Sonochemical synthesis and luminescence properties of single-crystalline BaF2:Eu3+ nanospheres

BaF2 nanocrystals doped with 5.0 mol% Eu3+ has been successfully synthesized via a facile, quick and efficient ultrasonic solution route employing the reactions between Ba(NO3)(2), Eu(NO3)(3) and KBF4 under ambient conditions. The product was characterized via X-ray powder diffraction (XRD), scanning electron micrographs (SEM), transmission electron microscopy (TEM), high-resolution transmission electron micrographs (HRTEM), selected area electron diffraction (SAED) and photoluminescence (PL) spectra. The ultrasonic irradiation has a strong effect on the morphology of the BaF2:Eu3+ particles. The caddice-sphere-like particles with an average diameter of 250 nm could be obtained with ultrasonic irradiation, whereas only olive-like particles were produced without ultrasonic irradiation. The results of XRD indicate that the obtained BaF2:Eu3+ nanospheres crystallized well with a cubic structure. The PL spectrum shows that the BaF2:Eu3+ nanospheres has the characteristic emission of Eu3+ D-5(0)-F-7(J) (J = 1-4) transitions, with the magnetic dipole D-5(0)-F-7(1) allowed transition (590 nm) being the most prominent emission line.

Facile sonochemical synthesis of single-crystalline europium fluorine with novel nanostructure

A single-crystalline EuF3 nanoflower with a novel three-dimensional (3D) nanostructure has been successfully synthesized via a facile, fast, efficient, and mild ultrasonic irradiation solution route employing the reaction of Eu(NO3)(3) and KBF4 under ambient conditions without any template or surfactant. The ultrasonic irradiation plays an important role and is necessary for the synthesis of EuF3 with the complex structure. The formation mechanism of this complex nanostructure is proposed in this paper. No template or surfactant is used in this method, which avoids the subsequent complicated workup for the removal of the template or surfactant. Furthermore, a substantial reduction in the reaction time as well as the reaction temperature is observed compared with the hydrothermal process.

Morphology of polyimide fibers derived from 3,3 ',4,4 '-biphenyltetracarboxylic dianhydride and 4,4 '-oxydianiline

As one member of high performance fibers, aromatic polyimide fibers possess many advantages, such as high strength, high modulus, high and low temperature resistance, and radiation resistance. However, the preparation of the high performance fibers is so difficult that the commercial fibers have not been produced except P84 with good flame retardancy. In this report, a polyimide was synthesized from 3,3',4,4'-biphenyltetracarboxylic dianhydride (BPDA) and 4,4'-oxydianiline (ODA) and the fibers were prepared from its solution by a dry-jet wet-spinning process. The formation of the as-spun fibers in different coagulation bath composition was discussed. Scanning electron microscope (SEMI) was employed to study the morphology of the as-spun fibers. As a result, the remnant solvent existed in the as-spun fibers generated from coagulation bath of alcohol and water. There were many fibrils and microvoids with the dimension of tens of nanometers in the fibers. One could observe the obvious fibrillation and the drawn fibers.

Thermal mechanical and dynamic mechanical property of biphenyl polyimide fibers

High-performance polyimide fibers possess man), excellent properties, e.g., outstanding thermal stability and mechanical properties and excellent radiation resistant and electrical properties. However, the preparation of fibers with good mechanical properties is very difficult. In this report, a biphenvl polyimide from 3,3',4,4'-biphenyltetracarboxylic dianhydride and 4,4'-oxydianiline is synthesized in p-chlorophenol by one-step polymerization. The solution is spun into a coagulation bath of water and alcohol via dry-jet wet-spinning technology. Then, the fibers are drawn in two heating tubes. Thermal gravimetric analysis, thermal mechanical analysis, and dynamic mechanical analysis (DMA) are performed to study the properties of the fibers. The results show that the fibers have a good thermal stability at a temperature of more than 400degreesC. The linear coefficient of thermal expansion is negative in the solid state and the glass transition temperature is about 265degreesC. DMA spectra indicate that the tandelta of the fibers has three transition peaks, namely, alpha, beta, and gamma transition. The alpha and gamma transition temperature, corresponding to the end-group motion and glass transition, respectively, extensively depends on the applied frequency, while the beta transition does not.

The morphology and thermal properties of multi-walled carbon nanotube and poly(hydroxybutyrate-co-hydroxyvalerate) composite

Nanocomposites based on poly(hydroxybutyrate-co-hydroxyvalerate) (PHBV) and multi-walled carbon nanotubes (MWNTs) were prepared by solution processing. Ultrasonic energy was used to uniformly disperse MWNTs in solutions and to incorporate them into composites. Microscopic observation reveals that polymer-coated MWNTs dispersed homogenously in the PHBV matrix. The thermal properties and the crystallization behavior of the composites were characterized by thermogravimetric analysis, differential scanning calorimetry and wide-angle X-ray diffraction, the nucleant effect of MWNTs on the crystallization of PHBV was confirmed, and carbon nanotubes were found to enhanced the thermal stability of PHBV in nitrogen.

Preparation and properties of microporous membrane from poly(vinylidene fluoride-co-tetrafluoroethylene) (F2.4) for membrane distillation

Flat-sheet microporous membranes from F2.4 for membrane distillation (MD) were prepared by phase inversion process. Dimethylacetamide (DMAC) and LiClO(4)(.)3H(2)O/trimethyl phosphate (TMP) were, respectively, used as solvent and pore-forming additives. The effects of casting solution composition, exposure time prior to coagulation and temperature of precipitation bath on F2.4 membrane structure were investigated. The morphology of resultant porous membrane was observed by scanning electron microcopy. Some natures of F2.4 porous membrane after drying in air, such as mechanical properties and hydrophobicity, were exhibited and compared with poly(vinylidene fluoride) (PVDF) membrane prepared by the same ways. Stress-at-break and strength stress of F2.4 microporous membrane are higher than that of PVDF membrane, and elongation percentage of F2.4 membrane at break is about eight-fold as great as that of PVDF membrane. Contact angle of F2.4 microporous membrane to water (86.6 +/- 0.51degrees) was also larger than that of PVDF mernbrane (80.0 +/- 0.78degrees). MD experiment was carried out using a direct contact membrane distillation (DCMD) configuration as final test to permeate performance of resultant microporous membrane.

Factors affecting pore structure and performance of poly(vinylidene fluoride-co-hexafluoro propylene) asymmetric porous membrane

Preparation of poly(vinylidene fluoride-co-hexafluoro propylene) (F2.6) flat-sheet asymmetric porous membrane has been studied for the first time. Factors affecting F2.6 membrane pore structure and permeate performance, such as macromolecule pore formers (polyethylene glycol-400, 1000, 1540, 2000 and 6000), the small molecule former (glycerol), swelling agent (trimethyl phosphate) in casting solution, precipitating bath component and temperature, exposure time and ambient humidity, were investigated in detail. Average pore radius and porosity were used to characterize F2.6 membrane structure, and respectively, determined by ultrafiltration and gravimetric method for the wet membrane. Morphology of the resultant membranes was observed by scanning electronic microscopy (SEM). Final test on permeate performance of F2.6 porous membrane was carried out by a direct contact membrane distillation (DCMD) setup. The experimental F2.6 membrane exhibits a higher distilled flux than PVDF membrane under the same operational situations. The determination of contact angle to distilled water also reveals higher hydrophobic nature than that of PVDF membrane.

Green electroluminescent device with a terbium beta-diketonate complex as emissive center

In this study, a terbium complex, Tb(acac)(3)bath (acac: acetylacetone, bath: 4,7-diphenyl-1,10-phenanthroline), was synthesized and its luminescent properties were investigated compared with the reported terbium complex, Tb(acac)(3)phen (phen: phenanthroline). When it was used as an emitting material in organic electroluminescent (EL) device, the triple-layer-type device with a structure of glass substrate/ITO (indium-tin oxide)/TPD (N,N'-diphenyl-N,N'-bis(3-methylphenyl)-1,1'-biphenyl-4,4'-diamine)/Tb(acac)(3)bath/Alq(3) (tris (8-hydroxyquinolinato) aluminum)/Al (aluminum) exhibited bright characteristic emission of terbium ion upon applying DC voltage. An apparent difference was observed between the photoluminescence spectrum and the EL spectrum. The EL device exhibited some characteristics of diode and the maximum luminance of 77 cd/m(2) was obtained at 17 V.

Determination of sulpiride by capillary electrophoresis with end-column electrogenerated chemiluminescence detection

Background: Capillary electrophoresis (CE) with tris(2,2'-bipyridyl)ruthenium(II) [Ru(bpy)(3)(2+)]-electro-generated chemiluminescence (ECL) detection is a promising method for clinical analysis. In this study, a method combining CE with Ru(bpy)(3)(2+) ECL (CE-ECL) detection that can be applied to amine-containing clinical species was developed, and the performance of CE-ECL as a quantitative method for determination of sulpiride in human plasma or urine was evaluated. Methods: Sulpiride was separated by capillary zone electrophoresis in uncoated fused-silica capillaries [510 cm x 25 mum (i.d.)] filled with phosphate buffer (pH 8.0 and a driving voltage of +15 kV, with end-column Ru(bpy)(3)(2+) ECL detection. A platinum disc electrode was used as working electrode. Sulpiride in human plasma or urine samples (100 muL) was extracted by a double-step liquid-liquid extraction procedure, dried under nitrogen at 35 degreesC in a water bath, and reconstituted with 100 muL of filtered water. The extraction solvent was ethyl acetate-dichloromethane (5:1 by volume). Results: Under optimum conditions (pH 8.0 phosphate buffer, injection for 6 s at 10 kV, and +1.2 V as detection potential), separation of sulpiride was accomplished within 4 min. The calibration curve was linear over a concentration range of 0.05-25.0 mumol/L, and the limit of detection was 2.9 x 10(-8) mol/L for sulpiride. Intra- and interday CVs for ECL intensities were <6%. Extraction recoveries of sulpiride were 95.6-101% with CVs of 2.9-6.0%. The method was,clinically validated for patient plasma and urine samples. Conclusions: CE combined with Ru(bpy)(3)(2+) ECL is reproducible, precise, selective, and enables the analysis of sulpiride in human plasma and urine. It thus is of value for rapid and efficient analysis of amine-containing analytes of clinical interest.

Preparation and properties of conductive polyaniline/poly-omega-aminoundecanoyle fibers

Historically, polyaniline (PANI) had been considered an intractable material, but it can be dissolved in some solvents. Therefore, it could be processed into films or fibers. A process of preparing a blend of conductive fibers of PANI/poly-omega-aminoun-decanoyle (PA11) is described in this paper. PANI in the emeraldine base was blended with PA11 in concentrated sulfuric acid (c-H,SO,) to form a spinning dope solution. This solution was used to spin conductive PANI/PA11 fibers by wet-spinning technology. As-spun fibers were obtained by spinning the dopes into coagulation bath water or diluted acid and drawn fibers were obtained by drawing the as-spun fibers in warm drawing bath water. A scanning electron microscope was employed to study the effect of the acid concentration in the coagulation bath on the microstructure of as-spun fibers. The results showed that the coagulating rate of as-spun fibers was reduced and the size of pore shrank with an increase in the acid concentration in the coagulation bath. The weight fraction of PANI in the dope solution also had an influence on the microstructure of as-spun fibers. The microstructure of as-spun fibers had an influence on the drawing process and on the mechanical properties of the drawn fibers. Meanwhile, the electrically conductive property of the drawn fibers with different percentage of PANI was measured.

Effect of physical aging on the microstructure and the crystallization of amorphous poly(aryl ether ether ketone ketone) (PEEKK)

Physical aging of poly(aryl ether ether ketone ketone) (PEEKK) has been investigated. Heat flow responses were measured after annealing the amorphous samples obtained by quenching the melt into an ice-water bath close to, but below, the glass transition temperature. The extent of aging is related to the supercooling from the glass transition temperature and to the aging time. The activation energy of the aging process, which was estimated by a Williams-Watt expression, is similar in magnitude to that obtained for the cold crystallization for the aged samples. The quenched glass is a metastable glass. The conformation of molecular chains rearranges with physical aging which results in the formation of a denser packing in the amorphous phase. The dense amorphous phase may form an initial nucleus for crystallization. Isothermal cold crystallization of the aged samples was carried out. The Avrami equation was used to determine the kinetic parameters, and the Avrami constant n is about 2. An Arrhenius expression was used to evaluate the activation energy of relaxation upon physical aging and the activation energy of transportation upon isothermal crystallization. The activation energy of relaxation is similar in magnitude to that of crystallization for aged samples. Results obtained are interpreted as kinetic effects associated with the glass formation process.

Physical aging and crystallization of amorphous poly(aryl ether ether ketone ketone)

Physical aging of poly(aryl ether ether ketone ketone) (PEEKK) was investigated. Heat flow responses were measured after annealing the amorphous samples that were obtained by quenching the melt into an ice-water bath at just below the glass transition temperature. Isothermal cold crystallization of the aged samples was carried out. The Avrami equation was used to determine the kinetic parameters, and the Avrami constant it is about 2. An Arrhenius form was used to evaluate the relaxation activation energy of physical aging and the transport activation energy of isothermal crystallization. The activation energy of physical aging was similar in magnitude to that observed for the temperature dependence of crystallization under conditions of transportation control. Results obtained were interpreted as purely kinetic effects associated with the glass formation process. (C) 1998 John Wiley & Sons, Inc.

The fabrication of dipped CdS and sputtered ITO thin films for photovoltaic solar cells

Stable bilayer thin films of indium tin oxide (ITO) on CdS and CdS on ITO were formed for the window material of solar cells by chemical bath and sputtering methods. Scanning electron microscopy and X-ray diffraction studies have shown that both the ITO and CdS films are continuous, homogeneous, with high compactness. Measurement of the CdS film thickness across the 2 x 4 cm(2) reveals the good uniformity of these films. Four-point probe measurements show that the resistivity of a CdS film on an ITO surface is much better than that of the single CdS film The thermal stability of an ITO/CdS bilayer, interfacial reaction and optical transmittance were investigated at different annealing temperatures and environments (air, vacuum and N-2 + H-2). The results showed that the ITO/CdS bilayer film is a good window material for the CuInSe2 and CdTe cells. It is a simple method using a small amount of the cadmium compound.

Relationship between the structure and catalytic activity of La2-xSrxNiO4-lambda(0<=x<=1) mixed oxides for NH3 oxidation

A series of samples having the composition of La2-xSrxNiO4(0 less than or equal to x less than or equal to 1) were prepared and used as catalysts for NH3 oxidation. It was found that the La and oxygen vacancies exist in the La2-xSrxNiO4-lambda(0 less than or equal to x less than or equal to 1). The unit cell volume decreases with the increase of x. For bath c and a parameters there appeared a turning point at x = 0.5. Doping with a lower valence cation Sr2+ in the case of La2NiO4 resulted in an increase of Ni3+, consequently the formation of oxygen vacancies, the increase of reducing ability and the increase of catalytic activity. In the oxygen TPD of La2-xSrxNiO4(0 less than or equal to x less than or equal to 1) appeared three peaks, the alpha' peak at about 400K was attributed to the surplus oxygen desorption, the a peak at 700K which approaches to a maxium at x = 0.6 was attributed to the oxygen adsorbed at oxygen vacancies. The beta peak at about 1000K which depends closely on the x and favors the catalytic activity was attributed to the reduction of Ni3+. The catalytic activity of La-2-x SrxNiO4 mixed oxides in the NH3 oxidation in general could be attributed to the extent of the redox reaction: 2Ni(2+) + O-2 + V-0(..) reversible arrow 2Ni(3+) + 20(-) where V-0(..) representes the oxygen vacancies and O- the oxygen species adsorbed at the vacancies.

ELECTRODEPOSITION OF POLYCRYSTALLINE CD-RICH HG1-XCDXTE AND PHOTOELECTRO-CHEMICAL BEHAVIOR OF HG0.09CD0.91TE THIN-FILM

Electrodeposition process of polycrystalline Cd-rich Hg_(1-z)Cd_xTe (x>0.5) in acidic bath of CdSO_4+HTeO_2~+HgCl_2 was investigated. The simultaneous electrodeposition technique of three kinds of ions at the same potential has been achieved. The XRD, SEM and EDAX analysis of the thin film electrodeposited on titanium substrate showed a typical cubic zinc blende polycrystalline structure and homogeneous dispersion. The photoelectrochemical behavior of (1-x)=0.09 polycrystalline thin film in a polysulfide re...