Synthesis and Characterization of Cerium-Doped Lutetium Aluminum Garnet Phosphors by Nitrate-citrate Sol-Gel Combustion Process

Nanosized cerium-doped lutetium aluminum garnet （LuAG：Ce） phosphors were prepared by nitrate-citrate solgel combustion process using 1：1 ratio of the citrate：nitrate. The prepared LuAG：Ce phosphors were characterized by XRD, TEM, photoluminescence and radioluminescence spectra excited by UV and X-ray, respectively. The purified crystalline phase of LuAG：Ce was obtained at 900 ℃ by directly crystallizing from amorphous materials. The resultant Lu- AG：Ce phosphors were uniform and had good dispersivity with an average particle size of about 30 urn. Both photoluminescence and radioluminescence were well-known Ce^3＋ emissions located in the range of 470 -600 nm consisting of two emission bands because of the transition from the lowest 5d excited state （2D） to the 4f ground state of Ce^3＋, which matched well with the sensitivity curve of the Si-photodiode. There was a little red shift for the emission components from the UV-excited emission spectrum to the X-ray-excited emission spectrum. The fast scintillation decay component of 26 ns satisfies the requirements of fast scintillators.     

Spectroscopy of Pr^3＋4f5d Configuration in LaF3 Nanocrystals／Oxyfluoride Glass Ceramics

Theinterestofinvestigatingthe 4fn -15delectronicconfigurationofthetrivalentrareearth (RE)ionsisbasedonavarietyofapplicationsinthevacuumultra violet (VUV)regionofthespectrum ,suchasthede velopmentofplasmadisplaypanelsandmercury freefluorescenttubes[1] .Amo…     

Preparation and Characterization of Red Luminescent Ca0.8Zn0.2TiO3: Pr3+, Na+ Nanophosphor

Nanophosphor with the nominal composition of Ca0.8Zn0.2TiO3∶Pr3 , Na (CZTOPN) was synthesized at relatively low temperature by the sol-gel method. Metal ions were dispersed by citric acid in ethylene glycol solvent and then react with Ti(OC4H9)4 to form sol and gel. The decomposition process of the precursor, and crystallization and particle size of CZTOPN were examined by thermal analysis (TG-DSC), powder X-ray diffraction (XRD), and scan election microscopy (SEM). Results of TG-DSC and XRD reveal that the composition of Ca0.8Zn0.2TiO3∶Pr3 , Na changes with the sintering temperature. SEM data indicate that the diameter of particles is under 50 nm even if the sintering temperature increases to 1000 ℃. In contrast to a solid state reaction, the excitation spectra of samples synthesized by the sol-gel method shift blue about 10 nm and the emission intensity at 617 nm increases significantly.     

Luminescence Properties of Tb^3＋ -Doped LuAG Films Prepared by Pechini Sol-Gel Method

Lu3Al5O12（LuAG） thin films with different Tb^3＋ concentration were prepared on carefully cleaned （111 ） silicon wafer by a Peehini process and dip-coating technique. Heat treatment was performed in the temperature range from 800 to 1100 ℃. The crystal structure was analyzed by XRD. The results show that LuAG film starts to crystallize at about 900 ℃, and the particle size increases with the sintering temperature. Excitation and emission spectra of Tb^3＋ doped LuAG films were measured. The effects of heat-treatment temperature and doping concentration of Th3 ＋ on the luminescent properties were also investigated. For a comparison study, Th^3＋-doped LuAG powders were also prepared by the same sol-gel method.     

Influence of In3＋ ions concentration on spectroscopic properties of Ho：LiNbO3 crystals

In:Ho:LiNbO3 crystals doped with various concentrations of In3+(0, 1 mol.%, 3 mol.%, 5 mol.%), fixed concentrations of Ho3+ (1 mol.%) were grown by Czochralski method. The X-ray powder diffraction, infrared and UV-visible absorption spectra were measured and modified. Judd-Ofelt approach was employed to study the effect of In doping on spectroscopic properties of Ho:LiNbO3 crystals. In concentrations in crystals were analyzed by an inductively coupled plasma optical emission spectrometry (ICP-OE/MS). For In (3 mol.%):Ho (1 mol.%):LiNbO3 crystal, the obtained intensity parameters were: Ω2=9.6563, Ω4=4.2195, Ω6=14.1526. The results showed that the Ω2 and Ω6 parameters increased with the increase of In3+ concentration. When the In doping concentration was up to 5 mol.%, Ω2 and Ω6 suddenly decreased. In2O3 incorporation had a strong effect on the radiative lifetime, but had less influence on fluorescence branching ratios. The effective distribution coefficient of In3+ in In:Ho:LiNbO3 crystals was less than 1 and increased with increasing concentration of In3+ in the melt.     

Ni-Al_2O_3粉末注射成形喂料的流变学研究

采用HAAKE Poly Lab QC转矩流变仪的密炼模块,制备了粉末装载量为55%(体积分数),粘结剂配方(质量分数)为60%石蜡+35%低密度聚乙烯+5%硬脂酸的不同Ni含量的Ni-Al_2O_3喂料,并在130℃、140℃、150℃条件下通过MLW-400型毛细管流变仪对其进行黏度测定,通过MATLAB曲线拟合、回归参数的方法确定了喂料的幂率指数与黏流活化能。结果表明:Ni含量的变化对幂率指数n影响较小,说明粘结剂配方合理,喂料的均匀性好;但是随着Ni含量的增加,喂料对温度的敏感性增强。实验结果为粉末注射成形制备Ni-Al_2O_3复合材料提供了流变学参考,从而为研究不同Ni含量对Al_2O_3陶瓷性能的影响奠定基础。     

Photoluminescence Characteristics of Gd2Mo3O9 ： Eu Phosphor Particles by Solid State Reaction Method

Eu^3＋-doped Gd2Mo3O9 was prepared by solid-state reaction method using Na2CO3 as flux and characterized by powder X-ray diffractometry. According to X-ray diffraction, this material belonged to a tetragonal system with space group I41/α. The effects of flux content and sintering temperature on the luminescent properties were investigated with the emission and excitation spectra. The results showed that flux content and sintering temperature had effects on the luminescent properties, the optimized flux content and the best temperature was 3 % and 800 ℃ respectively. The excitation and emission spectra also showed that this phosphor could be effectively excited by C-T band （280 nm）, ultraviolet light 395 nm and blue light 465 nm. The wavelengths at 395 and 465 nm were nicely fitting in with the widely applied output wavelengths of ultraviolet or blue LED chips. Integrated emission intensity of Gd2Mo3O9 ： Eu was twice higher than that of Y2O2S ： Eu^3 ＋ under 395 nm excitation. The Eu^3＋ doped Gd2Mo309 phosphor may be a better candidate in solid-state lighting applications.     

Controlled synthesis and tunable luminescence of NaYF₄:Eu³⁺

High quality NaYF4:Eu3+ luminescent materials were successfully synthesized via a facile template technique by hydrothermal method.The samples were characterized by X-ray powder diffraction(XRD),transmission electron microscopy(TEM) and fluorescence spectroscopy(FS).The incorporating of Eu3+ ions into NaYF4 crystal lattice influenced the symmetry types of NaYF4 crystals,resulting in phase transformation of NaYF4 crystals between α and β phase.The pure hexagonal phase of branched NaYF4:Eu3+ was obtained as the Eu3+ concentration reached 15 mol.%.In addition,the luminescence color was tuned by changing the doping concentration of Eu3+ ions.     

Preparation of Neodymium-Doped Yttrium Aluminum Garnet Transparent Ceramics by Homogeneous Precipitation Method

Neodymium-doped yttriumaluminumgarnet(Nd∶YAG)transparent polycrystalline ceramics,laser ce-ramic matrix materials,are gradually becomingsubsti-tutes for single crystals because they are provided withpredominantly chemical stability,highly doped ionconcentration,excellent optical performance and hightemperature stability[1,2].Presently,the conventionallyused methods to produce Nd∶YAG powders are solid-state processes[3],chemical precipitation methods[4,5]andlowtemperature combustiontechniqu…     

Luminescent properties of Ba3Gd（BO3）3：Eu^3＋ phosphor for white LED applications

Luminescent material Ba3Gd(BO3)3 doped with Eu3+ ion was prepared by high temperature solid-state method. The preparing conditions, luminescent properties, and particle morphology of Ba3Gd(BO3)3:Eu3 + phosphor were studied with X-ray diffraction (XRD), fluorescence spectroscopy, and scanning electron microscopy (SEM). The results obtained by XRD showed that pure phase of Ba3Gd(BO3)3 was obtained at 1000℃. Images from SEM displayed that the particles of Ba3Gd(BO3)3:Eu3+ phosphor had a spherical shape with an average diameter of about 200-400 nm. The luminescence spectra showed that Ba3Gd(BO3)3:Eu3+ phosphor was effectively excited by the near ultraviolet (UV) light (396 nm) and blue light (466 nm). The main emission peaks of Ba3Gd(BO3)3:Eu3+ phosphor were assigned to the supersensitive transition 5D0-7F2 (611 and 616 nm) of Eu3+ ion when samples were excited at 255 and 396 nm, respectively, and the luminescent intensity of Ba3Gd(BO3)3:Eu3+ at 611 and 616 nm reached to the maximum when the doped content of Eu3+ ion was 10mol.%. Therefore, this phosphor could be a promising red component for possible applications in the field of white LED.     

Effects of Annealing Treatments on Luminescence and Scintillation Properties of Ce：Lu3 Al5 O12 Crystal Grown by Czochralski Method

Lu3Al5O12 single crystals grown in pure N2 atmosphere by Czochralski method were annealed in oxidizing atmosphere （air）and reducing atmosphere （H2 ＋ N2）, respectively. Effects of annealing treatments on luminescence and scintillation properties of the crystals were investigated. The crystal annealed in air showed the highest luminescence intensity under blue light or vacuum ultraviolet excitation in comparison with that annealed in reducing flux or the as-grown crystal. Under X-ray excitation, crystal annealed in reducing atmosphere had the lowest light yield, and crystal annealed in air had the fastest decay time under ^137Cs 662 keV γ-ray excitation. Different annealing treatments resulted in different luminescence and scintillation properties, which might related with oxygen vacancies or defect existing in the crystals.     

Synthesis and luminescent properties of Ce~(3+) doped LuAG nano-sized powders by mixed solvo-thermal method

Polycrystalline LuAG:Ce3+(cerium3+-doped lutetium aluminum garnet) powders were prepared by mixed solvo-thermal method.Fourier-transform IR spectroscopy(FTIR) and X-ray diffraction(XRD) measurements showed that the precursors were ethanol derivatives AlO(OH) crystal with hydroxyl and carbonate group.XRD results showed that phase of Lu2O3 disappeared with the precursors were annealed at 400 °C,cubic phase LuAG:Ce3+ appeared but only one diffraction peaks of LuAP(LuAlO3) at calcination temperature to 700 °C,and the purified crystalline phase of LuAG:Ce3+ was obtained at 1000 °C.The scanning electron microscopy(SEM) analysis revealed that the synthesized LuAG:Ce3+ powders were uniform and had good dispersivity with an average particle size about 100 nm.Excitation and emission spectra of Ce3+ doped LuAG phosphors were measured.Many factors of affecting the intensity of emission spectra were discussed.     

微波消解-电感耦合等离子体质谱法测定氟化铈中13种稀土杂质

准确称取0.10 g(精确至0.000 1 g)待分析样品于微波消解罐中,加入3 mL盐酸,将微波消解仪由室温升温到120 ℃并保持5 min,再继续升温到180 ℃并保持15 min进行微波消解,以10 ng/mL Cs溶液为内标,建立了电感耦合等离子体质谱法(ICP-MS)测定氟化铈中13种稀土杂质(La、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu)含量的方法。实验表明,13种稀土杂质的线性范围为1.0~100 ng/mL,线性相关系数均不小于0.999 5,方法的检出限为0.002～0.050 μg/g。用所建立方法测定氟化铈粉末样品中La、Pr、Nd、Sm、Gd的结果与电感耦合等离子体原子发射光谱法(ICP-AES)基本一致。将方法应用于氟化铈粉末样品中13种稀土杂质的分析,相对标准偏差(RSD, n=7)均小于5.0%,加标回收率为95%~105%。     

Electrospinning synthesis and luminescent properties of Lu₂O₃:Eu³⁺ nanofibers

One-dimensional Lu2O3:Eu3+ nanofibers were prepared by electrospinning followed by high-temperature calcinations.Thermogravimetric and differential thermal analysis,X-ray powder diffraction,Fourier transform infrared spectroscopy,scanning electron microscopy,photoluminescent spectra and decay curves were used to characterize the samples.Results showed that samples began to crystallize at ～500 oC and crystallized completely around 1000 oC.The average diameter of nanofibers(1000 oC annealed) was about 55 nm and the particle size of Lu2O3:Eu3+ increased with increasing annealing temperature.Under ultraviolet excitation,nanofibers exhibited typical red emission of Eu3+ in Lu2O3.The effect of heat-treatment temperature on luminescent properties of nanofibers was also discussed.     

Optimization of BaMgAl₁₀O₁₇:Eu²⁺ phosphors by the substitution of Si-N bonds for Al-O bonds

We proposed a simple method to improve the thermal stability of BaMgAl10O17:Eu2+(BAM) phosphors by the substitution of Si-N bonds for Al-O bonds in the host lattice.Both photoluminescence properties and thermal stability under ultraviolet(UV) and vacuum ultraviolet(VUV) excitation could be significantly improved through Si-N incorporation.After thermal degradation at 600 °C for 1 h in air atmosphere,the Si-N doped sample(Ba0.88Eu0.12MgAl9.97Si0.03O16.97N0.03) had the highest emission intensity which was 22% and 40% stronger than that of as-received sample under UV and VUV excitation,respectively.This could be attributed to the stable local structure surrounding the Eu2+ ions and the lower electronegativity of nitrogen.     

Enhancement of luminescence and afterglow in Ca0.8Zn0.2TiO3:Pr3+ by Nb5+ substitution for Ti4+

Nb5+ doped Ca0.8Zn0.2TiO3:Pr3+ red long afterglow phosphors were synthesized by solid-state reaction methods. X-ray diffraction, photoluminescence spectroscopy and thermally stimulated spectrometry were used to investigate the effects of Nb5+ content on the crystal characteristics and luminescent properties of Ca0.8Zn0.2Ti1-xNbxO3:Pr3+ phosphors. The results showed that the addition of a small quantity of Nb5+ had negligible effect on the crystal characteristics of Ca0.8Zn0.2Ti1-xNbxO3:Pr3+, but it could change the trapping parameters (the depth of trap, frequency factors and the concentration of trapped charges at t=0) of Ca0.8Zn0.2Ti1-xNbxO3:Pr3+ phosphors, and then led to the enhance-ment of red fluorescence and phosphorescence at 612 nm originating from 1D2→3H4 transition of Pr3+. Both of the red fluorescence intensity and afterglow time reached the largest values in the sample of Ca0.8Zn0.2Ti1-xNbxO3:Pr3+ with x=0.05. The afterglow time of Ca0.8Zn0.2Ti0.95Nb0.05O3:Pr3+ phosphors lasted for over 24 min (≥1 mcd/m2) when the excited source was cut off.     

低温燃烧法制备Ce_(0.8)Sm_(0.2)O_(1.9)电解质固溶体及其烧结性能的研究

采用柠檬酸–硝酸盐低温燃烧合成法,以Ce(NO_3)_3·6H_2O为氧化剂,柠檬酸为还原剂,制备Sm_2O_3掺杂的Ce_(0.8)Sm_(0.2)O_(1.9)(SDC)超细粉体,利用XRD、TG-DSC、FT-IR、SEM及FESEM等手段对制备样品的晶相结构、热分解过程、微观形貌以及团聚情况进行研究.结果表明:柠檬酸与硝酸盐组成的干凝胶自蔓延燃烧点火温度为270.0℃;粉体经600℃焙烧2 h后,形成了单一立方萤石型结构的固溶体,平均晶粒度为18.80 nm.粉体的结晶性能完善,分散性能良好,粒子间仅有微弱的软团聚.将素坯在1 250℃烧结2 h,即可得到相对密度为95.5%的陶瓷烧结体.     

Synthesis and Luminescent Properties of GdAlO3:RE by Combustion Process

Pure GdAlO3: RE (RE = Eu, Pr or Tb) crystalline phase was formed at 900 ℃ with the precursor prepar by nitric-citric combustion process. The synthesis process was studied by XRD, TG-DSC and IR spectra. The analysis results show that there are three main stages in combustion process: ( 1 ) water evaporation and organic compound pyrolysis; (2) combusting reaction; (3)pure crystal formation. GdAlO3: RE powder shows good luminescent properties under 254 nm excitation and was proved to be a good kind of phosphors.     

Infrared to ultraviolet upconversion luminescence in Nd3+ doped nano-glass-ceramic

Nd3+ doped transparent oxyfluoride glass ceramic containing β-YF3 nanocrystals was prepared and the upconversion luminescence behaviors of Nd3+ in the precursor glass and glass ceramic were investigated. Under 796 nm laser excitation, ultraviolet upconversion emissions of Nd3+ ions at 354 nm (4D3/2→4I9/2) and 382 nm (4D3/2→4I11/2) were observed at room temperature. Power dependence analysis demonstrated that three-photon upconversion processes populated the 4D3/2 excited state. In comparison with those of the precursor glass, the ultraviolet emissions were enhanced by a factor of 500 in the glass ceramic, which was attributed to the change in the ligand field of Nd3+ ions and the decrease in phonon energy because of the partition of Nd3+ ions into the β-YF3 nanocrystals after crystallization.     

Up-conversion luminescence of Er~（3＋）-doped and Yb~（3＋）/Er~（3＋） co-doped 12CaO·7Al_2O_3 poly-crystals

The optical properties of Er3+-doped and Yb3+/Er3+ co-doped 12CaO·7Al2O3 (C12A7) poly-crystals, synthesized by high temperature solid state method, were investigated in detail. For Er3+-doped and Yb3+/Er3+ co-doped C12A7 poly-crystals, two main emission bands centered around 530/550 nm (green) and 660 nm (red) were observed under 980 nm diode laser excitation via an up-conversion process. The intensity of green up-conversion emission had a strong increase in Er3+ (1.0 mol.%, 1.5 mol.%, 3.0 mol.%), and the intensity ratio of red to green up-conversion emission had an increase in Yb3+ (1.0 mol.%, 2.0 mol.%, 10. 0 mol.%)/Er3+ (fixed at 1.0 mol.%). This detailed study of the up-conversion processes allowed us to identify the dominant up-conversion mechanisms in Er3+-doped and Yb3+/Er3+ co-doped C12A7 poly-crystals.