25 December 2011, Volume 42 Issue 12
    

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  • Progress in Preparation of Polymer Microporous Membrane via Thermally Induced Phase Separation
    Cheng Chen;Li-Ping Zhu;Bao-Ku Zhu;XU You Yi
    . 2011, 42(12): 2124-2129.
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    Thermally induced phase separation (TIPS) is an important approach to prepare polymer microporous membrane. Since it was invented, it has always been the hotspot in the research field of membrane technology. In recent years, tremendous efforts have been made to overcome its original shortcomings. Firstly, it is combined with other formation methods, including nonsolvent induced phase separation, stretching, supercritical carbon dioxide method and so on. Secondly, hydrophilic polymer and amphipathic additives are used in TIPS so as to improve its hydrophilicity. Thirdly, the selection scope of new polymer material is expanded from crystalline polymer to amorphous polymer. In this article, this new trend in preparing polymer microporous membrane via TIPS is reviewed.
    • 研究与开发
  • Investigation on the electrical conductivity and synthetic kinetics of TiO2 doped NiO-NiF2O4
    Shu-Lan Wang;Rong-Hai LiGuang-Chun Yao
    . 2011, 42(12): 2130-2132.
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    NiO-NiF2O4 and 0.5%TiO2 doped NiO-NiF2O4 were synthesized within temperatures of1173-1213K by the solid reaction method. X-ray diffraction technique was used to characterize the synthesized products. The electrical conductivity of the sample versus time was obtained by putting the sample in between two platinum plates and measuring the resistance of the sample during heating. The kinetic equation of the steady diffusion control was established and the synthetic rate and the influence of 0.5%TiO2 on the synthetic rate of NiFe2O4 was discussed. The rate coefficient and the activation as well as the average diffusion coefficient of Ni2+ and Fe3+ were obtained.
  • Analysis of Mechanical Effects for the Cracks in Large-scale KDP Crystals during Getting out from crystallizers with Numerical Simulation Method
    Ning Zhang;Qiang-Yong Zhang;Yun-Sun
    . 2011, 42(12): 2133-2136.
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    During getting the large-scale KDP (Potassium Dihydrogen Phosphate,KH2PO4) crystals out from crystallizers cracking phenomenon occurs frequently, which usually results in large financial losses, to investigate mechanical effects of the cracks in large-scale KDP crystals and propose a reasonable method to prevent cracks, this paper simulates the process getting the large-scale KDP crystals out from crystallizers with the finite element method, the changes of stress field in the KDP crystals have been got. The results show the maximum stress in the KDP crystals increases more than 100 times during the cooling process, while the maximum stress increases very little after the mechanical boundary conditions changed, those data indicate that the decrease of temperature resulting in the stress concentration is the main reason for the crystals crack. The discovery of those conclusions provides important theoretical basis for proposing crack control measures of the large-scale KDP crystals.
  • Hydrogen Desorption Properties of Ni Nanoparticles Doped Mg(NH2)2 Hollow Nanosphere Mixed with LiH
    Xuan-Zhou Zhang;Yun-Zhi Yang;Ping Song
    . 2011, 42(12): 2137-2140.
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    Mg3N2 nanocubes with particle size about 50 nm were synthesized by vaporized bulk magnesium with ammonia plasma metal reaction. Reacted the Mg3N2 nanocubes with NH3, Mg(NH2)2 hollow nanospheres with particle sizes of about 80 nm and the shell thickness of about 10 nm were successfully synthesized. Hydrogen desorption temperature of Mg(NH2)2 + 2LiH system was lowered by use of Mg(NH2)2 hollow nanospheres, and the desorption activation energy was lowered from 149.1 kJ mol-1 to 117.6 kJ mol-1. Furthermore, the desorption activation energy was lowered to 108.0 kJ mol-1 by doping with Ni nanoparticles. The particle size of resultant after dehydrogenation lied on the size of Mg(NH2)2. The factors on the hydrogen desorption kinetics of Mg(NH2)2 + 2LiH system were also discussed.
  • In situ study of the kinetics of growth steps on (100) faces of zinc(tris) thiourea sulphate crystal
    Hang Shi
    . 2011, 42(12): 2141-2145.
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    Abstract: In-situ observation of movement process of steps on the (100) face of ZTS crystal in aqueous solutions was performed by using optical microscopy. The displacement velocities under different conditions of predefined supersaturation, actual steps height, growth durations, and densities of kinks on the steps edge were obtained. The dependence of the rate difference between various steps on the supersaturation was explained by the “net flux model”. The values of activation energy for integration of growth unit in a step and kinetic coefficient for a unit-hight step were calculated. Results show that the average displacement rate of steps increases linearly with an increase in supersaturation, and the velocity of steps decreases with an increase in their height. The change of the step displacement rate with growth duration is related to the processes of reorganisation of step. Meanwhile the value and changing trend of step displacement rate are primarily determined by the density of kinks on step edge.
  • Preparation of Yb3+-doped ZnO nanopowders and its photocatalytic activity
    Tian-You Peng;Hong-Jin Lv;Jiang-Rong Xiao
    . 2011, 42(12): 2146-2149.
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    ZnO nanopowders were prepared through a direct precipitation method, and then dipped into Yb(NO3)3 aqueous solution to obtain the Yb3+-doped ZnO nanoparticles. The obtained ZnO nanopowders and its Yb3+-doped products were characterized by XRD, FESEM, HRTEM, XPS, diffuse reflection absorption spectrum and spectrophotometry. The experimental results show that the obtained ZnO nanoparticles after calcinations at 500℃ are hexagonal crystal phase with narrower particle size distribution. Moreover, the samples were employed for the photodegradation of Rhodamine B in an aqueous suspension, and it was found that suitable Yb3+-doping levels can efficiently improve the photocatalytic activity of the obtained ZnO nanoparticles.
  • Effect of metallic phase on relative density of NiFe2O4-10NiO based cermet for aluminum electrolysis
    Han-Bing He;Yi-Hong Qin;Han-Ning Xiao
    . 2011, 42(12): 2150-2152.
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    xNi/(NiFe2O4-10NiO), xCu/(NiFe2O4-10NiO)和x(80Cu-Ni)/(NiFe2O4-10NiO) cermets were prepared with the cold isostatic pressing?sintering process. The effect of metallic content and type on relative density was analyzed. The results show that the relative density of cermets is first increases and then decreases along with the increase of metallic content, while Obtains maximum at 5% metallic content. The influence degree of metallic type on relative density is different, but the change trend of relative density is consistent, so that the effect of metallic phase on relative density have promotion and obstruction dual role.
  • Effect of Ca/Si ratio on the microstructures and properties of CaO-B2O3-SiO2 glass-ceramics
    Hui Shao;Hong-Qing Zhou;;bing dai;
    . 2011, 42(12): 2153-2156.
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    Influence of Ca/Si on the crystallization, microstructure and dielectric properties of CaO-B2O3-SiO2 glass was studied by using XRD,DCS and SEM. The results indicate that When M (Ca/Si ratio) <1.08, calcium borosilicate glass sintering temperature higher than 900 ℃, but it is M> 1.08, CBS department of the sintering temperature of glass is far lower at 900 ℃. When M reaches 1.767, CBS can not be sintered; With the increase of CaO content, Ca2SiO4 crystals gradually increased, leading to the gradual reduction of wollastonite phase, resulting in gradual increase in quartz; The samples were C2,C5, C7 dielectric loss sintered <2×10-3 at 1MHz.
  • Synthesis and characterization of Some Novel Flame Retardants Polyphosphamides with Enhanced Phosphorus-Nitrogen Content
    Rui-Lan Fan;Guan-Qun Yun;Zhan-Xi Bian
    . 2011, 42(12): 2157-2161.
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  • Finite Element Analysis of Thermal Insulation in Double-ceramic-layer Thermal Barrier Coatings
    Guo-Dong Zhou;Shu-Hai Chen;Ji-Hua Huang
    . 2011, 42(12): 2162-2165.
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    Abstract: The opaque and translucent physical models of double-ceramic-layer thermal barrier coatings were established with theory of thermal conduction and convection and radiation. The steady temperature field was simulated with ANSYS software. The results show that when the double ceramic is opaque, the thickness of double or top ceramic layer increases, upper side temperature of top ceramic layer increases nearly linearly, and upper side temperature of second ceramic and bonding layer decrease nearly linearly. When the double ceramic is weakly translucent, the trend is similar to opaque. When the double ceramic is highly translucent, the thickness of top ceramic layer increases, upper side temperature of top ceramic layer is a little lower than opaque, and upper side temperature of second ceramic layer is higher than opaque, and upper side temperature of bonding layer firstly fast and slowly increases and keeps no change, but much higher than opaque, and reflection has some effect on reducing temperature of every layer.
  • Catalytic oxidation of 2-mercaptoethanol by Activated Carbon Fibers supported Cobalt Phthalocyanine
    Yu-Yuan Yao;Feng-Xiang Sheng;Xiong-Ping Wu
    . 2011, 42(12): 2171-2175.
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    ACF-CoPc was prepared by immobilizing Cobalt tetra (2,4-bichloro-1,3,5-triazine) aminophthalocyanines on the modified activated carbon fibers by covalent bond, characterized by Thermogravimetric Analysis, Atomic Absorption Spectrometry and Nitrogen Isothermal Adsorption. The loading amount of CoPc was 5.26μmol/g. The analysis by Nitrogen Isothermal Adsorption indicated that specific surface area of ACF-CoPc was 1235.9m2/g, and the pore size distributions was mainly micropore of about 2nm. Ultra Performance Liquid Chromatography was adopted to investigate the catalytic ability of 2-mercaptoethanol by ACF-CoPc. The results demonstrated that the removal rate of 2-mercaptoethanol was up to 100% by ACF-CoPc, and the product was 2-hydroxyethyl disulfide. In addition, the catalytic ability of ACF-CoPc remained essentially constant after six repetitive experiments, suggesting that ACF-CoPc could be reused.
  • Preparation and properties of MMT/PA6 intercalate composite
    Zheng-Hou Zhu;Su-Yun Ma;Xiao-Qin Liu
    . 2011, 42(12): 2176-2180.
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    The Nylon6/montorillonite intercalate composite were successfully direactly prepared by means of melting intercalation in twin-screw extruder, and their thermal stability hydroscopic properties and mechanical properties were measured. The results showed that the comprehensive mechanical properties were more better than those of Nylon 6. Especially,the flexural strength , Brinell hardness , yield strength , modulus of elasticity increased by33.8%，23%，21.7%,12% seprately than those of PA6，while the breaking elongation and impact strength decreased by 28%and 51.7% respectively，when the content of MMT was 3%.The hydroscopic quality decreased by 50% ,and thermal stability were also much better than those of Nylon 6.
  • Insulated performance of amorphousTa2O5 film prepared with the anodic oxidation process
    YANG Lan;GUO Tailiang
    . 2011, 42(12): 2181-2184.
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    The Ta2O5 isolation medium thin film was prepared with the anodic oxidation process. The morphology and composite of Ta2O5 film were characterized by scanning electron microscope (SEM), X-ray diffractions (XRD) and pectroscope (EDS), respectively. The results indicated Ta2O5 film was amorphous and had better surface. The electrical breakdown field intensity test system studied insulated performance of Ta-Ta2O5-Al composite films (MIM structure) in the FED component, indicated that the composite films had higher breakdown field intensity, which was 2.3Mv/cm. To analyze Ta-Ta2O5-Al composite films breakover mechanism, The Schottky Effect, F-N Effect were respectively regarded as the main mechanism.
  • Preparation of Mesophase Pitch by Simultaneous Hydrogenation-thermal Condensation
    Xin Su;Yan-Bo Yao;Wen-Li Xia;An-Hua LIU
    . 2011, 42(12): 2185-2188.
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    In this work, the mesophase pitch was prepared through simultaneous hydrogenation-thermal condensation of coal tar pitch in tetralin. The influences of the content of tetralin on the properties of mesophase pitch were systematically investigated. Results showed that the softening point and insoluble content of mesophase pitch were decreased while H/C was increased gradually with the increase the content of tetralin; Polarized light microscopy showed that the mesophase pitch was an uneven-distribution mixture of isotropic pitch and anisotropic pitch when the content of tetralin was less than 8%. With the increase the content of tetralin, the mesophase spheres became evenly distributed in isotropic matrix and the spinning ability of this mesophase pitch had been improved after further heat treatment. The ultimate carbon fiber from the mesophase had a cross-section of random-type.
  • Swelling Behaviors of β-Cyclodextrin – Acrylic acid – Acrylamide in Different Metal ions
    Zhan-Hua Huang
    . 2011, 42(12): 2189-2192.
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    The superabsorbent resin was synthesized by inverse suspension polymerization using β-cyclodextrin (β-CD), acrylic (AA) and acrylamide (AM) as materials. The swelling characteristics of resin was researched in different metal ions. The result s show that : the effect of competition swelling between metal ions and water to the resin is obviously，the effect of the swelling capability on the resin is NaCl> CaCl2>FeCl3 . The swelling behavior of the resin has overshoot phenomenon in CaCl2 and FeCl3, and the overshooting phenomenon to resin decrease with the increase of metal ionic intensity. When the anion solution concentration are 0.005~0.1mol/L, the swelling capability of the resin is NaAc>Na2CO3>Na3PO4. Anonic radius is bigger, hydration is stronger, the swelling capality of the resin is lower. The micro-morphology of resin in metal ion solution is classical 3-dimensional network structure, and the size of the network but all membranes in 3-dimensional gridding membrane structure. There was positive correlation between the size of the network and the absorptive capability.
  • The research on the Eu3+-doped concentration for the properties of a red-emitting LaInO3:Eu3+ phosphor and the self-quenching mechanism of Eu3+
    An Tang;Ding-Fei Zhang;Liu Yang
    . 2011, 42(12): 2193-2195.
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    A novel red-emitting LaInO3:Eu3+ phosphor was synthesized by the high temperature solid-reaction method. The structure phases and luminescence properties for the as-prepared phosphors were respectively characterized with XRD and fluorescence spectrometer. The analysis of XRD shows that the pure LaInO3:Eu3+ phase was obtained at 1150℃. The excitation and emission spectra indicate that the phosphors could be efficiently excited at 394nm or 464nm and the strongest emission peak was 610nn due to 5D0→7F2 transition of Eu3+ ions. The emission shape and location hardly changed with different Eu3+-doped concentration, but the emission intensity decreased greatly at the time of beyond 20mol% Eu3+ concentration. The mechanism for the concentration self-quenching of Eu3+ at 610nm emission results from the quadripole-quadripole reaction. From the results, the LaInO3:Eu3+ is suggested as a promising phosphor to fabricate white LEDs.
  • Preparation and Photoluminescence of Pure Amorphous Silica Nanowires by a Thermal Vapor Method
    Chuan-Yi Tao;Xue-Ming Li;Jian-Chun Yang
    . 2011, 42(12): 2196-2199.
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    A large quantity of silica nanowires were prepared by a non-catalytic and single-step thermal vapor method using polished p-Si wafers as substrates under nitrogen ambient at atmospheric pressure. Scanning electron microscopy (SEM) equipped with energy dispersive X-ray spectrometry (EDS), high-resolution transmission electron microscopy (HRTEM) and X-ray diffractometry (XRD) were used to characterize the morphology and structure of the product. The results indicated that silica nanorods were obtained at 1100 ℃, and smooth and uniform nanowires were observed at 1200 ℃ while nanowires with many curved segments at 1300 ℃. The EDS analysis indicated that nanowires consisted of mainly Si and O in an atomic ratio of about 1: 2 corresponding to SiO2. The XRD patterns and HRTEM study revealed amorphous character of the as-grown nanowires. Fine SiO2 cluster, which was formed by disproportionation and oxidation of SiO vapors, acts as nucleation centers for silica nanowires growth. Photoluminescence spectra of the silica nanowires recorded with 270 nm excitation showed two broad peaks of ultraviolet (UV) and blue light emissions centred at 364 and 467 nm, respectively. The blue and UV luminescence were attributed to the various structural defects in silica nanowires, which might have been generated during the nanowires growth.
  • Electrochemical hydrogen storage properties of as-spun nanocrystalline/amorphous Mg2-xLaxNi (x = 0-0.6) alloys
    Yang-Huan Zhang;;;Ying Cai;Yan Wang
    . 2011, 42(12): 2200-2205.
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    In order to improve the electrochemical hydrogen storage properties of the Mg2Ni-type alloys, Mg in the alloy was partially substituted by element La, and melt-spinning technology was used for the preparation of the Mg2-xLaxNi (x = 0, 0.2, 0.4, 0.6) alloys. The as-spun alloy ribbons with a continuous length, a thickness of about 30 μm and a width of about 25 mm were successfully obtained. The structures of the as-spun alloy ribbons were characterized by XRD, SEM and HRTEM. The electrochemical hydrogen storage performances and the electrochemical impedance spectra (EIS) as well as the hydrogen diffusion coefficients of the as-spun alloy ribbons were tested. It was found that the as-spun La-free alloy holds a typical nanocrystalline structure, whereas the as-spun alloys substituted by La exhibit an evident amorphous structure, suggesting the substitution of La for Mg facilitates the glass formation of the Mg2Ni-type alloy. For x≤0.2, the substitution of La for Mg, instead of changing major phase Mg2Ni, leads to forming small amount of secondary phases LaMg3 and La2Mg17. Both the La substitution and the melt spinning evidently ameliorate the electrochemical hydrogen storage properties of the alloy. Among of all the alloys, the as-spun Mg2La0.2Ni alloy possesses the superior electrochemical hydrogen storage properties. As the spinning rate is enhanced form 0 m/s (as-cast is defined the spinning rate of 0 m/s) to 30 m/s, the discharge capacity of the Mg2La0.2Ni alloy increases form 197.2 to 406.5mAh/g，the capacity retaining rate at 20th cycle rises from 52.7% to 81.4%, high rate discharge ability grows from 48.3% to 56.8%, and hydrogen diffusion coefficient (D) augments from 8.12×10?12 to 1.80×10?11 cm2/s。
  • Synthesis and characterization of a novel piperazine derivative microcrystal with specific optical property
    Mao-Lan Zhang;Chang-Shun Ruan;Guo-Ming Zeng
    . 2011, 42(12): 2206-2208.
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    Using piperazine and maleic anhydride as raw materials, we synthesized a novel piperazine derivative (4, 4'-(1, 4-piperazinediyl) bis (4-oxo-2-butenoic acid), PBBA) under the mild conditions. Optical microscope, FT-IR, HPLC-EMS and atomic force microscopy were employed to characterize the PBBA microcrystal. The results showed that the PBBA microcrystal had a specific optical property, and its molecular structure was symmetrical.
  • Preparation of TiO2(B)@Anatase Hybrid Nanowires and Their Lithium Storage Properties
    Yang Zunxian;Li Song;Guo Zaiping
    . 2011, 42(12): 2209-2212.
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    Abstract: Novel anatase@TiO2(B) hybrid nanowires have been synthesized by a facile aqueous alkali hydrothermal method, followed by acid washing and heating. The nanowires have a bicrystalline structure consisting of a TiO2(B) core encapsulated in an anatase shell. This hybrid nanowire has one column of entangled interface between the (001) plane of anatase and the (100) plane of TiO2(B), where a high conductivity column layer or belt comes into being, owing to the one way transfer of electron-hole carriers during the heterojunction formation. The as-prepared anatase@TiO2(B) hybrid nanowires deliver a highly reversible capacity of 196 mAhg-1 after 100 cycles at 30 mAg-1 (0.1C) and excellent rate capability as high as 125 mAhg-1 when cycled at 4500 mAg-1 (15C). Owing to the excellent electrochemical performance, anatase@TiO2(B) hybrid nanowires could be promising anode materials for lithium ion batteries.
  • Wavelet analysis study of the K24 application of cutting force
    Kun Qiu;Xin-Yong Wang;Si-Qin Pang
    . 2011, 42(12): 2213-2216.
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    In this paper, orthogonal experimental nickel-base cast superalloy K24 conducted a study of cutting force, cutting force applied to the wavelet analysis of signal processing. Using the wavelet analysis of cutting force for denoising and for different tool wear state of cutting force signal wavelet decomposition, energy detection. Results show that, with the tool wear increases, the scale increased vibration frequency of the signal, but also the corresponding increase in energy.
  • Preparation and photocatalytic property of iron doped TiO2 photocatalyst
    Gang Dong;Zhong-Qi Zhu;Qing-Ju Liu
    . 2011, 42(12): 2217-2220.
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    Abstract: The TiO2 photocatalyst samples doped with iron were prepared by sol-gel method. The samples were analyzed by XRD, FT–IR, UV–Vis, PL et al. The photocatalytic activity of the samples doped with different Fe content and sintered at different temperature were investigated by measuring the methyl blue （MB）degradation rate under the fluorescent lamp irradiation. The results show that Fe-TiO2 samples are a mixed phase of anatase and rutile and the threshold wavelength is red shift about 68nm. The Iron doping inhibits the growth of crystallite size and transformations of crystallite phase from anatase to rutile, and the photocatalytic activity is improved. The activity of the sample prepared at 500℃, n (Fe）: m（TiO2）=1: 200 is the best under fluorescent lamp and is obviously highter than that of Degussa P25.
  • Preparation and characterization of a cationic flocculant based on modified collagen
    Xue-Chuan Wang;Sha Zhang;Liang Zhou;Long-Fang Ren
    . 2011, 42(12): 2221-2224.
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    The gelatin was hydrolyzed by trypsin and the collagen protein solution was obtained. Then Fe（Ⅲ）was combined on it for iron tanning mechanism in tanning chemical. So modified collagen flocculant was prepared and used in the treatment of waste drilling water. The influence of different conditions on the treatment effect was studied by CODcr removal rate and suspended solids content. IR、XRD and fluorescence spectrum were used to characterized the structure of product. The result indicated that the best reaction condition on the preparation of flocculant was: reaction time was 4h, pH was 2.6, the quality ratio of collagen and Fe2(SO4)3 was 1︰1.4, the temperature was 35℃. When the flocculant prepared under this condition was used in the treatment of waste drilling water, CODcr removal rate was 73.1% and suspended solids content decreased from 2115mg/L to 330mg/L.
  • Complex impedance spectroscopy analysis of CdCl2 annealing on the CdTe polycrystalline thin films
    Wen-Bo Fu
    . 2011, 42(12): 2225-2228.
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    The complex impedance spectroscopy was measured for the Cadmium Telluride polycrystalline thin films of as-deposited and annealed under CdCl2 atmosphere. Then the complex impedance spectroscopy was fitting with using constant phase element (CPE) equivalent circuits model, and the dependence of grain bulk resistance，grain boundary resistance and time constantτon the annealing process was realized. The results show that, grain bulk resistance increases，grain boundary resistance and time constantτdecrease with the increased temperature.
  • Preparation and Characterization of hydrophilic polyurethane composite
    LIU Haohuai;ZHANG Jianhua;XU Qingling
    . 2011, 42(12): 2229-2232.
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    In this study, nano-hydroxyapatite (HA) slurry and aliphatic polyurethane (PU) were selected to fabricate hydroxyapatite/polyurethane (HA/PU) nano-composites by solvent casting and evaporation methods. The morphology and properties of the nano-composites were characterized by SEM, XRD and mechanical testing. The results show that HA crystals with nano size are distributed uniformly in the PU matrix, but the high loading levels of nano-HA are prone to agglomerate and make against homogeneous dispersion. The addition of hydrophilic poly(ethylene glycol) in raw materials enhances the surface and bulk hydrophilicities of PU;. The tensile strength and modulus of the nano-composites increase with the augment of hard segment content, while the broken elongation decreases; Increasing the content of poly(ethylene glycol) in soft segment, tensile strength and broken elongation first increase and then decrease, while the tensile modulus decreases all the time; The tensile strength and broken elongation of the nano-composites are all reinforced with the addition of HA nano-particles. When incorporated of 30wt% HA nano-particles into PU matrix, the comprehensive performance of the composite reaches optimality.
  • Preparation and Properties of Molecularly Imprinted Polymeric Microspheres for Recognition of Omethoate
    Chang-Jun Hou;Qing-Qing Huang;Dan-Qun Huo
    . 2011, 42(12): 2233-2236.
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    Molecularly imprinted microspheres (MIPMs) for recognition of omethoate and Non-molecularly imprinted microspheres (NMIPMs) were synthesized by suspension polymerization. Methacrylic acid was used as functional monomer. Then, morphologies of MIPMs and NMIPMs were characterized by scanning electron microscopy (SEM), which showed that the diameters were between 5~25μm. The isotherm binding of MIPMs and NMIPMs at different concentrations of omethoate demonstrated that MIPMs absorbed more substrates than NMIPMs. The data obtained in equilibrium adsorption experiment was processed by Scatchard analysis, which displayed that the MIPMs had two different affinity binding sites. The dissociation constants were calculated to be 0.131mmol/L and 5.178mmol/L, and the maximum absorption quantities were estimated to be 3.890μmol/g and 62.232μmol/g respectively. MIPMs also showed good selectivity for omethoate through the isotherm binding test of three other different substrates which were diomethoate, isocarbophos and phorate.
  • Photoluminescence properties and energy transfer of Sr2Al2SiO7 phosphor doped with Eu2+and Ce3+
    Sheng-Chang Chen;Jin Tan;Ai-Hua Zhong;
    . 2011, 42(12): 2237-2240.
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    The phosphors of Sr2Al2SiO7: Re(Re=Eu2+, Ce3+) were synthesized by high temperature solid state reaction. The luminescence properties of Eu2+, Ce3+ and the energy transfer between them were studied. The results indicate that Sr2Al2SiO7:Eu2+ phosphors show a broad excitation band and the main emission peak of the sample is located at 513 nm. The emission intensity reaches the maximum value when the concentration of Eu2+ is 5 mol%. The excitation spectrum is composed of two peaks which locate at 300 nm and 337 nm, respectively. The strongest emission peak locates at 406 nm and the strongest emission intensity is obtained when the concentration of Ce3+ is 2 mol%. Besides, co-doping of Ce3+ and Eu2+ enhances the emission intensity by transferring Ce3+ emission energy to Eu2+, which contributes to photoluminescence performance.
  • The luminescence properties of Ni2+-doped CdWO4 Crystal
    Yue-Feng Zhong
    . 2011, 42(12): 2241-2244.
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    The Ni2+-doped CdWO4 ( CWO) single crystals were grown by the vertical Bridgman technique. The absorption and emission spectra were measured. The crystal field strength of Ni2+ doped in CWO crystal , Dq = 1054cm-1, the Racah parameter B=1280cm-1 and C=5982cm-1 were calculated according to the absorption spectrum and crystal splitting theory. The emission band at 350nm-600nm was observed under excitation by 314nm, which were the intrinsic emission of WO66+.The emission band at1068nm was observed under excitation by 808nm and 980nm lights, which was attributed to the 3T2g(3F)→3A2g(3F) transition of Ni2+ in octahedral sites.
  • Effect of electric field on ferroelectric ferroelectric properties in (Ba0.90Ca0.10)TiO3 ceramics
    Li-Ren Han
    . 2011, 42(12): 2245-2248.
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    Barium calcium titanate (Ba0.90Ca0.10)TiO3 ceramics were prepared by sol–gel technique. The evolution of the ferroelectric hysteresis loops was analyzed at frequencies ranging from 0.01 to 10 Hz and in a field of 1.5-20 kV/cm. The results show that the electric field and frequency dependence of hysteresis loops are obvious. At low field, coercive field (Ec) decreases monotonically with frequency increasing, and remanent polarization increases at low frequency. But at high field, Ec increases monotonically with frequency increasing, and the evolution of the hysteresis loops is not obvious with different testing frequency when the hysteresis loops become saturated.
  • Synthesis of Nano-sized Li4Ti5O12 via a sol-gel method and its electrochemical performance study
    Ya-NanLi;Ying-Ying Hu;Jin Wang
    . 2011, 42(12): 2249-2252.
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    With lithium acetate and tetrabutyl titanate [Ti(OC4H9)4] as starting materials, and PEG as a surfactant, anode material Li4Ti5O12 for lithium-ion batteries has been prepared by a sol–gel method. The effects of the calcining temperature and calcining time on the electrochemical performance of obtained Li4Ti5O12 were investigated. The results showed that using PEG-6000 as surfactant， a single phase material with good crystallinity was obtained by calcining the gel precursors at 700 ℃ in air for 10 h which exhibited the a narrow size distribution (100nm to 300nm). The nano-sized Li4Ti5O12 power shows excellent rate capability. Its 1st discharge capacities at 0.1C and 5C were 164mAh/g and 127mAh/g, respectively, and could be retained at 162 mAh/g and 120 mAh/g after 50 cycles.
  • Preparation of the Quartz Fiber Coated Al2O3 and Applied in Phosphoric Acid Chromium Aluminum Through Wave System
    Yi-Xia Chou;Ji-Chuan Huo;Yong-Lin Lei
    . 2011, 42(12): 2253-2256.
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    The phase transition laws of Al2O3 preparing by sol-gel method were researched. The changes of the acid resistance, the tensile strength and the oxidation resistance and other effects of quartz fiber coating Al2O3 were researched. The changes of the tensile strength and dielectrical property in the phosphoric acid chromium aluminum through wave materials coating Al2O3 were researched.The results showed that: the Al2O3 prepared in the optimum preparation conditions was good quality. The coating process was suitable. The coating of the quartz fiber surface can be uniform. The Al2O3 coating can enhance the acid resistance, tensile strength and oxidation resistance of quartz fibers, can improve the binding of the coating and the acid phosphate matrix material, can enhance the tensile strength of the composite material. The dielectric constant and dielectric losses of the composite material coated Al2O3 are rather stable.
  • Effects of Zr addition on the microstructure and magnetostriction of the as cast Tb0.3Dy0.7Fe1.95 alloys
    Xiao-Cheng Li;Yu-Tian Ding;Yong Hu
    . 2011, 42(12): 2257-2260.
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    The Tb0.3Dy0.7Fe1.95-xZrx (x=0, 0.03, 0.06, 0.09) alloys were prepared by arc melting furnace. The crystal structure, microstructure and the magnetostriction of the Tb0.3Dy0.7Fe1.95-xZrx (x=0, 0.03, 0.06, 0.09) alloys were studied. Results demonstrated that the matrix phase of the Tb0.3Dy0.7Fe1.95-xZrx (x=0.03, 0.06, 0.09) alloys consisted predominantly of the cubic Laves phase with MgCu2(C15-type) structure. After Zr addition, the lattice parameter of the Laves phase in the alloys decreased by substituting rare earth elements Tb and Dy. The formation of the ZrFe2 phase as the primary phase made the solidifying liquid become rich in rare earths and suppressed the formation of the deleterious RFe3 phase. Zr was found to be limited soluble in the matrix RFe2 phase and negligible soluble in Re-rich phase. ZrFe2(C15-type) phase could dissolve into the RFe2 phase which crystal structure is C15-type and form the matrix (Re,Zr)Fe2 phase. The solubility of Zr in the matrix phase was found to be supersaturated(x=0.09), and Zr-rich phase formed as a new phase on the matrix (Re,Zr)Fe2 phase. The concentration of the element Zr affected the magnetostriction significantly. The improvement in magnetostriction was remarkably for the element Zr addition alloys with a low concentration as compared to the parent alloy Tb0.3Dy0.7Fe1.95. However, the decrease in magnetostriction at a higher concentration (x=0.09) was due to the formation of Zr-rich and Re-rich phases affecting magnetostriction. Whereas the magnetostriction had little improvement as compared to the parent alloy Tb0.3Dy0.7Fe1.95.
  • Research on the dynamic characteristics of La0.75Mg0.25Ni3.5Si0.10 alloy under high temperature
    Yu-Fang Lin;Pei-Pei Guo;Shi-Hai Guo;Yanghuan Zhang
    . 2011, 42(12): 2261-2264.
    Abstract ( ) Knowledge map Save
    Hydrogen storage alloys will show especial characteristics under high temperature. In this paper, the high-rate discharge ability and dynamic characteristic of La0.75Mg0.25 Ni3.5 Si0.10 alloy under 30~70℃ has been researched, by using electrochemical impedance spectrum (EIS) and constant potential-step discharge technique. The results show: the dynamic characteristic of the alloy is controlled by both the electrochemical reaction rate and the speed of hydrogen diffusion. The charge transfer resistance is decreased with testing temperature, and the electrode surface electrochemical reaction rate is increased at high testing temperature. But for La0.75Mg0.25 Ni3.5 Si0.10alloy, hydrogen diffusion coefficient will be decreased when the testing temperature is above the optimal temperature(45℃), due to the escape of the finite hydrogen in alloys being accelerated and the oxide film becomes thicker at high testing temperature. The increase of electrochemical reaction rates and the decrease of hydrogen diffusion speed together determine the high-rate discharge ability of La0.75Mg0.25 Ni3.5 Si0.10 alloys gets its best at 45℃.
  • Synthesis and Mechanism of Polytitanocarbosilane from LPCS and Ti(OBu)4
    Guo-Mei He;Xue-Chuan Lu;Ma-Tai Ding
    . 2011, 42(12): 2265-2268.
    Abstract ( ) Knowledge map Save
    Polytitanocarbosilane was synthesized from liquid polycarbosilane (LPCS) and tetrabutyl titanate (Ti(OBu)4). They were characterized by gel permeation chromatography (GPC), nuclear magnetic resonance (NMR) and Fourier transform infrared spectroscopy (FTIR). Based on these characterizations, the reaction mechanism was proposed as follows: the silicon free radicals were generated from Si-H group and then attacked the tetrabutyl titanate to form a branched or cross-linked network of silicon-containing fragment linked by Si-O-Ti group. The ceramic yield of the PTCS prepared in this way is very good. It can be used as the precursor for SiC ceramic composite matrix.
  • Study on the bonding mechanism of Ag/MWNTs-wool antibacterial fiber
    Li Zhang
    . 2011, 42(12): 2269-2272.
    Abstract ( ) Knowledge map Save
    With Ag/MWNTs antibacterial agent as functional material, antibacterial wool fiber was prepared by the method of ultraviolet irradiation. The morphologies of samples were observed by scanning electron microscopy. The structures of specimens were characterized by Fourier Transformation Infrared Spectrum. Moreover, the characteristics of wool fiber were measured before and after antibacterial treatments. The results show that wool fiber could firmly combine with the Ag/MWNTs composite which had excellent antibacterial effect. Furthermore, an antibacterial layer was formed on the surface of wool fiber by covalent bonding through the bridge action of coupling agent. Compared with original wool fiber, the Ag/MWNTs-wool fiber was longer and thinner with higher crimp recovery and crimp elasticity.
  • Simultaneous Removal of Acid Orange 7 and Cr(Ⅵ) by Strippable TiO2 Nanotube Array Photocatalytic
    Xiao-Jing Wu
    . 2011, 42(12): 2273-2276.
    Abstract ( ) Knowledge map Save
    Well-ordered strippable TiO2 nanotube array was prepared by two-step anodization in 0.5 wt % NH4F/HF/glycerol. The performances of the TiO2 nanotube array was studied, such as crystal form, morphology, photocatalytic effect, et al. The X-ray diffraction(XRD) result shows that the samples annealing at 500 ℃ and 800 ℃ are anatase and rutile, respectively. The Scanning electron microscopy(SEM) result reveals that the length of the TiO2 nanotubes with pore diameter about 100nm is approximately 25 μm. Under UV light, the aqueous solutions containing azodye acid orange 7 and hexavalent chromium were degradated by using TiO2 nanotube arrays as catalyst. The photocatalytic effect of using different crystal forms, different pH values and unlike initial concentrations of acid orange 7(AO7) and hexavalent chromium were investigated. The result shows that the photocatalytic of anatase is better than the rutile. The synergistic effect in the ternary system of TiO2/AO7/ Cr(Ⅵ) was outstanding, and the acidic condition were favorable for the removal of AO7 and Cr(Ⅵ).
  • Coaxial Dry-spinning of Regenerated Silk Fibroin/Sericin Aqueous Solution
    Yi-Chun Hang;Yao-Peng Zhang;Yin-Ying Li
    . 2011, 42(12): 2277-2280.
    Abstract ( ) Knowledge map Save
    To biomimick the composition，core-shell structure and spinning process of the natural Bombyx mori silk, regenerated silk fibroin/sericin (RSF/SS) fiber with a core (RSF) –shell (SS) structure was preliminarily prepared by coaxial dry-spinning process. The morphology, secondary structure and mechanical property of the resultant fiber were characterized by fluorescence microscope, scanning electron microscope, Raman Spectroscopy and material test machine, respectively. It was found that the coaxial dry-spun RSF/SS fiber had a clear core-shell structure, wrinkled surface and greater diameter. Although its properties were not yet good enough as those of natural silk, RSF/SS fiber had much superiority in the secondary structure and the mechanical property compared with the RSF fiber.
  • Preparation and electrical conductivity of Cu-30wt%Ag composite nanopowders
    Wei-Min Sun;Li-Jun Zhao;Gui-Mei Shi
    . 2011, 42(12): 2281-2284.
    Abstract ( ) Knowledge map Save
    Cu-30wt%Ag composite nanopowders were prepared by a both gas and liquid phase stabilizing method in H2﹢He, and conductive paste was prepared using composite nanopowders as conductive phase. The structure ,morphology , surface layer and oxidation resistance as well as electrical conductivity of the nanoparticles were studied using X-ray diffraction(XRD),high-resolution transmission electron microscopy(HRTEM),infrared spectrum analysis ,chemical analysis,gas analysis,differential thermal and thermogravimetry analysis. The results show that the nanoparticle size ranged from 10nm to 60nm.The surface of nanoparticles are consisted of bi-layer including a 2-(2-Butoxyethoxy)ethyl acetate molecules(C10H20O4) layer and a oxide layer,the bi-layer prevents the particles from a further oxidation in air. The 2-(2-Butoxyethoxy)ethyl acetate molecules of nanoparticles surface are desorption at about 200℃ in air.At the temperature below 200℃,the oxidation resistance of the composite nanoparticles are prepared by a both gas and liquid phase stabilizing method is better than that of gas phase stabilizing method.The Cu-30wt%Ag composite nanopowders conductive paste sintered at 200℃ for 50min under 5Pa can be obtained a thick film with resistivity is（1.56-3.92）×10-4Ω?cm.
  • Microwave hydrothermal synthesis of ZnO nanospheres and its modified pure acrylic emulsion
    Zhen-Feng Zhu;Xiao-Feng Wang;Hui Liu;;Juan Du
    . 2011, 42(12): 2285-2288.
    Abstract ( ) Knowledge map Save
    Well monodispersed ZnO nanospheres have been prepared by using triethanolamine (TEA) as complexant and znic nitrate hexahydrate as znic source under microwave hydrothermal conditions. The structure and morphology of the samples were characterized by XRD, SEM and TEM. Results show that each ZnO nanospheres (~150nm) is composed of numerous ZnO aggregates nanocrystallines with diameters of 10-20nm. Moreover, TEM observations indicate that the structure of ZnO nanospheres is loose. In the SEM images, the products obtained at different temperatures (140-180℃) and different times (1-60min) have the similar morphologies under the otherwise identical conditions. The composite latex was obtained by pure acrylic emulsion mixed with a small amount of modified ZnO nanoparticles. Water absorption ratio of composite films decrease by 10% after soaking 48h, in addition, both elongation at break and tensile strength of composite films significantly improve.
  • Preparation, Characterization and Gas Sensitivity Studies of Polyaniline and its Doped Materials
    Hai-Ying Du;Jing Wang;Juan Wang
    . 2011, 42(12): 2289-2293.
    Abstract ( ) Knowledge map Save
    Polyaniline (PANI) and its doped materials (In2O3-PANI, TiO2-PANI and SnO2-PANI) were synthesized by chemical polymerization of protonic acid method in 0℃ water bath. Aniline was oxidized by ammonium persulfate in hydrochloric acid solutions. The polyaniline and its composite materials were characterized by using X-ray diffraction (XRD), field emission scanning electron microscope (FE-SEM) and FT-IR spectromete (FI-IR). The gas sensors were fabricated based on polyaniline and its doped materials to detect NH3 at the room temperature. The response sensitivity of the gas sensors to NH3 was measured in NH3 concentration range of 10 ppm ~ 150 ppm. The relationships of the sensitivity of the sensors vs the NH3 concentration basically showed linearity. The sensitivity of the gas sensor based on In2O3 doped PANI was the highest and it is 50 for 150 ppm NH3 at room temperature. While response times of the gas sensor based on TiO2 doped PANI was the shortest in these four kinds of gas sensors and the response times was 60 s. The gas sensitive mechanism of polyaniline and its doped materials was analyzed. The doping of metal oxides has great effect on the properties of PANI materials such as response sensitivity, response and recovery times and selectivity.
  • Effect of Gd3+ doping on Phase Structure, Magnetic and Electrical Properties of double perovskite Sr2FeMoO6
    Yong-Qing Qu;Jing Qiao;Zhang Zhang
    . 2011, 42(12): 2294-2297.
    Abstract ( ) Knowledge map Save
    Double perovskite Sr2-xGdxFeMoO6（x=0, 0.1, 0.2, 0.3） were synthesized by microwave sintering method using SrCO3, Fe2O3, MoO3 and Gd2O3 as raw materials. The phase structure, magnetic and electrical properties of all the samples were investigated by X-ray powder diffraction (XRD) and vibrating-sample magnetometer (VSM) respectively. XRD analysis shows that the as-synthesized sample is Sr2FeMoO6 with tetragonal crystal structure and I4/mmm space group. With the increase of doped Gd3+, cell volume increases firstly and then decreases, accompanied by a small amount of impurity phase Gd2O3. Magnetism testing results show that the samples Sr2-xGdxFeMoO6 are ferromagnetic, the magnetic transition temperature is above room temperature. The saturation magnetization of Sr2-xGdxFeMoO6 is 16.528, 12.542, 10.616 and 12.040 A?m2/kg for x=0, 0.1, 0.2, 0.3 respectively under 1.0 T magnetic field at room temperature，and the magnetoresistance ratio of the samples is 28.02%, 29.39%, 30.36% and 61.66% respectively. Therefore，the saturation magnetization is decreased with the doping of Gd3+, but magnetoresistance ratio can be improved significantly when the doping concernt of Gd3+ x=0.3. Electrical performance testing results show that the samples exhibit typical semiconductor behavior. The conductive mechanism of Sr2-xGdxFeMoO6（x=0, 0.1, 0.2） is variable range transation of small polaron model in the range of 100~300 K. The conductive mechanism of Sr1.7Gd0.3FeMoO6 is variable range transation of small polaron model in the range of 150~300 K; but it is ascribed to the adiabatic small polaron conduction mechanism in the range of 100~150 K.
  • Effects on Structure of Nickel Hydroxide Doped with Zinc
    Jin-Yu Zhang;Jian-Yong Chang;Wang Miao
    . 2011, 42(12): 2298-2300.
    Abstract ( ) Knowledge map Save
    Nickel hydroxide was prepared through different methods such as chemical coprecipitated with zinc, mechanically mixed with Zn(OH)2 powder or undoped, and effects of doped form and amount of zinc on crystal type and structure were investigated. The measurement results of XRD indicated that the samples prepared by chemical coprecipitated with zinc were β-Ni(OH)2 when the amount of zinc is less than 11% ， with better crystal structure, and more crystal defects, all of these will improve the electrochemical performance of Ni(OH)2. But the characterize lines arised in the XRD patterns ,when the amount of zinc is more than 11% by chemical coprecipitation 、1% by mechanical mixing with Zn(OH)2. This result shown that there is two phases in the sample, which will not beneficial to improving the electrochemical performance of nickel hydroxide.
  • Construction for Processing Map Based on DMM and Identification for the stable hot-working parameters of Ti-6Al-2Zr-1Mo-1V Alloy
    Quan-Guo Zheng;Yang Wang;Yan-Wei Zhang
    . 2011, 42(12): 2301-2306.
    Abstract ( ) Knowledge map Save
    Abstract: Several series of billet samples were compressed on heat physical simulation machine under deformation temperatures 1073～1323K and strain rates 0.01～10s-1, then the true stress-strain data collected resulted the performance of calculations for strain rate sensitivity ( -value), power dissipation efficiency ( -value) and instability parameter ( -value). A series of 3D surfaces reveal the dramatic response of m-value to the transferring and coexisting of several deformation mechanisms induced by the enhanced effect of stress, temperature, strain rate and strain, from which the stable and unstable deformation parameter regions were indentified preliminarily. In further, the maps of power dissipation efficiency were plotted, from which the unstable ( ≤0) deformation parameter regions were indentified furtherly. Finally, based on the map of instability criterion, stable region ( ), unstable region ( ) were clarified clearly. According to the comprehensive identification, the stable deformation parameter regions with higher -value level, higher -value level, higher -value level are recommended, while the unstable deformation parameter regions with negative -value level, negative -value level, negative -value level should be avoided.
  • Study on Al/Ag/Al Electric Composite Films Applied in FED
    YANG Lan;GUO Tailiang
    . 2011, 42(12): 2307-2310.
    Abstract ( ) Knowledge map Save
    Abstract: The Al/Ag/Al electric composite films were prepared by magnetron sputtering and treated at 480 ℃ due to the ability of oxidation resistance of Ag. The morphology and composite of Al/Ag/Al composite films were characterized by scanning electron microscope (SEM) and X-ray spectroscope (EDS), respectively. The results indicated the surface of composite films was oxidized in the process of heat treatment. The Ag-Al alloy with rich Ag and Ag3Al compound were produced for the interdiffusion between Ag and Al atoms during the magnetron sputtering and heat treating. The resistivity of Al/Ag/Al composite films was largened as a result of an Al layer at the surface, and which was about 19.4×10-6 Ω?cm after heat treatment.
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