Grain boundary conductivity of high purity neodymium-doped ceria nanosystem with and without the doping of molybdenum oxide

Solid solutions of Ce1-xNdxO2-x/2 (0.05 <= x <= 0.2) and (Ce1-xNdx)(0.95)MO0.05O2-delta (0.05 <= x <= 0.2) have been synthesized by a modified sol-gel method. Both materials have very low content of SiO2 (similar to 27 ppm). Their structures and ionic conductivities were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM) and electrochemical impedance spectroscopy (M). The XRD patterns indicate that these materials are single phases with a cubic fluorite structure. The powders calcined at 300 degrees C with a crystal size of 5.7 nm have good sinterability, and the relative density could reach above 96% after being sintered at 1450 degrees C. With the addition Of MoO3, the sintering temperature could be decreased to 1250 degrees C. Impedance spectroscopy measurement in the temperature range of 250-800 degrees C indicates that a sharp increase of conductivity is observed when a small amount of Nd2O3 is added into ceria, of which Ce0.85Nd0.15O1.925 (15NDC) shows the highest conductivity. With the addition of a small amount Of MoO3, the grain boundary conductivity of 15NDC at 600 degrees C increases from 2.56 S m(-1) to 5.62 S m(-1).

Synthesis and morphology of polyethylene chains grafted onto the surface of crosslinked polystyrene microspheres

The bifunctional comonomer 4-(3-butenyl) styrene was used to synthesize crosslinked polystyrene microspheres (c-PS) with pendant butenyl groups on their surface via suspension copolymerization. Polyethylene chains were grafted onto the surface of c-PS microspheres (PS-g-PE) via ethylene copolymerizing with the pendant butenyl group on the surface of the c-PS microspheres under the catalysis of metallocene catalyst. The composition and morphology of the PS-g-PE microspheres were characterized by means of Fourier transform infrared spectroscopy, Fourier transform Raman spectroscopy, X-ray photoelectron spectroscopy, and field-emission scanning electron microscopy. It is possible to control the content of PE grafted onto the surface of c-PS microspheres by varying the polymerization time or the initial quantity of pendant butenyl group on the surface of c-PS microspheres. Investigation on the morphology and crystallization behavior of grafted PE chains showed that different surface patterns could be formed under various crystallization conditions. Moreover, the crystallization temperature of PE chains grafted on the surface of c-PS microspheres was 6 degrees C higher than that of pure PE. The c-PS microspheres decorated by PE chains had a better compatibility with PE matrix.

Electrocatalytic reduction of oxygen at multi-walled carbon nanotubes and cobalt porphyrin modified glassy carbon electrode

The multi-walled carbon nanotubes (MWNTs) modified glassy carbon electrode exhibited electrocatalytic activity to the reduction of oxygen in 0.1 M HAc-NaAc (pH 3.8) buffer solution. Further modification with cobalt porphyrin film on the MWNTs by adsorption, the resulted modified electrode showed more efficient catalytic activity to O-2 reduction. The reduction peak potential of O-2 is shifted much more positively to 0.12 V (vs. Ag/AgCl), and the peak current is increased greatly. Cyclic voltammetry (CV), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM), were used to characterize the material and the modified film on electrode surface. Electrochemical experiments gave the total number of electron transfer for oxygen reduction as about 3, which indicated a co-exist process of 2 electrons and 4 electrons for reduction of oxygen at this modified electrode. Meanwhile, the catalytic activities of the multilayer film (MVVNTs/CoTMPyP)(n) prepared by layer-by-layer method were investigated, and the results showed that the peak current of O-2 reduction increased and the peak potential shifted to a positive direction with the increase of layer numbers.

Sol-gel-derived BPO4/Ba2+ as a new efficient and environmentally-friendly bluish-white luminescent material

In this paper, BPO4 and Ba2+-doped BPO4 powder samples were prepared by the sol-gel process using glycerol and poly(ethylene glycol) as additives. The structure and optical properties of the resulting samples were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, field emission scanning electron microscopy (FESEM), diffuse reflection spectra, photoluminescence (PL) excitation and emission spectra, quantum yield, kinetic decay, and electron paramagnetic resonance (EPR), respectively. It was found that the undoped BPO4 showed a weak purple blue emission (409 nm, lifetime 6.4 ns) due to the carbon impurities involved in the host lattice. Doping Ba2+ into BPO4 resulted in oxygen-related defects as additional emission centers which enhanced the emission intensity greatly (> 10x) and shifted the emission to a longer-wavelength region (lambda(max) = 434 nm; chromaticity coordinates: x = 0.174, y = 0. 187) with a bluish-white color. The highest emission intensity was obtained ;when doping 6 mol % Ba2+ in BPO4, which has a quantum yield as high as 31%. The luminescent mechanisms of BPO4 and Ba2+-doped BPO4 were discussed in detail according to the existing models for silica-based materials.

Tunable photoluminescent and cathodoluminescent properties of ZnO and ZnO : Zn phosphors

ZnO and ZnO: Zn powder phosphors were prepared by the polyol-method followed by annealing in air and reducing gas, respectively. The samples were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), X-ray photoelectron spectra (XPS), electron paramagnetic resonance (EPR), and photoluminescence (PL) and cathodoluminescence ( CL) spectra, respectively. The results indicate that all samples are in agreement with the hexagonal structure of the ZnO phase and the particle sizes are in the range of 1-2 mu m. The PL and CL spectra of ZnO powders annealed at 950 degrees C in air consist of a weak ultraviolet emission band ( similar to 390 nm) and a broad emission band centered at about 527 nm, exhibiting yellow emission color to the naked eyes. When the sample was reduced at the temperatures from 500 to 1050 degrees C, the yellow emission decreased gradually and disappeared completely at 800 degrees C, whereas the ultraviolet emission band became the strongest. Above this temperature, the green emission ( similar to 500 nm) appeared and increased with increasing of reducing temperatures.

Morphology-controllable synthesis and characterization of single-crystal molybdenum trioxide

Molybdenum trioxide nanobelts and prism-like particles with good crystallinity and high surface areas have been prepared by a facile hydrothermal method, and the morphology could be controlled by using different inorganic salts, such as KNO3, Ca(NO3)(2), La(NO3)(3), etc. The possible growth mechanism of molybdenum trioxide prism-like particles is discussed on the basis of the presence of HI and the modification of metal cations. The as-prepared nanomaterials are characterized by means of powder X-ray diffraction (PXRD), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), Fourier transformation infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), and ultraviolet and visible spectroscopy (UV-vis). TEM and HRTEM micrographs show that the molybdenum trioxide nanobelts and prism-like particles have a relatively high degree of crystallinity and uniformity. BET specific surface areas of the as-prepared molybdenum trioxide nanocrystals are 67-79 m(2)g(-1). XPS analysis indicates that the hexavalent molybdenum is predominant in the nanocrystals. UV-vis spectra reveal that the direct band gap energy of the annealed molybdenum trioxide prism-like particles shows a pronounced blue shift compared to that of bulk MoO3 powder.

ZnO-based hollow microspheres: Biopolymer-assisted assemblies from ZnO nanorods

Many efforts have been made in fabricating three-dimensional (3D) ordered zinc oxide (ZnO) nanostructures due to their growing applications in separations, sensors, catalysis, bioscience, and photonics. Here, we developed a new synthetic route to 3D ZnO-based hollow microspheres by a facile solution-based method through a water-soluble biopolymer (sodium alginate) assisted assembly from ZnO nanorods. The products were characterized by X-ray diffraction, field emission scanning electron microscopy, transmission electron microscopy, selected area electron diffraction, and X-ray photoelectron spectroscopy. Raman and photoluminescence spectra of the ZnO-based hollow microspheres were obtained at room temperature to investigate their optical properties. The hollow microspheres exhibit exciting emission features with a wide band covering nearly all the visible region. The calculated CIE (Commission Internationale d'Eclairage) coordinates are 0.24 and 0.31, which fall at the edge of the white region (the 1931 CIE diagram). A possible growth mechanism of the 3D ZnO superstructures based on typical biopolymer-crystal interactions in aqueous solution is tentatively proposed, which might be really interesting because of the participation of the biopolymer.

Rapid self-assembly of oligo(o-phenylenediamine) into one-dimensional structures through a facile reprecipitation route

The self-assembly of oligo(o-phenylenediamine) (OPD) into 1-D nanostructures on a macroscopic length scale was found when they were transferred from N-methyl pyrrolidone to deionized water. Field emission scanning electron microscopy and confocal fluorescence microscopy were used to investigate the morphology of the precipitates. Results showed that large amounts of OPD 1-D supertructures could be obtained through the simple reprecipitation route, and the length of the fibers could be tuned from microscale to macroscale by adjusting the ratio of two solvents. X-ray diffraction patterns and UV-vis spectra revealed that pi-pi interactions between OPD molecules that facilitated the formation of 1-D structures became predominant when they were transferred from a good solvent to a bad one. Accordingly, a possible formation mechanism was proposed.

Sol-gel synthesis and characterization of SiO2@CaWO4, SiO2@CaWO4 : Eu3+/Tb3+ core-shell structured spherical particles

Nanocrystalline CaWO4 and Eu3+ (Tb3+)-doped CaWO4 phosphor layers were coated on non-aggregated, monodisperse and spherical SiO2 particles by the Pechini sol-gel method, resulting in the formation of SiO2@CaWO4, SiO2@CaWO4:Eu3+/Tb3+, core-shell structured particles. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), photoluminescence (PL), low-voltage cathodoluminescence (CL), time-resolved PL spectra and lifetimes were used to characterize the core-shell structured materials. Both XRD and FT-IR indicate that CaWO4 layers have been successfully coated on the SiO2 particles, which can be further verified by the FESEM and TEM images. The PL and CL demonstrate that the SiO2@CaWO4 sample exhibits blue emission band WO42- with a maximum at 420 nm (lifetime = 12.8 mu s) originated from the 4 groups, while SiO2@CaWO4:Eu3+ and SiO2@CaWO4:Tb3+ show additional red emission dominated by 614 nm (Eu3+:D-5(0)-F-7(2) transition, lifetime = 1.04 ms) and green emission at 544 nm (Tb3+:D-5(4)-F-7(5) transition, lifetime = 1.38 ms), respectively.

Sol-gel synthesis and photoluminescence properties of spherical SiO2@LaPO4 : Ce3+/Tb3+ particles with a core-shell structure

LaPO4: Ce3+ and LaPO4: Ce3+, Tb3+ phosphor layers have been deposited successfully on monodispersed and spherical SiO2 particles of different sizes ( 300, 500, 900 and 1200 nm) through a sol - gel process, resulting in the formation of core - shell structured SiO2@ LaPO4: Ce3+/ Tb3+ particles. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microcopy (SEM), transmission electron microscopy (TEM), and general and time-resolved photoluminescence (PL) spectra as well as lifetimes were used to characterize the resulting SiO2@ LaPO4: Ce3+/ Tb3+ samples. The XRD results demonstrate that the LaPO4: Ce3+, Tb3+ layers begin to crystallize on the SiO2 templates after annealing at 700 degrees C, and the crystallinity increases on raising the annealing temperature. The obtained core - shell phosphors have perfectly spherical shape with a narrow size distribution, non-agglomeration, and a smooth surface. The doped rare-earth ions show their characteristic emission in the core - shell phosphors, i.e. Ce3+ 5d - 4f and Tb3+5D4 - F-7(J) (J = 6 - 3) transitions, respectively. The PL intensity of the Tb3+ increased on increasing the annealing temperature and the SiO2 core particle size.

Direct electrochemical generation of conducting polymer micro-rings

Self-doped polyaniline (PANI) micro-rings have been successfully generated electrochemically. The polymer forming rings were about 100 nm wide, and the ring diameter is tunable from several to dozens of micrometres depending on deferent current densities. The morphology of such nanostructured polyaniline rings was investigated and further confirmed with field-emission scanning electron microscopy (FE-SEM). Furthermore, the film was characterized using UV/visible spectroscopy and cyclic voltammetry. The bubble template formation mechanism of the micro-rings was also proposed. Such nanostructured materials synthesized electrochemically open up a new approach to surface morphology control.

Precursor induced synthesis of hierarchical nanostructured ZnO

As-synthesized ZnO nanostructures with a bladed bundle-like architecture have been fabricated from a flower-like precursor ZnO (.) 0.33ZnBr(2) (.) 1.74H(2)O via a mechanism of dissolution - recrystallization. Experimental conditions, such as initial reactants and reaction time, are examined. The results show that no bladed bundle-like ZnO hierarchical nanostructures can be obtained by using the same molar amount of other zinc salts, such as ZnBr2, instead of the flower-like ZnO (.) 0.33ZnBr(2) (.) 1.74H(2)O precursor, and keeping other conditions unchanged. The products were characterized by field emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The ZnO nanostructures are mainly composed of nanowires with a diameter around 40 - 50 nm and length up to 1.5 - 2.5 mu m. Meanwhile, ZnO nanoflakes with a thickness of about 4 - 5 nm attached to the surface of ZnO nanowires with a preferred radially aligned orientation. Furthermore, the photoluminescence (PL) measurements exhibited the unique white-light-emitting characteristic of hierarchical ZnO nanostructures. The emission spectra cover the whole visible region from 380 to 700 nm.

Crystallization and phase behavior of crystalline syndiotactic 1,2-polybutadiene/isotactic polypropylene blends in solution-cast thin films

Crystallization and phase behavior in solution-cast thin films of crystalline syndiotactic 1,2-polybutadiene (s-1,2-PB) and isotactic polypropylene (i-PP) blends have been investigated by transmission electron microscopy (TEM), atomic force microscopy (AFM) and field-emission scanning electron microscopy (FESEM) techniques. Thin films of pure s-1,2-PB consist of parallel lamellae with the c-axis perpendicular to the film plane and the lateral scale in micrometer size, while those of i-PP are composed of cross-hatched and single-crystal-like lamellae. For the blends, TEM and AFM observations show that with addition of i-PP, the s-1,2-PB long lamellae become bended and i-PP itself tends to form dispersed convex regions oil a continuous s-1,2-PB phase even when i-PP is the predominant component, which indicates a strong phase separation between the two polymers during film formation. FESEM micrographs of both lower and upper surfaces of the films reveal that the s-1,2-PB lamellae pass through i-PPconvex regions from the bottom, i.e. the dispersed i-PP regions lie on the continuous s-1,2-PB phase. The structural development is attributed to an interplay of crystallization and phase separation of the blends in the film forming process.

Silica supported submicron SiO2@Y2SiO5 : Eu3+ and SiO2@Y2SiO5 : Ce3+/Tb3+ spherical particles with a core-shell structure: Sol-gel synthesis and characterization

X-1-y(2)SiO(5):Eu3+ and X-1-Y2SiO5:Ce3+ and/or Tb3+ phosphor layers have been coated on nonaggregated, monodisperse, submicron spherical SiO2 particles by a sol-gel process, followed by surface reaction at high temperature (1000 degrees C), to give core/shell structured SiO2@Y2SiO5:Eu3+ and SiO2@Y2SiO5:Ce3+/Tb3+ particles. X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), TEM, photoluminescence (PL), low voltage cathodoluminescence (CL), and time-resolved PL spectra and lifetimes are used to characterize these materials. The XRD results indicate that X-1-Y2SiO5 layers have been successfully coated on the sur- face Of SiO2 particles, as further verified by the FESEM and TEM images. The PL and CL studies suggest that SiO2@Y2SiO5:Eu3+, SiO2@Y2SiO5:Tb3+ (or Ce3+/Tb3+), and SiO2@Y2SiO5:Ce3+ core/shell particles exhibit red (Eu3+, 613 rim: D-5(0)-F-7(2)), green (Tb3+, 542nm: D-5(4)-F-7(5)), or blue (Ce3+, 450nm: 5d-4f) luminescence, respectively. Pl, excitation, emission, and time-resolved spectra demonstrate that there is an energy transfer from Ce3+ to Tb3+ in the SiO2@Y2SiO5:Ce3+,Tb3+ core/shell particles.

Luminescence properties of sol-gel derived spherical SiO2@Gd-2(WO4)(3): Eu3+ particles with core-shell structure

Monodisperse, core-shell structured SiO2@Gd-2(WO4)(3):Eu3+ particles were prepared by the sol-gel method. The samples were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy, transmission electron microscopy, photoluminescence (PL) and low-voltage cathodoluntinescence (CL). PL and CL study revealed that the core-shell structured SiO2@Gd-2(WO4)(3):Eu3+ particles show strong red emission dominated by the D-5(0)-F-7(2) transition of Eu3+ at 615 nm with a lifetime of 0.89 ins. The PL and CL emission intensity can be tuned by the coating number of Gd-2(WO4)(3):Eu3+ phosphor layers on SiO2 particles, the size of the SiO2 core particles, and by accelerating voltage and the filament current, respectively.