30 May 2013, Volume 44 Issue 10
    

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    综述·进展
  • An overview on the progress of catalysts for methanol to gasoline
    GAO Xiao-xia;WANG Xiao-dong;HUANG Wei
    . 2013, 44(10): 1369-1374.
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    In this paper, from the point of the existing problems in the ZSM-5 zeolite catalyst for methanol to gasoline (MTG), and from the two aspects that how to improve the catalytic properties and extend its life，it is reviewed in detail that the process of researching and exploring of the ZSM-5 zeolite catalyst since methanol to gasoline come out. We think that research and development of two-dimensional layer, one-dimensional line, as well as zero-dimensional unit cell molecular sieve materials is the focus of MTG catalyst in the future.
    • 研究·开发
  • Research of mold erosion of alkyd resin coating and the effect of chlorothalonil on the mouldproof properties
    ZHANG Yi-xuan;LI Song-mei;LIU Jian-hua;YU Mei
    . 2013, 44(10): 1375-1380.
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    Abstract: The impact of mold erosion on the appearance and performance of alkyd resin coating used in aviation and the inhibition of fungicide (chlorothalonil, TPN)added to the coatings were studied through mold test.The mildew situation of coatings were observed by using stereo microscope. The morphology of the coatings removal of mold were investigated by using scanning electron microscopy (SEM) and atomic force microscope(AFM). The change of corrosion resistance of the coatings were studied by electrochemical impedance spectroscopy (EIS).The results demonstrated that mildew situation is related to mold test time and the amount of TPN. With the mold test time increased, The roughness and the undulation of the coating microscopic surface increased, the pit corrosion generated in the thick region of the mold growth. Corrosion resistance of coating dropped significantly. Within the selected concentration range, the effect is more pronounced with increasing of TPN concentration.Mold test 84 days ,the mildew rating of coatings without TPN is 4.When the dosage of TPN is 0.5%,1%, 1.5%, the mildew grade is 3,1,0 respectively.
  • Electrochemical performance Research of Mg ion doped LiMnPO4/C
    LIU Xue-wu;LI Xin;DENG Yuan-fu;SHI Zhi-cong;CHEN Guo-hua
    . 2013, 44(10): 1381-1384.
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    LiMn1-xMgxPO4/C(x=0，0.01，0.04，0.05，0.1) were synthesized by using wet-ballmilling and solid-state calcining with phenolic resin as the carbon source. All samples are single phase with a similar morphology, but the cation substitution results in a crystal lattice shrink because of the smaller ionic radii of Mg2+, the particles are small and homogeneous. CV、EIS and charge/discharge measurement shows that the Mg substitution leads to a significantly increased reversible capacity due to the enhanced electrochemical kinetics. LiMn0.96Mg0.04PO4/C calcined at 600℃ has a discharge capacity of 144mAh/g at 0.05C. When charging-discharging by CC-CV-CC mode at high rates, LiMn0.96Mg0.04PO4/C composite exhibits a good cyclability and rate capability.
  • Electrical impedance spectroscopy Analysis on the electrode interface of Dye-sensitized solar cells
    LI Yan;ZHUANG Quan-chao;WANG Hong-tao;FANG Liang
    . 2013, 44(10): 1385-1389.
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    Electrical impedance spectroscopy (EIS) is a important technology to investigate electronic and ionic processes in dye-sensitized solar cells(DSSCs). EIS of DSSCs with different PEG content, setting time and light intensity were tested. A suitable model was used to fit the EIS. Each part of EIS was discussed and parameters were determined, for example, effective rate constant for recombination, lifetime of electrons, electron diffusion coefficient in TiO2, charge transfer resistance and electron transport resistance in TiO2, et al. Based on these parameters, effect of experimental condition on the electrode interface of DSSCs were discussed.
  • Experimental Study on the Porous Foam Iron-nickel Metal Inhibition of Gas Explosion Wave
    SUN Jian-hua;LI Yan-xia;WEI Chun-rong;WANG Shu-tong;XING Shu-ren
    . 2013, 44(10): 1390-1394.
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    To seek barrier device and develop explosion suppression material for coalmine gas explosion， effects of porous foam iron- nickel metal material’s attenuation of gas explosion overpressure on the different parameters was studied experimentally by using self-designed square experimental pipeline which section is 30 cm × 30 cm. The results show that the absorbing ability, strong capability of resisting impact, good effect on the attenuation of shock wave of gas explosion do the porous foam iron-nickel metal material have, attenuation rate is between 12.9% and 73.8%.Aperture, relative density and the thickness are important factors of attenuation performance. Properly reducing aperture and increasing relative density and thickness help to improve attenuation performance of porous foam iron- nickel metal material , well the proportion of material composition has little effect on it.
  • Preparation and Properties of Reflection Infrared Radiant for Core/Shell style ATO/Hollow Glass Microspheres Composites
    ZENG Guo-xun;ZHANG Hai-yan;CHEN Yi-ming;XIONG Xuan
    . 2013, 44(10): 1395-1398.
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    Core-shell structure ATO/hollow glass microspheres composites(HGMs) as heat reflectance materials were prepared by a novel mixing slurry-sintering method. Hollow glass microspheres were mixed with sub-Micro SnO2 and Sb2O3 oxide powder slurry which were prepared by ball milling. After drying and sintering at 530℃, Core-shell ATO/HGMs were obtained. The size distribution of the SnO2 and Sb2O3 oxide powder slurry after ball milling were tested by Laser particle size analyzer；and the structures and morphology of the Core-shell ATO/HGMs were characterized by SEM, XRD. A composite coating was prepared by mixing Core-shell ATO/HGMs with silicone resin(SR). Reflective properties of Core-shell ATO/HGMs- SR composites coatings were investigated by Fourier transform infrared spectrometer in NIR and MIR. The results showed that the content of the oxide particles with size distribution less than 0.6 μm is about 93% ; The thickness of ATO shell on the HGMs was about 600nm, which were synthesized by the reaction of SnO2 and Sb2O3 at 530℃. The reflectance of the Core-shell ATO/HGMs- SR composites coatings are 50%-41% in the infrared wavelength rang of 0.8-2.1 μm, and the absorption are more than 90 % in the infrared wavelength rang of 2.5-16 μm, which indicated that Core-shell ATO/HGMs can be applied as a good cool pigment.
  • Influence of Shrinkage Reducing Admixture on Drying Shrinkage of Concrete with Manufactured-Sand
    GAO Li-xiong;KONG Li-juan
    . 2013, 44(10): 1399-1403.
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    In order to reduce the cracking sensitivity of concrete with manufactured-sand and enhance the application technology, the influence of shrinkage reducing admixture (SRA) in the different using-way on drying shrinkage of concrete with manufactured-sand containing the different stone dust (SD) content were studied by testing drying shrinkage of concrete with manufactured-sand and analyzing the water retention of mortar and microstructure of scanning electron microscope (SEM). The results indicate that for the same concrete specimen with SRA in the different using-way, the mixing with SRA (SRA-M) and coating with SRA (SRA-C) can decrease the drying shrinkage of the specimen, but the reductions of drying shrinkage are different for the different specimens; for the different concrete specimen with SRA in the same using-way, SRA-M is more conducive to reducing drying shrinkage of the concrete with manufactured-sand containing 5% of SD, and however, SRA-C corresponding to the concrete with manufactured-sand containing 10% of SD; SRA can retard the migration seepage of internal free water, and thus improve the water retention to decrease drying shrinkage.
  • Preparation and Properties of Water blown Polyurethane Rigid Foam With Halogen Free Flame Retardance
    WU Deng-hui;ZHAO Pei-hua;WANG Xiao-feng;LIU Ya-qing;LI Tian-kai;LIAO Deng-xiong
    . 2013, 44(10): 1404-1408.
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    A water blown RPUF, the ODP equal to zero, was prepared by the best research technology. The compression strength of the RPUF reached the requirements of GB10800-89. The halogen free flame retardant RPUFs were prepared with SPDPA as flame retardant by the foaming technology and the performance of flame retardant RPUFs with different addition of SPDPA was discussed. SEM shows SPDPA can be evenly dispersed in RPUF matrix, the water resistance test shows the SPDPA can exist in the RPUF matrix stably, the above results confirm there is a favorable compatibility between SPDPA and RPUF. Flame retardant test indicates the LOI of the RPUF-SPDPA(30) is 26.0 and UL-94 V-0 rating can be reached. TGA shows RPUF-SPDPA(30) has a high yield of residual char at high temperatures. The compact charred layers can be seen in the surface of the char by SEM. When the phr of SPDPA is 30, the compression strength of the flame retardant RPUF still reaches the requirement of GB10800-89.
  • Preparation of methotrexate-loaded PLLA microspheres by a high-voltage electrostatic antisolvent process
    CHEN Ai-zheng;YANG Yue-mei;WANG Shi-bin;LIU Yuan-gang;DANG Ting-ting
    . 2013, 44(10): 1409-1413.
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    Using the supercritical CO2 technology-based methotrexate (MTX) nanoparticles as small molecular drug model, the MTX-loaded poly (L-lactide) (PLLA) microspheres were prepared by a high-voltage electrostatic antisolvent process. The resulting MTX-loaded PLLA microspheres were characterized by scanning electronic microscopy (SEM) and Fourier transform infrared spectrophotometry (FTIR), and their drug load, encapsulation efficiency and drug release profiles were also investigated. The results show that the MTX-loaded PLLA microspheres have a smooth surface with a mean size range from 10 μm to 50 μm; Fourier transform-infrared (FTIR) spectra revealed that no alteration of chemical structure occurred during the high-voltage electrostatic antisolvent process, which is favorable for drug carries; with an increase in theoretical drug load (2.5%, 5.0%, and 10.0%), the encapsulation efficiency decreased (18.0%, 7.1%, and 2.3%, respectively); the MTX-loaded PLLA microspheres released the drug with a long sustained-release effect without a burst release.
  • Preparation and Characterization of modified polyacrylonitrile fiber by collagen
    HU Xue-min;XIAO Chang-fa;FENG Yan
    . 2013, 44(10): 1414-1417.
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    With polyacrylonitrile fiber and collagen as the basic raw material, collagen modified polyacrylonitrile fibers with a high moisture regain and durability were prepared by hydrolysis–baking method. The structures and properties of collagen modified polyacrylonitrile fiber were analyzed by means of FTIR、TG、X-Ray、DMA、SEM techniques. Results show that: compared with unmodified fiber, the surface of modified fiber is smooth and covered by a large number of collagen composition, the moisture regain increased from 2% to 6.1%，thermal decomposition temperature decreased from 318℃ to 296℃. The breaking strength and elongation of collagen modified polyacrylonitrile fiber are decreased too.
  • Reactive Force Field Study of the Effect of Subtract Temperature on the ZnO Film Growth Process and Microstructure
    LIU Yong-li;LIU Huan;QI Yang
    . 2013, 44(10): 1418-1421.
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    The understanding of the growth process and formation mechanism of ZnO film on the atomic scale is crucial in adjusting and controlling the film depositing conditions. Using the reaction force field based molecular dynamics method, we theoretically studied the effect of depositing velocity (150, 250 and 350m/s) on the quality of ZnO film with the temperature of 500K, and some results agree with the experimental observation. It is found that, when depositing velocity is 350m/s, the radial distribution function curve of the deposited structure are sharp and highly ordered, and the finally formed thin film possesses the most stable and ordered structure than the other conditions. The film grew with an island mechanism.
  • Morphological Features and Adsorption for Phenol of P(MMA-BA) Hollow Microspheres Prepared by Spray Drying
    HUANG Kai-bing;SHI Min;LI Wei;ZHOU Hong
    . 2013, 44(10): 1422-1427.
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    Hollow poly(methyl methacrylate-butyl acrylate) microspheres with shells of nanoparticles were fabricated by the combination of seed emulsion polymerization and spray drying method. The formation mechanism of the microspheres was analyzed, as well as the influences of prepolymer content、monomer ratio(MMA:BA)、crosslinking agent content on morphological features and specific surface area. The results revealed that hollow microspheres with regular shape were fabricated when the condition as follows：emulsion concentration of 2%, inlet temperature of 125 ° C, outlet temperature of 50 ° C, feed rate of 250ml / h, prepolymer amount of 2 wt%, monomer ratio (MMA: BA) around 7: 3, crosslinking agent amount of 10~20 wt%. In addition, the phenol adsorption properties of hollow microspheres were discussed. The results show that adsorptive capacity in low microspheres concentrations was up to 7.8568mg?g-1. Especially，the adsorptive capacity improved with the increase of monomer ratio and specific surface area.
  • Preparation of HNTs based Thermo-sensitive Composite-microspheres and Their Adsorbability
    CAI Li-feng;LIN Wang;LIN Su-ying;CAI Li-fang;HUNG Xu-xin
    . 2013, 44(10): 1428-1430.
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    Seed emulsion polymerization was carried out to encapsulate halloysite nanotubes (HNTs) with poly(N-isopropylacrylamide) (PNIPAM) to fabricate thermo-sensitive composite-microspheres HNTs/PNIPAM. The structure and morphology of microspheres were characterized by fourier transform infrared spectrometer (FTIR), particle size analyzer and BET specific surface area. Spectrophotometer was employed to investigate adsorption behavior of microspheres using methylene blue (MB) as model organics. It is indicated that the diameter of microspheres is about 1.8μm, and the specific surface area is about 18.2m2/g. The microspheres possess thermo-sensitive characteristics, and the volume phase transition temperature (VPTT) is about 33.6℃. Under the experimental conditions, about 99.4% of methylene blue was absorbed by microspheres. After regeneration under room temperature for 60min, desorption of MB on the adsorbed microspheres achieves equilibrium. Additionally, more MB was released from the microspheres when such regeneration was further carried out under 40℃.
  • Preparation and Magnetic Properties of 6.5%Si Steel Iron Core with Core-Shell Structure
    WU Chao-yang;FAN Xi-an;LI Guang-qiang;GAN Zhang-hua;LU Lei;CAI Xin-zhi
    . 2013, 44(10): 1431-1436.
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    The paper takes preparation 6.5%Si Steel with high induction, low core loss and removing rolling as the starting point, amorphous Fe-Si ribbons was synthesized by melt spinning method, 6.5%Si steel nanopowders with high resietivity core shell structure was prepared by the slight oxidation process and 6.5% Si Steel Iron Core with evaluating internal was sintered by Spark Plasma Sintering process(SPS). The essay focuses studies the effects of different oxidation cladding time on sample density, phase composition, micro structure and static magnetism. It showed that micro structure was best when oxidation cladded 5 hours and sintered at 800℃, the saturated magnetization was 128.84emu/g, coercive force was 28.25Oe and remanent magnetism was 3.47emu/g. The saturated magnetization is equivalent to that silicon steel prepared by DPR, but the coercive force reduced one third.
  • The effect of shale and fly ash on the dehydration property of sewage sludge
    XIE Cong-bo;QIAN Jue-shi;ZHANG Zhi-wei;YUE Yan-fei;YANG Hai-lin
    . 2013, 44(10): 1437-1441.
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    It is beneficial for disposal and utilization to improve the dehydration property of sewage sludge. Aimed at using sewage sludge as building materials, the dehydration property of sludge with adding shale and fly ash in sludge sedimentation process was investigated in this paper. The results indicated that the addition of shale or fly ash could markedly improve dehydration property of sewage sludge. The specific resistance of thickened mixture decreased from 1013 magnitude to 1011. And the moisture content of sludge after settlement and dehydration became low, which was beneficial to the subsequent processing. The volume of sludge after dehydrating was increased, but this increased volume is still acceptable taking into account the utilization of sludge as building materials. The positive effect on dehydration property of sludge with adding both shale and fly ash was better than the one by adding either. And when the dosage of shale and fly ash was respectively 5%, the dehydration property of sludge got best improvement and the volume of dehydrated sludge is not obviously increased.
  • Controlled polymerization and properties of linear heat vulcanizing Polysinglephenylsiloxane
    SHI Dong-lin;SHU Yuan-jie;YU Feng-mei;LU Ai;LUO Shi-kai;DENG Zhi-hua
    . 2013, 44(10): 1442-1446.
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    The high molecular weight ((M_w ) ? > 6.5×105 g/mol) polysinglephenylsiloxane (HP-1) was designed and synthesized in this paper. The molecular structure of HP-1 was characterized by Fourier transform infrared spectrometer (FT-IR), Solid-state nuclear magnetic resonance (29Si SS-NMR) and Liquid nuclear magnetic resonance (1H-NMR). Low temperature thermal property and high temperature rheological properties of HP-1 were studied by Differential scanning calorimetry (DSC) and Rotational rheology (RS). The results showed that the vinyl group and phenyl group content and molecular weight of HP-1 were 0.997 mol%, 9.98mol% and 8.23×105 g/mol, which coincided with the designed values. HP-1 belonged to the class of non-crystalline polymer with glass transition temperature -119.85 ℃, and it possessed excellent stability and elastic under 250 ℃. In addition, HP-1 had outstanding damping property at T ≤ 250 ℃and ω < 7.7 rad/s.
  • Synthesis of Fe3O4 nanoparticles and magnetic properties by chemical reduction
    FENG Hui-xia;CHEN Bai-yi;ZHANG De-yi;LUO He-ming
    . 2013, 44(10): 1447-1450.
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    In this paper, magnetite nano-particals were rapidly prepared using a chemical reduction method. The effects of dispersant type and its dosage, calcining temperature and calcining time were studied by X-ray powder diffraction(XRD). The results present that the conditions to obtain the magnetite nano-particals with a perfect inverse spinel type structure are the dispersant type of PEG(6000), the dispersant dosage of 50g/L, the calcining temperature of 700℃, the calcining time of 120min. The VSM analysis demonstrate that the saturation magnetization of the magnetite nano-particals was 85emu/g, and the samples showed strong paramagnetism due to its coercivity tending to 0.
  • Study on High-temperature phase change composites of NaNO3-LiNO3/expanded graphite by saturated water solution method
    LI Yue-feng;ZHANG Dong
    . 2013, 44(10): 1451-1456.
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    The NaNO3-LiNO3/expanded graphite high-temperature phase change composite were prepared by saturated water solution method, with agitating the suspension in a water bath at a temperature of 90℃ and then drying it in an electric heating drying oven at a temperature of 120℃ over 24 hour. The composites with EG amount of 10%, 20% and 30% were prepared in the similar method. The morphology, phase change temperature and latent heat, thermal conductivity and endothermic and exothermic behavior during thermal cycling of EG composites were characterized by scanning electron microscopy (SEM), differential scanning calorimetry (DSC), Hot Disk thermal constants analyzer and self-designed automatic cycle equipment. The results show that the composites are uniform and well dispersed with the NaNO3-LiNO3 eutectic adsorbed during the graphite laminar, and the thermal storage performance of the eutectic does not weaken with added EG. At increasing graphite amount, the thermal conductivity of the composite is found to progressively increase with intensifications up to 10 but the effective latent heat is found to reduce. The composite with lower graphite amount displays better thermal stability behavior. It is proven that saturated water solution method is a simple and efficient technique for improving the salt thermal conductivity. It is necessary to optimal selection and design between heat storage and thermal conductivity in practical applications.
  • Catalytic performance of Ce–Ni–Mn-O mixed oxide for combustion of benzene
    LI Bing;WANG Zhi-liang;WU Hai-suo;HUANG Qiong;YAN Xiao-kang;CHEN Ying-wen;SHEN Shu-bao
    . 2013, 44(10): 1457-1460.
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    Abstract: A series of Ce-Ni-Mn-O catalyst samples supported on cordierite honeycomb were prepared by the citric acid wet impregnation method with using Ce(NO3)2, Ni(NO3)2 and Mn(NO3)2. The effects of the molar ratio on Ce, Ni and Mn, calcinations temperature and time for the complete oxidation of benzene were investigated. The catalysts were characterized by specific surface area (BET), scanning electron microscope (SEM) and X-ray diffraction techniques (XRD). The results showed that the Ce-Ni-Mn-O complex oxides catalysts with Ce, Ni and Mn molar ratio of 1:0.5:0.5, calcining at 500℃and 7 h exhibited high catalytic performance. With the concentration of benzene of 4.8 g/m3 and the gaseous hourly space velocity of 15000 h-1, the conversion of toluene was 91.8% at the reaction temperature of 300℃．
  • Study on Preparation and Properties of Capric- Myristic Acid/Diatomite Form-stable Phase Change Energy Storage Materials
    FU Lu-jun;DONG FA-qin;HE Ping;YANG Yu-shan
    . 2013, 44(10): 1465-1468.
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    Capric acid-myristic acid eutectic mixture/diatomite form-stable phase change energy (FSPCM) storage materials were prepared by using vacuum impregnation method. Capric acid was mixed with myristic acid to prepare binary fatty acid eutectic, which was selected as energy storage element material and diatomite was selected as supporting material. The structure, microstructure, thermal properties and thermal stability of FSPCM were characterized by infrared spectroscope, scanning electronic microscope, differential scanning calorimeter and thermogravimetric analysis apparatus, respectively. It was shown that the CA-MA was well adsorbed into the porous of diatomite, and they were physical interaction in nature between CA-MA and diatomite. The maximum absorption of CA–MA in the FSPCM was determined as 45 wt. % without melted PCM seepage from the FSPCM when FSPCM change from solid to liquid state. The melting temperature and latent heat of the FSPCM is 22.75 ℃ and 67.03 J/g, respectively. The freezing temperature and latent heat of the FSPCM is 14.52 ℃ and 66.85 J/g, respectively, and FSPCM have a good thermal stability. So the FSPCM was applied to building field.
  • Synthesis the BiFeO3 film on Si substrate by PLD method with SPS-ed target
    HUANG Yan-qin
    . 2013, 44(10): 1469-1471.
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    In order to prepare preferred orientation and high quality BiFeO3 films, the low-cost Si (100) was chose as substrate and bottom electrode. A pure phase BiFeO3 target was prepared by spark plasma sintering (SPS) technique. The preferred orientation and high crystallization BiFeO3 films were prepared by pulsed laser deposition (PLD) method at the substrate temperature was 650 ℃, deposition pressure was 2 Pa O2 pressure, 5 cm target substrate distance and the laser energy was 350 mJ laser energy with 7 Hz laser frequency. A series of BiFeO3 film with different thickness were obtained and the measurement results show that the ferromagnetic and ferroelectric properties of thin films are different with thickness-dependent. It was found that the film with the thickness 300 nm in this experiment is the optimal film.
  • Correlation of the PCDL, PCL and Water-Borne polyurethane specialty paper surface sizing agent performance
    FEI Gui-qiang;ZHU Ke;WANG Hai-hua;LI Jing-yi;LI Qing-long
    . 2013, 44(10): 1472-1475.
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    A series of paper surface sizing agent of waterborne polyurethane which have Different flexible segment were successfully prepared by using polytetrahydrofuran（PTMG1000）and polycaprolactone diols (PCL1000), Fourier transform infared spectrometer (FTIR) , Atomic Force Microscope(AFM) and Thermogravimetr-y Analysis(TGA) were used to characterize the structure of the polymer; PCDL-type facilities glue, PCL-type facilities glue for paper folding endurance and wet strength were systematically studied. The results showed that the emulsions were stable and transparent and the emulsion particle size ranges from 70nm to 100 nm when n(NCO)/n(OH)=1.6, w(DMPA)=9.25%;The atomic force microscope indicated that PCL type surface film more smoothness compared to the PCDL type films ;TG showed that PCDL type films thermal stability better than PCL type films. Compared with the performance after the paper sizing discovered that PCDL type sizing agent have high folding endurance and PCL type sizing agent have high wet strength.
  • The influence of retarders on the hydration process of C3A-gypsum system
    MA Bao-guo;XIAO Jun;XIA Yong-fang;HU Jia-bing
    . 2013, 44(10): 1476-1479.
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    Using a variety of retarders to regulate the hydration process of C3A-CaSO4.2H2O system, and research their mechanism. We use hydration heat, XRD and raman spectroscopy testing the hydration heat rules and hydration process law. The results show that: Sodium tripolyphosphate has the strongest delaying effect, while boric acid is better able to inhibit the hydration heat emission amount for the hydration process of C3A-gypsum system. Sodium tripolyphosphate can inhibit the gypsum dissolving rate, delay the early hydration reaction, and infusibility calcium phosphate salt will adsorb and cover on the surface of C3A and gypsum, while inhibiting its dissolution and hydration; Sodium gluconate can hinder the hydration of C3A through electrostatic adsorption and infusibility calcium salt’s package action, and boric acid can precipitate in surface of C3A through forming a insoluble calcium borate complexes parcel layer.
  • High Thermal Conductivity and Corrosion Resistant SiCx Coating on Mg-3Sn Alloy
    LIU Xia;CHEN Yun-gui;XIAO Su-fen;TANG Yong-bai;DING Wu-cheng;WANG Chun-ming;HE Dai-cheng;TANG Yong-qing
    . 2013, 44(10): 1480-1483.
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    A coating with high thermal conductivity and corrosion resistant is considered of great significance to magnesium alloy especially when they are used as light metal heat sink devices. In this paper, a SiCx film was deposited on Mg-3Sn alloy by magnetron sputtering and its structure and properties of heat conduction as well as corrosion resistance were researched. The results show that the SiCx film deposited on Mg-3Sn alloy is amorphous. In addition, compared with bare Mg-3Sn alloy substrate corroded through salt spray test, the thermal conductivities of coated Mg-3Sn alloy with SiCx film after corrosion are improved by 23 and 16 W/m.K at 25℃and 100℃ respectively. This coated Mg-3Sn alloy shows us good corrosion resistance at the same time.
    • 工艺 ·技术
  • The regulation of graphene oxide on micromorphology of cement hydrate crystals and and its impact on mechanical properties
    LV Sheng-hua;MA Yu-juan;QIU Chao-chao;JU Hao-bo
    . 2013, 44(10): 1487-1492.
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    Graphene oxide (GO) was prepared by Hummers method and its nano-lamellae disperse liquid was obtained by ultrasonic. The dispersing result was characterized by XRD and AFM. Meanwhile, effects of GO with different oxygen content on the micromorphology of cement hydrate crystals and the folding strength and compression strength of the mortar were investigated, respectively. The results indicated that the GO with oxygen content of 18.65% and 25.53% can make the cement hydrate form the flower shape crystals with uniform shape and distribution evenly. The results also showed that the flower shape hydrate crystals have strong toughening and reinforcing effects on mortar. The experiment results suggested that nano-GO lamellae has promotion and template role for cement hydration reaction and can control the shape and size of cement hydrates. The research result has the positive significance consequence to improving of crack resistance and prolonging life of concrete.
  • Facile synthesis of hollow microspheres of LiMn2O4 as high-performance cathodes for Lithium-ion batteries
    WEI Xiu-ge;LI Bao;TANG Hong-wei;GUO Dong-lei;CHANG Zhao-rong
    . 2013, 44(10): 1493-1496.
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    A LiMn2O4 cathode material with hollow microsphere is combination of spinel single crystals, which is successfully synthesized by γ-MnO2 with multilayer core shell structure. The structure and morphology of the sample are characterized by XRD and SEM separately. Furthermore , the electrochemical properties were studied by cyclic voltammetry (CV)、electrochemical impedance spectroscopy (EIS) and galvanostatic charge-discharge measures. The results of SEM indicate that the size of the prepared hollow spherical LiMn2O4 particles is uniform, whose diameter is about 8μm in average and the particles are all made of well-distributed octahedron-like spinel single crystals. The electrochemical test results reveal that the hollow spherical LiMn2O4 possess outstanding high specific capacity 、high rate capability and excellent cycle stability in room temperature when tested at 0.2C and 10C.The initial discharge capacity are up to 145.9mAh/g and 113.3 mAh/g respectively between 3.3V and 4.3V. In addition, the capacity retention both are over 95％ after 60 cycles.
  • Investigation of the doping properties of ZnO:H thin film prepared by RF magnetron sputtering
    CHEN Yi-chuan;HU Yue-hui;CHEN Jun;CHEN Xin-hua;MA De-fu
    . 2013, 44(10): 1497-1501.
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    This paper investigated the properties of ZnO:H thin films. We found that hydrogen played an important role on structural and properties of ZnO:H thin films. With the changing of H doping amount, the effects of H doping manifested as passivating vacancy defects, shallow donor doping and etching action. (1) When the doping concentration R (R=H2/ (H2+Ar)≤0.02) was low, samples grown along the (002) preferential orientation; In this condition, H atoms did mainly play a role of shallow donor doping of passivating oxygen vacancies and substituting zinc ion, so the unit cell volumes became smaller and the crystallinity of ZnO:H thin films increased; In addition, H atoms passivated oxygen vacancies, which made the band tails became narrower, so the optical band gap became wider; We could observe the grains size became bigger and homogeneous distribution on the rough films surface from the SEM figure; Besides, the resistivity of thin film decreased, which was mainly attributed to the electron mobility increased from the crystallinity increasing and the electron concentration increased from the shallow donor doping. (2) When the doping concentration was more than 0.04 (R≥0.04), the (002) peak of XRD quenched, the unit cell volumes became bigger and the quality of crystallization decreased. In the FT-IR spectra, which were observed an absorption band at 3400-3900 cm-1. It exhibited to the typical O-H bonding local vibrational modes (LVM) absorption band. Owing to the charges unbalance was caused by polar molecular clusters (hydroxy), which produced oxygen vacancies and increased the electron concentration, and result in the decreasing of the film resistivity in the high doping concentration. In this condition, the optical band gap became narrower, which caused by the H etching action.
  • One-Pot hydrothermal Synthesis of N-(S,F) codoped Titanium Nanotubes and Its Visible Light Responsive Photocatalytic Properties
    WANG Jian-ye;ZHAO Zhi-huan;FAN Ji-min;ZHU li-xiao
    . 2013, 44(10): 1502-1506.
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    Different non-metal co-doped titanium dioxide nanotubes (TiO2NT) were preformed by one-pot hydrothermal synthesis with urea, thiourea and ammonium fluoride as dopant source respectively. The samples were characterized by SEM, TEM, XRD, BET, FT-IR, UV-Vis and DRS. The photo-catalytic activity under visible light was evaluated by photocatalytic degradation of methyl orange. The adsorption performance of catalyst to methyl orange was studied, and the relationship between nitrogen doping behavior and visible light photo-catalytic property was investigated by the experiment of degradation of methyl orange waste water. The results showed that nanotubular titania prepared by hydrothermal processing using different non- metal elements as dopant in the strong alkaline solution had larger surface area (193.93 m2/g) and lower band gap energy (2.76eV) than that of TiO2, and nonmetal- doping can activate its visible-light activity. Photo-catalytic degradation of methyl orange tests showed that the thiourea doped titania nanotubes (N,S-TiO2NT) under the visible light had the best degradation rate, methyl orange degraded by 81.5% with illumination of 90 min. The reaction followed a first-order kinetics equation.
  • Effect of dealuminted NaY zeolite carrier on the encapsulation of phospho-tungstic acid
    GUI Qin-zhang;LIU Bi-yu;YUAN Xia;WU Jian
    . 2013, 44(10): 1507-1510.
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    NaY zeolite was modified by dealumination using the hydrotherm treatment and SiCl4 gas phase method, respectively. The dealuminted NaY zeolite was used as carrier for the in-situ encapsulation of phospho-tungstic acid. The structure of dealuminated NaY zeolite was characterized by the means of XRD diffraction, N2 physical adsorption, ICP-AES and SEM. The results showed that when Si/Al ratio was up to 5.5, the dealuminated zeolite by the hydrotherm treatment had the higher crystallinity, larger surface areas and pore volume, higher ratio of micropore than the sample modified by SiCl4 gas phase method. In the process of encapsulation of phospho-tungstic acid, the amount of encapsulation was up to 0.0569gPW/g dealuminted NaY carrier by the hydrotherm treatment, which was much higher than that using the dealuminated zeolite by the SiCl4 gas phase method as carrier.
  • Preparation and the particle size study of polyurethane microcapsules containing photochromophores
    FAN Fei;WANG Chao-xia
    . 2013, 44(10): 1511-1514.
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    Polyurethane was used as wall material. Azo dyes were dispersed in butyl acetate as core materials. The photochromic compound microcapsules coated by polyurethane were prepared via in-situ polymerization. The influences of emulsifier type and its dosage, core/wall ratio, homogenization speed, stirring speed and synthesis temperature on the particle size of the microcapsules were investigated. The experimental results showed that Peregal O emulsifier was more suitable for the preparation of polyurethane microcapsules than Tween80, OP-10 and PVC, the average particle size of microcapsules decreased from 0.6171um to 0.5236um as the Peregal O concentration increased from 5% to 15%. With the reduction of the core/wall weight ratio in the range from 1:1 to 1:8, the average particle size improved from o.4731um to o.7147um.The average particle size of the microcapsules was inverse to the speeds while homogenization speed and stirring speed increased.20～60℃ prepolymerization temperature and 90-100℃ chain extension temperature were appropriate for polymerization and average particle size of microcapsules.
  • First-principles study on electronic structure and optical properties of TiNx
    HUANG Tao;ZHOU Bai-yang;ZHANG Wei;WU Bo
    . 2013, 44(10): 1515-1519.
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    Abstract：The electronic structure and optical properties of TiNx system in different N content (X = 0, 0.5, 0.6 and 1) corresponding to the TiNx super cell structure were calculated by the first principle method. The calculation results showed that: TiNx were typically metal properties,but this properties of TiNx were weakened according to the increase of the content of N. The dielectric function and reflectivity function of TiNx (X = 0, 0.5, 0.6 and 1) crystal were accurately calculated. The calculation results coincided with the existing theory well,which offered theoretical data for TiNx materials in molecular atomic scale design and application in further .
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