Preparation of Nanometer Nd~(3+),Y~(3+) Co-doped CaF_2 Powder by Coprecipitation-azeotropic Distillation Technique

The synthesis of Nd~(3+),Y~(3+):CaF_2 nanopowder was conducted by azeotropic distillation method,which effectively dehydrated hydrous CaF_2 and prevented forming hard agglomerates.X-ray diffraction(XRD),scanning electron microscopy(SEM),scanning calorimetries-thermalgravimetry(DSC-TG),Fourier transform infrared spectroscopy(FT-IR) and absorption spectroscopy were performed to characterize the powder properties.The experimental results showed that products obtained by azeotropic distillation were single phased,rather monodispersed,successfully prevented the hard agglomerate formation and effectively removed the residual water inside the as-prepared precipitate than that of the direct drying.The absorption spectra showed a wider and stronger absorption bands around 792 nm,which should be profitable for LD pumping.     

Preparation and optical properties of Er<Superscript>3+</Superscript>: Na<Subscript>2</Subscript>O-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-SiO<Subscript>2</Subscript> transparent glass-ceramics

Na₂O-Al₂O₃-SiO₂ glass-ceramics doped with Er³⁺ ions were synthesized by the conventional melt quenching technique at a low melting temperature. The samples were characterized by differential scanning calorimetry (DSC), X-ray diffraction (XRD), scanning electron microscopy (SEM), UV-vis-NIR scanning spectrophotometry, and fluorescence spectrometry. The results show that the main crystalline phase of glass-ceramics is nepheline.The best heat-treatment process is at 520 °C for 2 h. Because the up-conversion luminescence and near infrared luminescence properties of glass doped with Eu³⁺ are studied in detail.     

Interaction of rare earth ions in Sr<Subscript>2</Subscript>MgSi<Subscript>2</Subscript>O<Subscript>7</Subscript>: Eu<Superscript>2+</Superscript>, Dy<Superscript>3+</Superscript> material

To discuss the function of Eu and Dy and their interaction in Sr₂MgSi₂O₇: Eu²⁺, Dy³⁺ long afterglow material, the Eu and Dy single doped and their co-doped Sr₂MgSi₂O₇: Eu²⁺, Dy³⁺ were prepared. The samples were characterized by X-ray diffraction (XRD), decay curves, photoluminescence (PL), and thermoluminescence (TL). The results indicate that Sr₂MgSi₂O₇: Eu has afterglow properties, and the doping of Eu ion in Sr₂MgSi₂O₇: Eu²⁺, Dy³⁺ can lower the depth of traps. Eu ion can not only serve as luminescence center, but also produce traps in the matrix, meanwhile, it also exerts certain influences on the traps produced by Dy in Sr₂MgSi₂O₇: Eu²⁺, Dy³⁺. The Dy ion can not act as luminescence center but relates to the change of the traps in the Sr₂MgSi₂O₇ matrix.     

Fluorescence detection for H<Subscript>2</Subscript>PO<Subscript>4</Subscript><Superscript>-</Superscript> based on carbon dots/Fe<Superscript>3+</Superscript> composite

A novel fluorescent probe for H₂PO₄ ^- was designed and fabricated based on the carbon dots/Fe³⁺ composite. The carbon dots were synthesized by an established one-pot hydrothermal method and characterized by transmission electron microscope, X-ray diffractometer, UV-Vis absorption spectrometer and fluorescence spectrophotometer. The carbon dots/Fe³⁺ composite was obtained by aqueous mixing of carbon dots and FeCl₃, and its fluorescence property was characterized by fluorescence spectrophotometer. The fluorescence of carbon dots was quenched by aqueous Fe³⁺ cations, resulting in the low fluorescence intensity of the carbon dots/Fe³⁺ composite. On the other hand, H₂PO₄ ^- reduced the concentration of Fe³⁺ by chemical reaction and enhanced the fluorescence of the carbon dots/Fe³⁺ composite. The Stern-Volmer equation was introduced to describe the relation between the relative fluorescence intensity of the carbon dots/Fe³⁺ composite and the concentration of H₂PO₄ ^-, and a fine linearity (R ²=0.997) was found in the range of H₂PO₄ ^- concentration of 0.4-12 mM.     

Crystallization and luminescence properties of Sm<Superscript>3+</Superscript>-doped SrO-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-SiO<Subscript>2</Subscript> glass-ceramics

The Sm³⁺-doped SrO-Al₂O₃-SiO₂ (SAS) glass-ceramics with excellent luminescence properties were prepared by batch melting and heat treatment. The crystallization behavior and luminescent properties of the glass-ceramics were investigated by DTA, XRD, SEM and luminescence spectroscopy. The results indicate that the crystal phase precipitated in this system is monocelsian (SrAl₂Si₂O₈) and with the increase of nucleation/crystallization temperature, the crystallite increases from 66 % to 79 %. The Sm³⁺-doped SAS glass-ceramics emit green, orange and red lights centered at 565, 605, 650 and 715 nm under the excitation of 475 nm blue light which can be assigned to the ⁴G_5/2→⁶ H _j/2 (j=5, 7, 9, 11) transitions of Sm³⁺, respectively. Besides, by increasing the crystallization temperature or the concentration of Sm³⁺, the emission lights of the samples located at 565, 605 and 650 nm are intensified significantly. The present results demonstrate that the Sm³⁺-doped SAS glass-ceramics are promising luminescence materials for white LED devices by fine controlling and combining of these three green, orange and red lights in appropriate proportion.     

Synthesis of M (M=Co<Superscript>2+</Superscript>, Co<Superscript>2+</Superscript>/Ni<Superscript>2+</Superscript>)-doped FeS<Subscript>2</Subscript> Nanospheres with Enhanced Visible-light-induced Photocatalytic Activity

Nano-spherical Co²⁺-doped FeS₂ was synthesized through a simple solvothermal method. The products were investigated using XRD, FE-SEM, BET, ICP, EDS, TEM, HRTEM, XPS, and UV-vis spectroscopy. The results indicated that Co²⁺ ion could change the particle nucleation process and inhibited the particle growth of FeS₂. In addition, when the content of doped Co²⁺ was 15%, the degradation efficiency of methylene blue (MB) achieved 60.72% after 210 min irradiation, which increased by 52.01% than that of the undoped FeS₂. Moreover, comparison experiments also demonstrated that the M (M=Co²⁺, Co²⁺/Ni²⁺)-doped FeS₂ photocatalytic activity efficiency sequence was Co²⁺ > Ni²⁺>Co²⁺/Ni²⁺. This is ascribed to the fact that the Co²⁺ doping could induce the absorption edge shifting into the visible-light region and increased the surface area of the samples. The effect mechanisms of M-doping on the band gap and the photocatalytic activity of FeS₂ were also discussed.     

Microstructures and fatigue-free properties of the La<Superscript>3+</Superscript> and Nd<Superscript>3+</Superscript> doped Bi<Subscript>4</Subscript>Ti<Subscript>3</Subscript>O<Subscript>12</Subscript> thin films prepared by modified sol-gel technique

Ferroelectric Bi_3.25La_0.75Ti₃O₁₂ (BLT) and Bi_3.15Nd_0.85Ti₃O₁₂ (BNT) thin films were fabricated on Pt/TiO₂/SiO₂/Si (100) substrates by a modified sol-gel technique. X-ray diffraction indicated that these films were of single phase with random polycrystalline orientations. The surface morphologies of the films were observed by scanning electron microscope, showing uniform, dense films with grain size of 50–100 nm. Well-saturated hysteresis loops of the films were obtained in metal-ferroelectric-metal type capacitors with Cu top electrodes at an applied voltage of 400 kV/cm, giving the remanent polarization (2P _r) and coercive field (2E _c) values of the films of 25.1 μC/cm² and 203 kV/cm for BLT, and 44.2 μC/cm² and 296 kV/cm for BNT, respectively. Moreover, these capacitors did not show fatigue behaviors after up to 1.75×10¹⁰ switching cycles at the test frequency of 1 MHz, suggesting a fatigue-free character. The influences of the La³⁺ and Nd³⁺ doping on the properties of the films were comparatively discussed. Supported by the National Key Basic Research and Development Program of China (Grant No. 2006CB932305) and the Natural Science Foundation of Hubei Province, China (Grant No. 2004ABA082)     

Frequency up-conversion luminescence properties and mechanism of Tm<Superscript>3+</Superscript>/Er<Superscript>3+</Superscript>/Yb<Superscript>3+</Superscript> co-doped oxyfluorogermanate glasses

Oxyfluoride glasses were developed with composition 60GeO 2 ·10AlF 3 ·25BaF 2 ·(1.95-x)GdF 3 · 3YbF 3 ·0.05TmF 3 ·xErF 3 (x=0.02,0.05,0.08,0.11,0.14,0.17)in mole percent.Intense blue(476 nm),green(524 and 546 nm)and red(658 nm)emissions which identified from the 1G 4 →3H 6 transition of Tm3+and the(2H 11/2 ,4S 3/2 )→4I 15/2 ,4F 9/2 →4I 15/2 transitions of Er3+,respectively,were simultaneously observed under 980 nm excitation at room temperature.The results show that multicolor luminescence including white l...     

Preparation and Upeonversion Lumineseenee ofNanoerystailine Gd2O3： Er^3＋, Yb^3＋

Nanocrystalline Gd1.77Yb0.2Er0.03O3 samples were prepared by combustion and precipitation methods. Structures and upconversion luminescence properties of samples were studied. The results of XRD show that all samples are cubic structure, the average crystallite size could be calculated as 23 nm and 39 nm, respectively. The lattice constants were obtained. The FT-IR spectra were measured to investigate the vibrational feature of the samples. Upconversion luminescence spectra of samples under 980 nm laser excitation were investigated. The strong red emission of samples were observed, and attributed to 4F9/2→4I152 transitions of Er^3＋ ions, the emission intensity for sample synthesized by precipitation method is stronger compared to that of combustion method. The possible upconversion luminescence mechanisms in nanocrystalline Gd1.77Yb0.2Er0.03O3 were discussed.     

Phase transition and photoluminescence properties of Eu<Superscript>3+</Superscript>-doped ZnMoO<Subscript>4</Subscript> red phosphors

Eu³⁺-doped ZnMoO₄ with different doping concentrations were synthesized by a hydrothermal method. The effects of Eu³⁺ doping on the phase structure and photoluminescence (PL) properties of ZnMoO₄ were investigated. The result showed that the introduction of Eu3+ could lead to phase transition of ZnMoO₄. With the increase of Eu³⁺ doping amount, β-ZnMoO₄ was transformed to α phase gradually, which led to different photoluminescence performances. The optimized doping concentration of Eu³⁺ was 6 mol% for the highest emission intensity at 615 nm. Its CIE chromaticity coordinates were (0.667, 0.331), which were very close to the values of standard chromaticity (0.67, 0.33) for National Television Standards Committee (NTSC) system. Therefore, Eu³⁺-doped ZnMoO₄ is considered to be a promising red-emitting phosphor for white LED applications.     

Synthesis and luminescence of nano fluorescent powder of Y<Subscript>4</Subscript>Al<Subscript>2</Subscript>O<Subscript>9</Subscript>: Eu<Superscript>3+</Superscript>

Nano fluorescent powder of Y₄Al₂O₉: Eu³⁺ was synthesized by sol-gel method. The XRD shows that the product prepared at 900°C is pure-phase Y₄Al₂O₉: Eu³⁺. The Y₄Al₂O₉ powder is nano-size crystal testified by BF and ED analysis of TEM. The grain diameter of Y₄Al₂O₉ is in the range between 20 and 50nm, and its average is 30 nm. The luminescent spectra show that Eu³⁺ ious occupy two kinds of sites in Y₄Al₂O₉ crystal lattice. One is in the strict inversion center, and the other is in off lying inversion center. When excited with UV light (λ=254nm), Y₄Al₂O₉: Eu³⁺ exhibits an orange emission bond at λ=590 nm due to the⁵D_o→⁷F₁ transition and a red emission band at λ=610 nm due to⁵D_o→⁷F₂ transition. YUAN Xi-ming: Born in 1951 Funded by Key Scientific and Technological Project of Hubei Province (2001 AA102A03)     

Roles of Eu^2＋, Dy^3＋ Ions in Persistent Luminescence of Strontium Aluminates Phosphors

The polycrystalline Eu^2＋ and Dy ^3＋ co-doped strontium aluminates SrAl2O4： Eu^2＋, Dy^3＋ with different compositions were prepared by solid state reactions. The UV-excited photoluminescence, persistent luminescence and thermo-luminescence were studied and compared. Results show that the doped Eu^2＋ ion in SrAl2O4： Eu^2＋, Dy^3＋ phosphors works as not only the UV-excited luminescent center but also the persistent luminescent center. The doped Dy^3＋ ion can hardly yield any luminescence under UV-excitation, but effectively enhance the persistent luminescence and thermo-luminescence of SrAl2O4： Eu^2＋. Dy^3＋ co-doping can help form electron traps with appropriate depth due to its suitable electro-negativity, and increase the density and depth of electron traps. Based on above observations, a persistent luminescence mechanism, electron transfer model, is proposed and illustrated.     

Fabrication and photocatalytic activity of Ag<Subscript>3</Subscript>PO<Subscript>4</Subscript>-TiO<Subscript>2</Subscript> heterostructural nanotube arrays

To extend the absorption capability of TiO₂ into visible light region and inhibit the recombination of photogenerated electrons and holes, we put forward an effective strategy of the coupling of TiO₂ with a suitable semiconductor that possesses a narrow band gap. Meanwhile, Ag₃PO₄-TiO₂ heterostructural nanotube arrays were prepared by the two-step anodic oxidation to obtain the TiO₂ nanotube arrays and then by a deposition-precipitation method to load Ag₃PO₄. The samples were characterized by field emission scanning electron microscopy (FESEM), energy dispersive spectrometry (EDS), X-ray diffraction (XRD), and UV-vis diffuse reflectance spectroscopy (UV-vis DRS). The experimental results showed that Ag₃PO₄ nanoparticles were uniformly dispersed on the highly ordered TiO₂ nanotube arrays, which increased the visible-light absorption of TiO₂ photocatalyst. The photocurrent density and photocatalytic degradation of methyl orange indicated that the performance of Ag₃PO₄-TiO₂ heterostructural nanotube arrays was better than that of the TiO₂ nanotube arrays, which could be attributed to the effective electron-hole separation and the improved utilization of visible light.     

Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>@PAM@NTA-Ni<Superscript>2+</Superscript> Magnetic Composite Nanoparticles for Highly Specific Separation of His-tagged Proteins

A facile approach has been developed to synthesize Fe₃O₄@PAM (polyacrylamide) nanoparticles (NPs) with carboxyl groups on the surfaces by copolymerization with acrylamide and acrylic acid in Fe₃O₄ NPs aqueous suspension. Nitrilotriacetic acid (NTA) was conjugated to the magnetic NPs via well-known carboniimide chemistry using EDC and NHS. The Ni²⁺ ions loaded on the surface of NPs provide abundant docking sites for immobilization of His-tagged green fluorescent proteins (His-tagged GFP). The high magnetic property of Fe₃O₄@PAM@NTA-Ni²⁺ allows an easy separation of the NPs from solution under an external magnetic field, with high His-tagged protein binding capacity (42 μg protein/mg of NPs). The NPs can be recycled for at least four times without significant loss of binding capacity to proteins. These materials show great potential to separate His-tagged protein with low-cost purification at industrial scale.     

Electrochemical preparation of V<Subscript>2</Subscript>O<Subscript>3</Subscript> from NaVO<Subscript>3</Subscript> and its reduction mechanism

Vanadium trioxide (V₂O₃) was directly prepared by NaVO₃ electrolysis in NaCl molten salts. Electrolysis products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). The existing state and electrochemical behavior of NaVO₃ were also studied. The results indicated that V₂O₃ can be obtained from NaVO₃. VC and C were also formed at high cell voltage, high temperature, and long electrolysis time. During electrolysis, NaVO₃ was dissociated to Na⁺ and VO₃ ^? in NaCl molten salt. NaVO₃ was initially electro- reduced to V₂O₃ on cathode and Na₂O was released simultaneously. Na₂CO₃ was formed due to the reaction between Na₂O and CO₂. The production of C was ascribed to the electro-reduction of CO₃ ^2?. VC was produced due to the reaction between C and V₂O₃.     

Preparation and Performance of Si<Superscript>4+</Superscript>-doping Rod-shaped TiO<Subscript>2</Subscript> Powder by Nonhydrolytic Sol-gel Method

Titania (TiO₂) nanorod powder was prepared by nonhydrolytic sol-gel method using titanic chloride (TiCl₄) as titanium source, methylene dichloride (CH₂Cl₂) as solvent, absolute ethyl alcohol (CH₃CH₂OH) as oxygen donor. The effects of Si⁴⁺ doping on the TiO₂ nanocrystalline phase transformation temperature were systematically researched. The results showed that when the molar ratio of Ti⁴⁺ to Si⁴⁺ is 1 to1.3, TiO₂ prepared by calcination at 1100 °C for 1 hour exhibits rod shape and has good photocatalytic activity. Doping of Si⁴⁺ makes glass phase core-shell structure forming on the surface of anatase crystal particles, which can inhibit crystal phase transformation and raise the transformation temperature, making TiO₂ stable in anatase phase at 1200 °C.     

Structure and Electric Conductivity of Ce-doped Bi<Subscript>2</Subscript>O<Subscript>3</Subscript> Electrolyte Synthesized by Reverse Titration Chemical Coprecipitation

Ce-doped Bi₂O₃ nanopowders were prepared by reverse titration chemical coprecipitation from Bi³⁺ and Ce⁴⁺ containing aqueous solution. Techniques of X-ray diffraction (XRD), transmission electron microscopic (TEM) and Fourier transform infrared spectroscopy (FTIR) were employed to characterize the as-synthesized materials. The XRD patterns indicated that the peaks can be easily indexed to β-Bi₂O₃ and no diffraction peaks of Ce or other impurity phases were detected in the prepared samples. The calculated average crystalline size decreased from 31.72 to 11.96 nm when the Ce content increased from 1 wt% to 10 wt%. The morphology changed from flake-like into the spherical-like with increase in Ce content. The electric conductivity of Ce-doped Bi₂O₃ electrolyte was also investigated by two probe DC method. Conductivity analysis exhibited that the rate of conductivity increased with increasing Ce²⁺ ratio, when the Ce concentration was up to 5 wt%, the as-synthesized Ce-doped Bi₂O₃ electrolyte showed the maximum value of conductivity(0.295 S·cm^–1).     

Preparation of Functionalized Graphene Nano-platelets and Use for Adsorption of Pb<Superscript>2+</Superscript> from Solution

Functionalized graphene nano-platelets (FGN) were obtained via treating graphene nanoplatelets (GN) with HNO₃, and served as adsorbent for the removal of Pb²⁺ from solutions. We investigated the FGN adsorption capacity for Pb²⁺ at different initial concentrations, varying pH, contact time and temperature. The characterization results of scanning electron microscopy (SEM), thermal analysis (TG/DTG), Fourier transform infrared spectroscopy (FT-IR) and Brunauer-Emmett-Teller (BET) method indicated that FGN layers were thin and possess large specific area with oxygen-containing functional groups grafted onto their surface. Meanwhile, the determined equilibrium adsorption capacity of FGN for Pb²⁺ was 57.765 mg/g and adsorption isotherms well confirmed to Langmuir isotherms models. The results reveals that the FGN has better effect of water treatment.     

Preparation and characterization of CeO<Subscript>2</Subscript>-TiO<Subscript>2</Subscript>/SnO<Subscript>2</Subscript>:Sb films deposited on glass substrates by R.F. sputtering

CeO2-TiO2 films and CeO2-TiO/SnO2：Sb （6 mol%） double films were deposited on glass substrates by radio-frequency magnetron sputtering （R.F. Sputtering）, using SnO2：Sb（6 mol%） target, and CeO2- TiO2 targets with different molar ratio of CeO2 to TiO2 （CeO2：TiO2-0：1.0; 0.1：0.9; 0.2：0.8; 0.3：0.7; 0.4：0.6; 0.5：0.5; 0.6：0.4; 0.7：0.3; 0.8：0.2; 0.9：0.1; 1.0：0）. The films are characterized by UV-visible transmission and infrared reflection spectra, scanning electron microscopy （SEM）, Raman spectroscopy, X-ray photoelectron spectroscopy （XPS） and X-ray diffraction （XRD）, respectively. The obtained results show that the amorphous phases composed of CeO2-TiO2 play an important role in absorbing UV, there are Ce^3-, Ce^4- and Ti^4- on the surface of the films; the glass substrates coated with CeO2-TiO2 （Ce/Ti=0.5：0.5; 0.6：0.4）/SnO2：Sb（6 mol%） double films show high absorbing UV（〉99）, high visible light transmission （75%） and good infrared reflection （〉70%）. The sheet resistance of the films is 30-50 Ω/□. The glass substrates coated with the double functional films can be used as window glass of buildings, automobile and so on.     

Effect of ZnO-B<Subscript>2</Subscript>O<Subscript>3</Subscript> glass addition on the microwave dielectric properties of BaO-Nd<Subscript>2</Subscript>O<Subscript>3</Subscript>-TiO<Subscript>2</Subscript>-Bi<Subscript>2</Subscript>O<Subscript>3</Subscript> system

The effect of ZnO-B₂O₃(ZB) glass addition on the sintering behavior, microstructures and microwave dielectric properties of BaO-Nd₂O₃-TiO₂-Bi₂O₃ (BNTB) system was investigated with the aid of X-ray diffraction, scanning electron microscopy and capacitance meter. It is found that the ZB glass addition, acting as a sintering aid, can effectively lower the sintering temperature of BNTB system to 850 °C. The dielectric constant of BNTB-ZB ceramics increases with the increase of soaking time and the value of dielectric loss decreased with increasing soak time. The optical dielectric properties at 1 GHz of ɛ=74, tan δ=4×10⁻⁴, and TCC=25 ppm/°c were obtained for the BNTB system doped with 25 wt% ZB glass sintered at 850 °C for 2 h, representing that the BNTB-ZB ceramics could be promising for multilayer low temperature co-fired ceramics applications.