Ca2+、La3+掺杂纳米Y2O3∶Eu3+的超声波制备及光致发光性能

采用超声波作用下的均匀沉淀法制备Ca2 、La3 掺杂的纳米Y2O3∶Eu3 荧光粉.通过正交实验研究掺杂浓度、溶液pH、超声功率、反应时间、干燥温度、煅烧温度等因素对其光致发光(PL)性能的影响,得到制备Ca2 、La3 掺杂纳米Y2O3∶Eu3 的最佳条件.结果表明,超声功率、Eu(NO3)3浓度、尿素体积、氨水浓度、煅烧温度是影响样品PL强度的主要因素.Ca2 、La3 离子单一掺杂效果优于两种元素的复合掺杂,最佳条件下制备的Ca2 、La3 分别掺杂的纳米Y2O3∶Eu3 荧光粉的发光性能均显著优于未掺杂样品.     

纳米Gd_2O_3:Tb~(3+)的多元醇法制备及发光特性

以DEG为溶剂,分别配置一定比例的GdCl_3, TbCl_3作为前驱液,利用多元醇法合成可用于生物探针的Gd_2O_3:Tb~(3+)纳米晶;将一定量的APTES和TEOS加入制备好的溶液中,使得纳米晶Gd_2O_3:Tb~(3+)的表面包裹聚硅氧烷层。本实验通过马尔文粒度仪、 X射线衍射仪(XRD)、场发射扫描电镜(SEM)、透射电镜(TEM)、荧光分光光度计等检测方法研究不同煅烧温度和不同Tb~(3+)掺杂浓度对纳米晶Gd_2O_3的粒径、物相结构、和发光性能的影响。将真空干燥过的纳米晶Gd_2O_3:Tb~(3+)置于马弗炉中分别以600, 800, 1000℃进行煅烧,得到的样品经XRD表征后发现:当煅烧温度为800℃时,得到立方相结构的纳米Gd_2O_3:Tb~(3+)。通过研究不同Tb~(3+)离子掺杂浓度下纳米晶Gd_2O_3:Tb~(3+)的荧光强度表明:当Tb~(3+)离子浓度为5.0%时,纳米晶Gd_2O_3:Tb~(3+)的发射强度最强,尤其是在主发射峰545 nm附近Tb~(3+)的~5D_4→~7F_5能级跃迁峰,其峰值强度比掺杂浓度为2.5%时提高了39%; Tb~(3+)掺杂浓度升高至7.5%时,样品发生了浓度猝灭导致光谱强度下降。     

高分子网络凝胶法合成纳米Sr2CeO4荧光体及其发光性能研究

采用高分子网络凝胶法合成了Sr2CeO4纳米荧光粉. 利用X射线粉末衍射（XRD）、紫外-可见吸收光谱（UV-Vis）、荧光光谱（PL）、透射电镜（TEM）等测试手段对Sr2CeO4的成相过程、发光性能及形貌特征进行了研究. XRD结果表明, 用高分子网络凝胶法合成的样品的晶化温度低于固相法, 但结晶度高于固相法制得的样品（在相同的烧结温度下）, 且所含杂相极少. 透射电镜照片看出样品的颗粒大小比较均匀, 粒径为30～45 nm. Sr2CeO4纳米荧光粉的紫外-可见吸收光谱表明它是一个有效的紫外吸收剂, 有利于它的激发和发射. 发光光谱测试表明, Sr2CeO4纳米荧光粉具有宽带荧光谱, 出现了多个激发峰, 发射主峰位于470 nm, 因而是一种极具前途的荧光材料和发光基质.     

化学共沉淀法制备Sc_2O_3-Y_2O_3-ZrO_2纳米陶瓷粉末及其高温相稳定性

以(ZrOCl2·8H2O、Y(NO3)3·6H2O和Sc2O3为原料,聚乙二醇(PEG)为分散剂,采用化学共沉淀法制备YSZ(yttrium stabilized zirconia)(名义成分为4.5%Y2O3-ZrO2)与Sc-YSZ(名义成分为0.6%Sc2O3-YSZ)2种纳米复合陶瓷粉末(Y2O3和Sc2O3的含量均为摩尔分数),经过压制成形后在不同温度下烧结。通过透射电镜、X射线衍射等对粉末进行表征,研究其高温下相的稳定性。结果表明:前躯体粉末在600℃煅烧2 h后都呈单一的非平衡四方相结构。采用正向滴定法制备的0.6%Sc2O3-YSZ粉末粒径约为30 nm,粉末团聚严重,有许多大的团聚体,反向滴定法制备的0.6%Sc2O3-YSZ粉末粒径约20 nm,粉末团聚少。YSZ在1 200℃烧结100 h后,呈平衡四方相,并有立方相产生在1 300℃烧结100 h后,平衡四方相不稳定,产生立方相和少量单斜相;在1 400℃烧结100 h后,四方相全部转变为单斜相和立方相。而Sc-YSZ粉体在1 200、1 300和1 400℃下烧结100 h后都始终保持单一的非平衡四方相结构。因此在YSZ中添加少量Sc2O3可提高其相的稳定性。     

燃烧法合成稀土纳米长余辉发光材料SrO·xAl2O3:Eu2+,Dy3+

应用燃烧法在空气中较低的温度(<900℃)下成功地合成了SrO·xAl2O3∶Eu2+,Dy3+稀土纳米长余辉发光材料,并研究了炉温、反应物中铝锶比、助溶剂和可燃物等对发光材料性能的影响。研究结果表明,反应物置于温度为600℃的高温炉中时燃烧得到的产物性能最好,发光粉的粒径在70nm左右,发射光谱的最大波长在520nm左右。与其它合成方法相比,该方法具有合成温度低、反应时间短,获得的产物疏松、硬度小、粒度小等优点。     

水热-还原法合成球形Gd_2O_2S:Pr~(3+)闪烁体粉末

采用Gd2O3、Pr6O11、H2SO4和尿素为实验原料,通过水热-还原法合成了Gd2O2S:Pr3+闪烁体粉末。利用X射线衍射(XRD)、红外光谱(FT-IR)、热重分析(DTA-TG)、扫描电子显微镜(SEM)和光致发光(PL)光谱等手段对合成的粉末进行了表征。研究表明尿素与Gd2(SO4)3的摩尔比(m)对前躯体的物相组成和形貌有很大影响,最佳的m值为2.5。最佳的前躯体在流动的90%Ar+10%H2气氛中800℃煅烧1 h能转变成单相的Gd2O2S粉末。所获得的Gd2O2S粉末呈球形,分散性良好,粒径尺寸约为1μm。在307 nm的紫外光激发下,Gd2O2S:Pr3+闪烁体粉末的主发射峰位于516 nm,归属于Pr3+的3P0-3H4跃迁。在Gd2O2S基质中,Pr3+的猝灭浓度为1%(摩尔分数),猝灭机理为电偶极-电四极相互作用引起的。     

Dy2O3纳米颗粒的制备及其光学特性

以四水碳酸镝(Dy_2(CO_3)_3·4H_2O)为镝源,Dy_2(CO_3)_3·4H_2O在空气中热重-热差(TGDTA)分析为依据,利用X射线衍射仪(XRD)、扫描电镜(SEM)和紫外-可见分光光度计(UVVis)分别表征了Dy_2(CO_3)_3·4H_2O在空气中热分解产物的物相、形貌和光学特性。研究结果表明,Dy_2(CO_3)_3·4H_2O在空气中的热分解过程主要分为两个阶段,第一阶段是在室温～285℃之间Dy_2(CO_3)_3·4H_2O失去结晶水变为Dy2(CO3)3,第二阶段是在285～700℃范围内Dy2(CO3)3经过受热分解生产了Dy_2O_3,在700℃下保温15 min获得了Dy_2O_3纳米颗粒。Dy_2O_3纳米颗粒具有较强的光吸收能力。此外,在波长为300～400 nm的范围内,Dy_2O_3纳米颗粒具有较宽的光吸收带。     

低温燃烧法合成白光LED用新型红色荧光粉SrMoO_4:Pr~(3+)及其发光性质

以硝酸锶、七钼酸铵、氧化镨为原料,采用低温燃烧法合成白光发光二极管(white light emitting diode,简称WLED),用新型红色荧光粉SrMoO4:Pr3+,并研究其光谱性质。结果表明,SrMoO4:Pr3+激发光谱中Pr3+在449 nm处有一最强3H4--3P0激发峰,其激发范围与蓝光LED芯片相匹配,能被蓝光有效激发;发射光谱在644nm处有最强峰,属于Pr3+的3P0--3F2跃迁,发红光,说明SrMoO4:Pr3+荧光粉是1种潜在的白光LED用蓝光激发的红色荧光粉。同时还研究了燃烧温度、尿素用量、稀土Pr3+掺杂量对荧光粉发光强度的影响,得出制备SrMoO4:Pr3+的最佳条件为:燃烧温度600℃,尿素用量为理论尿素用量的3倍,稀土Pr3+离子掺杂摩尔分数为2%。     

α-Fe2O3纳米颗粒的水热法合成及其光吸收特性

以硝酸铁为铁源、以氢氧化钠溶液(或浓氨水)为沉淀剂,在不同条件下,利用水热法合成α-Fe2O3纳米颗粒.用X射线衍射(XRD)、透射电子显微镜(TEM)和紫外可见分光光度计(UV-VIS)对试样进行分析.结果表明:用氢氧化钠溶液作沉淀剂比用浓氨水作沉淀剂更有利于α-Fe2O3颗粒粒径变小,反应温度升高更有利于α-Fe2O3颗粒粒径细化.以氢氧化钠溶液作沉淀剂,在240℃下反应24 h,获得粒径小于20 nm的α-Fe2O3颗粒.不同条件下水热法合成的α-Fe2O3的紫外可见光吸收光谱表明:随着α-Fe2O3颗粒粒径变小,颗粒对光的屏蔽程度增大;特别是当α-Fe2O3颗粒粒径小于20 nm时,它对光完全屏蔽.     

用于白光LED的荧光粉Sr3MgSi2O8:Eu2+的发光特性

使用高温固相法制备不同NH4Cl(作为助熔剂)加入量和不同Eu2+浓度的Sr3MgSi2O8:Eu2+,并研究其成相和发光性质.研究结果表明:NH4Cl加入量为24%时,样品为纯相,发光最强.Sr3MgSi2O8:Eu2+样品在近紫外区存在强激发带(250～400 nm),谱峰位于366 nm相应的发射谱带位于蓝光区(420～500nm),为一个不对称宽带,谱峰位于457 nm,该发射带由两个发射峰组成,其位置较接近,因此不能复合出白光,Sr3MgSi2O8:Eu2+仅适合作为紫外LED芯片激发的蓝光荧光粉.     

Photoluminescent properties of LaF3：Eu^3＋ and GdF3：Eu^3＋ nanoparticles prepared by co-precipitation method

LaF₃:Eu³⁺ and GdF₃:Eu³⁺ nanoparticles were prepared by a co-precipitation method in the presence of the chelating agent, citric acid. The structural properties of the products were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The average crystallite size was estimated from the full-width at half-maximum (FWHM) of the diffraction peaks by the Scherrer equation. The sizes of the nanoparticles were 12 nm for LaF₃:Eu³⁺ and 17 nm for GdF₃:Eu³⁺. The luminescent properties of the nanoparticles were investigated by excitation and emission spectra. Energy transfer from Gd³⁺ to Eu³⁺ was observed.     

Sol-gel synthesis and photoluminescence properties of BaSO_4/Y_2O_3:Eu~(3+) core-shell submicrospheres

Europium-doped nanocrystalline Y2O3 phosphor layers were coated on the surface of preformed submicron BaSO4 spheres via the sol-gel process.The obtained BaSO4/Y2O3:Eu3+ core-shell phosphors were characterized by X-ray diffraction(XRD),scanning electron microscopy(SEM),transmission electron microscopy(TEM),energy dispersive spectroscopy(EDS) and photoluminescence spectra.The results showed that the obtained BaSO4/Y2O3:Eu3+ core-shell phosphors consisted of well-dispersed submicron spherical particles with na...     

Influence of annealing temperature on luminescent properties of Eu~(3+)/V~(5+) co-doped nanocrystalline Gd_2Ti_2O_7 powders

Nanosized Gd2(1-x)Eu2xTi2O7:yV5+ phosphors were prepared via sol-gel method and characterized with X-ray diffraction,Raman spectroscopy,diffuse reflectance spectra and photoluminescence spectra.Their PL properties were investigated as functions of the Eu3+ doping concentration and annealing temperature.The results indicated that the as-prepared samples showed a strong emission of Eu3+ under the irradiation of 303 nm.For Eu3+-doped Gd2Ti2O7,the orange emission at 586 nm was the strongest,which was correspond...     

Gd_2O_3-Yb_2O_3-Y_2O_3-ZrO_2热障涂层材料及涂层性能研究

使用化学共沉淀法合成了纳米Gd2O3-Yb2O3-Y2O3-ZrO（2GYYZO）粉末,并最终制备了超细晶团聚的多元稀土氧化物掺杂的GYYZO热喷涂粉末,系统的研究了材料及涂层的基本性能,重点研究了材料及涂层的高温稳定性,材料和涂层的高温相稳定性相对传统纳米8YSZ材料明显提高,对高温热处理过程中涂层孔隙收缩、晶粒长大...     

Luminescent properties of MMgP_2O_7：Eu~（3＋）（M=Ca,Sr,Ba） phosphor

A series of red phosphors Eu3+-doped MMgP2O7(M=Ca,Sr,Ba) were synthesized by solid-state reaction method.X-ray powder diffraction(XRD) analysis confirmed the formation of pure CaMgP2O7,SrMgP2O7 and BaMgP2O7 phase.Photoluminescence spectra of MMgP2O7(M=Ca,Sr,Ba):Eu3+ phosphors showed a strong excitation peak at around 400 nm,which was coupled with the characteristic emission(350-400 nm) from UV light-emitting diode.The CaMgP2O7:Eu3+,SrMgP2O7:Eu3+ and BaMgP2O7:Eu3+ phosphors showed strong emission bands peaking at 612,593 and 587 nm,respectively.Due to the difference of the ion sizes between Ba2+(0.142 nm),Sr2+(0.126 nm),Ca2+(0.112 nm),Mg2+(0.072 nm) and Eu3+(0.107 nm),Eu3+ ions were expected to substitute for different sites in CaMgP2O7,SrMgP2O7 and BaMgP2O7 lattice.     

Preparation and luminescent properties of CaAl_2O_4:Eu~(3+),R~+(R=Li,Na,K) phosphors

CaAl2O4:Eu3+,R+(R=Li+,Na+,K+) red phosphors were synthesized by solid state reaction method.X-ray diffraction(XRD) and photoluminescence(PL) were employed to characterize their structural and luminescent properties.It was found that the optimal sintering temperature and sintering time were 1200 °C and 4 h,respectively.The optimal concentration of doped Eu3+ was 3 mol.%.Furthermore,under ultraviolet excitation with a wavelength of 254 nm,these samples showed red luminescence which were probably attributed to the transitions from 5D0 excited state to 7FJ(J=0-4) ground states of Eu3+ ions.The feature and the high intensity of hypersensitive transition from 5D0→7F2 indicated that Eu3+ preferred to occupy a low symmetry site.The incorporation of alkali metal ions greatly enhanced the luminescence intensity probably due to the influence of charge compensation of alkali metal ions.     

Hydrothermal synthesis and luminescence properties of YW2O6（OH）3：Tb^3＋ green phosphors

YW2O6(OH)3:Tb3+ green phosphors were synthesized at different pH values via a facile hydrothermal method. The structure and optical properties of as-synthesized samples were studied by X-ray diffractometer (XRD), scanning electron microscopy (SEM), photolumi-nescence spectra and luminescence decay curve. The results showed that pure monoclinic YW2O6(OH)3:Tb3+ green phosphors could be ob-tained at pH 2-5. Uniform spherical micro-phosphors of ~5 μm in diameter with narrow size distribution could be prepared at pH 5. pH value had dramatic influence on morphologies, which could be ascribed to the various spatial configurations of different poly-tungstates existing at different pH values. The emission spectra under 261 nm excitation exhibited dominant green emission at 546 nm. The green emission inten-sity reached the maximum value at pH 5 due to the high packing density of the obtained phosphor.     

Promising red phosphors LaNbO4:Eu3+,Bi3+ for LED solid-state lighting application

La0.75NbO4:Eu3+0.25 and La0.65NbO4:Eu3+0.25,Bi3+0.10 phosphors were synthesized by solid-state reaction method,and their photoluminescence properties were discussed in detail.With the increased incorporation of the co-activator Bi3+,the charge transfer(CT) bands of Nb5+→O2-and Eu3+→O2-(-280 nm) weakened and a new and significant broad band Bi3+-O2-(-330 nm) appeared,while the peaks at 395 and 466 nm assigned to f-f transitions of Eu3+ was slightly changed.Compared with the commercial phosphor Y2O2S:0.05Eu3+...     

Citrate sol-gel combustion preparation and photoluminescence properties of YAG:Ce phosphors

Yellow-emitting YAG:Ce3+ nanocrystalline phosphors were prepared by citrate sol-gel combustion method using citric acid as the fuel and chelating agent. The influence of mole ratio of citric acid to metallic ions (MRCM), pH value of the solution, calcination temperature and Ce-doped concentration on the structures and properties of as-prepared powders were investigated in detail. Higher crystallinity and better luminescence performance powders were obtained at MRCM=2, pH=3 and the calcination temperature of 1200 °C. The phosphors exhibited the characteristic broadband visible luminescence of YAG:Ce. The optimum concentration of Ce3+ was 1.0 mol.%, and the concentration quenching was derived from the reciprocity between electric dipole and electric quadrupole (d-q). Especially, the pH value of the solution was a key factor to obtain a stable sol-gel system and then obtain pure and homogeneous rare earth ions doped YAG phosphors at a lower tem-perature. The Y3Al5O12:Ce0.03 phosphor with optimized synthesis-condition and composition had a similar luminescence intensity with the commercial phosphor YAG:Ce.