30 September 2015, Volume 46 Issue 18

    

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工艺 技术
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  functional assembly and medicines performance of cucurbiturils with Zinc tetraphenylporphyrin

  Yang Qin ;;;Ying JIANG

  . 2015, 46(18): 1-0.

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  Abstract: The functional assembly between Q[7]、Q[8] with Zinc tetraphenylporphyrin (ZnTPP) were investigated by ultraviolet-visible absorption spectrum, infrared spectrum and scanning electron microscopy. The results show that the assembly rate is about 1:1 respectively between Q [7,8] and ZnTPP; When pH value of solution is in the range of 5.0-11.0, assembly is more stable; The thermodynamic data shows that assembly process is spontaneous, exothermic, and giving?priority to entropy driven; Fluorescence?quantum of?assembly?is not significantly decreased when compared with ZnTPP; The solubility of ZnTPP have been improved extremely as a result of assembled with?Q [7, 8].
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  Magnetic Spectum Properties of NiCuZn Ferrites Appliied for NFC

  shuoqing yan;;;;;;

  . 2015, 46(18): 2-0.

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  The influence of the Fe2O3 content in the formula, grain size and the Co2O3 addition quantity on the magnetic spectra of NiCuZn ferrite materials for the NFC applications was investigated. Micrographs of the sintered samples were obtained by using scanning electron microscope, the magnetic spectra were measured by Agilent E4991A impedance analyzer. By using the theory of critical size of grain, magnetic spectral component and combining with the microstructure of the samples, the magnetic spectra had been carried on the detailed study. The difference between the magnetic spectra had been analyzed. The results show that when the Fe2O3 content in the formula of is closer to 50% and the grains are single-domain, the material is favor to the attainment of better performance. When the grains are single-domain, Co2O3 apply little contribution to improving the resonance frequency, but it can reduce the gap between the resonance frequency and cutoff frequency in application, and also improve the performance of materials.
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  Fabrication and photoelectrochemical performance of large diameter anodic TiO2 nanotube

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  . 2015, 46(18): 3-0.

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  Anodic TiO2 nanotubes have been studied for decades, and the preparation of TiO2 nanotubes with small diameter (100-200 nm) have been reported for many times, however, the fabrication of TiO2 nanotubes with large diameter is still a challenge. In order to fabricate TiO2 nanotube with large diameter, the influence of water content contained in electrolyte on the diameter of TiO2 nanotubes has been investigated in detail. The results show that nanotube diameter increases significantly with the increase of water content (from 8 vol% to 12 vol%) . However, when the water content increases to 13 vol%, the well-defined nanotubular structure cannot be obtained by anodization. Further increasing the water content to 20 vol%, the compact titanium oxide film can be obtained. Besides, the investigation of voltage affect on the diameter of TiO2 nanotube was carried out in ethylene glycol electrolyte containing 0.3 wt% NH4F and 12 vol% H2O. The results indicate that the largest diameter (~600nm) can be obtained at a voltage of 170 V, which has never been reported in the literature. The photoelectrochemical (PEC) water splitting measurements of the TiO2 nanotube fabricated at different voltages show that the increase of the nanotubes’ diameter is beneficial to their PEC water splitting performance.
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  Pyrolytic Kinetics Analysis of Boron Modified Phenol-formaldehyde Resin

  Hai-yun JIANGJigang Wang;Shen-qing Wu;;Zhong Liang HU

  . 2015, 46(18): 4-0.

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  Boron carbide and phenol-formaldehyde resin were mixed together at some mass ratio. Being cured at 200℃, a composite B4C- PF was obtained. Non-isothermal pyrolysis kinetics of B4C-PF was investigated using thermogravimetric analysis (ТGA) at controlled heating rates. The research indicates that the pyrolysis process consists of two stages. In the first stage, the diffusion rate of B4C is the main factor deciding the velocity of pyrolysis process whose the most probable mechanism function g(α) is 1–(1–α)1/4. In the second one, the most probable mechanism function g(α) is (1–α)-2–1, which means the main factor deciding the velocity of pyrolysis process is the reactivity of B4C and other reactants. At the same time, the diffusion rate of B4C has some influence on the pyrolysis process but not the key one.
研究 开发
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  Research on the Performance and Microstructure of Asphalt under Salt Freezing Cycle

  Ji-Wei HAN ; ;

  . 2015, 46(18): 5-0.

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  The three routine indicators for the matrix asphalt, SBS modified asphalt and rubber powder modified asphalt were tested before and after the salt freezing. The influence factors that would change the high and low temperature performance of the asphalt were analyzed through range analysis method and grey relation entropy method, and the scanning electron microscope (SEM) was used to observe the microstructure of the three kinds of asphalt before and after the salt freezing. The analysis results showed that freezing temperature, concentration of salt solution, freezing and thawing cycles would affect the temperature sensitivity, reduce the high and low temperature performance and change the microstructure of the asphalt greatly. But the study also indicated that the performance of the asphalt itself is more important than others especially for penetration value of asphalt. So how to select suitable asphalt for road in the cold region should be strictly controlled.
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  Study on the crystal structure refinement and magnetic properties of Al doped NdFeO3 system

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  . 2015, 46(18): 6-0.

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  Al doped orthoferrites NdFe1-xAlxO3 is synthesized by solid state reaction. X-ray powder diffraction and the Rietveld refinement results show a decrease in the lattice parameters as Al doping content x increasing. Higher Al doping level leads to significant change on Fe-O bond length as well as Fe-O-Fe bond angle in the unit cell, and such change shows different behaviors in the directions of a, b and c axis. Magnetic properties of the sample are significantly affected by the structure change of the sample, which is caused by Al doping. Magnetic measurement results indicate that weak ferromagnetic ordering resulted from Dzyaloshinsky-Moriya (D-M) interaction is reduced with the increasing Al doping content and the phase transition temperature of spin reorientation interaction owing to the interaction between Nd ion and Fe ions moves to lower temperature with higher Al doping level. Furthermore, magnetization of the sample is decreased along with the increasing Al-doping content, indicating that the canted antiferromagnetic structure is evidently modulated by the nonmagnetic Al-doping in Fe site.
工艺 技术
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  Study on the process and properties of LDHs films prepared by in situ electrochemical anodic oxidation

  . 2015, 46(18): 7-0.

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  Ni/Al-NO3-LDHs film was prepared by in-situ electrochemical anodic oxidation of aluminium oxide template to provide Al3+ in the NH4NO3 solution. sulfosalicylic acid /LDHs composite films were prepared by introducing sulfosalicylic acid anions into the Ni/Al-NO3-LDHs layers with ion exchange method in weak acid conditions. The process conditions were optimized. The structure and morphology of the film were characterized by XRD, FT-IR and SEM. The results showed that sulfosalicylic acid anions were successfully intercalated into LDHs layers with the layer spacing increased from 0.883nm to 1.153nm. The characteristic peak of NO3- ion at 1384 cm-1 disappeared while a new peak for sulfosalicylic acid anion appeared. SEM images showed that LDHs film grown vertically on Ni substrate. Electrochemical corrosion and UV-Vis analysis showed that LDHs film had good corrosion resistance and excellent UV blocking properties.
研究 开发
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  Inference of SCR catalyst microstructure and De-NOx property over different amount of cerium doped

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  . 2015, 46(18): 8-0.

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  This paper discussed a recent study of NOx removal by novel Ce doped low vanadium SCR catalysts with TiO2 as support under a bench scale condition. The catalysts were characterized by brunauer-emmett-teller ( BET) ，X-ray diffraction ( XRD) ，scanning electron microscope ( SEM) ，FT-Raman ，comparison with the traditional catalyst. The result shows that，BET surface areas and porous volume didn’t have a significant influence on catalytic performance .The amount of doped cerium didn’t affect the structure characteristics of the carrier. When the CeO2 loaded exceeds 5%，cubic crystalline structure of CeO2 exists in the catalyst surface and trace Ce2(WO4)3 is formed. The NOx conversion is up to 95% in the activity temperature range with 1% cerium doped at the gas hourly space velocity of 125，000 h-1，n( NH3) /n( NO) =1．
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  Study on the Activated Carbon Preparation and Pyrolysis Process of Sugarcane Leaves

  MENG Mian-Wu ;;;;

  . 2015, 46(18): 9-0.

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  The pyrolysis reactions of sugarcane leaves activated by NH4H2PO4 were carried out using the thermo-gravimetric analyzer to analysis the pyrolysis mechanism, the influencing factors on the yield and adsorption capacity of the activated carbon such as activator concentration, the ratio of activator solution to sugarcane leaves, soaking time, activating temperature and time were systematically investigated, and the microstructure of samples was characterized by means of scanning electron microscope(SEM). The results show that the activation mechanism of sugarcane leaves is as follow: 4C+2NH4H2PO4→P2O3+CH4↑+CO2↑+2CO↑+ 2NH3↑+H2O↑. The iodine adsorption value of the samples would increase with prolong the activation time, and increase first and then decrease with the increase of activator concentration, the ratio of activator solution to sugarcane leaves, soaking time or activation temperature. The suitable preparation conditions is as follows: sugarcane leaves is infused 20h in 2.5 wt% ammonium dihydrogen phosphate with the ratio of activator solution to sugarcane leaves 5:1, and treated 60 min at 700℃, the sugarcane leaves-based activated carbon has abundant porous microstructures, and the yield and iodine adsorption value of the specimen were 29.33 % and 987.69 mg/g, respectively.
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  Effects of steam explosion pretreatment on rice straw particleboard

  Peng LuoChuanmin Yang;

  . 2015, 46(18): 10-0.

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  Rice straw, whose outer surface is covered with smooth, water-repellent wax layer, has a high contentof silica. Conventional urea formaldehyde (UF) cannot be used to make rice straw particleboard. This study adopted steam explosion to pretreat rice straw with temperature being 160 and 170 ℃ and residence time being 2, 4, 6 min, respectively. Rice straw particleboards were made from steam exploded rice straw with UF. The results showed the steam explosion effectively got rid of the silica and wax layer on the outer surface of rice straw as well as lowered the pH value of rice straw. As intensity of pretreatment increased, the physical and mechanical properties of panel increased. Particleboards made from rice straw pretreated under 160 ℃/6 min, 170 ℃/4 min and 170 ℃/6 min met the strength requirement of GB/T 4897-2003.
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  Performance analysis of pH values/ salt concentration double sensitivity SPM hydrogel microspheres

  ;Ji-juan Guo;;;

  . 2015, 46(18): 12-0.

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  Intelligent hydrogel is a kind of crosslinked polymer which can response to external stimuli such as temperature, pH values, light, electricity and ionic strength. These p sensitive gel ball can be used in the biological medicine, environmental protection and other fields.The authors mainly studied the swelling and deswelling performance of SPM hydrogel microspheres made from sodium alginate(SA), polyvinyl alcohol (PVA) and montmorillonite(MMT). The sensitivity to the pH values, salinity and temperature was also tested. The experimental results show that the SA concentration was positively correlated with swelling performance while MMT had the negatively effect. The content of carbonyl groups and other groups in alkane chains reduced and the possible chemical reaction can occur. These gel balls are sensitive to alkaline environment and high salt concentration, but not sensitive to temperature.
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  A study on low-temperature growth of AZO thin films by atomic layer deposition

  Jia-Heng FENG

  . 2015, 46(18): 13-0.

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  Al-doped zinc oxide (AZO) films were prepared on quartz glass substrates by atomic layer deposition at 150℃with improved Al-doped model. The growth rate was illustrated by spectroscopic ellipsometer. And surface morphology, crystal structure, films composition and electric properties were characterized by atomic force microscopy, X-ray diffraction, Raman spectroscopy, X-ray photoelectron spectroscopy and Hall measurement, respectively. The results showed that all of AZO films with hexagonal wurtzite structure were continuous and homogeneous on the substrate surface. The intensity of ZnO (002) crystal plane diffraction peak reduced with increasing Al atom doping content. Al is substituted for Zn in lattice position uniformly distributes and disperses in ZnO crystal structure by the mode of Al-O coalition, the O vacancies exist in the crystal . The lowest resistivity of 4.61×10-4Ω?cm were obtained in AZO films when Al and Zn circulating ratio is 1:19.
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  CHARACTERISTIC RESEARCH ON SIMULATIVE WALLBOARD OF PHASE CHANGE AND HUMIDITY STORAGE UNDER NATURAL VENTILATION

  . 2015, 46(18): 14-0.

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  With building gypsum as basis material, double-shell phase change micro-nano capsules mixed with gypsum-based, preparation of phase change and humidity storage wallboard, and use it build simulation room in order to acquire inner wall temperature and relative humidity change under natural ventilation, analysis of regulating temperature and humidity effects of wallboard to indoor environment. The results show phase change and humidity storage wallboard has good phase change performance and efficient humidity storage performance, as building envelope parts, it can remarkably reduce the fluctuation range of the indoor temperature and relative humidity, improve the indoor thermal environmental quality, enhance the indoor comfort and reach the aim of energy-efficient building.
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  3Y-TZP ceramics simulation of the fluorescence properties of natural teeth by doping Eu2+

  Lian-Shui SHI;;;;;

  . 2015, 46(18): 15-0.

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  Eu2+-doped 3Y-TZP dental bioceramic was prepared by immersing the presintering 3Y-TZP in Eu(NO3)3 solution, followed with calcination under reducing atmosphere. The surface microstructure, phase constitution, fluorescence spectrum and cytotoxicity were analyzed by X-ray diffraction (XRD), scanning electron microscope (SEM), fluorescence spectrometer and MTT test. The results showed that Eu2+-doped 3Y-TZP presented a densification morphology and the average grain size was 450nm. There were no other crystal structure other than t-ZrO2 was found. The emission spectrum excited by 365 nm showed a characteristic blue broad band with the peak at about 470nm, which corresponded to 4f65d1→4f7(8S7/2) transition of Eu2+. This emission spectrum was similar to the natural tooth which can be used to simulation of the fluorescence emission of natural teeth. The cytotoxicity grade of Eu2+-doped 3Y-TZP was I, which can be used for clinical with biological safety.
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  Investigation of technologyand mechanism of removing ash from Camellia oleifera shell charcoal material

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  . 2015, 46(18): 16-0.

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  Using Camellia oleifera shell as raw material, technology and mechanism of removing ash from camellia oleifera shell charcoal were explored by the method of hydrochloric acid washing. The results shoewd that the ash content gradually increased with an increase in carbonized temperature and a decrease in acid washing time, however,after acid washing for more than 2h, ash content was not significantly changed. In the process of removing ash from Camellia oleifera shell charcoal using hydrochloric acid washing, de-ashing reaction mainly occurred on the surface of charcoal and effective pore expanding was not be formed. Pore structure of all charcoal was not well-developed in the experiment range of carbonization temperature, hydrochloric acid washing could significantly reduce the ash content but hardly benefit the formation of new pore structure. After Camellia oleifera shell charcoal were activated by steam, acid washing could decrease ash content and also increase about 20% pore volume without changing the pole size by removing inorganic substances blocking porous channel。
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  Research on rapid analysis method of the foreshortening property of vascular stents

  . 2015, 46(18): 17-0.

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  Based on the finite element analysis, experimental design and metamodeling techniques, this paper presents a fast analysis method of stent mechanical properties. Response surface methodology (RSM) and radial basis function artificial neural network (RBFANN) was selected respectively to construct an analysis model of stent foreshortening. The results showed that the RSM and RBFANN model established herein were able to quickly analysis the stent axial shortening rate and their root mean square error were 1.0974 and 0.2789, respectively. Compared to RSM model, RBFANN model had higher analysis accuracy. Therefore, the fast analysis method of stent mechanical properties presented in this paper is feasible and reliable, greatly improving the efficiency of analysis of stent mechanical properties.
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  One-dimensional CdTe nanorod arrays preparation by the magnetron sputtering method

  BIng-Wei LUOYuan Deng;;

  . 2015, 46(18): 18-0.

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  The different microstructures of CdTe thin films are prepared by magnetron sputtering method through changing the substrate temperature, working pressure and sputtering power. The XRD and SEM results show that the abilities of growth and surface diffusion of CdTe particles are directly determined by the substrate temperature. Meanwhile, the working pressure can affect the energy of incident CdTe particles and the quantities of the CdTe particles are determined by the sputtering power. Finally, the uniform one-dimensional CdTe nanorod arrays with diameter about 150 nm are achieved at sputtering power of 84 W, working pressure of 0.4 Pa and the temperature of quartz substrate within 200-450 ℃.
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  Preparation and photocatalysis property of sulfur doped TiO2 hollow spheres

  jiang xueliang

  . 2015, 46(18): 19-0.

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  Sulfur-doped titanium dioxide (S-TiO2) hollow spheres were prepared by the reaction of tetrabutyl titanate and thiourea as the main raw material with polystyrene-hydroxyethyl acrylate copolymer (P (St-HEA)) microspheres templates. The morphology, crystal type and state of elemental sulfur doping of S-TiO2 hollow spheres was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). Study the catalytic properties of S-TiO2 hollow spheres using methanal solution simulated wastewater. The results showed that TiO2 hollow spheres were obtained by removing P (St-HEA) microspheres template successfully, the particle size and morphology of TiO2 hollow spheres are little effected by sulfur-doping, the crystallite dimension of TiO2 hollow spheres diminished and the crystal shape of TiO2 hollow spheres was changed from pure anatase into anatase/rutile. Sulphur was present in the form of S4+ which substitutes Ti4+ in the titania lattice, forming Ti1-xSxO2 solid solution.The performance of photocatalysis of doped sample was superior to the pure TiO2 hollow spheres, while they both preceded TiO2 powder. The catalytic efficiency of synthesized photocatalyst is 60% for degrading methanal under UV-light..
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  Effect of SiCp electroless plating on the microstructure and thermal properties of SiCp/Al composites

  Duosheng Li

  . 2015, 46(18): 20-0.

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  Abstract: To improve the interface of between SiC particles and Al matrix, under alkaline condition, the surface of SiC particles was plated with Cu using electroless plating, and then the SiCp/Al composites were prepared by pressureless infiltration technology. Surface and interface morphology, microstructure and phase of SiC particle and SiCp/Al composites were analyzed by X-ray diffraction, 3D stereo video microscope and scanning electron microscope respectively. The surface element of SiC particles coating and composites was analyzed by EDS, meantime, thermal conductivity of SiCp/Al composites was measured by the laser flash method. The results show that, compared with a single KNaC4H4O6?4H20 complexant, double complexants (KNaC4H4O6?4H20 + EDTA-2Na) can more effectively plate a dense, no oxidation and good combined interface Cu coating on the surface of SiCp. The interface thickness of Cu is approximatively 2.5-3μm. AlCu2 phase was detected in the interface, however Al4C3 brittle phase was not found. The thermal conductivity of SiCp/Al composites is 181W/m-1?k-1 at 20 ℃. It is much higher than that (102W/m-1?k-1) of SiCp/Al composites without surface modification of SiCp.
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  Study on Preparation and Microwave Absorbing Properties of Carbon nanotubes/PANI composites

  wang peng

  . 2015, 46(18): 21-0.

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  Abstract：Carbon nanotubes/PANI composites were prepared by the in-situ polymerization. The morphology, constitution and thermal stability of the products were characterized by TEM,FT-IR and TGA respectively. The electromagnetism parameters of the composites were investigated by Vector Network Analyzer. On the basis of the parameters, the influence of polymerization time, polymerization temperature, acid concentration and coating thickness on the microwave absorbing properties were evaluated. Results show that the core-shell structure composites are obtained. When the polymerization time is 6h, the polymerization temperature is 20℃ and the acid concentration is 0.05mol/L respectively, the samples have good microwave absorbing properties in the frequency range from 8 to18 GHz.
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  Effects of ethylene segments with different adding time and different adding amount on the properties of polyurethane-acrylate microemulsions and films

  ; ;WANG Yong Chao

  . 2015, 46(18): 22-0.

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  A series of Polyurethane-acrylate microemulsion (PUA) with different adding time and different adding amount of ethylene segments was prepared through in-situ polymerization, using isophorone diisocyanate (IPDI), polycaprolactone diols(PCL1000), methyl methacrylate(MMA), butyl acrylate(BA), 2,2-dimethylolbutyric acid(DMBA) and 2-Hydroxyethyl Methacrylate(HEMA) as raw materials. Effects of the ethylene segments with different adding time and different adding amount on rheology study of polyurethane prepolymer and properties of polyurethane-acrylate microemulsion and films were systematically studied, as well as the scattering intensity of the dispersion under different reaction times. The hybrid emulsion was characterized by FTIR and NMR. It was found that the dispersion particle displayed as core/shell spherical morphology. At the same time, the particle size of PUA microemulsion increased from 62.96 nm to78.86 nm by TEM, submicron particle size analyzer and water absorption of PUA coating film decreased from 12.19% to 8.22%, while the coagulation ratio decreased from 4.21% to 0.11% and the viscosity also decreased，presenting non-Newtonian flow behavior as increasing the amount of pre-added ethylene segments. The emulsion polymerization process of PUA was studied by dynamic light scattering method.
综述 进展
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  Advances in biocompatibility of mesoporous silica nanoparticles

  Ji-Sheng GU;Xiao-Bing Cai

  . 2015, 46(18): 23-0.

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  Because of the good Physical and chemical properties of mesoporous silica nanoparticles (MSNs), MSNs Have broad prospect of application in disease diagnosis and treatment, but before it can be successfully applied in the human body，the biocompatibility of it must be improved. The cytotoxicity of MSNs is related to the way and quantity it can be uptaken into the cells.Those depend on the cell type and character of the MSNs. By improvement of Physical and chemical methods, the biocompatibility of mesoporous silica nanoparticles can be obviously improved,and its hemolysis can be reduced too.MSNs distribute mainly in the liver,spleen,lungs,kidney, intestines,stomach, muscle and heart. The toxicity depend on the concentration.As a foreign matter, a certain extent hypersensitivity can be induced when the MSNs enter into the body (in vivo), MSNs exhibit good biocompatibility in vitro and in vivo, but the way to be adopted needs further study.
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  Research Progress of Nano Materials Applied in Luminol Chemiluminescent Analysis

  Kai-En XU;

  . 2015, 46(18): 24-0.

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  The theory of chemiluminescence（CL）has been increasingly mature, but the popularization and application of CL technology are still limited by low luminous efficiency, poor selectivity, extreme conditions. Because nano materials have the features of quantum size effect, large specific surface area and high surface energy, chemical activity and biocompatibility are well performed. Nano materials can be used as catalysts, nanosized reaction platforms, ion markers, energy acceptors. in CL analysis. In this review, we report the recent progress of luminol CL system with nano materials involved, combined with some modern separation and immunoassay technology.
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  A review on prediction and mechanism of rubber fatigue research

  . 2015, 46(18): 25-0.

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  A literature review on rubber fatigue research is presented from two aspects: fatigue life prediction and the mechanism of rubber fatigue. Mathematical models include crack nucleation approaches, crack growth approaches and artificial neural network approach. While mechanism of the rubber fatigue focus on the effect of inclusion and fatigue life enhancement of the strain crystallizing rubbers. Finally, a prospect of remained problems is presented at the end of the paper.
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  Structural Characteristics and Functional Modification Methods of Natural Organic Fiber Oil Sorbents: an overview*

  ;;Zheng-Jun LI

  . 2015, 46(18): 26-0.

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  Natural organic fibers, a renewable biomass resource, possess biological degradability and a certain amount of oil absorption capacity, have gained widely attention as oil sorption materials in recent years. In this context, we firstly outline the development trends and oil absorption mechanism of organic oil sorbents. Subsequently, a detailed elaboration on the structural characteristics and functional modification techniques of natural organic fibers are made. This review attests that utilizing natural organic fiber as a substrate, a novel environmental friendly oil sorbent material with excellent oil absorption properties and controllable degradability could be acquired by establishing a super-hydrophobic-oleophilic surface through hydrophobic modification and surface roughness fabrication, building an appropriate porous structure and introducing new degradation patterns, such as photodegradation and thermal degradation. Particularly, the prospects and challenges of the potential application of protein fiber (especially for collagen fiber) as oil sorbents are briefly addressed.