20 November 2011, Volume 42 Issue 11
    

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  • WANG Xiaotao;BI Shuguang;PENG Haiyan
    . 2011, 42(11): 1927-1930.
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    The review summarized the researching progress on phase behaviors of LCs under chemical confinements such as polymer blocks, carbon nanotubes (CNTs) and polyhedral oligomeric silsesquioxanes (POSS) which are covalently linked with LCs. The researching results showed that the confinements of polymer blocks decrease the order degree and phases transition temperature of liquid crystalline phases in the blocking copolymers. For liquid crystalline polymer grafted CNTs, the confinements of CNTs destroy the LC ordering, and there exists no liquid crystalline phase in them. The incorporation of POSS in LCs via covalent bonds enhance the thermal stability of LC phases. However, as the content of POSS is higher the critical value, the LC molecules exhibit the monotropic liquid crystallinity, and their liquid crystallinity disappears.
  • 研究与开发
  • GU Tao;SHI Haishan;YE Jiandong
    . 2011, 42(11): 1931-1935.
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    Reinforced calcium phosphate cement (CPC) composed of three compartments was prepared by orthogonal test to improve the properties in this study. The effects of tetracalcium phosphate on the mechanical properties, setting time, phase evolution, microstructure, and exothermal behavior of CPC were systematically investigated. The results demonstrated that with the tetracalcium phosphate reacting lowly, the compress strength of CPC was enhanced remarkably. New content obviously increased the setting time, reduced the porosity and enhanced the compressive strength of CPC by about 50%, the exothermal peak during reaction dropped by 40% while cumulative heat liberation maintained constant. This ternary CPC system should be a promising material for bone repair and bone reconstruction.
  • CHU Huijuan;WEI Hongliang;ZHU Baoku
    . 2011, 42(11): 1936-1938.
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    To explore low dielectric polyimide, cellular polyimide films were prepared from pyromellitic dianhydride and 4,4′-diaminodiphenyl ether via a combined technique of solution induced phase separation and thermal imidization. These polyimide films displayed good thermal stability. SEM analyses showed that the obtained polyimide films had various cellular structures with the different conditions, such as the composition and temperature of coagulation bath, staying time, etc. The films with sponge–like cellular structures exhibited lower dielectric constants than those with finger–like structures. When the film was prepared in the conditions the coagulation bath of DMAc/H2O of 20/80, the temperature of 25?C and the staying time of 20 minutes, the film was full of sponge-like structure and its dielectric constant was low to 1.45.
  • YU Miao;JU Benxiang
    . 2011, 42(11): 1939-1942.
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    Magnetorheological elastomer(MRE) is a new member of the magnetorheological materials,dynamic mechanical properties of MRE is an important part of studing MRE materials,The establishment of dynamic mechanical properties testing system is the problem must to be solved. This work design a device for testing dynamic mechanical properties of MRE, which steady sinusoidal signal was provided by electromagnetic vibration, magnetic field strength can be changed by adjusting the spacing of NdFeB permanent magnet during the experiment. Force sensor and accelerometer installed on the testing system to get shear stress and acceleration signal of MRE in shear motion, displacement data can be calculated from two acceleration integration. Dynamic shear stress-strain relationship of MRE established through the force and displacement data, therefore, dynamic mechanical properties of MRE under shear mode were obtained by combining theoretical model of viscoelastic material. The system will provide a necessary guidance for preparation high performance MRE.
  • ZHU Yutian;XU Qin;CHEN Maolin
    . 2011, 42(11): 1943-1946.
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    Based on a photo-induced bending material which has two-way shape memory function, a novel micropump with valves was designed and made. Combined with material deformation principle, the micropump’s finite element model was built by using the finite element software ANSYS, and the pumping capacity calculated by ANSYS was gained and compared with the one came from the pump prototype’s experimental results, then the consistency of which validates this micropump design’s rationality. The material application on micropump has some reference values for relative engineering application and the photo-induced bending effect equivalent also provides research methods for similar problems.
  • ZHANG Lei;SHEN Honglie;HUANG Haibin
    . 2011, 42(11): 1947-1950.
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    Poly-crystalline silicon thin films were prepared on quartz glass, AZO, Si(100) and Si(111) substrates using SiH4 and H2 by hot wire chemical vapor deposition (HWCVD). Crystalline fraction, orientation and stress in the films deposited on different substrates were characterized by XRD, Raman spectrum and FT-IR, surface morphology was observed by SEM. The results show that all the samples are (111) oriented. Si substrate can promote the crystallization of the films deposited on them, and Si(111) substrate has better induction effect than Si(100) substrate. AZO which is (002) oriented also shows induction effect. Raman spectra are fitted and crystalline fraction for all the films are calculated. The result shows that except the film deposited on quartz glass, all the other samples have crystalline fraction above 90%, especially higher for films on Si substrates. There exist compressive stress in the samples except the film deposited on Si(111).
  • ZHANG Lei;LIU Danmin;DENG Xiaojun
    . 2011, 42(11): 1951-1953.
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    Mn1.2Fe0.8P0.75Ge0.25 compound has been prepared by mechanical alloying and subsequent spark plasma sintering (SPS) technique. XRD and VSM were used to analysis the phase composition and MCE .The results show that the sintered bulk sample has a hexagonal Fe2P-type crystal structure, the thermal hysteresis of M-T is about 4K. The Curie temperature Tc is 292K, and the maximum magnetic entropy change of the compound reaches to 18J/kg.k and adiabatic temperature change △Tad is 4K in a field change from 0 to 1.5T. The properties of this compound meet room temperature magneto-caloric requirements.
  • WU Leigang;WU Jing;HOU Ruixia
    . 2011, 42(11): 1954-1957.
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    One kind of tacrolimus eluting stent coated with biodegradable poly(1,3-trimethylene carbonate) (PTMC) was developed. The results of Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD) analysis proved the chemical stability of tacrolimus loaded in PTMC matrix. Stent coating were examined by scanning electron microscopy (SEM), indicating that the coating not only was very smooth and uniform but also had the ability to withstand the compressive and tensile strains. In vitro drug release of tacrolimus-eluting stents was similar to the Weibull’s release mode . The result of in vitro platelets adhesion and human umbilical cord artery smooth muscle cells (HUCASMCs) culture showed the PTMC loaded by tacrolimus could significantly prohibit the adhesion of platelets and the proliferation of HUCASMCs. This work aims to find a better biodegradable polymer which is surface erosion and can be applied as drug-eluting stent coatings.
  • HE Yongjia;LV Linnv;JIN Shun
    . 2011, 42(11): 1958-1961.
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    Conductive cement-based composite material was prepared by using carbon fiber and conductive functional aggregate calcined by graphite particles and clay matrix as composite conductive components. The pressure sensitivity of the composite material was investigated with Instron5882 materials testing machine, dynamic resistance strain gauge and DC power supply systems, and the results show that its resistivity was obviously affected by the pressure stress; during the process of loading beginning to failure, the change of resistivity showed even decrease, balance and rapid increase phases. In low level stress loading cycles, the variation of resistivity change had good correlation with pressure stress, but in high level stress loading cycles, the resistivity showed irreversible increase due to the unrecoverable damage cracks. Loading speed also affected the variation of resistivity change, under low loading stress the loading speed had minor effect on the variation of resistivity change, but under high loading stress the effect was relative obvious.
  • TIAN Zuzhi;HOU Youfu;WANG Nannan
    . 2011, 42(11): 1962-1964.
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    To ensure the torque transmission properties of magnetorheological transmission device, the experimental method is used to analyze the effect of material, rough, surface morphology of disk, slip speed and working gap on the torque transmission properties. The results indicate that material of wall has a significant influence on the properties, the lower the permeability of material, the smaller the torque transmits, and the wall effect will appear; the surface morphology of disk has also an important influence on the transmission properties, the concave convex concentric circles surface reduces the torque; when the slip speed is higher, the process of particles chains formed is complex and the torque will be lower, the working distance has little effect on the transmission properties.
  • TANG Ruihe;WU Zhangben;YANG Zhigang
    . 2011, 42(11): 1965-1968.
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    Co-C nanocomposite thin films with Co contents of 13.0~24.6 at.% were deposited by magnetron sputtering. Co-C thin films were annealed at 400 ℃ for 2 h in vacuum. Magnetic hysteresis loops of the as-deposited and annealed samples were measured at 5 K, 77 K and 300 K. Annealing and composition dependence of microstructure and magnetic properties of Co-C nanocomposite thin films were investigated systematically. The as-deposited thin films show weak magnetization. After annealing, magnetic properties are enhanced. Samples with low Co content exhibit ferromagnetic properties at low temperature while superparamagnetic properties at room temperature, which is characteristic granular nature. Magnetization, coercivity, associated with the blocking temperature of Co-C thin films increase with increasing Co content.
  • WEI Yongfeng;ZHANG Jiuxing;BAO Lihong
    . 2011, 42(11): 1969-1971.
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    The DyHx nano-powders were prepared by hydrogen arc plasma method, and then the mixed of DyHx nano-powders and micron boron were sintered by Spark Plasma Sintering (SPS) method to fabricate high-properties polycrystalline DyB6 bulk. The influence of SPS sintering temperature on the microstructure and property was investigated. It is shown that the pure phase DyB6 bulk can be easily fabricated by SPS when the sintering temperature is 1275℃. The values of density, Vickers hardness and bend strength respectively reach 5.191g/cm3,23.32GPa and 112.8MPa when the sample was sintered at 1425℃ and 60MPa. Thermionic emission measurement of the sample was performed. The emission current density of the DyB6 is 3.6A/cm2 at 1933K.
  • CUI Xuemei;WANG Yan;DENG Min
    . 2011, 42(11): 1972-1976.
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    This paper we proposed a novel technology of CNT field emitters fabrication—Planting Technology. The morphologies of CNT field emission cathode fabricated using this method were observed by field emission scanning electron microscopy(FESEM). The effects of ball milling time, etch time, weight ratio between CNTs and polymer media on the field emission property were investigated. The results showed that cathodes fabricated by planting technology have good field emission properties, such as low turn-on field(1.7 v/μm) and high current density(26 mA/cm2 at an applied electric field of 3.6v/μm). Planting Technology combined the advantages of direct growth and screen printing. Structures with high conhesiveness bwteen CNTs and metal substrate have been obtained, and this structures as core module have a high potential to be applied to emission devices.
  • Shao Hui;ZHOU Hongqing;ZHU Haikui
    . 2011, 42(11): 1977-1980.
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    Glass-ceramics were prepared by sintering method. The effect of glass composition on sintering and crystallization behavior as well as properties of the glasses were investigated by using (Thermogravimetry- differential scanning calorimetry, DSC), X-ray diffraction (XRD), scanning electron microscopy (SEM) and property measurements. The results show that the optimal sintering temperature for this glass-ceramic is 875 ℃ for 15 min, and the major phases of this material are β-CaSiO3, CaB2O4 and SiO2. The glass-ceramic possesses excellent dielectric properties: εr = 5.3, tanδ=0.003 at 10 kHz and density about 2.48g.cm-3.The crystallization process occurred prior to densification the process, which is not favorable for densification. The CBS Glass-ceramics of sintering is crystallization sintering, viscous flow sintering. Crystallization during the sintering and the densification are competing processes.
  • YI Qianning;HU Chenguo
    . 2011, 42(11): 1981-1984.
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    Square-like WO3 Nanoporous pillar arrays were prepared by a hydrothermal process at 160℃ for 48h. The phase and morphology of the product were characterized by scanning electron microscopy and x-ray diffraction spectroscopy. A micro-humidity sensor based on a single piece of WO3 square was fabricated, for proving the superiority of the as-synthesized material in structure. It was shown that the resistance of the sensor decreased almost in a linear way, with the increase of the relative humidity from 20% to 75%. It was also found that when the relative humidity in atmosphere changed periodically between 20% and 60%, the sensor responded fast (~2s) with excellent stability and repeatability. Analysis indicated that the protonic conductivity played a leading role in the sensing process of the humidity sensor.
  • LI Qiang;YANG Xianjin;CUI Zhenduo
    . 2011, 42(11): 1985-1988.
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    The ingots with composition of Ti-24 at.%Nb -(0,2,4) at.%Zr were prepared by non-consumble arc melting methods. They were homogenized, solution treated, cold rolled, and annealed in turn. Tensile tests and loading-unloading tests were carried out at room temperature. Changes of microstructure before and after tensile tests were observed by optical microscope, X-ray diffraction and transmission electron microscope. Deformation Mechanisms were determined by analyzing microstructure and tensile curves. The results showed that {112} <111> twinning appeared in Ti-24 at.%Nb alloy with low strength. The addition of Zr improved the strength of alloys and stability of β phase. In this case, {112} <111> twinning disappeared with the formation of {332} <113> twinning. Due to the appearance of a stress-induced α” martensite transformation, the alloys showed super-elasticity in tensile loading-unloading tests. Ti-24 at.%Nb-2 at.%Zr with a super-elastic recovery of 3.6% is potential to be applied as biomaterials.
  • DONG Gang;ZHU Zhongqi;LIU Qingju
    . 2011, 42(11): 1989-1992.
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    Abstract: The TiO2 photocatalyst samples co-doped with iron and nitrogen were prepared by sol-gel method and microwave chemical 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-N-TiO2 samples are a mixed phase of anatase and rutile, and the threshold wavelength is red shift about 45nm. The co-doping of iron and nitrogen inhibit the phase transformation from anatase to rutile and the photocatalytic activity is improved. The activity of the sample prepared at 600℃, n Fe): m(TiO2)=1: 200 is the best under fluorescent lamp and is obviously higher than that of Degussa P25.
  • YANG Baoping;ZHONG Xiaohua;ZHANG Xiaoliang
    . 2011, 42(11): 1993-1997.
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    Using sol-gel method with the simple starting reagents of SnCl4·5H2O and SbCl3, antimony doped tin oxide (ATO) nanoparticles were synthesized. The microstructure, composition and conductivity properties were characterized by FESEM, X-ray diffraction (XRD), Fourier transform infrared spectrophotometer (FTIR), X-ray photoelectron spectroscope (XPS) and four-probe resistivity/square resistance tester, and the effects of the Sb content on the crystalline microstructure, the crystalline size and the resistivity of the ATO nanoparticles were investigated systematically. The results show that The as-synthesized ATO was with tetragonal cassiterite crystalline structure of SnO2, and the preferred orientation was observed as (110), and its resistivity was obtained to be as lowest as 12.85 Ω?cm when the Sb content was 15%. The complete doped ATO can be obtained with the Sb contents less then 28%. The conductivity of the ATO was related with the concentration of Sb5+, and there is an optimal value of Sb contents that is beneficial for Sb converting to Sb5+, and it make the carrier concentration to the maximum, so it deserves the optimum conductivity.
  • YAN Mifang;XUE Lihong;YAN Youwei
    . 2011, 42(11): 1998-2000.
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    Red emitting phosphor α-Sr2P2O7: Eu3+ was prepared by a combustion-assisted synthesis method. The luminescence, crystallinity and particle sizes were investigated by using luminescence spectrometry, x-ray diffractometer, and field scanning electron microscopy. The emission spectrums shows that the most intense peak is located at 613 nm, which correponds to the 5D0→7F2 transitions. The phosphors has two main excitation peaks located at 394 and 464 nm, which mathch the emission of UV and blue light-emitting diodes , respectively.
  • MA Suyun;ZHU Zhenghou;LIU Xiaoqin
    . 2011, 42(11): 2001-2004.
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    Montmorillonite(MMT) is treated by the intercalation of organic using the method of solution intercalation. It included acidification and organization treatment. The results showed that the acidification can not only expand the interlayer spacing of MMT, but also effectively improve the compatibility of organic montmorillonite in toluene, xylene and other organic solvents.The microstructure and morphology of organic montmorillonite were investigated by TGA, XRD and FTIR. Furthermore, the acidification mechanism was aslo studied.
  • YU Honghao;XUE Xiangxin;HE Yan
    . 2011, 42(11): 2005-2008.
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    Using the iron ore tailings as the silica source and n-hexadecyltrimethyl ammonium bromide (CTAB) as the template, highly ordered mesoporous molecular sieves MCM-41 were successfully synthesized by hydrothermal synthesis. The technique of X-ray diffraction was used to identify the effects of the systhesis pH, CTAB/ SiO2, crystallization time and crystallization temperature on the crystal structure of MCM-41. The results showed that the synthesis conditions for getting suitable mesoporous molecular sieves MCM-41 were CTAB/SiO2 of 0.05~0.60, pH of 8~11, minimum crystallization time of 24 h and crystallization temperature 60~100 ℃. The pore structure of MCM-41 was well-ordered and symmetrical hexagonal structure, which pore diameter of MCM-41 was changed between 2 nm to 4 nm. Silicon-oxygen tetrahedron skeletons were confirmed by FT-IR.
  • LIANG Ye;HAN Baoqin;LIU Wanshun
    . 2011, 42(11): 2009-2013.
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    A novel chitosan-based membrane made of hydroxyethyl chitosan, gelatin and chondroitin sulfate was used as a carrier of corneal endothelial cells. The characteristics of the blend membrane, such as transparency, equilibrium water content, cytotoxicity were determined. To study the effects of cell attachment and growth on the membrane, rabbit corneal endothelial cells were cultured on the artificial membrane. And The in vivo biodegradability and histocompatibility of the blend membrane were evaluated by implantation into the muscle of the rats and the anterior chamber of rabbits. As a result, the optical transparency of the membrane was as good as the natural human cornea. The water content of this scaffold was 74.25% which was remarkably close to the native cornea. The membrane is belonged to non-cytotoxicity materials. The cultured rabbit corneal endothelial cells formed a monolayer on the membrane which demonstrated that it was suitable for corneal endothelial cells to attach and grow. In addition, the membrane could be degraded in vivo steadily with less inflammation and showed a good histocompatibility property. These results demonstrated that the hydroxyethyl chitosan-chondroitin sulfate-gelatin blend membrane can potentially be used as a carrier for corneal endothelial cell transplantation.
  • TANG Yuanyuan;TANG AiDong
    . 2011, 42(11): 2014-2016.
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    Volatile organic compounds contained chlorine (Cl-VOC) like dioxins is a kind of highly toxic gas phase environmental pollutants. For the purpose of choosing high efficiency and stable catalysts which is used for catalytic combustion of Cl-VOC, a series of (Fe,Co,Cu,V)-Mn catalysts supported on cordierite were synthesized and used for catalytic combustion of o-dichlorobenzene. The results showed that Cu-Mn/cordierite catalyst had the best catalytic performance in all catalysts. XRD results indicated that a new CuMn2O4 spinel phase presented in the Cu-Mn/cordierite catalyst and SEM results demonstrated that the particle distributed well. However, EDS results showed that the catalyst after reaction had a small amount of residual chlorine on its surface compared with before reaction. Further stability test result demonstrated that the degradation rate of o-dichlorobenzene is about 65% after 20 h continued reaction, which showed that Cu-Mn/cordierite catalyst maybe have a good promise for catalytic combustion of volatile organic compounds contained chlorine.
  • LIU Huan;GONG Shuping;LIU Jianqiao
    . 2011, 42(11): 2017-2020.
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    V-doped TiO2 films were prepared by the sol-gel method starting from tetrabutyl titanate and vanadium(III) 2,4-pentanedionate. Their properties were characterized by XRD, UV-Vis absorption spectra, FTIR, and XPS with the undoped film samples as the control. Both the V-doped and undoped TiO2 films are anatase and the band gap decreases from 3.28 eV to 3.15 eV, with a red shift in the absorption of V-doped TiO2 film compared to the undoped samples. The V-doped films consist of vanadium atoms in the V4+ and V5+ oxidation states, generating deep defect levels and the valence bandedge might extend into the forbidden band gap, inducing the band gap narrowing effect and enhancing the bandedge absorption. At the grain boundaries of TiO2, those impurity defects located deep inside the gap become closer to the top of the valence band and hence tend to trap the photo-generated holes, which would contribute to inhibit the recombination of photogenerated carriers and become highly attractive for application in photocatalytic materials.
  • HANG Yichun;ZHANG Yaopeng;JIN Yuan
    . 2011, 42(11): 2021-2025.
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    To biomimic the composition and core-shell structure of natural Bombyx mori silk, regenerated ultra-fine fibers with a core (silk fibroin, SF) –shell (silk sericin, SS) structure were prepared by coaxial electrospinning. The influences of core flow rate (Qc), applied voltage (V), distance from capillary to collector (D) and the strength of electric field (E) on the morphology and core-shell structure of RSF/SS fibers were studied using scanning electron microscope (SEM) and transmission electron microscope (TEM). It was found that the RSF/SS fibers had clear core-shell structure with average diameters from 1400 to 2100 nm. The Qc had a great influence on the formation of the core-shell structure. A larger Qc induced an off axis of core fiber or non-coaxiality because of uneven adhesion of SS (shell) on the SF (core) component. Furthermore, with increasing E (increasing V or decreasing D), both the average diameter and the diameter deviation of the RSF/SS fiber were decreased and the core-shell structure became clearer. While at the same E, the higher V orlonger D facilitated the formation of the uniform RSF/SS fiber and core-shell structure.
  • YU Juan;WEI Yan;WANG Jigang
    . 2011, 42(11): 2026-2029.
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    Abstract:The hydrothermal synthesis method was employed to prepare the magnesium-aluminium layered double hydroxides (LDHs) by using Mg(NO3)2?6H2O and Al(NO3)3?9H2O as the raw materials. Considering the hydrogen bonding interactions existing in the LDHs, the co-solvents of polyhydric alcohols will have a great influence on the preparation of the LDHs. To investigate these effects, we respectively employed five kinds of solvents: pure water, water/ethanol, water/glycol, water/glycerin, and water/pentaerythritol. The microstructures and thermal properties of the prepared LDHs were contrastively investigated by XRD, SEM, IR, and DSC. With the increasing number of the hydroxyl groups in the co-solvents, the hydration levels of the crystal water in the LDHs were elevated. The interactions between the co-solvent and the LDHs affect the nucleation and subsequent growth of LDHs, resulting in the variation of crystallinity and thermal stability. The LDHs prepared using water/ethanol and water/glycol as solvent, respectively, have similar crystalline shapes to that synthesized with pure water. But for the LDHs respectively synthesized using glycerin and pentaerythritol as co-solvents, the crystalline shapes became irregular with smaller grain size and the aggregation of grains. In addition, as the number of the hydroxyl groups in the co-solvents is increased, the temperatures for releasing crystal water were elevated, but the corresponding temperatures for the dehydration of basic layer and the release of carbon dioxide were decreased.
  • ZHU Mingyuan;CHEN Huiming;HU Yemin
    . 2011, 42(11): 2030-2033.
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    Olivine-structured LiFePO4 is a promising cathode material for lithium-ion batteries. A two-step carbothermal reduction method was used in synthesizing LiFePO4 cathode materials in this study. Decreasing high-temperature sintering time of the two-step method restrained the growth of the particle. At the same time, carbon was wrapped on the surface of LiFePO4 particle. And a LiFePO4/C composite cathode material was formed. The results showed that the initial discharge capacity of this sample was 149.4 mAh/g at 0.1C rate and the discharge efficiency reached 93.5%.On contrary, the one-step carbothermal reduction sample had an initial discharge capacity for 99.1mAh/g. And the discharge efficiency is 81.4%. Then the mechanism of synthesis reaction and electrochemical result was analyzed.
  • TANG Aidong;HU Liqin;WANG Duo
    . 2011, 42(11): 2034-2037.
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    Cuprous oxides (Cu2O) with different shapes, such as spheres and octahedron, have been synthesized by facial wet-solution method at room temperature. Its structure, morphology and photo-catalytic performance were characterized by X-ray powder diffraction (XRD), scan electron microscope (SEM) and spectrophotometer. The concentration of NaOH has significant effects on the formation and growth of these Cu2O particles. The possible growth mechanism of the Cu2O crystal was discussed. Its photo-catalytic activities in the degradation of methyl orange as the model pollutant using incandescence light as an energy source were investigated. The result indicates that the spherical Cu2O shows a superior photo-catalytic activity to methyl orange than octahedral Cu/Cu2O composite material at initial reaction time. However, octahedral Cu/Cu2O composite demonstrated better photo-catalytic activity and structure stability when presented in methyl orange solution for a long time about 25 days.
  • ZHOU Chao;ZHANG Huiting;CHEN Junying
    . 2011, 42(11): 2038-2041.
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    In this paper, after being sonic cleaned by acetone, ethanol and distilled water, the quartz glass was chemically activated for obtaining hydroxyl functional groups on its surface. Silanization was then performed by incubating the activated quartz glass in 3% solution of (3- aminopropyl) -triethoxysilane (APTE) (from Sigma-Aldrich) in anhydrous alcohol for 12 hours at room temperature. Fibronectin (Fn) was dissolved in physiology saline water for achieving different concentrations. To immobilize Fn molecule onto the silanized quartz glass surface, the samples were respectively incubated into 5, 25, 50μg /ml Fn solution containing NHS/MES/EDC system for 4 hours at 37℃. The water contact angle measurement, X-ray photoelectron spectroscopy (XPS) and Atomic force microscope (AFM) were used to investigate the characteristics of the surface after each modification procedure. Especially, the immobilized fibronectin was quantificated by the micro-bicinchoninic acid (MicroBCA) protein assay (from Pierce) method. The results indicated that, the fibronectin was successfully immobilized on the silanized quartz glass surface. The density of the immobilized Fn molecule on surface was positively correlated with the input concentration of the incubating Fn solution in a certain range. The work supplied a new assay to quantify the immobilized biomolecule on biomaterials surface.
  • LIU Xuyang;HU Meilong;BAI Chenguang
    . 2011, 42(11): 2042-2046.
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    The FeTi alloy can be prepared directly by electrolysis in CaCl2 molten salt.The raw material is ilmenite concentrate from Panzhihua area. The main purpose of the paper is tracking deoxideation process through interrupted experiments at different time. The results show that the iron and perovskite are first obtained during the process of preparing FeTi alloy through electrolysis ilmenite concentrate in CaCl2 molten salt. Then the titanium suboxide can be obtained by electrolysis the perovskite . Finally, FeTi alloy can be obtained by electrolysis the titanium suboxide. The weight loss experiments of the cathode verified the conclusion of the previous studies.The final part of the paper studies the formation mechanism of perovskite through experiments. There have two ways, the main reason is reaction of salt, and another reason attributed to the hydrolysis of CaCl2 molten salt.
  • LILi;WANG Feifei;NIU Zongwei
    . 2011, 42(11): 2047-2049.
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    Electroplating Ni–P alloys process on sintered NdFeB was studied which involves with ultrasonic. The influence of ultrasonic on electroplating Ni–P alloy on NdFeB was studied by using microscope, adhesion test and NaCl solution immersion test. The results showed that the Ni–P alloy deposit on NdFeB is rough and has poor adhesion without ultrasonic agitation; however, the Ni–P alloy deposit on NdFeB with ultrasonic agitation has more compact and uniform microstructure, smoother morphology. At the same time, the adhesion and corrosion resistance are greatly enhanced.
  • WU Wenjuan;XIAO Dingquan;WU Jiagang
    . 2011, 42(11): 2050-2052.
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    In this paper, the relationship between the calcined temperature and the phase structure for the 0.94Bi0.5Na0.5TiO3-0.06BaTiO3 (BNT-6BT) ceramic powders was systematically studied, and the BNT-6BT ceramic powder was successfully synthesized at low temperature (600 °C). The BNT-6BT lead-free piezoelectric ceramics made from these powders have been prepared by using traditional solid-state synthesis method, and the effect of the calcined temperature of the powders on the electrical properties for the ceramics was also studies. The results show that BNT-6BT ceramics powder can be synthesized at 600 °C, which significantly reduces the calcined temperature compared to the usually used at 900 °C; the electrical properties of the piezoelectric ceramics slightly increase with the decreasing of the calcined temperature; and the BNT-6BT ceramics made from the powder synthesized at low temperature (600 °C) exhibits excellent electrical properties with ?=5.87 g/cm3, d33=141 pC/N, kp=0.30, Qm=141, Tc=278 °C, Td=132 °C, εr=1643, Pr=23 μC/cm2, and Ec=32 kV/cm.
  • ZHU Zhenfeng;ZHANG Yanli;LIU Hui
    . 2011, 42(11): 2053-2056.
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    α-Ni(OH)2 percursor was synthesized using PVP as surfactant and nickel nitrate as nickel source through a microwave-assisted hydrothermal method. The NiO with micro-nano structure was obtained after calcined of the precursor α-Ni(OH)2 at 500℃.The chemical structure and surface morphology of the as-obtained products were well characterized by XRD, SEM, TEM, UV-Vis, and the electrochemical character was initially explored. The experimental results shown that the as-prepared products was cubic system and the morphology was microballoon sphere. The CV shows that the sample had obvious faraday quasi capacitance and stabilized electrochemical character.Also,The results indicated that it was reversible.
  • LU Yingdong;CHANG Yongqin;ZHANG Jingmin
    . 2011, 42(11): 2057-2059.
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    Ga doped ZnO nanowires with large length-diameter ratio were synthesized by chemical vapor deposition method using Sn catalyst. The diameter of the nanowires is around 25~90 nm. Room temperature photoluminescence results of the Ga doped ZnO nanowires show that the intensity of the ultra violet emission increases, and the position of the ultra violet emission shift to short wavelength with the doping of Ga. While the blue-shift degree decrease with Ga doping, and turn to red-shift with heavy doping. The doping of Sn only affects on the blue-green emission of the Ga doped ZnO nanowires.
  • YAN Jialei;SUN Yan;SHI Liang
    . 2011, 42(11): 2060-2063.
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    In this paper, nano-TiO2 powder doped with rare earth Ce3+ (nano-Ce/TiO2) was prepared through sol-gel method and characterized by XRD, BET and SEM. The results show that the nano-Ce/TiO2 is anatase with the grain size 19.95nm, specific surface area 43.302m2?g-1. Carboxymethyl chitosan(CMC) was synthesized in ultrasonic as catalyst and was composited with the nano-Ce/TiO2 to prepare a kind of antibacterial composite film(CMC/Ce/TiO2). FT-IR is successfully used to characterize the CMC/Ce/TiO2 composite. Antibacterial property of nano-Ce/TiO2, common nano-TiO2, CMC/Ce/TiO2 and CMC were tested preliminarily. The antibacterial activity of nano-Ce/TiO2 to E-coli and staphylococcus aureus are 55%, 53% and the antibacterial activity of common nano-TiO2 are 99% and 95%. The antibacterial activity of CMC/Ce/TiO2 to E-coli and staphylococcus aureus are 99% and 95% and the antibacterial activity of CMC are 90% and 80%. It can be known that doping Ce3+ can improve bacteriostasis of nano- TiO2 and CMC/Ce/TiO2 composite is an excellent antimicrobial with better antibacterial activities than CMC.
  • HAN Shiyan;SONG Zhanqian;YU Fangdan
    . 2011, 42(11): 2064-2067.
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    Abstract: A novel gemini surfactant was synthesized from dehydroabietic acid, and its chemical structure was confirmed by Fourier transform infrared spectroscopy (FT-IR) and 1H nuclear magnetic resonance (NMR) analysis. Then anatase nanometer TiO2 (average size was 8.81nm) was prepared from tetra-n-butyl titanate (TNB) and this gemini surfactant via hydrothermal synthesis. The prepared TiO2 nanoparticle was characterized by FT-IR,transmission electron microscopy (TEM) and X-ray diffraction (XRD). Moreover, its photocatalytic activity was determined with RhB as model pollutant under UV irradiation. The results showed that its photocatalytic activity was greater than that of the nano TiO2 prepared without surfactants. The model pollutant RhB was almost totally degraded (99.7% of degradation rate) after 3h under UV irradiation.
  • MI Chaohui;CUI Bin;YOU Qiaoming
    . 2011, 42(11): 2068-2072.
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    In this study, X7R type BaTiO3-based ceramics were prepared by the nano-doping process and directly doping method respectively by using Li2O-SiO2(LSO) nano-composites as sintering aids. The effect of nano-doping and directly doping of Li2O-SiO2 sintering aids on the microstructure and dielectric properties of the ceramics were studied. And we studied the effect of LSO amounts and sintering temperature on the microstructure and dielectric properties of the ceramics. The sintering mechanism was also discussed by defect chemistry theory. The results indicate that, the doping elements enter the crystal lattice by directly doping method and produce ion vacancies. This can decrease the diffusion activation energy and then leads to an effective densification as well as significant microstructure improvement, when compared with the performance obtained on the nano-doping process. Dielectric constant of the specimens were enhanced with an increase of LSO up to 0.08mol% and then decreased. The specimens with 0.08mol% LSO sintered at 1200°C for 4 h showed εr of 4855 and met X7R character. The sintering aids can be uniformly distributed in the ceramics by directly doping method and the amounts of sintering aids can be decreased apparently. Finally, the sintering temperature of ceramics has been lowered significantly and the properties of ceramics have been improved obviously.
  • WANG Yan;MIN Jiahua;LIANG Xiaoyan
    . 2011, 42(11): 2073-2077.
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    The Cd0.9Zn0.1Te crystal growth (LPVB--Low Pressure Vertical Bridgman) was numerically simulated and analyzed by the simulation software of Comsol Mutiphysics. The influence of curvature on solid-liquid interface is studied, and the radial solute segregation is calculated. Three kinds of growth methods divided as following: 1.constant velocity; 2.changed velocity; and 3.remelting growth are studied on the radial solute segregation. Energy dispersive X-ray detector of scanning electronic microscopy is used to test the concentration of Zinc. And all the calculated data are agreements with the results of the experiments.
  • ZHANG Xiaoqing;LOU Kexing;WANG Jiaxing
    . 2011, 42(11): 2078-2080.
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    The electromechanical properties of the piezoelectrets based on the irradiation cross-linked polypropylene (XPP) were investigated. The Young’s modulus of the XPP films were determined from the dielectric resonance spectra. The piezoelectric d33 coefficients in such piezoelectret films were measured by using quasi-static method. The thermal stability of d33 coefficients were investigated by isothermal annealing and thermally stimulated discharge. The time spectrum of piezoelectric response was analyzed. The experiments of the mechanical fatigues in the XPP piezoelectret films were also taken. The result shows that the Young’s modulus of the XPP films is around 1.3 MPa. The d33-coefficients exhibit good linearity in the range of applied pressure from 10 to 60 kPa. The d33 values decrease with the increase of the charging temperature. The time spectrum of piezoelectric response reveals a viscous flow feature in XPP films. The relation between the output voltage and applied force is linear. No significant change in d33 coefficients was observed after 600000 cycles of applying force.
  • SHI Dongjian;REN Shenyue;XIONG Wanbin
    . 2011, 42(11): 2081-2084.
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    Poly(N-vinylacetamide) (PNVA) grafted polyacrylonitrile/polystyrene (PNVA-g-PAN/PSt) polymer spheres were prepared by dispersion copolymerization of acrylonitrile(AN), styrene (St), and PNVA macromonomer using AIBN as an initiator. Palladium nanoparticles were homogenously located onto surfaces of the PNVA-g-PAN/PSt polymer spheres, which was confirmed by transmission electron microscopy (TEM), by reduction method using PdCl2 as metal and ethanol as reducing agent. The amorphous diffraction peak of the polymeric particles and obvious palladium cubic crystal diffraction peaks were appeared in the powder of X-ray diffraction (XRD) pattern. The diameter of palladium nanoparticles, calculated from the XRD, was about 9 nm. Moreover, the weight percentages of palladium nanoparticles stabilized onto the microspheres were about 15 to 30, which were calculated from the thermogravimetric analysis (TGA). Glucose could convert to sodium gluconate easily in the present of the pd@PNVA-g-PAN/PSt spheres, suggesting the nanoparticles had excellent catalytic oxidization.
  • YAO Bo;FANG Zebo;ZHU Yanyan
    . 2011, 42(11): 2085-2088.
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    Er2O3 films have been prepared on p-type Si (001) substrate by Molecular Beam Epitaxy (MBE). High-resolution transmission electron microscope (HRTEM) images show that the samples are uniform single crystals with perfect epitaxy on the substrate. It is found that the accumulation capacitances take on the frequency dispersion at high frequency when taking C-V test for MOS capacitor with Er2O3/p-Si. A new model for explaining the frequency dispersion effect is proposed .The capacitance-frequency equations are obtained by deriving the impedance expression of the model equivalent circuit. The equation and the experimental data are fitted by the MATLAB. The result shows that the interfacial layer, which is not fully oxidized, is the main reason of the frequency dispersion effect. Accordingly, we need to minimize or avoid the formation of the interfacial layers in order to eliminate the frequency dispersion effect of Er2O3 in accumulation.
  • LIU Jinlong;SHA Yuhui;ZHANG Fang
    . 2011, 42(11): 2089-2091.
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    High silicon steel thin sheets with thickness of 0.3mm were successfully produced by conventional rolling and annealing methods. Recrystallization texture was investigated by means of X-ray diffraction. It is found that recrystallization texture is mainly composed of γ fiber(<111>//ND)with peak at {111}<112> and {001} fiber with peak at {001}<210> after annealing at 700℃, while strong {001}<210> component dominates recrystallization texture after annealing above 900℃. It is during grain growth that {001}<210> is significantly enhanced and finally develops to the main texture component.
  • LIU Changyou;GU Zhi;WANG Tao
    . 2011, 42(11): 2092-2095.
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    ZnO microcrystal growth were investigated under a low temperature hydrothermal process with a relatively low concentration of N2H4&#8226;H2O(0.01-0.20 M). The nucleation and the growth rates of various crystal planes are strongly affected by the weak alkalinity of N2H4&#8226;H2O and the co-ordinative activity of N2H5+ ion. ZnO microcrystals change from oatmeal-like plate to hexagonal plate, and then to hexagonal rod-like cluster with increasing of N2H4?H2O concentrations, respectively. The nucleations of ZnO microcrystals are influenced by the alkaline dispersant and ultrasonic treatment. The solution of 0.20 M N2H4&#8226;H2O with the alkaline dispersant has a strong reducibility, which changes the mechanism of nucleation and growth of ZnO microcrystals. The center-hollow hexagonal rod-like ZnO clusters were obtained through the N2 bubble template-growth route.
  • LI Xuan;SHEN Yiding;LI Xiaorui
    . 2011, 42(11): 2096-2099.
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    A series of anionic waterborne polyurethane emulsion were successfully prepared by the reaction of Polycaprolactone diols (CAPA),   Toluene diisocyanate(TDI),dimethylolpropionic acid (DMPA). A kind of waterborne polyurethane / Carboxy1ated styrene-butadiene rubber1etex compound Latex was synthesized by polyurethane, Carboxy1ated styrene-butadiene rubber1etex and aziridine as crosslinker. The factors affecting its synthetic condition were discussed, and the synthetic process was optimized. The results show that the compound emulsion owns excellent sizing property when n(TDI):n(CAPA)=1.4,w(DMPA)=6%,m(PU)/m(XSBRL)=2/1, w(aziridine)=2%. The papers’ sizing value can reach 30s, folding endurance reach 86 times and surface strength reach 2.5m/s with 0.5% compound emulsion addition. And the polymer was characterized with TG and DLLS.
  • BAI Xiaohui;SHEN Yiding;LI Peizhi
    . 2011, 42(11): 2100-2103.
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    Organic/inorganic fluorinated and siloxane acrylates soap-free emulsion was prepared by the organic/inorganic hybrid polymerization.With tetraethyl orthosilicate(TEOS)and γ-methacryloxy propyl trimethoxysilane(KH570)as silicon monomers,2-(perfluoroalkyl)ethyl acrylate(FM) as fluorine monomer.The FT-IR results indicate that TEOS has hydrolied into SiO2,the acrilyic ester molecules、fluoro agent and silicon sol have participated in the copolymerization.The morphology structure of latex particles were characterized by TEM and AFM,the results indicate that the latex particles are well-distributed,the roughness and density have greatly improved.The DLS analysis shows the average particle size is about 49.49nm.The CA results illustrate that the add of FM、silicon sol and KH570 have significantly improved the waterproof property of the coatings.
  • Wang Pan;ZHENG Yuying;LI Baoming
    . 2011, 42(11): 2104-2106.
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  • Luo Zijiang;ZHOU Xun;HE Yequan
    . 2011, 42(11): 2107-2111.
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    A series of InxGa1-xAs films were grown on GaAs(001) substrates over the compositions range from InAs to GaAs(100%、39%、29%、19%、0%) by MBE. During the process of growing InxGa1-xAs, the growth rate and status was measured and monitored via RHEED oscillations and patterns respectively. Compared the RHEED oscillations and patterns, the growth mode turned rapidly from 2D to 3D with increasing of In composition. We draw a reasonable assumption to determine the composition of the InxGa1-xAs, and obtained ideal results. For the sample of composition of In0.19Ga0.81As, after growth and subsequent annealing, the STM images confirmed that the surface of this sample was atomically flat and (2×3) reconstructed.
  • CHEN Chunming;CHEN Zhonghua;ZENG Xingrong
    . 2011, 42(11): 2112-2115.
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    Abstract: The phase change nanocapsules (PCNs) with n-dodecanol as core and St-BA-AM co-polymer as shell were prepared by miniemulsion polymerization. The influence of emulsifier, co-monomer and the mass ratio of styrene to n-dodecanol on the structure and properties of nanocapsules were studied. The particles size and distribution, structure, properties and micro-morphology of nanocapsules were characterized by using DSC, TG, TEM, and laser particle diameter analyzer. The results showed that co-monomer acrylamine (AM) is helpful for encapsulation of n-dodecanol. As the mass ratio of styrene to n-dodecanol was 1:1, the phase change latent heat of nanocapsule and encapsulation efficiency of n-dodecanol reach to the highest value of 109.3 J/g and 92.1 %, respectively.
  • LEI Li;ZHAO Gaoyang;XU Hui
    . 2011, 42(11): 2116-2118.
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    Zn2+-doped YBCO thin films were prepared on LaAlO3 (LAO) single-crystal substrates by sol-gel process. The microstructure and growth orientation of the Zn2+-doped YBCO thin films were analyzed by X-ray Diffraction (XRD) and Transmission Electron Microscopy (TEM) respectively. The standard four-probe method was used to measure the superconducting properties of the pure and doped YBCO thin films. The results show that the critical current density Jc of the Zn2+-doped YBCO films was improved with the increase of Zn2+ concentration, although critical transition temperature Tc was decreased and transition width ΔT was broadened. When the Zn2+ doping percentage is over 0.5 mol%, the YBCO films exhibit deteriorated superconducting properties due to bad c-axis growth orientation. It is found that YBCO film doped with 0.5 mol% Zn2+ show the best superconducting performance with Tc of 91.3 K, ΔT of 1.1 K and Jc of 1.54 MA/cm2 (77K, 0T).