20 October 2011, Volume 42 Issue 10
    

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    研究与开发
  • Crystal growth and lasing properties of Tm:YAP laser crystal
    ZHANG Hao;SONG Pingxin;ZHANG Yingjiu
    . 2011, 42(10): 1735-1737.
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    High quality Tm-doped YAlO3 (Tm:YAP) single crystal with 4 at% doping concentrations was grown by the Czochralski method. X-ray power diffraction studies of Tm:YAP crystal con?rm that the as-grown crystal is isostructural with the YAP crystal. The absorption spectra show that Tm:YAP crystal has strong absorption peaks at 688 and 794 nm. A 793 nm laser diode pumping Tm:YAP crystal was applied to realize 2010nm laser output, the maximum output power was 5.1W, the optical conversion efficiency was 37% and the slope efficiency was 43.5%. Continuous tunable range from 1894 nm to 2066 nm is achieved with the maximum laser output power of 1.84W at 2010 nm.
  • Sol-gel Method Synthesize of High Temperature Stable Marcroporous TiO2
    LI Yingpin;LI Junxin;HAO Yanzhong
    . 2011, 42(10): 1738-1741.
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    Butyl titanate was used as titanium precursor, 95% ethanol water mixture as solvent, through simple sol-gel method macroporous TiO2 was synthesized. The products were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, thermogravimetry differential thermal analysis (TG-DTA), and N2 adsorption –desorption method. The results indicated that the macropore diameter was about 2 um. This material with big specific surface, and could withstanding 800 °C high temperature. The macroporous material calcinationed at 550 ℃ could degradation Rhodamine B. 95% ethanol water mixtures were favorable to macroporous TiO2 formation. Macroporous TiO2 formation was the coordination of micro- phase separation and chelating function.
  • Preparation and Characterization of MWNT-g-PEG/ZnO Nanocomposites
    WU Wenwen;ZHANG Li;SUI Kunyan
    . 2011, 42(10): 1742-1745.
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    MWNT-g-PEG enclosed by petal-like zinc oxide (ZnO) particles were prepared by sol-gel method at ambient pressure and low temperature (T=70℃). The hybrid nanocomposites were characterized by XRD, FTIR,SEM and TEM. The results obtained exhibited intimate contact between the ZnO nanoparticles and MWNT-g-PEG and ZnO crystallites had a very uniform size distribution of 80–150 nm. It was suggested that the PEG chains on MWNT surface act as the active sites for the in-situ growth of ZnO.
  • Effects of carbonization temperatures on the adsorption properties and pore structure of carbon fibers from liquefied wood
    MA Xiaojun;ZHAO Guangjie;LIU Xinyan
    . 2011, 42(10): 1746-1749.
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    After melt-spinning by adding hexamethylenetetramine and the curing treatment, carbon fibers were prepared from the phenolated Chinese Fir (Cunninghamia Lanceolata) by using of direct carbonization method. The adsorption properties of carbon fibers were studied. The results show that the isotherms adsorption of carbon fibers belongs to the typical I type, and the closed hysteresis loops belongs to H4 type. Carbon fibers from liquefied wood mainly contain micropores, and the maximum micropores content up to73.4%. With increasing heat-treatment temperature, BET surface area，micropore area and micropore volume of carbon fibers increased. Temperature rang 600～800℃ was the critical stage at which the pore structure of carbon fiber changed. wood/phenol ratio of raw have no influence on specific surface area, micropore volume and pore diameter of carbon fibers.
  • The diffusion characteristics of TiO2 nanotubes bio-membranes
    LIU Xi;ZHU Wen;LIU Huiqiong
    . 2011, 42(10): 1750-1753.
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    The paper introduce the preparation process of TiO2 nanotubes array membrane,the analysis of morphology and the etching parameters to get throughhole membrane.On the basis,different solutions were injected in a selfmade experimental setup to study the diffusion characteristics of the membrane.Photoelectric colorimeter and UV spectrophotometer are respectively used to research the influence produced to the diffusion characteristics of phenol red and bovine serum albumin(BSA) of different time and different nanotubes.
  • Sol-gel preparation and properties of V2O5-TiO2 electrochemic ionic storage films
    KONG Qinghu;ZHU Quanyao;HU Siping
    . 2011, 42(10): 1754-1757.
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    V2O5-(TiO2)x composite ionic storage electrode films were successfully perpared by the modified inorganic solgel route.The microstructures and morphologies,stoichiometry,Li+ intercalation and optical properties of the films were investigated by XRD,AFM,raman spretra,cyclic votammetry measurement and UVVis transmission spectra,respectively.The results indicated that the films have a layered V2O5 matrix structure,however,the orientation along caxis decreased with the inhanced content of TiO2.The grain size and surface roughness of the composite films remarkablely reduced.Meanwhile TiO2 incorporation also introduced some degree of nonstoichiometry in V2O5,increased the number of oxygen vacancies.The V2O5-(TiO2)x thin films with x=0.2 have relatively higher ion storage capacity and stability,and excellent transmission characteristics in the visible region as the ion intercalation and deintercalation.
  • Hydrothermal Synthesis of Tungstate and Molybdate Phosphor Powder-Structural and properties investigations
    WEI Yanyan;LAI Xin;QIN Dan
    . 2011, 42(10): 1758-1761.
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    A0.925(MoO4)0.5(WO4)0.5:Dy3+0.05(A=Ca,Sr,Ba) solid solution microcrystallines were synthesized by hydrothermal method; the crystal structure, surface morphology and room temperature photoluminescence properties of the microcrystallines were investigated by through X-ray diffraction(XRD), scanning electron micrograph(SEM) and fluorescence analysis(FA). The results show that the A0.925(MoO4)0.5(WO4)0.5:Dy3+0.05(A=Ca,Sr,Ba) microcrystallines all are typical scheelite structure with tetragonal symmetry. The emission peeks located at 480nm and 575nm respectively correspond to the transition of 4F9/2→6H15/2 and 4F9/2→6H13/2. The Ca0.925(MoO4)0.5(WO4)0.5:Dy3+0.05 microcrystallines with spherical morphology(grains size:0.7μm) give the maximum emission intensity, and it has wide potential application in optical materials.
  • Mechanical Properties and Hygroscopicity of Poly(lactic acid)/Wood-Flour Composite
    HUA Jin;ZHAO Zhimin;YU Wei
    . 2011, 42(10): 1762-1764.
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    The wood-flour was modified by polylactic acid (PLA) and maleic anhydride (coupling agent, MAPP). Composite materials were prepared by melt blending. The mechanical properties and water absorption of the wood-flour/PLA composite were researched, and the relationship between the macroscopic properties and the micro-characteristics was also analyzed. The results showed that with the wood-flour contents varied from 10g to 25g, the maximum tension increased four times, and the tensile strength increased three times. With the addition of MAPP, the increments of maximum tension and tensile strength were doubled. With the increase of wood components, the water absorbing capacity increased simultaneously, the maximum increment after 2 hours was 2.85%, and after 24 hours was 8.12%. The use of MAPP decreased the water absorbing capacity, the maximum increment after 2 hours was 0.72%, and after 24 hours was 3.58%. With scanning electron microscope(SEM), we can find that when the MAPP was added into the wood-flour, the interface became more smooth, and the adhesion between the PLA and wood-flour became more closely.
  • Surface hydrophilic modification of medical silicon rubber
    QU Xiangjun;WEI Zhiyong;REN Zhenchu
    . 2011, 42(10): 1765-1767.
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    We successfully prepared a PVP hydrophilic coating on medical silicon rubber surface by appropriate treatment and silane coupling agent.The surface morphology and the thickness of coating were investigated by SEM(scanning electron microscope),and hydrophilic properties of the samples were characterized by water contact angle.The tendency of hydrophilic coating in water was observed by measuring water contact angle of different samples with soaking time in 100mL water at 37℃.The results indicated that the hydrophilicity of the sample treated by coupling agent and hydrophilic solution was modified significantly.The obtained coating was very smooth(the thickness was about 110μm),and the hydrophilicity soaking of modified samples in water 7d was much better than that of the matrix.
  • Study on Electrodeposited ZnO Nanorod Arrays Assisted with PEG as Additive
    SUN Bao;HAO Yanzhong;GUO Fen
    . 2011, 42(10): 1768-1771.
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    Well-aligned ZnO nanorod arrays were successfully fabricated directly on indium doped tin oxide coated conducting glass (ITO) substrate by a facial electrodeposited process assisted with PEG -400 as additive. SEM and XRD were employed to characterize the nanostructures and their photoelectrochemical properties were also investigated. The results indicated that the as-prepared ZnO nanorod displayed a pure hexagonal wurtzite structure and a regular hexagonal cylindrical shape. The influence of PEG-400 on ZnO seed layers and ZnO NR arrays was discussed in detail. With the addition of 2% PEG-400, a dense and better-dispersed ZnO seedlayer was obtained, and a preferential oriented ZnO NR array with regular morphology, better crystallinity and higher photocurrent was presented.
  • Ring-opening polymerization of D, L-lactide to synthesize polylactic acid catalyzed by Schiff-base titanium complex
    LI Xiang;HU Chengbo;FU Ya
    . 2011, 42(10): 1772-1775.
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    Binuclear Schiff-base titanium complex was synthesized and used to catalysis bulk ring-opening polymerization of D, L-lactide. The synthetic products were characterized by FTIR, NMR and GPC. The results show that this Schiff-base complex has relatively high catalytic activity and controllability of molecular weights (PDI=1.09-1.24) in catalyzing ring-opening polymerization of D, L-lactide. The effects of molar ratio of monomer and catalyst, the polymerization temperature and polymerization time on polymerization were studied in detail. In the conditions of monomer and catalyst is 2600, polymerization time is 16h, polymerization temperature is 160℃, D,L-polylactic acid with Mn=9.058×104, PDI=1.16 can be obtained.
  • Effects of alloying element Mg on micro-arc oxidation ceramic coatings formed on three aluminum alloy substrates
    DAN Min;TONG Honghui;SHEN Liru
    . 2011, 42(10): 1776-1779.
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    Ceramic coatings were fabricated on three aluminum alloy substrates by micro-arc oxidation (MAO) at the constant current density of 10A/dm2 in Na3PO4 solution. The microstructure, composition, phase constituent of the coatings were investigated by means of SEM 、EDS and XRD; The protective properties of the coatings were evaluated by hardness, friction and wear. The results show that, the coatings are mainly composed of γ-Al2O3,α- Al2O3,AlPO4,and a few alloying elements such as Mg、Cu、Zn、W; The large-diameter bugs of the coatings decreases with increasing the content of Mg, and the coatings become more smooth and denser; With the increases of the content of Mg, the content of α- Al2O3 decreases, the hardness and wear of coating decreases too, when Mg content ≥2.5 wt.% only the γ- Al2O3.
  • Preparation, Characterization and Cytotoxicity of Hydroxyethyl Chitosan and N-Succinyl-hydroxyethyl Chitosan
    LI Minyu;HAN Baoqin;LIU Wanshun
    . 2011, 42(10): 1780-1785.
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    A water-soluble chitosan derivative hydroxyethyl chitosan (HECTS) was synthesized by chitosan (CTS) and chlorethanol. HECTS reacted with succinic anhydride and generated N-Succinyl- hydroxyethyl chitosan (Suc-HECTS). The best reaction condition was selected by analyzing the experiment conclusions in different conditions to obtain the supreme binding rate of succinic anhydride. The acquired products were characterized by FTIR. The deacetylation degree, binding rate of succinic anhydride and substitution degree of hydroxyethyl were measured by 1H NMR and Elemental analysis. Cytotoxicity of HECTS and Suc-HECTS were evaluated, and the results showed that two materials both had noncytotoxicity. The experimental conclusions offered a theoretical basis for the application of HECTS and Suc-HECTS as biopharmaceutical material and drug carrier.
  • Fabrication and characterization of novel water-soluble chitosan hydrochloride microspheres
    GAO Shibo;ZUO Yi;ZOU Qin
    . 2011, 42(10): 1786-1789.
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    Microspheres of water-soluble chitosan hydrochloride were fabricated by emulsion cross-linking method. The properties including surface morphology, interaction, crystallization, size distribution, thermal stability and cytocompatibility were analyzed by different analysis methods and cell culture with MG63 cells. The results show that schiff’s base reaction takes place between chitosan hydrochloride and glutaraldehyde. The chitosan hydrochloride microspheres have a spherical shape with smooth surface, poor crystallinity and small size (about 5-10μm by SEM). Compared with the chitosan microspheres, the chitosan hydrochloride microspheres have better balling property and thermal stability. Cell culture indicates that the chitosan hydrochloride microspheres have good cytocompatibility and are beneficial for adhesion, migration and growth of MG63 cells. Because of its water soluble property, there is a broad foreground for its application in drug loading and releasing.
  • A study on La2O3-doped SnO2 thick-film gas sensors based orthogonal experiment
    XU Hongyan;CHEN Xingqiao;YU Qingjiang
    . 2011, 42(10): 1790-1794.
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    In this thesis, using high energy ball mill method and orthogonal experiment design, SnO2 nanopowder and La2O3 nanopowder were milled and mixed. Therefore, pure SnO2 nanopowder and La2O3 doped-SnO2 nanopowder were prepared. SnO2 thick-film gas sensors and La2O3-doped SnO2 thick-film gas sensors were show that, the primary and secondary sequence affecting the comprehensive gas-sensing properties is: La2O3–doping concentration> sintering time> aging time> sintering temperature. By analysis, an optimum preparation condition was found. Gas sensors exhibit the best comprehensive gas-sensitive properties when the preparation condition was: La2O3–doping concentration 5wt.%，sintering time 2h, aging time 7d and sintering temperature 650℃. The sensitivity to 1000 ppm ethanol vapor is 107.2, and the best selectivity to interference gas (gasoline vapor or acetone vapor) with the same concentration is S乙醇/S汽油=11.3，S乙醇/S丙酮=9.1, respectively.
  • Study on Preparation and Properties of Crosslinked Anionic Waterborne Polyurethane
    YUE Jie;SHEN Yiding;LAI Xiaojuan
    . 2011, 42(10): 1795-1798.
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    Abstract: A new crosslinked aqueous anionic polyurethane was prepared by toluene diisocyanate(TDI), polycaprolactone(PCL), dimethnololpropionic acid(DMPA) and neutralized by triethylamine(TEA). Then the aqueous polyurethane reacted with hexamethoxymethyl melamine (HMMM) as a cross-linking agent.The product was characterized by FITR. And the particle size distribution of the polyurethane was researched, the water resistance, mechanical properties, thermal stability and crystallinity of the film were also tested. The FITR spectrum indicated that HMMM was crosslinked with polyurethane, and when m(HMMM):m(-COOH)=2.25, tensile strength is up to 30.3MPa, water absorption rate and ethanol absorption rate decreased to 17.2% and 10.9% , contact of angle increased to 69.6°, Tmax is 301.5℃, crystallinity decreased from 3.77% to 1.10%.
  • Synthesis of Fluoride Ion Probe based on the DCC modified Pyrrolo[2,1-a]isoquinoline Derivative
    LIU Lei;HAN Qiaorong;JIANG Yuliang
    . 2011, 42(10): 1799-1801.
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    Abstract: A novel DCC modified pyrrolo[2,1-a]isoquinoline compound 4 has been synthesized and characterized by 1H NMR, FT-IR and elemental analysis.The solvent effects on its UV /Vis and fluorescence spectra were studied. The influence of some metal ions and halogen ions on its fluorescence properties were also studied. The results showed that its fluorescence can be decreased evidently by the fluoride ion, so this compound is promising to be the fluorescent probe for fluoride ion .
  • Study on Properties of Organic Solar Cells Based on P3HT
    HUANG Long;XU Xiangdong;ZHOU Dong
    . 2011, 42(10): 1802-1805.
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    Abstract: Poly(3-hexylthiophene)(P3HT) is a novel material for application in organic photovoltaic solar cell donor. By using vacuum evaporation and spin coating, a novel organic photovoltaic cell based on P3HT with a structure of ITO/Buffer layer/P3HT/C60/Bphen/Ag was fabricated, and was analyzed by the semiconductor test instrument for the characteristics parameters of solar cells. The optimal thicknesses for P3HT and C60 are 30nm and 40nm, respectively. It was also demonstrated that the open-circuit voltage of the device is significantly enhanced when molybdenum trioxide (MoO3) is used as the anode buffer layer. Therefore, by optimizing the preparation process and introduction of new metal oxides, the parameters of solar cells could be better controlled.
  • Microstructure analyses of mesophase pitch-based carbon fibers with high thermal conductivity
    YUAN Guanming;LI Xuanke;DONG Zhijun
    . 2011, 42(10): 1806-1809.
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    Mesophase pitch-based carbon fibers are most attractive candidates for thermally conductive materials and heat dissipation materials due to their low electrical resistivity and high thermal conductivity, but there are few research reports on their microstructrues and properties in our country. In contrast to the mesophase pitch-based carbon fibers with different transverse shapes fabricated in our laboratory, the microstructure and morphology of high conductive mesophase pith-based carbon fibers prepared by foreign country are analyzed in the paper.
  • Microwave absorbing propertiesof Z-type hexaferrite Ba3(MnZn)xCo2(1-x)Fe24O41
    ZHOU Kesheng;CHEN Ying;QIN Xianming
    . 2011, 42(10): 1810-1813.
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    The samples of MnZn-doped Z-type barium ferrite Ba3(MnZn)xCo2(1-x)Fe24O41（x=0.1,0.2,0.3,0.4,0.5）were prepared by sol-gel process．The crystal structure and surface morphology of the particles were characterized by X-ray diffraction （XRD ）and scanning electron microscope （SEM）, respectively. Their complex dielectric constant and complex permeability were measured by microwave vector network analyzer in the frequency range from 2 to 18GHz, the reflection coefficient and loss tangent were calculated according to measurements,and the microwave absorbing properties and the electromagnetic loss mechanism of samples were studied. The results showed that Z-type hexaferrite crystal structure was formed and powder morphology was micro-hexagonal flake for this samples, and the absorption peak was 38.5dB at 3.9GHz and the bandwidth above 10dB was 3.8GHz when sample thickness was 2.20mm and x=0.4.This material that can effectively achieve the microwave absorption in1-5.8GHz low frequency range had both magnetic loss and dielectric loss, but the former was more significant.
  • Research of waterborne polyurethane modified with silane coupling agent γ-Methacryloxypropyl trimethoxy silane
    WANG Xiaorong;SHEN Yiding;LAI Xiaojuan
    . 2011, 42(10): 1814-1816.
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    Silane modified waterborne polyurethane was synthesized by isophorone diisocyanate(IPDI),polytetrahydrofuran glycol(PTMG), γ-Methacryloxypropyl trimethoxy silane and aziridine was aslo used to improve the quality of the film.The structure was characterized by ATR-FTIR.The effect of MEMO content on emulsion size,the film property of water resistence,mechanical properties,thermal stability,crystallinity and contact angle were studied.The results showed that when w(MEMO)=5.67%，w(AZ)=2%，water resistence rate was low to 14.84%,the maximum tensile strength was 17.334Mpa,the breaking elongation was 232.56%,the surface engery and the crystallinity of the polyurethane film was decreased while the thermal stability was enhanced.
  • Synthesis, structure and electrochemical properties of LiFePO4 Prepared by Solvothermal Process
    SU Yuchang;SHAO Bing;CHENG Hongyan
    . 2011, 42(10): 1817-1820.
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    The pure, well-developed prism shapes and well-crystallized LiFePO4 was synthesized by solvothermal process using Li1+:Fe2+:PO43+=1:1:1 as starting material. Adding the phenolic resin, LiFePO4/C was obtained during the high temperature process, which had high tap density and good machinability. The effects of solvothermal process temperature and process time on microstructure and electrochemical properties of LiFePO4 and LiFePO4/C were investigated by the methods of X-ray Diffraction(XRD), scanning electron microscope(SEM), and constant current charge-discharge. The results showed that the sample prepared at 190℃/24h performs good properties, whose tap density was 1.25g?cm-3 and discharge specific capacity was 151.3mAh?g-1 at 0.1C and 120mAh?g-1 at 1C under room temperature.
  • Study on a Novel Cross-Linkable Polymer for Second-order Nonlinear Optics
    HOU Wenjun;GAO Wu;CHEN Zhuo
    . 2011, 42(10): 1821-1824.
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    A novel cross-linkable poly(arylene ether), which was used in second-order nonlinear optical material, has been synthesized by polycondensation and post functional reaction. This cross-linkable poly(arylene ether) has excellent film-forming. The Diels-Alder（DA）cross-linking process of polymer film doped with N,N-(methylene diphenyl) bismaleimide was investigated by UV-vis method. Results show that the cross-linking condition of polymer film was 110℃, 15min. The second-order nonlinearity of polymer film combined by poly(arylene ether) and N,N-(methylene diphenyl) bismaleimide and chromophore-1 was measured with simple reflection mothed. The value of electro-optic coefficient (r33) was 6.5pm/V （1.31 μm）with 10wt% loading in polymer film and maintained more than 85% initial value after 10 days .
  • Studies on skincore structure of stabilized PAN fibers by ultrasonic etching method
    HU Xiuying;WANG Chengguo;YU Meijie
    . 2011, 42(10): 1825-1828.
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    After ultrasonic etching treatment, the morphology and the chemical constitution difference between the skin and the core of the stabilized fibers from different temperature zones were studied by SEM and Raman spectrum respectively. The fibers stabilized at 195225℃ had low stability, in which almost no difference in structure appeared between the skin and the core. The core in the fibers stabilized at 235265℃ was dissolved by ultrasonic etching due to lower stability compared with the skin, which led to significant morphology difference between the skin and the core. After stabilized at 275℃, the stabilization of the core was improved, and the skin and the core showed infusibility. The characteristic Ramanscattering peaks of graphite broadened in the final stabilized fibers, while the peaks of the skin was broader, indicating the chemical constitution difference between the skin and the core.
  • Microhardness measurement of KDP Crystal grown by point-seed technique
    SUN Yun;WANG Shenglai;GU Qingtian
    . 2011, 42(10): 1829-1832.
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    Abstract: Potassium dihydrogen phosphate (KDP) crystal was rapidly grown by “point-seed” technique. Indentation experiments on different faces of KDP crystal were carried out at a serial of loads. The anisotropy of microhardness has been studied. The results show that the microhardnesses of KDP crystal on (001), (101) and (100) faces were 187kg/mm2, 156.7 kg/mm2, 151.3 kg/mm2 , respectively. The hardness indentation size effect (ISE) phenomenon was also found at loads varying from 5 to 200g. The results show that the microhardnesses decreased with increasing of load for all crystal faces. The cracks appeared and expanded in the radiation form when the loads were higher than 25g. The edges of indentation appeared cataclasms with the disintegration shape. In this paper, It was believed that 25g was the optimal load for KDP crystal.
  • Fabrication of a microscale ordered-reinforced composite and its mechanical characterization
    ZHANG Zhenjie;WANG Hong;YANG Zhuoqing
    . 2011, 42(10): 1836-1839.
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    Abstract：Polyurethane modified epoxy resin is selected as matrix, an PMC reinforenced by micro-ordered electroplated nickel wire is fabricated through microfabrication. Results of ANSYS simulation show that matrix can relieve stress concentration if the matrix wraps up entirely on the reinforcement. The lowest stress concentration is generated in the deformation of composite when the angle of reinforcement is 45°and the volume content of reinforcement is 62.5%. Results of tension testing on DMA show that the tensile strength and Young'modulu of composite are 4 times and 3 times higher than the pure polymer, reasonable fracture processing has been analyzed by SEM. Keywords：MEMS；Composite；ANSYS；ordered reinforcement；Microscale
  • Study on the drug release mechanism in vitro of antimicrobial material controlled degradation
    LI Chunyan;HU Congcong;WEN Zhiguo
    . 2011, 42(10): 1840-1843.
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    Based on the preparation and characterization of controlled release antibacterial materialciprofloxacinpolyurethanes (CFPU)，the method of HPLC was established to determine the content of antibacterial agentciprofloxacin (CF) in the degradation solution of CFPU and investigate the drugrelease mechanism in vitro by plotting and fitting the cumulative release curves to inspect the effects of different medium and different concentrations on drug release. The results showed that the HPLC method is accurate, reliable and simple. The drugrelease of CFPU was bioresponsive and could be accorded with first order kinetics. It was observed that CF was released from CFPU by a combination of diffusion and erosion mechanism by modeling in the RitgerPappas equation (0.45＜n＜0.89), mainly in the manner of diffusion in the absence of infection while erosion mechanism in the presence of infection. And the worse the inflammation was, the more erosion mechanism dominated. 
  • on Electromagnetic Shielding Cement Paste with Graphite and Carbon Fiber
    YANG Yushan;DONG Faqiang;DENG Qiang
    . 2011, 42(10): 1844-1846.
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    graphite and carbon fiber as unit for electromagnetic shielding, adding they into cement paste to replace sand, and the cement paste has the functions of shielding and absorbing the electromagnetic wave by adjusting the contents of functional materials. The influence of the contents of electromagnetic shielding material to electromagnetic shielding effectiveness of cement paste was analyzed by contrasting the electromagnetic shielding effectiveness of different samples. The results show that electromagnetic shielding effectiveness is higher in 30MHz～200MHz frequency range, electromagnetic shielding effectiveness reduce fastly with frequency increasing. Electromagnetic shielding effectiveness changes to mild in 200MHz～1.8GHz frequency range, electromagnetic shielding effectiveness is lower. SEmin up to 10 dB to carbon fiber electromagnetic shielding cement paste in 1.8GHz.
  • Study on the preparation of the SiC-MoSi2-TiSi2 coating made by pack cementation method
    JIAO Gengsheng;LI Hejun;LU Guofeng
    . 2011, 42(10): 1847-1850.
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    Abstract : The internal SiC-MoSi2-TiSi2 coating for C/C composites made by pack cementation was studied. The influencing factor was analyzed when the coating was made. It is discovered that the optimum temperature was 2573K, the prepared time was 2h and the mixture ratio of MoSi2 and TiC was 5:2. Oxidation test shows that the weight loss of the SiC-MoSi2-TiSi2 coated C/C composites characterized by excellent thermal shock resistance is only 2.18% (the weight loss rate is 1.17×10-4g/cm2?h) at 1773 K for 49h.
  • Fabrication of a porous CuAlMn shape memory alloy by sintering-dissolution technique
    LI Nuo;WANG Qingzhou;CUI Chunxiang
    . 2011, 42(10): 1851-1854.
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    A porous CuAlMn shape memory alloy has been successfully fabricated by replication of NaCl space-holders via sintering-dissolution technique. Examination of macroscopic and microscopic morphologies，phase identification as well as investiation on the martensitic transformation of the resultant material were also carried out. It is shown that the resultant material exhibits uniformly distributed and interconnected pores. Flexural fractograph exhibits ductile characteristic, indicating that an effective bonding between CuAlMn powders has been achieved. Endothermic and exothermic peaks on the DSC curves show that the resultant porous CuAlMn alloy has good martensitic transformation behaviours.
  • Study on structure and character of Polyacene quinine radical polymer
    ZHENG Huaqing;TANG Xianzhong;JIANG Yadong
    . 2011, 42(10): 1855-1860.
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    A kind of molten salt NaCl /AlCl3, rarely reported in the synthesis of polymer, is used to synthesize PAQR, which is compared with the one got in nitrobenzene. The structure and thermal stability of polymers have been studied as well as the dielectric constant. The results indicate that PAQR shows good thermal stability. The polymer synthesized in NaCl /AlCl3 exhibits huge dielectric constant which is over 10,000 when the frequency is 20Hz while the one of polymer synthesized in nitrobenzene is below 10.The dielectric constant of PAQR decreases rapidly as the frequency increases. Besides, two new monomers of anthraquinone 1, 4-bis (octyloxy) anthracene-9, 10-dione and 1, 4-dibutoxyanthracene-9,10-dione are synthesized and characterized by FITR, H1NMR spectra and elemental analysis. Results of DSC and TG indicate melting points of two monomers are blow 130℃ and the 5% thermal decomposition temperatures are more than 200℃.
  • Synthesis and Characterization of Titanium Opaque Porcelain
    GUO Litong;DENG Changcheng;WANG Yao
    . 2011, 42(10): 1861-1863.
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    The titanium opaque porcelain was synthesized through normal melting-derived route using SnO2 glass-ceramic system. The porcelain was characterized by thermal expansion, X-ray diffraction and cytotoxicity tests. The results of XRD showed that the main crystal phase of the opaque porcelain was SnO2. Its' average coefficient of thermal expansion (α25-350) was 8.9×10-6/℃, which was lower than that of bonding porcelain (9.2×10-6/℃) and pure titanium (9.5×10-6/℃). The optimal fusion temperature was 780℃. The methyl thiazolyl tetrazolium assay results demonstrated that the cytotoxicity of the titanium porcelain was ranked as 0. At the same time, the titanium porcelain did not result in hemolysis. It was believed that the titanium opaque porcelain synthesized in this research was a biocompatible material and could be used for dental implant materials.
  • Preparation of Cu-diamond composite using inter-sand co-deposition
    LI Weiping;WEI Youyang;LIU Huicong
    . 2011, 42(10): 1864-1868.
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    Cu-diamond composite are expected to combine the advantages of copper and diamond to achieve the performance of low density, high thermal conductivity, and low thermal expansion. Composite electrolytic deposition is a promising technique for preparing Cu-diamond composite. The influences of inter-sand process parameters towards diamond content and bulk density for composites were studied, and then the inter-sand process parameters were optimized. Cu-diamond composite with uniform distribution diamonds inside and a high bulk density were achieved under optimized inter-sand process parameters. The relationships between optimized inter-sand process parameters and diamond diameter were also simulated in this paper.
  • Preparation, Microstructure, Piezoelectric and Ferroelectric Properties of Piezoelectric Ceramics with Low-lead Component
    LI Ziyuan;HE Zijun;XIAO Dingquan
    . 2011, 42(10): 1869-1872.
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    Abstract: xPbTi0.4716Zr0.4834(Mn1/3Sb2/3)0.0450O3-(1-x)(K0.485Na0.485Li0.03)NbO3 [xPMS-(1-x)KNLN] ceramics with low-lead Component were prepared by using conventional ceramics method. Microstructure, piezoelectric and ferroelectric properties of the low-lead ceramics with different stoichiometry x fabricated at varied sintering temperature were studied. The XRD patterns of the ceramics show that the microstructure of the ceramics transform from a coexistence state of pyrochlore and pseudo-cubic pervoskite to tetragonal pervoskite while sintering temperature increases. The SEM analysis shows that a liquid-phase formed by the (K0.485Na0.485Li0.03)NbO3 component appeared during the sintering process and while the sintering temperature increases the holes appeared on the surface of the ceramics and disappeared when the ceramics were sintered at even higher sintering temperature. The electric measurement results obtained show that xPMS-(1-x)KNLN ceramics possess good piezoelectric and ferroelectric properties, and when sintered at 1250 ℃, the xPMS-(1-x)KNLN ceramics with x=0.75 ceramic possess the properties of d33=182 pC/N， kp=34.5 %， Tc=165 ℃， Pr=21.2 μC/cm2， Ec=1.47 kV/mm, εr=1879， and tanδ=0.92%.
  • Resistance temperature characteristic of non-crystalline polymer composites / carbon department of fillers
    HUANG Ying;ZHAO Xing;GAO Feng
    . 2011, 42(10): 1873-1875.
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    The differences of the resistance temperature characteristic of the different composites which non-crystalline polymers-silicone rubber as a substrate material, carbon black, graphite and carbon fiber as conductive fillers are analyzed. The composite samples of carbon black as fillers do not show resistance temperature characteristic. Graphite samples has obvious resistance temperature characteristic in a smaller temperature range (55℃-75℃) .While carbon fiber samples shows the more obvious features of resistance temperature characteristic in a large temperature range (25℃-90℃), and there is approximately linear change in resistance with temperature. It was concluded that the shape of the carbon department fillers is the main factor of the resistance temperature characteristic of conductive composites.The resistance temperature characteristic of non-crystalline polymers / carbon fiber composite has good linearity, so it can be used as sensitive materials of flexible temperature sensors.
  • The study on preparation and properties of biogradable bone-cement compounded with bioactive glass fiber
    WANG Huiyu;ZHOU Nai;YAO Weifang
    . 2011, 42(10): 1876-1880.
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    In this study, the bone-cement with high porosity is strengthened by borate glass fiber as reinforce materials. The microstructure of the glass fiber’s surface was investigated by SEM. And mechanical strengths were tested as well. The results indicate that the degradation of borate glass contributes growth of HAP in the SBF solution. After 30 days, the interface between glass fiber and bone cement is not obvious existence and both of them come into being the one whole unity. During this 30 days, the strength testes show that the mechanical strength of bone cement is in the steady growth.
  • Effects of deposition temperature on the growth behavior of and optical properties N-doped Cu2O films
    LI Hongjing;MA Chunyu;LI Shuai
    . 2011, 42(10): 1881-1885.
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    N-doped Cu2O films were firstly deposited in the mixture of Ar and N2 by using reactive-frequency magnetron sputtering a CuO target. We have investigated the feature of structure, growth mechanism and optical properties of N-doped Cu2O films at different deposition temperatures. It is found that the Cu2O samples are highly (100) textured at the low deposition temperatures, and gradually change to be highly (111) textured at the deposition temperature of 500℃. With increasing the deposition temperature, the increase of free energy of critical nucleation is suggested to dominate the change of film texture. The analysis of the atomic force microscopy shows that the surface morphologies of all the films deposited at different temperatures have the spatial scaling exponents greater than 1 (?>1), indicating that the film growth can be attributed to the surface-diffusion-dominated growth. The spatial scaling exponent and characteristic length of the film surface morphologies are found to correlate to the textured factors of the films. The bandgaps of N-doped Cu2O films deposited at different temperatures are determined to be 2.52±0.03 eV.
  • Hydrothermal synthesis of N-acetyl-L-crysteine stabilized CdxZn1-xSe quantum dots
    GU Lemin;HU Lang;YAO Aihua
    . 2011, 42(10): 1889-1892.
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    In this paper, ZnxCd1-xSe quantum dots with tunable photoluminescence emission, uniform particle size and good crystallinity were synthesized by hydrothermal method, in which N-acetyl-L-crysteine was used as a stabilizer. UV-vis absorption spectroscopy (UV-vis), photoluminescence (PL) spectroscopy, X-ray diffraction (XRD) spectroscopy, and high-resolution transmission electron microscopy were used to characterize their structures and properties. The effects of Cd2+/Zn2+ ratio, pH of the precursor solution, hydrothermal temperature and time on the photoluminescence properties of ZnxCd1-xSe quantum dots were significantly investigated in the present work. The results showed that the content of heavy metals in the quantum dots could be increased, which contribute to improving biocompatibility of the quantum dots. At the same time, the obtaining quantum dots possessed high photoluminescence yield (up to 35%) and narrow fluorescence full-width (FWHM<50nm). Therefore, the ZnxCd1-xSe quantum dots would be a promising fluorescent probe for biological and biomedical imaging.
  • Extracting geometric parameters of nanotemplates with MATLAB
    LEI Jinglei;WU Shengmao;LI Lingjie
    . 2011, 42(10): 1893-1897.
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    Nanotemplates with high-qualities play an important role in preparing well-aligned functional nanomaterials. However, it is difficult to evaluate the quality of nanotemplates quantitatively at present. In this paper, a computer program based on the general software MATLAB was proposed to extract quantitatively the geometric feature parameters from the morphology images of the nanotemplates. The proposed program can not only calculate the size parameters of the pores of the nanotemplates such as the porosity, the diameters and their variance by mathematical morphological operations, but also obtain the angle parameter of the pores arrangement by analyzing the morphology images with 2-dimensional fast Fourier transforms (FFT) and 1-dimensional FFT successively. After the accuracy and reliability of the proposed program was confirmed by processing a standard image, several scanning electron microscope (SEM) images of anodic aluminum oxide (AAO) templates, one of the most important nanotemplates, were analyzed. A reliable conclusion about the quality of the templates can be drawn based on both the size and angle parameters extracted with the proposed program. The application of the program will be helpful to optimize the templates preparation conditions and prepare functional nanomaterials in the future.
  • Synthesis and optical properties of CdS:Mn/ZnS core/shell nanocrystals
    ZHAI Hui;CAO Lixin;LIU Wei
    . 2011, 42(10): 1898-1901.
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    With 3-Mercaptopropionic acid as stabilizer，CdS:Mn nanocrystals were synthesized by a co-precipitation technique in aqueous phase, and then CdS:Mn/ZnS core/shell nanocrystals were prepared by ZnS epitaxial coated on the surface of CdS:Mn nanocrystals. The crystal structure, morphology and optical property of the nanocrystals were characterized by X-ray diffraction, transmission electron microscopy and UV-Vis absorption spectroscopy. The results showed that nanocrystals were nearly monodisperse and confirmed that ZnS was grown on the surface of CdS:Mn nanocrystals. Luminescence and photostability of the nanocrystals were researched with photoluminescence emission spectroscopy. Luminescence intensity of the core/shell nanocrystals was significantly enhanced up to eight times, and the Mn2+ photoluminescence peak was gradually red-shifted as the ZnS shell increased. Furthermore, a strongly improved photostability of the optical properties was observed.
  • Effect of Heat Treatment on Microstructure and Damping Capacity of Mn-Cu Alloy
    WANG Jingfeng;LING Chuang;HU Yaobo
    . 2011, 42(10): 1902-1906.
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    The phase structures, microstructure and damping capacity of rolled CuMn50 alloy were tested using X-ray diffractometer, scanning electron microscopy and dynamic mechanical thermal analyzer. The effect of heat treatment on damping capacity and microstructure of rolled CuMn50 alloy was study. The result indicated that the damping capacity increased slowly at first and then increased rapidly with Strain amplitude increasing. Manganese-copper alloy began to appear grains with the cooling rate increasing, and the damping capacity of rolled CuMn50 alloy decreased with the cooling rate increasing, the slow cooling rate is conducive to the production of manganese-rich, played a role in aging. After aged at 420℃ for different time, the damping capacity of furnace cooling specimens is further increased, however, aging time did not affect the damping properties of the sample. After aged at 420℃ for different time, With the aging time increases, the grain first becomes coarse, followed by precipitation of second phase α-Mn, and the damping capacity of water cooling specimens increased to the peak value first and then slightly reduced with the aging time increasing. When the aging temperature is about 420℃,the aging time is about 8h,the best damping capacity of water cooling specimens is obtained.
  • Influence of substituting Mg with La on hydrogen storage kinetics of as-quenched nanocrystalline/amorphous Mg2Ni-type alloys
    ZHANG Yanghuan;LI Xia;ZHANG Guofang
    . 2011, 42(10): 1907-1912.
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    In order to improve the gaseous and electrochemical hydrogen storage kinetics of the Mg2Ni-type alloys, Mg in the alloy was partially substituted by element La, and rapid quenching technology was used for the preparation of the Mg2-xLaxNi (x = 0, 0.2, 0.4, 0.6) alloys. The structures of the as-cast and quenched alloys were characterized by XRD, SEM and HRTEM. The gaseous hydrogen storage kinetics of the alloys was measured using an automatically controlled Sieverts apparatus. The electrochemical hydrogen storage kinetics of the alloys was tested by an automatic galvanostatic system. The results show that that the as-quenched binary Mg2Ni alloy holds a typical nanocrystalline structure, whereas the as-quenched alloys substituted by La exhibit an evident amorphous structure, implying the substitution of La for Mg facilitates the glass formation of the Mg2Ni-type alloy. The substitution of La for Mg visibly changes the phase composition of the alloys. For x≤0.2, the substitution leads to forming small amount of secondary phases LaMg3 and La2Mg17 without changing major phase Mg2Ni. The major phase of the alloys are changed to the (La, Mg)Ni3+LaMg3 phases by increasing La content to x≥0.4. The gaseous and electrochemical hydrogen storage kinetics of the alloys is dependent on both the amount of La substitution and the rapid quenching technology. The substitution of La for Mg causes a decrease in the hydrogen absorption kinetics of the alloy, but it significantly ameliorate the hydrogen desorption kinetics and the high rate discharge ability of the alloy. The influence of substituting Mg with La on the hydrogen storage kinetics of the alloy is strongly dependent its preparation technology, meaning that the structure of the alloy is a crucial factor of the hydrogen storage kinetics of the alloy.
  • Synthesis of Immunomagnetic Microspheres and Their Applications in the Detection of Hepatitis C Virus Antigen
    YANG Mingzhu;GUAN Yueping;LAI Xianhong
    . 2011, 42(10): 1913-1915.
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    Superparamagnetic poly(methyl acrylate) microspheres were synthesized by suspension-emulsion polymerization. Amino group was modified on the surface of the magnetic polymer and the slide by ammonolysis and silanized chemical reaction，respectively，then the Hepatitis C Virus Antibody was immobilized. The obtained magnetic microspheres were characterized by means of vibrating sample magnetometry(VSM)，biological microscope and atomic adsorption spectrophotometer(AAS).The results showed that the magnetic microspheres were spherical with a narrow size distribution，a mean diameter of 4μm，and superparamagnetic with the saturation magnetization of 7.181emu/g，and the concentration of the amino groups was 0.433mmol/g. Negative, positive distinction has been very good to reach a better detection results through the immunoreaction between the Antibody on the surface of microspheres, antibody on the slides and hepatitis C Virus Antigen.
  • Synthesis and photocatalytic activities of BiVO4 microspheres with different crystalline forms
    ZHU Zhenfeng;DU Juan;LI Junqi
    . 2011, 42(10): 1916-1919.
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    Bismuth vanadate(BiVO4) microspheres were prepared with Bi(NO3)3 and NH4VO3 as starting materials and with NaOH to adjust pH through the microwave hydrothermal method at 180 ℃. The effect of different calcination temperatures on the crystalline phase and morphology was investigated, and the relationship between crystalline phase of BiVO4 and its photocatalytic performance was further studied. The as-prepared BiVO4 samples were characterized by XRD, SEM and UV-Vis. The photocatalytic activity of the BiVO4 microspheres was determined by degradation of methylene blue molecules under visible light irradiation. The results indicate that the crystalline phase of as-prepared BiVO4 microspheres is tetragonal phase, and the diameter of microspheres is 1-3 μm. It is found that the phase transition has undergone after being calcined at 500 ℃, and monoclinic scheelite BiVO4 microspheres obtained by being calcined at 600 ℃ has the excellent visible-light photocatalysis. Besides, BiVO4 with different crystalline forms can affect the degradation of methylene blue molecules.
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