magneto-optical properties of Sr₃Tb(BO₃)₃ are comparing to the ones of TGG.     

Growth and magnetic‐optical properties of Sr3Gd(BO3)3 and Sr3TbxGd1‐x(BO3)3 single crystals

Single crystals of Sr₃Gd(BO₃)₃ (SGB) and Sr₃Tb_xGd_1‐x(BO₃)₃ (TSGB) with dimension Ø 20 mm×20 mm have been grown by Czochralski method. The grown crystals were characterized by X‐ray powder diffraction analysis which showed the crystals belong to hexagonal structure with lattice parameters of a=b=1.254 nm, c=0.926 nm (SGB) and a=b=1.253 nm, c=0.925 nm (TSGB). In TSGB, x=17.7% was obtained by X‐ray fluorometry which showed the segregation coefficient of Tb is closed to 1. The transmission spectrum was measured, which indicated the crystals have high transmittance in 400‐1100 nm region. The Faraday rotation of single crystals at 532 nm wavelength was measured at room temperature. Finally, the Verdet constants were investigated, (SGB) V=17.9 degcm^‐1T^‐1 and (TSGB) V=21.3 degcm^‐1T^‐1. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Tb3+,Yb3+共掺杂LuBO3荧光粉的下转换发光

利用水热法成功合成了近红外量子剪裁荧光粉LuBO3∶15;Tb3+,x; Yb3+(x=0,1,2,4,8,12).通过X射线衍射(XRD)、光致发光谱(PL)、激发谱(PLE)和荧光寿命测试了合成物质的物相结构与发光性质.在286 nm(Tb3+∶7 F6→5D)紫外光激发下,观察到了Tb3∶5D4→7Fj(J=6,5,4,3)可见波段特征发射光和Yb3+:2F5/2→2F7/2的近红外光.研究了Yb3+浓度与激发发射光谱和荧光寿命之间的关系,表明Tb3+和Yb3+之间存在能量传递.当Tb3和Yb3+掺杂摩尔浓度分别为15;和2;时,近红外发射最强.计算得知,其最大下转换量子效率为160.74;.     

3-Methyl-3a,4-Dihydro-3H-Thiochromeno[4,3-c]isoxazol

Abstract  The crystal structure of the title compound, C₁₁H₁₁NOS, was determined by an X-ray diffraction analysis. The compound crystallizes in the monoclinic space group P2₁/c with cell parameters a = 10.533(2) ?, b = 12.7826(19) ?, c = 7.6491(17) ?, β = 107.997(17)^°, V = 979.5(3) ?³ and Z = 4. The S containing heterocycle adopts a sofa conformation, whereas the 5-membered ring adopts an envelope conformation. The crystal packing is characterized by weak C–H···N contacts and π-stacking interactions. Graphical Abstract  The title compound, 3-methyl-3a,4-dihydro-3H-thiochromeno[4,3-c]isoxazol was synthesized by an 1,3 dipolar cycloaddition reaction and its crystal structure determined. Single crystal X-ray diffraction analysis reveals that the aromatic 6-membered ring is planar, whereas the ring containing the S atom adopts a sofa conformation and the 5-membered ring an envelope conformation. The methyl group is in an equatorial position.      

Second harmonic generation in Na3Gd2(BO3)3 crystals

Na₃Gd₂(BO₃)₃ crystals with dimensions up to 22 × 20 × 5 mm³has been grown from NaBO₂ flux by the top‐seeded solution growth (TSSG) method for the first time. Differential scanning calorimetry (DSC) result shows that Na₃Gd₂(BO₃)₃ melts incongruently. The infrared spectrum indicates that Na₃Gd₂(BO₃)₃ contains characteristic triangular [BO₃]^3– groups responsible for the nonlinear optical effect. For the as‐grown crystal, the transmittance exceeds 80% in the wavelength range of 315 nm to 2670 nm, and the UV cutoff wavelength is 207 nm. The damage threshold is 0.47 GW cm^–2 at 1064 nm. Moreover, Na₃Gd₂(BO₃)₃ crystal exhibits an optical second harmonic generation effect which is 1.3 times as large as that of KH₂PO₄ (KDP). (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)