Three-color upconversion luminescence of rare earth codoped oxyhalide tellurite glasses

The red, green, and blue upconversion properties of Er^3＋/Tm^3＋/Yb^3＋-codoped oxyhalide tellurite glasses were studied under 980 nm LD excitation. The intense red （657 nm）, green （530 and 545 nm）, and blue （476 nm） emissions were simultaneously observed at room temperature. The results showed that the mixed halide modified tellurite glass （TZFCB） had strong upconversion emissions. The effect of halide on upconversion intensity was observed and discussed, and possible upconversion mechanisms were evaluated. The intense red, green, and blue upconversion luminescence of Er^3＋/Tm^3＋/Yb^3＋-codoped oxyhalide tellurite glasses might be a potentially useful material for developing three-dimensional displays applications.     

Preparation and characterization of NaYF_4:Er~(3+),Tm~(3+)@NaYF_4:Ce~(3+),Tb~(3+) microcrystals with dual-mode emissions at the single-particle level

Under hydrothermal environment,we synthesized lanthanide ions doped sodium yttrium fluoride(NaYF_4:Er,Tm@NaYF_4:Ce,Tb) luminescent microcrystals via an epitaxial growth technique.The structure and morphology of these microcrystals were examined by SEM,TEM,EDS and XRD measurements.These particles show dual-mode emissions with red upconversion(UC) and green down conversion(DC) as single particles level.The mean length and diameter of these microparticles increase from 0.43 to2.26 μm and from 1.33 to 1.86 μm,respectively.Most interestingly,the photoluminescence properties of NaYF_4:Er,Tm@NaYF_4:Ce,Tb phosphor crystals are highly dependent on the crystallite size.The microcrystals fluoresce emit dual-mode emissions when they are solid or dispersed in solvents.Benefiting its intensive fluorescence and uniform morphology,these materials hold great potential for security and anti-counterfeiting applications.     

Rate equation model analysis on the infrared and upconversion emission of Er/Yb co-doped borate-silicate glass

Er/Yb co-doped borate-silicate glasses with various Yb concentrations were fabricated by high-temperature solid-reaction method.The photoluminescence spectra around 1.55 μm and the visible upconversion spectra were measured.The radiative lifetime of Er-4I13/2,com-pared with the measured one,was obtained by Judd-Ofelt theory based on the absorption spectra.A rate equation model for Er/Yb co-doped system has been established based on the data obtained from the measurements,including the absorption and emissio...     

电感耦合等离子体原子发射光谱法测定镝铁电解粉尘中15种稀土元素

用硝酸和氢氟酸溶解试样,高氯酸冒烟除氟,在硝酸介质中用电感耦合等离子体原子发射光谱法(ICP-AES)测定了镝铁电解粉尘中La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu、Y 15种稀土元素。为了提高高含量元素的测定准确度,在测定基体元素Dy时,采用铟作内标;为了消除基体效应对稀土杂质元素测定的影响,采用基体匹配的校准曲线。镝铁电解粉尘中铁含量很低(铁的质量分数不超过1%),对测定没有影响。实验方法测定了一镝铁电解粉尘样品,结果表明,La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Ho、Er、Tm、Yb、Lu和Y 14个稀土杂质元素测定值与ICP-MS的测定值基本一致,镝和14个稀土元素的合量与重量法测得的稀土总量吻合。     

ICP-AES法测定镝铁合金中稀土杂质

研究了以ICP-AES法测定镝铁合金中稀土杂质,采用基体匹配和光谱拟合技术消除基体光谱干扰,分析范围,La、Ce、Pr、Nd、Sm、Eu、Tm、Yb、Lu:0.0050％～0.50％,Gd、Tb、Ho、Er、Y:0.010％～0.50％,精密度RSD为0.40％～10.32％.对不同含量样品,经与等离子质谱法对照,结果吻合.     

NaYF4:Yb,Er材料的制备及其上转换发光性能

通过沉淀法制备Yb3+和Er3+共掺的NaYF4上转换发光材料,考察了主要制备工艺条件对材料上转换发光性能的影响,并探讨了其上转换发光的机理。利用x射线衍射(XRD)、透射电镜(TEM)、荧光光谱仪对样品进行了表征。结果表明,Yb3+和Er3+的掺杂浓度分别15%(摩尔分数,下同)、3%,焙烧温度为600℃时可得到发光性能较好的六方相NaYF4:Yb,Er上转换材料,其主要上转换途径是Yb3+和Er3+之间的能量转移,且Er3+的红、绿光发射均为双光子过程。     

共沉淀分离-电感耦合等离子体原子发射光谱法测定含难熔金属岩石中12种稀土元素

准确测定稀土元素含量,对是否开采含难熔金属岩石的矿山中稀土元素具有重要指导意义。实验采用Na₂O₂在750℃马弗炉中熔融样品,熔融体冷却后用盐酸(1+4)转入烧杯中,往溶液中加入氨水,以样品做载体,共沉淀分离除去钠盐及能与氨水形成络氨离子的金属元素,沉淀物用稀氨水洗涤、热稀盐酸溶解,以电感耦合等离子体原子发射光谱法(ICP-AES)测定试液中La、Ce、Sm、Eu、Gd、Tb、Ho、Er、Dy、Tm、Yb、Y,建立了含难熔金属岩石中12种稀土元素的测定方法。各元素校准曲线的线性范围为0.10~25μg/mL,方法的检出限0.20~1.0μg/g。按照实验方法测定含难熔金属岩石物料中La、Ce、Sm、Eu、Gd、Tb、Ho、Er、Dy、Tm、Yb、Y等12种稀土元素,结果的相对标准偏差(RSD,n=9)为3.2%~6.2%,加标回收率为90%~110%。实验方法可用于含难溶金属岩石中稀土元素含量为0.001%~0.50%(质量分数)的测定。     

共沉淀分离-电感耦合等离子体原子发射光谱法测定含难熔金属岩石中12种稀土元素

准确测定稀土元素含量,对是否开采含难熔金属岩石的矿山中稀土元素具有重要指导意义。实验采用Na₂O₂在750℃马弗炉中熔融样品,熔融体冷却后用盐酸(1+4)转入烧杯中,往溶液中加入氨水,以样品做载体,共沉淀分离除去钠盐及能与氨水形成络氨离子的金属元素,沉淀物用稀氨水洗涤、热稀盐酸溶解,以电感耦合等离子体原子发射光谱法(ICP-AES)测定试液中La、Ce、Sm、Eu、Gd、Tb、Ho、Er、Dy、Tm、Yb、Y,建立了含难熔金属岩石中12种稀土元素的测定方法。各元素校准曲线的线性范围为0.10~25μg/mL,方法的检出限0.20~1.0μg/g。按照实验方法测定含难熔金属岩石物料中La、Ce、Sm、Eu、Gd、Tb、Ho、Er、Dy、Tm、Yb、Y等12种稀土元素,结果的相对标准偏差(RSD,n=9)为3.2%~6.2%,加标回收率为90%~110%。实验方法可用于含难溶金属岩石中稀土元素含量为0.001%~0.50%(质量分数)的测定。     

Upconversion Luminescence Properties of Ho^3＋, Tm^3＋, Yb^3＋ Co-Doped Nanocrystal NaYF4 Synthesized by Hydrothermal Method

Nanocrystal of upconversion （UC） phosphor Ho^3＋, Tm^3＋ , and Yb^3＋ co-doped NaYF4 was prepared by the hydrothermal method in the presence of the complexing agent EDTA. Under 980 nm diode laser excitation, the impact of different concentrations of Ho^3＋ ion on the UC luminescence intensity was discussed. The law of luminescence intensity versus pump power shows that the 474 nm blue emission, 538 nm green emission, and 642 nm red emission are all due to the two-photon process, while the 450 nm blue emission is a three-photon process. The UC mechanism and processes were also analyzed. The sample was characterized by transmission electron microscopy （TEM） and X-ray diffraction （XRD）. The result shows that Ho^3＋ ,Tm^3＋ , and Yb^3＋ co-doped NaYF4 prepared by the hydrothermal method exhibits a hexagonal nanocrystal.     

Upconversion luminescence of Yb3+/Ho3+/Er3+/Tm3+ co-doped KGd(WO4)2 powders

Different lanthanide ions (Yb3+/Ho3+/Er3+/Tm3+) codoped KGd(WO4)2 phosphors were prepared by high-temperature solid-state reaction. The upconversion luminescence properties of two-ion and three-ion co-doped KGd(WO4)2 phosphors were investigated in detail. The concentration quenching effect of the two-ion co-doped KGd(WO4)2 phosphors was studied, and the optimum concentration of Ho3+, Er3+ and Tm3+ are 2 mol.%, 2 mol.% and 3 mol.%, respectively. The Yb3+/Ho3+/Tm3+ co-doped KGd(WO4)2 sample is the best white ...     

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%。     

镧铁合金中14项稀土杂质含量的测定—电感耦合等离子体发射光谱法

采用电感耦合等离子体发射光谱法（ICP-OES）测定镧铁合金中铈、镨、钕、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥、钇稀土杂质元素。镧铁合金试料在硝酸介质中,以近似基体匹配法校正基体对测定的影响,直接以氩等离子体光源激发,用标准曲线法进行光谱测定。为选择合适的分析线,先根据光谱波长表预选几条强度大,激发电位低的谱线,然后对此谱线进行轮廓扫描,从而选出一条背景平坦,信背比大,基体及共存元素干扰少或无干扰的谱线作为分析线。用基体匹配法配制标准溶液,根据产品标准XB/T 407—2020指标,以铁（85 %）与镧（15 %）配制成混合基体,配制6个系列标准溶液进行曲线绘制。该方法适用于铈、镨、钕、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥、钇含量在0.005 %~0.25 %的分析测定。方法的相对标准偏差（n=11）在0.74 %~2.58 %之间,用标准加入法对方法的回收率进行试验,测得回收率在91.75 %与107.75 %之间, 能满足产品测定要求。      

Analysis of Response Surface in the Study of RE(NO_3)_3-HNO_3-P507-Kerosene Extraction System

RE(NO_3)_3-HNO_3-P507-kerosene extraction system(RE=La,Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu,Y)was studied by the response surface technique.14 models for extracting single rare earth ele-ment in a broad range of acidity and initial rare earth concentration were obtained by using the stepwiseregression method.Three-dimensional display of the response surface of the model of extracting Er~(3 )wasshowed as an example,which reveals clearly the dependence of distribution ratio upon both initial acidity and ini-tial rare earth concentration.     

Influence of B2O3 on Spectroscopic Properties of Er^3＋/Yb^3＋ Co-Doped Tungsten-Tellurite Glasses

A series of novel Er^3＋/Yb^3＋ co-doped （85- x ） TeO2-15WO3-xB2O3 （TWB;x=2%,5%,8%（mole fraction） ） glasses were prepared. Influence of B203 on the spectroscopic properties of Er^3＋/Yb^3＋ co-doped tungsten-tellurite glasses were investigated. It is found that the intensity of 1.5μm fluorescence, lifetime of the ^4I13/2 level and upconversion fluorescence all decrease with the increase of B2O3 content. The product of full width at half maximum （FWHM） and stimulated emission cross-section （σe^peak） of Er^3＋ ：^4I13/2→^4I15/2 transition has an optimum when B203 is 5% （mole fraction）. The emission spectra of Er^3＋ ： ^4I13/2→^4I15/2 transition was analyzed using peak-fit routine, and an equivalent four-level system was proposed to estimate the stark splitting for the 411512 and ^4I13/2 levels of Er^3＋ ions in TWB glasses at room temperature.     

电感耦合等离子体原子发射光谱法测定磷矿中微量稀土元素

样品经碱熔,溶液提取,沉淀富集后得到只含稀土元素的溶液,采用电感耦合等离子体原子发射光谱(ICP-AES)法测定磷矿中15种稀土元素La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu、Y。主要考察了共存元素间的干扰情况,选择无干扰或干扰量对分析结果可以忽略不计的谱线为最佳分析线,标准曲线法直接测定磷矿中稀土元素。本法测定结果与ICP-MS测定结果相符合,可满足日常分析要求。     

Energy transfer and frequency upconversion in Er~（3＋）-Yb~（3＋） codoped oxy-fluoro-tungstosilicate glasses

Er3+-Yb3+ codoped oxy-fluoro-tungstosilicate glasses with infrared-to-visible frequency upconversion luminescence were prepared by melting quenching in air.The effects of Er3+ doping on the optical properties of the samples were measured by means of techniques such as optical absorption spectra and photoluminescence spectra.The results showed that intense green and red signals centered at 546 and 665 nm,corresponding to the 4S3/2 → 4I15/2 and 4F9/2 → 4I15/2 transitions of Er3+ by a multiphoton stepwise phonon-assisted excited-state absorption process,respectively,were simultaneously observed by exciting the samples with a diode laser operating at 980 nm at room temperature.The upconversion process was found very sensitive to Er3+ content at a constant Yb2O3 content of 5 mol.%.With the increase of Er3+ content from 0.5% to 1.5%,the upconversion intensity increased gradually.Further increasing of Er3+ content to 3.0% resulted in a significant fluorescence quenching.Moreover,the possible upconversion mechanisms were discussed based on the energy-matching conditions and the quadratic dependence on excitation power.     

Synthesis and Characterization of Rare Earth Complexes of Ferrocenylcarbonylhydrazine

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Remarkable fluorescence enhancement of upconversion composite film and its application on mercury sensing

To achieve a stable, sensitive, and high-efficiency biological probe, a novel NaYF_4:Yb,Er nanocrystals/TiO_2 inverse opal composite film was designed by self-assembly and solvent evaporation methods. 32-fold enhanced upconversion(UC) emission was investigated under 980 nm excitation. According to size-dependency, excitation power density-dependency as well as photonic stop band(PSB)-dependency upconversion spectra, the enhancement mechanism of the composite film was put down to the stochastical diffraction of IOPCs multi-layered structure to the excitation laser. On the basis of the enhancement effect of the composite film, energy transfer between upconversion nanoparticles(UCNPs) and quantum dots(QDs), and the sensitive sensing of CdTe QDs on mercury, the UC composite film was used for sensing of Hg~(2+) in serum. The solid sensor as a mercury detector owns lots of superiorities such as feasible operation, good linear relationship(R=0.997), low limit of detection(70.5 nmol/L) and thus may have broad prospects in the biosensing field.     

Synthesis and luminescent properties of lanthanide-doped ScVO_4 microcrystals

High quality and monodispersed ScVO_4 microcrystals were successfully synthesized via a mild hydrothermal route using NH_4VO_3 as vanadium source. The X-ray power diffraction(XRD) and field-emission scanning electron microscopy(FE-SEM) results indicated that the size, shape, and phase formation of the ScVO_4 microcrystals could be tuned by altering the reaction temperature, reaction time, and p H value of the initial solution. Furthermore, the down- and upconversion luminescence of ScVO_4:Ln(Ln=Eu, Dy, Sm, Yb/Ho, Yb/Er, and Yb/Tm) microcrystals were characterized and the respective energy transfer processes were also discussed. The experimental results demonstrated that reactions at 200 oC, 24 h, and pH=6 could generate perfect ScVO_4 microcrystals, which were then used for luminescence studies.     

Raman spectra of RE2O3 （RE=Eu,Gd, Dy,Ho, Er,Tm, Yb,Lu, Sc and Y）：laser-excited luminescence and trace impurity analysis

Raman spectra of a series of cubic rare earth sesquioxides RE2O3 （RE=Eu, Gd, Dy, Ho, Er, Tm, Yb, Lu, Sc and Y） were investigated by Raman spectroscopy with both 532 and 785 nm laser lines. Abundant additional bands due to laser-excited lumines-cence were observed. For Eu2O3, Dy2O3, Ho2O3, Er2O3, Tm2O3 and Yb2O3, the luminescence mainly came from the intrinsic trivalent lanthanide ions, while for Gd2O3, Lu2O3, Sc2O3 and Y2O3, their luminescence were attributed to the trace impurities of other lumines-cent lanthanide ions such as Eu3＋, Nd3＋and Er3＋. This investigation confirmed Raman spectroscopy as a useful tool for detecting trace luminescent lanthanide impurities.