30 April 2014, Volume 45 Issue 08
    

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    综述 进展
  • ;Xiao-Jie CHENG;
    . 2014, 45(08): 1-0.
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    Chitosan based thermosensitive hydrogel is a type of intelligent gel that is nonchemical-crosslinked, whose structures are closely correlated with specific ingredients. Its mild preparation, desirable bioactivity and biocompatibility make it broadly applied in tissue engineering and drug controlled release. Notably, its applications as fluid embolizing agent and cell culture matrix for ready harvest have attracted numerous attentions recently. This review intends to summarize its categorization, gelling behavior, mode of gelation and novel applications.
  • 研究 开发
  • yun wangJun-Feng WU;;
    . 2014, 45(08): 2-0.
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    Bipolar plate is one key component of proton exchange membrane fuel cell (PEMFC), and it is also an important factor which affects cost performance of battery stack. It is difficult to form flow channel of bipolar plate under the micro scale. This paper puts forward the method of accumulative, and set up the corresponding experimental apparatus, selecting aluminum alloy 3003 sheet metal with the size of 11 mm×11 mm×0.6 mm as bipolar plate, and conducting heat treatment on sheet metal under room temperature and 260 ℃, 360 ℃, 450 ℃ four different temperatures, then we can complete straight flow channel by forming device. The paper studies the impact of different heat treatment temperatures on forming force, forming depth and the resilient rate. Results show that we can consider the influence factors of forming force and flow channel forming depth, and adopting sheet metal after the process of completely annealing in the later forming, it can improve the forming performance and forming accuracy.
  • ;Jin Wang
    . 2014, 45(08): 3-0.
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    Abstract: The dexamethasone-loaded poly(lactic-co-glycolic acid) (PLGA) was prepared by casting method. The result of Fourier transform infrared spectroscopy (FTIR) indicated that the dexamethasone-loaded film had the peaks of PLGA and dexamethasone, which proved that the chemical stability of dexamethasone loaded in PLGA. The water contact angle test directly showed the hydrophilicity of the drug loaded film was improved compared with PLGA film. The results of in vitro drug release behavior indicated that the dexamethasone existed burst release within1 day, but it had linear release characteristics after 6 days. In vitro biological evaluation showed that the drug loaded film can not only inhibit the adhesion and activation of platelets, but also significantly prohibit the adhesion of smooth muscle cells. Finally, dexamethasone eluting stent were prepared using ultrasonic atomization spray method. The stent coating was smooth, uniform and integrated. After stent expansion, there were still no cracks.
  • Yu Xie
    . 2014, 45(08): 4-0.
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    4,7-dibromo-n-octylcarbazole(M1) and 1,5-bis(tri-n-butyltin)-4, 8-di(n-dodecylalkoxy) benzo [1,2-b:4,5-b']dithiophene(M2) were synthesized from carbazole and 3-thenoic acid. The conjugated polymer(P1) was synthesized via Suzuki coupling reaction by M1 and M2. And the polymer P1 were used to characterize the structure and properties by a series of tests. The results have showed that the the optical band gap of P1 is 1.56eV, the electrochemical band gap of P1 is 1.57eV, and 5% weight loss temperature is 314 ℃. The polymer P1 shows the good optical properties, thermal stability and electrochemical oxidation of reduction performance.
  • Ting-Ting Tan;;;
    . 2014, 45(08): 5-0.
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    The micro-structure of three kinds of high-strength and middle-modulus carbon fiber including two homemade carbon fibers and Toray carbon fibers T800H, were characterized by using scanning electron microscope, X-ray diffractometer, transmission electron microscope and small angle X-ray scattering system. Their surface structure, fracture morphology, graphic micro-crystal structure and micro-pore size were compared. The results indicant that the surface structure of two homemade carbon fibers is better than T800H. But other micro-structure of the homemade high-strength and middle-modulus carbon fibers have some differences with the Toray carbon fiber. The preparation technology of the homemade carbon fiber need further improved.
  • . 2014, 45(08): 6-0.
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    Well-crystalline graphite was ground by roller vibration milling for different milling time, and the samples were examined by XRD, Raman scattering, SEM and BET. The result indicated that the grain size of graphite declined as milling time increasing, and a great many of defects were induced with the destruction of the structure of the pristine well-crystalline graphite. High graphitization degree of graphite nanosheets were expected after milling for 10h. This provided a new method of preparation of nanographite with high graphitization degree.
  • Bao-Ying QIAO
    . 2014, 45(08): 7-0.
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    Composite film was prepared by amorphous Fe73Si18B9 powder, 300 mesh, as sensitive phase and silicone rubber as matrix phase. The content of powder of film is 25wt%, 75wt% and83.3wt% and thickness is 200μm.The data of Impedance-Z were collected by TH2816LCR digital bridge while the data of stress-σ were collected by LYYL-500N high-grade type microcomputer control pressure testing machine when frequency was 1kHz and speeds of the continuous loading/unloading stress were 0.05mm/min, 0.1mm/min and 0.5mm/min. The force-sensitive properties of the film were studied when stress loading and unloading was continuous in different speed and the force-sensitive properties were compared between FeCuNbSiB powder/silicone rubber composite film and FeSiB powder/silicone rubber composite film. The results show that when speed of continuous loading and unloading is less than 0.1mm/min in the stress range from 0.03 to 1.0MPa, composite film has excellent force-sensitive stability and sensitivity. When stress is no more than 0.2MPa, the film is more sensitive. With the content of the powder increasing, the variable trend of the force-sensitive properties is alike while the value of sensitivity-k is up. When stress is from 0.03 MPa to 0.2 MPa , the value of SI% of film with the 83.3wt% powder content is from 36.51% up to82.48%, the value of sensitivity-k is from 42.91 down to1.889. When stress is from 0.2 MPa to 0.7 MPa , the value of k of film with the 83.3wt% powder content is between 1.889 and 0.6.As the stress reaches 1MPa , the value of k gradually approaches to 0 .
  • Xiao-Gang YOU;;Jia-Yang Li ;Su-Xia GUO
    . 2014, 45(08): 8-0.
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    Study on the effect of porous silicon gettering by electron beam injection was conducted. Preparation of porous silicon was carried out by electrochemical etching in both electrobath. The morphology of porous silicon changed after electron beam injection. Through 3 min gettering treatment, the resistivity changed significantly and greater than the resistivity of the silicon wafers from rapid heat treatment under the same condition, which fully improves that electron beam injection play a dual role of thermal effects and electrical effects, and electron beam injection have a certain effect on the removal of impurities. The time of the electron beam injection shows certain effect on the removal effectiveness of boron.
  • Xue-Feng LICheng Jiang;
    . 2014, 45(08): 9-0.
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  • 综述 进展
  • Bo-Yu ZHENG
    . 2014, 45(08): 10-0.
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    Abstract:Many characteristics of the microscale materials could result in change of thermal diffusivity, which could characterize these parameters in turn. For example, thermal diffusivity could change with the irradiation dose which has a direct effect on positron annihilation lifetime, thermal diffusivity could also change considerably at some metal's phase transition point. Besides, elemental composition, grain size and film thickness have been studied as a function of thermal diffusivity as well . Accordingly, in this paper, characterization methods for microscale properties based on thermal diffusivity have been summarized, theory of each method has been used to analyze and application prospects have been indicated which are expected to provide new ways and methods for microscale property test.
  • ;
    . 2014, 45(08): 11-0.
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    Abstract: Graphene is a single atomic layer thickness of graphite material, with good electrical, mechanical and thermal properties. When it was used as the electrode materials for lithium ion batteries, could effectively improve the various electrochemical performance, and it had a good application prospect. This paper summarized the preparation method of anode material of metallic oxide based graphene in the lithium ion battery, and different composite structure between graphene nanosheets and metal oxide, the structure had strong synergistic effect in improving the electrochemical performance of anode material of metallic oxide based graphene.
  • 研究 开发
  • ;;ZHAO Jian-Hao ;;
    . 2014, 45(08): 12-0.
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    A new liquid crystal material, octanoylated/acryloylated hydroxypropyl cellulose (OPPC), was synthesized by the combination of octanoylation and acryloylation on hydroxypropyl cellulose (HPC) and then followed by grafting heparin on the substrate surface via Michael addition. Fourier transform infrared spectrum analysis confirmed the successful grafting of heparin that was quantified to be 9.42 μg/cm2 by Toluidine blue method. A cholesteric liquid crystal texture was observed for heparinized OPPC films at room temperature by polarizing optical microscopy. The heparinization on the surface could improve the hydrophilicity of OPPC film. The hemolysis rate and platelet adhesion experiments proved that heparin-functionalized OPPC liquid crystal film had excellent blood compatibility.
  • ;;;;;TANG YONGJIAN
    . 2014, 45(08): 13-0.
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    Pd-doped MF aerogels is prepared by radiation method in 500kGy radiation dose, which has been confirmed by XRD, SEM and TEM. SEM and TEM images show that not only a great number of Pd particles presented in the network of MF but also some agglomerated particles of Pd presented on the surface of MF. Nitrogen adsorption data analysis shows that the specific surface area, total pore volume, micropore volume and mesopore volume of MF aerogels decreased after Pd doping. The decrease of mesopore volume was more than micropore volume, which means most of Pd particles filled the mesopore of MF aerogels.
  • . 2014, 45(08): 14-0.
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    The corrosion kinetics of NZ2 and NZ8 alloys were investigated by static autoclave test in 400℃/10.3MPa steam; The matrix microstructures of the two alloys were tested by TEM and neutron diffraction method. The crystal structure of oxide films of NZ2 and NZ8 alloys after corroded was investigated by XRD and Raman spectra methods in this paper. The results of corrosion kinetics indicated that the corrosion resistance of NZ2 alloy in 400℃/10.3MPa steam was better than that of NZ8 alloy; TEM studies on the matrixes showed that the precipitates of NZ2 were Zr(Fe,Cr)2 and Zr(Fe,Cr,Nb)2, and Nb content in the matrix was less than solid solution limit. However, the precipitates of NZ8 were Zr-Fe-Nb, and Nb was supersaturated in the matrix. The neutron diffraction result confirmed that the Zr(Fe,Cr)2 precipitates of NZ2 matrix were C14 structure. A great deal of Zr-Fe-Nb precipitates and the supersaturated Nb content in NZ8 matrix increased the local volume expansion and accelerated the crack formation, which resulted in the higher corrosion rate of NZ8. Moreover, the less than solid solution Nb content in the matrix and Zr(Fe,Cr)2, Zr(Fe,Cr,Nb)2 precipitates improved the corrosion resistance of NZ2 alloy.
  • Chang-Gai FAN; ;;Faqin Dong
    . 2014, 45(08): 15-0.
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    In this paper, numerical simulations are performed to study the solubility, diffusion, permeability of gas molecules in Fluorine substituent polymers (Parylene AF4 and Parylene AF8). A model of the molecular chain for Parylene AF4 and Parylene AF8 polymer with 300 repeat units was established and structural optimized with energy minimization and annealing based on the condensed-phase optimized molecular potentials for atomistic simulation studies (COMPASS) force field in Material Studio (MS) software of Accelrys. The free volume and its distributions in the polymeric model indicated that the Parylene AF4 and Parylene AF8 has small free volume, it is not easy to form the available channel for gas molecules permeation. The diffusion, solubility and permeability coefficients of some gaseous molecules in the model were also calculated based on the combined methods of Molecular Dynamics (MD) with Great Canonical Monte Carlo methods (GCMC). In contrast with the results of previous research on Parylene C, the simulated data showed that Parylene AF4 and Parylene AF8 have better barrier for the larger size molecules (such as H2O, H2S, SO2, Cl2, etc.). The trajectories of penetrant molecules diffusing in the model demonstrated that the molecules transferred or moved in polymer with a “hopping diffusion” behavior.
  • 工艺 技术
  • . 2014, 45(08): 16-0.
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    A kind of novel MCC/PPy composite hydrogel has been prepared using the cross-linking network of microcrystalline cellulose (MCC) as the matrix of the hydrogel, which is dissolved in ionic liquid (chloride-1-butyl-3-methylimidazolium, BMIMCl) and cross-linked by N,N-methylene-bis-arcylamide, and pyrrole (Py) as the monomer of conductive polymer. The chemical structure and morphology of the MCC/PPy composite hydrogel were characterized by FTIR and SEM, meanwhile, the conductivity, swelling ratio and thermal stability were studied. Results showed that the MCC/PPy composite hydrogel was semi-IPN conductive hydrogel with honeycomb-like structure. Conductivity of the composite hydrogel was between 10-4-10-3 S/cm, and doping of TsONa increased the conductivity significantly. The equilibrium swelling ratio (ESR) decreased with higher MCC content for both pure MCC hyrogel and the composite hydrogel; and ESR of the composite hydrogel could maintain at the level of 500% which was lower than that of the pure MCC hydrogel. Besides, the thermal stability of the composite hydrogel was reduced than the pure MCC hydrogel.
  • Lun-Wei ZHOU
    . 2014, 45(08): 17-0.
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    Abstract: In this paper, two kinds of flower-like Co3O4 hollow microspheres were synthesized by solvothermal process. The scanning electron microscopy(SEM), X-ray diffraction(XRD), Nitrogen adsorption instrument, UV-visible diffuse reflectance spectroscopy (UV-Vis), Infrared spectrometer(FTIR) were used to characterize the size, crystal structure, pore properties of the Co3O4 hollow microspheres. The results showed that the two kinds of Co3O4 microspheres are micron-sized, cubic phase spinel structure, and the specific surface area were 26.77 m2/g and 2.51 m2/g, respectively. The adsorption and regeneration properties of the two kinds of Co3O4 microspheres to basic fuchsin were compared. The study results showed that the two kinds of Co3O4 microspheres exhibited high adsorption capacities and excellent regeneration ability to basic fuchsin. The adsorption efficiency was increased with the specific surface area of the microspheres.
  • ;;;
    . 2014, 45(08): 18-0.
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    In-situ Al-Cr/Al composite was prepared by the ultrasonic vibration aided casting method in this paper. Microstructure was characterized by XRD,SEM and EDS. The wear resistance of composites was investigated by M-2000 wear tester. The results show that the ultrasonic vibration significantly refines the Al-Cr intermetallic compound reinforcement. With the increase of Cr, the content and size of Al-Cr intermetallic compound reinforcement increase. The Al-Cr hybrid intermetallic compound reinforcement exists in the matrix at the same time. With increase of the Cr powder particle size, the wear resistance of in-situ Al-Cr/Al composite and in situ reinforcement size both have minimum value. When the content of Cr is 8%, the particle size is 75μm, the fine Al-Cr intermetallic compound reinforcement distributes in the composites evenly; meanwhile, the wear rate is minimum, which is 0.294%. The wear resistance of composites is 8.5 times that of pure aluminum. The wear mechanism is mainly abrasive wear.
  • ; ;;;;
    . 2014, 45(08): 19-0.
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    During the indirect selective laser sintering of stainless steel parts, the precision of forming parts will be reduced. Due to the temperature gradient field, greater residual stress and warpage will be produced. To improve the sintering quality of stainless steel parts, the paper presented numerical analysis on coupled thermal stress field of 316L sintering. Then the results were compared with experiments. These results demonstrated the simulation was consistent with the physical deformation trend of sintering experiments. It verifies the correctness of the simulation. Using the simulation program and orthogonal test method, four process parameters (laser power, scan spacing, scan speed and preheating temperature) are optimized. A group of optimum process parameters is obtained. These results provide a powerful criterion to get good process parameters of SLS with important economic value and promising application.
  • Jian Bing Jiang; ;;
    . 2014, 45(08): 21-0.
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    LiMn2O4 has been successful synthesized by the mechanical-activation-oxidation method from high purity manganese powder and Li2CO3. The crystal structure, morphology and electrochemical performance of LiMn2O4 have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), charge-discharge test and AC impedance. The results show that the LiMn2O4 has spinel structure and exhibits uniform particle size distribution. The initial discharge capacities of the LiMn2O4 are as high as 125.8 mAh/g at 0.1C and 120.1 mAh/g at 1C in the voltage range of 3.0?4.4 V at 25℃, especially, the discharge capacity retains 103.9 mA?h/g at 1C after 500 cycles. Besides, the as-prepared LiMn2O4 presents good high temperature performance and smaller electrochemical impedance.
  • ;; ;; Wei Li
    . 2014, 45(08): 22-0.
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    , Cd1-xZnxTe crystalline thin films were deposited by magnetron co-sputtering with ZnTe and CdTe targets at different temperature, pressure and sputtering power. The properties of films were characterized by SEM, XRD and XRF to investigate the structure, composition and surface morphology. The optical and electrical properties of the films were also investigated. The results show that the films prepared at 300℃ were cubic phase with a dense surface and an average particle size of about 50nm. A linear relationship was obtained between Zn composition and lattice constant as well as Zn composition and the band gap of the film. With the decrease of the pressure from 8Pa to 1Pa the grain size increased and a denser surface was shown. The as-deposited Cd1-xZnxTe polycrystalline films show weak p-type conduction with the conductivity of about 8.61×10-11(Ω.cm)-1 at room temperature.
  • ;
    . 2014, 45(08): 23-0.
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    Ni-SiC nanocomposite coatings were prepared on A3 steel by ultrasonic-electrodeposition method. The microstructures of Ni-SiC nanocomposite coatings were investigated using CA model. The results illuminate that there is Ni and SiC phase in Ni-SiC nanocomposite coatings. And the coating has a compact and fine microstructure with increasing of the ultrasonic power. It is found that Nickel grains in NC-1, NC-2 and NC-3 coatings are 188.2, 135.7 and 70.5 nm, respectively. And that of SiC particles is 105.4, 80.9 and 36.2 nm, respectively. CA model shows that there is little difference between the predicted and measured results, and the maximum relative error is 5.0%.
  • ;
    . 2014, 45(08): 24-0.
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    Abstract: Graphene oxides was first prepared by hummers method, and then reduced using dextran as green reducing agent to produce graphene. Graphehen modified glassy carbon electrode combined with differential pulse stripping voltammetry to establish a trace cadmium detection method. The prepared graphene was characterized and studied by UV spectrophotometer, Fourier transform infrared spectroscopy, atomic force microscopy and X-ray photoelectron spectroscopy, and the electrical conductivity and electrochemical properties were also studied with cyclic voltammetry and AC impedance spectroscopy. The results showed dextran posses good reducing capacity which could successfully reduce graphene oxides to produce graphene with good conductivity, simultaneously, dextran can also be embedded into graphite inter-layers to increase the inter-layer spaces to achieve good dispersion of graphene in aqueous solution. At pH = 6 acetic acid - sodium acetate buffer solution, Cd2+ ion exhibit a sensitive stripping peak at -0.87V, and the linear calibration curve ranged from 0.5~120 ppb with the detection limit of 0.15ppb. The method uses non-toxic, environmentally friendly dextran can quickly prepare well dispersed graphene with excellent electrochemical characteristics, which can be used for rapid detection of trace amounts of cadmium.
  • Ji-Guo ZHANG;;;Sheng-Ming ZHANG;
    . 2014, 45(08): 25-0.
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    In this paper the sorbent of Lignin-polyethyleneimine (Lignin-PEI) was successfully synthesized by means of crosslinking Lignin and polyethyleneimine (PEI) by glutaraldehyde. We characterized Lignin-PEI by SEM, XRD, FT-IR and XPS, then investigated the use of Lignin-PEI for the removal of Cu2+ from water. These results indicated that the nitrogen content of prepared Lignin-PEI was 10.61 wt% at Lignin, PEI and GA reaction ratio m (g): V (mL): V (mL) of 2:5:20, at 25 ℃ for 2 hr. We found sorption isotherms for Lignin-PEI better fitted Langmuir equation. Sorption of Cu2+ ion on Lignin-PEI followed pseudo second-order kinetics. The maximum sorption capacity was 54.15 mg?g-1 for Cu2+ ion.
  • ;Qing LI ;;
    . 2014, 45(08): 26-0.
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    Abstract:Trepang-like PbWO4 microcrystals have been prepared by an aqueous solution method at room temperature with Pb(NO3)2 and Pb(NO3)2 as raw materials and β-CD as surfactant. The products were characterized by powder X-ray diffraction (XRD), energy-dispersive X-ray spectrometry (EDX), scanning electron microscopy (SEM). The effects of reaction conditions have also been investigated, which showed that the reaction temperature, pH and the concentration of surfactant have great influence to the morphology of products. A three-step formation mechanism was proposed. Besides, the photocatalytic performance of the products were studied which exhibited good photocatalytic effect toward rhodamine.
  • 研究 开发
  • . 2014, 45(08): 28-0.
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    Study on the surface morphology, chemical structure, degree of crystallinity and thermal properties of the para-aramid fibrid by SEM, AFM, FT-IR, XRD and TGA. Lay the experimental foundation for the study of para-aramid fibrid structural performance, and it is beneficial to its extensive use of composite reinforced materials. And the results show that para-aramid fibrid is non-granular and size is small, its shape like as fiber or film, surface is roughness, shape is supple. fiber has a secondary amide structure. the crystallinity of fiber is 28.55 percent, more amorphous composition and grain size smaller. The initial decomposition temperature of fiber is 490℃, TG10% is 550 ℃, its molecular chain structure is stability,and thermal properties excellent.
  • ;
    . 2014, 45(08): 29-0.
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    The key performance of modified epoxy resin prepared from epoxy resin (4,4'-diamino diphenyl methane), silicon carbide, diatomite and curing agent (4,4'-diamino diphenyl sulfone ) was researched. Besides viscosity, gel time of resin and mechanical properties of casting body was tested. Experiment showed that the viscosity of the modified resin was higher than the original one, and the gel time was much less. And with the addition of packing the mechanical properties of the modified resin enhanced firstly then decreased.
  • ;
    . 2014, 45(08): 30-0.
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    The surface of diatomite particles was modified using titanate coupling agent and the activation mechanism was discussed, the composite materials were fabricated with methyl vinyl silicone rubber and diatomite. The diatomite surface and fracture of composite materials were charactered by SEM. The compression properties of simple silicone rubber and composite materials were researched. The results showed that the average activation grade of diatomite particles modified was 98%, the maximum compression deformation springback of composite materials was obtained while the content of diatomite was up to 30%.
  • . 2014, 45(08): 31-0.
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    Based on the quasi-static compressive test of close-cell aluminum foam, mechanical properties and energy absorption under different porosities were investigated and deformation mechanism was analyzed. Results show that the quasi-static compressive process of closed-cell aluminum foam was characterized by three deformation stages: linear elastic stage, plastic platform stage and densification stage. Yield strength、Young's modulus and compaction stress of closed-cell aluminum foam are both decreased with the increase of porosity. Energy absorption efficiency and ideal energy absorption efficiency are both increased and then decreased in the compressive process. Porosity has great impact on the absorption efficiency, while for maximum ideal energy absorption efficiency has little effect. Combine ideal energy absorption efficiency curves with energy absorption efficiency curve can select the appropriate cushioning material, bring to bear the best energy absorption properties of aluminum foam. Close-cell aluminum foam has good plastic deformation capacity under quasi-static compression. Deformation has characteristics that poles were destroyed layer by layer.