Nd~(3+)掺杂对LiFePO_4结构及电化学性能的改善

采用两步加热高温固相法合成了掺杂Nd3+的LiFe1-xNdxPO4/C复合材料(x=0,0.01,0.02,0.04,0.06,0.08)。用TG-DSC对前驱体进行分析和SQUID(超导量子干涉仪)对样品中Fe3+的磁性测定,优化了合成工艺条件;采用XRD、FE-SEM、EDS等方法分析了样品的结构并对其电化学性能进行了测试。结果表明:LiFe1-xNdxPO4/C复合材料具有橄榄石型结构;当Nd3+的掺杂量6%(物质的量分数)、煅烧温度700℃、煅烧时间16 h时,样品在0.2C(1C=170.0 mA.g-1)电流密度下的最大放电比容量可达165.2 mAh.g-1,循环100次后的容量保持率仍为92.8%,在1C、2C、5C下的最大放电比容量分别为146.8、125.7和114.8 mAh.g-1。通过测定样品在不同较低倍率下的放电比容量,采用外推法得出制备样品的实测理论比容量为168.7 mAh.g-1。

快充MH-Ni电池AB3型负极合金与隔膜相互匹配的研究

(ML_(0.70)Mg_(0.12)Zr_(0.07)Gd_(0.05)MY_(0.06))Ni_(2.87)Al_(0.08)Co_(0.15)是具有快速充电能力的AB_3型负极合金材料,将此负极合金与正极以及尼龙或聚丙烯隔膜组成的快充形MH-Ni电池,研究了负极合金与隔膜的相互匹配性。结果表明:用交联型聚丙烯酸盐对隔膜改性生成的聚丙烯隔膜与该AB_3型负极合金有良好的匹配性。

Random lasing emission from a red fluorescent dye doped polystyrene film containing dispersed polystyrene nanoparticles

The authors report a random lasing emission from 4-(dicy-anomethylene)-2-t-butyl-6(1,1,7,7-tetramethyljulolidyl-9-enyl)-4H-pyran doped polystyrene thin films by introducing polystyrene nanoparticles. The aspects of concentration and diameter of polystyrene nanoparticles have been intensively investigated and found that the lasing occurs due to the scattering role of polystyrene nanoparticles. The devices emit a resonance multimode peak centered at a wavelength of 630 nm with a mode linewidth of less than 0.35 nm and exhibit threshold excitation intensity of as low as 0.06 mJ pulse(-1) cm(-2). The microscopic laser cavities formed by multiple scattering have been captured. The demonstration of random laser opens up the possibility of using organic scattering as alternative sources of coherent light emission.

Synthesis and photoluminescence properties of erbium-doped BaF2 nanoparticles

Erbium-doped BaF2 nanoparticles were prepared from the microemulsion of cetyl trimethyl ammonium bromide (CTAB), n-butanol, n-octane and water. The X-ray diffraction (XRD) patterns were indexed to a pure BaF2 cubic phase. Transmission electron microscopy (TEM) images showed that BaF2 products were monodispersed with 15-20 nm in size at the dopant concentration of 0.06 mol%. At higher dopant concentration, there was no significant increase in particle size, but more polydispersed. Photoluminescence (PL) properties of the final products were examined. We can observe fluorescence of Er3+ around 1540 nm and with the increase of dopant concentration, the fluorescent intensity increases.

Synthesis and fluorescence of europium-doped barium fluoride cubic nanocolumns

Europium-doped barium fluoride cubic nanocolumns were synthesized from the quaternary water in oil reverse microemulsions In this process, the aqueous cores of water/cetyl trimethyl ammonium bromide (CTAB)/n-butanol/n-octane reverse microemulsions were used as microreactors for the precipitation of europium doped barium fluoride. XRD analysis shows that under the dopant concentration of 0.06% (molar fraction), the products are single phase. The result products are cubic column-like with about 30 similar to 50 nm edge length of cross section, and about 200 nm of length obtained from the transmission electron microscopy (TEM), and atomic force microscopy (AFM). Under the 0.06 % (molar fraction) of dopant concentration I the fluorescence of Eu2+ and Eu3+ under the 589 of excitation wavelength is observed.

A new luminescent material: Li2CaSiO4 : Eu2+

In our study, the Eu2+ doped Li2CaSiO4 phosphors were initially synthesized by high temperature solid state method, and their luminescent properties were also investigated. Eu2+ ions occupied 8-coordinatid distorted dodecahedral Ca sites, leading to strong crystal field splitting. The strong crystal field splitting made the broad excitation band extending from UV to visible region. In addition, the high concentration of Li+ ions in the structure constrained the distortion of the emission centers, then resulted in a small stokes shift, similar to 1100 cm(-1). Under excitation, the Li2CaSiO4:Eu2+ phosphors emitted bluish green light with peak of 480 nm, FWHM of 31 nm and color coordination of (0.06, 0.44). The Eu2+ doped Li2CaSiO4 phosphor would be suitable for bluish green phosphor of white LEDs due to its excellent excitation profile and chromaticity.

Isothermal crystallization of poly(3-hydroxybutyrate-co-3-hydroxyvalerate)

Isothermal crystallization behavior of poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) was investigated by means of differential scanning calorimetry and polarized optical microscopy (POM). The Avrami analysis can be used successfully to describe the isothermal crystallization kinetics of PHBV, which indicates that the Avrami exponent n = 3 is good for all the temperatures investigated. The spherulitic growth rate, G, was determined by POM. The result shows that the G has a maximum value at about 353 K. Using the equilibrium melting temperature (448 K) determined by the Flory equation for melting point depression together with U-* = 1500 cal mol(-1), T-infinity = 30 K and T-g = 278 K, the nucleation parameter K-g was determined, which was found to be 3.14+/-0.07 x 10(5) (K-2), lower than that for pure PHB. The surface-free energy sigma = 2.55 x 10(-2) J m(-2) and sigma(e) = 2.70+/-0.06 x 10-2 J m(-2) were estimated and the work of chain-folding (q = 12.5+/-0.2 kJ mol(-1)) was derived from sigma(e), and found to be lower than that for PHB. This implies that the chains of PHBV are more flexible than that of PHB.

Alkali metal ions transfer across a water/1,2-dichloroethane interface facilitated by a novel monoaza-B15C5 derivative

In this paper, a novel monoaza-B15C5 derivative, N-(2-tosylamino)-isopentyl-monoaza-15-crown-5 (L), is used as an ionophore to facilitate alkali metal cations transfer across a water/1,2-dichloroethane (W/DCE) interface. Well-defined voltammetric behaviors are observed at the polarized W/DCE interfaces supported at micro- and nano-pipets except Cs+. The diffusion coefficient of this ionophore in the DCE phase is calculated to be equal to (3.3+/-0.2) x 10(-6) cm(2) s(-1). The experimental results indicate that a 1:1 (metal: ionophore) complex is formed at the interface with a TIC/TID mechanism. The selectivity of this ionophore towards alkali ions follows the sequence Na+ > Li+ > K+ > Rb+ > Cs+. The logarithm of the association constants (log beta(1)(0)) of the LiL+, NaL+, KL+ and RbL+ complexes in the DCE phase are calculated to be 10.6, 11.6, 9.0 and 7.1, respectively. The kinetic parameters are determined by steady-state voltammograms using nanopipets. The standard rate constants (k(0)) for Li+, Na+, K+ and Rb+ transfers facilitated by L are 0.54+/-0.05, 0.63+/-0.09, 0.51+/-0.04 and 0.46+/-0.06 cm s(-1), respectively. The pH values of aqueous solution have little effect on the electrochemical behaviors of these facilitated processes. The results predicate that this new type of ionophore might be useful to fabricate electrochemical sensor of sodium ion.

End-column amperometric detection of aesculin and aesculetin by capillary electrophoresis

Determination of aesculin (AL) and aesculetin (AT) by capillary electrophoresis with end-column amperometric detection using a 33 mu m microdisk carbon fiber electrode is described. The HDVs, the effect of pH, buffer concentration, injection voltage, injection time and separation voltage on the peak current response (i(p)) of the analytes and the number of theoretical plates (N) were studied. The method has high sensitivity and good reproducibility. Under the optimum condition - 10 mM, pH 9.00 phosphate buffer, 4 s at 9 kV injection, separation at 15 kV and +1.0 V as the detection potential - low detection limits (S/N = 3) of 0.06 and 0.3 mu M were obtained for AL and AT, respectively. The calibration curve was linear over three orders of magnitude. The relative standard deviations (n = 15) of peak current and migration time were 3.9% and 4.6%, and 0.96% and 0.75% for 15 consecutive injections of 5 mu M AL and AT, respectively. The use of this method for the separation and detection of the two compounds present in the traditional Chinese medicine and human urine samples is also reported. (C) 1999 Elsevier Science B.V. All rights reserved.

Simultaneous voltammetric determination of acetophenetidin, aminopyrine, acetaminophenol and aminophenol on a glassy carbon electrode

The voltammetric behaviour of acetophenetidin(A(1)) aminopyrine(A(2)) acetaminophenol(A(3)) and aminophenol(A(4)) was investigated by linear-sweep, differential-pulse, cyclic voltammetry at a glassy carbon electrode. In a medium of 0.1 mol/L NaOH solution, 4 high sensitivity and resolution anodic peaks were obtained. Their peak potentials are about at 0.68 V, 0.51, 0.22 and - 0.06 V( vs. Ag/AgCl). They can be used for direct determination of A(1), A(2),A(3),A(4) in samples respectively. The method is simple and rapid. The mechanism of the electrode reaction was discussed.

多组分有机物在玻碳电极上的伏安法测定

对乙酰氨基苯乙醚、氨基比林、乙酰氨基苯酚、氨基苯酚等4种有机物在玻碳电极上的伏安行为进行了研究.在0.1mol/L氢氧化钠溶液中得4个灵敏度和分辨率良好的阳极氧化峰,E_p分别为0.68,0.51,0.22,-0.06 V(vs.AgCl/Ag)左右,样品不需分离直接测定.20多种有机生化物质不干扰,方法简便快速.并对电极反应进行了探讨.

Structure and luminescent properties of YAG : Eu, Bi synthesized by sol-gel method

(Y1-xEux)(3)Al5O12 and (Y1-x-yEuxBiy)(3)Al5O12 were prepared by so-gel method. Their structures of the luminophor are similar to that of YAG, which is recorded on the ASTM card and belongs to a cubic system. The luminescent properties show that the reaction temperature of the current sol-gel method is in the range of 400-500 degrees C, which is lower than that of the conventional solid state reaction. The luminophors have the strongest emission intensity when the values of x and y are 0.06 and 0.013, respectively.

Fractal roughness characterization of super-ground Mn-Zn ferrite single crystals

The surface of superground Mn-Zn ferrite single crystal may be identified as a self-affine fractal in the stochastic sense. The rms roughness increased as a power of the scale from 10(2) nm to 10(6) nm with the roughness exponent alpha = 0.17 +/- 0.04, and 0.11 +/- 0.06, for grinding feed rate of 15 and 10 mu m/rev, respectively. The scaling behavior coincided with the theory prediction well used for growing self-affine surfaces in the interested region for magnetic heads performance. The rms roughnesses increased with increase in the feed rate, implying that the feed rate is a crucial grinding parameter affecting the supersmooth surface roughness in the machining process.

The rheological properties of polyaniline solution

This paper presents our work on the rheological properties of the solution of polyaniline (PAn) in N-methyl-2-pyrrolidone (NMP). The results indicate that the solution's non-Newtonian property becomes more prominent with the increase in solution concentrations exhibiting the behavior of pseudo-plastic fluid. Besides, there is a critical concentration C-v (around 0.06 g/ml), beyond which the viscosity of the PAn/NMP solution takes a sudden increase. with temperature rising, both the viscosity and the thixotropy of the solution decrease, implying that there exist physical cross-linking interactions between the molecular chains in the solution.

ELECTROCHEMICAL DETECTION OF COBALT IN HAIR FOLLOWING ON-COLUMN DERIVATIZATION WITH 1-(2-PYRIDYLAZO)-2-NAPHTHOL-6-SULFONIC ACID AND REVERSED-PHASE LIQUID-CHROMATOGRAPHY

A method for the specific determination of cobalt based on reversed-phase liquid chromatography with amperometric detection via on-column complex formation has been developed. A water-soluble chelating agent, 1-(2-pyridylazo)-2-naphthol-6-sulphonic acid (PAN-6S), is added to the mobile phase and aqueous cobalt solutions are injected directly into the column to form in situ the cobalt-PAN-6S chelate, which is then separated from other metal PAN-6S chelates and subjected to reductive amperometric detection at a moderate potential of -0.3 V. Because the procedure eliminates the interference of oxygen and depresses the electrochemical reduction of the mobile phase-containing ligand PAN-6S, by virtue of the quasi:reversible electrode process of the cobalt-PAN-6S complex, a low detection limit of 0.06 ng can be readily obtained. Interference effects were examined for sixteen common metal species, and at a 5- to 8000-fold excess by mass no obvious interference was observed. The feasibility of the method as an approach to the specific analysis of cobalt in a hair sample has been demonstrated.