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Progress in the Periodic Mesoporous Organosilicas
YANG Qi-Hua,LIU Jian,ZHONG Hua,WANG Pei-Yuan
2009 Vol. 24 (4): 641649
Abstract(
4149 )
PDF(2848KB)(
2575
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The integration of organic and inorganic fragments within the pore wall of the periodic mesoporous organosilicas (PMOs) represents one of the recent breakthroughs in the fields of material science. The organic moieties distributed uniformly in the mesoporous framework will not block the pore, which is beneficial to the diffusion of guest molecule. The surface hydrophilicity/hydrophobicity, mechanical and hydrothermal stability of the PMOs could be easily tuned. The unique features of the PMOs make them attractive in many applications. The recent progresses in the synthesis, characterization and application of the PMOs are summarized, with special emphasis on their applications in catalysis, adsorption, separation, and photoelectricity. The future development of the PMOs is also prospected.
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Point Defects and Applications of Chemical Sensors Ceramics
ZHOU Zhi-Gang,TANG Zi-Long
2009 Vol. 24 (4): 650660
Abstract(
4001 )
PDF(1970KB)(
2201
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Chemical sensors, an important green sensor, in view of the relation of the structure-sensitive and the physico-chemistry interaction with the surrounding environment for the point defects on the change of chemical surrounding in redox, additive and optical-electro-color fields are the key of the new applications and new developments in this paper. The knowledge of how the point defects influence the ceramics/device performance was revealed and provides very useful tools for understanding their basic characteristics and to open up their potentiality of the new applications in the near future.
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Visible-light Photocataltic Activity of Cr-doped TiO2 Nanoparticles Synthesized by Flame Spray Pyrolysis
TIAN Bao-Zhu,LI Chun-Zhong,GU Feng,JIANG Hai-Bo,HU Yan-Jie
2009 Vol. 24 (4): 661665
Abstract(
3277 )
PDF(1592KB)(
1905
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Cr-doped TiO2 nanoparticles were synthesized by one-step flame spray pyrolysis technique. The effects of Cr3+ doping on the microstructure, light absorption property, and photocatalytic activity of the samples were investigated. It is found that increasing Cr3+ concentration restrains the formation of anatase and simultaneously favors the formation of rutile. At low concentration (≤1%), Cr is mainly incorporated into the crystal lattice of TiO2 in the form of Cr3+, while high Cr concentration promotes the formation of Cr2O3 clusters. The result of photocatalytic degradation of 2,4-dichlorophenol demonstrates that appropriate Cr3+ doping can evidently enhance the visible-light photocatalytic activity of TiO2. The optimal Cr3+ concentration to obtain the highest photocatalytic activity is 1at%. The improvement of visible-light photocatalytic activity derived from Cr doping is mainly related to the enhancement of visible light absorption, appropriate crystalline composition, and improved transfer efficiency of photogenerated electrons and holes.
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Preparation and Photocatalytic Hydrogen Production of NiO(CoO)/N-SrTiO3 Heterojunction Complex Catalyst under Simulated Sunlight Irradiation
YAN Jian-Hui,ZHANG Li,ZHU Yi-Rong,TANG You-Gen,YANG Hai-Hua
2009 Vol. 24 (4): 666670
Abstract(
3068 )
PDF(1810KB)(
2224
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Nitrogen doped SrTiO3 was prepared by solid phase method, and NiO(CoO)/N-SrTiO3 heterojunction complex catalysts with different NiO or CoO loading contents were further obtained via impregnation-hydrogen reduction method. The as-obtained photocatalysts were characterized by XRD, SEM, UV-Vis DRS and Fluorescence spectrum techniques. The photocatalytic hydrogen generation activity and the variation laws under simulated sunlight irradiation were investigated. The effect of different treatment methods of loading NiO on hydrogen generation activity of nitrogen doped SrTiO3 was also studied. The results demonstrate that the photocatalytic activity of the oxides loaded complex catalyst treated by hydrogen reduction firstly and then oxidation is higher than that of the oxides loaded complex catalyst treated by direct oxidation. Comparing with the single catalysts, the asprepared NiO/N-SrTiO3, CoO/N-SrTiO3 complex photocatalysts exhibit higher photocatalytic hydrogen generation activity under simulated sunlight irradiation. The optimal photocatalytic activity of hydrogen production is achieved when the loaded mass percentage is 1.0wt%, 0.5wt% respectively and the amount of hydrogen within 6h is 4.2, 4.9 times more than that of unloaded samples. The reason is that the heterojunction structure formed at the interface of two phases can act as the convenient unilateralism channel for the transfer of photogenerated electrons and holes in the process of photocatalytic reaction after loading the metal oxides, leading to the effective separation of photogenerated carriers, so as to enhance the photocatalytic activity of catalysts.
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Synthesis and Photocatalytic Activity of Vanadium Doped Titania Hollow Microspheres
JIA Jin-Yi,LIU Jing-Bing,ZHANG Wen-Xiong,CHANG Lin,JING Qi
2009 Vol. 24 (4): 671674
Abstract(
3287 )
PDF(1265KB)(
2227
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Vanadium doped titania hollow microspheres were successfully prepared using polystyrene latex particles as template and using organmetallic Ti (Ⅳ) as precursor. The resulting samples were characterized by FT-IR,SEM,TEM, XRD and UV-Vis DRS. The results show that the morphology of titania hollow microspheres do not exhibit remarkable change when adding low concentration of vanadium. The wall thickness of these hollow microspheres is in the range from 20nm to 30nm. The vanadium promotes the phase transformation of TiO2 hollow microsphere from anatase to rutile phase. With increasing concentration of vanadium, the adsorption edge of as-prepared titania hollow microspheres show stronger absorbance of light with longer wavelength. The moderately vanadium doped titania hollow microspheres(1.0%)exhibit better photocatalytic activity for the decomposition of methyl orange in aqueous solution.
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Preparation of Anatase TiO2 Nanorods Sol by the Hydrothermal Treatment of Peroxotitanium Acid
LI Shuang,ZHANG Qing-Hong,LI Yao-Gang,WANG Hong-Zhi
2009 Vol. 24 (4): 675679
Abstract(
3796 )
PDF(2588KB)(
2367
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Transparent anatase titanium dioxide sol was prepared by the hydrothermal treatment of the peroxotitanium acid (PTA) as precursor, PTA was synthesized by the reaction of hydrogen peroxide with the wellwashed wet titania precipitates. The TiO2 nanoparticles were characterized by XRD, UV-Vis, PL, FT-Raman and TEM. It is confirmed the nanoparticles are shuttlelike and in the anatase phase with average diameter less than 10nm, most of which grow along the c-axis. The TiO2 sol shows a band-gap emission at the wavelength of 368nm. Prolonging the hydrothermal time makes TiO2 nanoparticles align and form the longer nanorods with aspect ratio more than 10 via the oriented attachment mechanism. Moreover, more stronger emission is observed in the sol prepared for a prolonged hydrothermal duration due to the formation of more longer nanorods.
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Photoelectrocatalytic Degradation of Methylene Blue by TiO2 Nanotube Array Prepared by Anodic Oxidation
CHEN Yi,SHI Li-Yi,YUAN Shuai,WU Jun,ZHANG Mei-Hong,FANG Jian-Hui
2009 Vol. 24 (4): 680684
Abstract(
3091 )
PDF(2218KB)(
1924
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TiO2 nanotube array material was prepared by anodic oxidation of a pure titanium sheet. The average length and the diameter of the nanotubes were 1.8μm and 80-90nm respectively. After calcination at 400℃ for 2h, the amorphous nanotube walls converted to anatase phase without distortion and collapse. The TiO2 nanotube array material was used as photocatalyst to degrade methylene blue solution under UV light irradiation and UV lightelectric field respectively. The synergetic effects of UV light and electric field on the degradation of methylene blue were investigated by changing the voltage from 0V to +3V. The highest synergetic efficiency of 124% is obtained under +1.4V. The degradation activity of the TiO2 nanotube array material used for several times decreases little, which reveals that the TiO2 nanotube array is adhered to the metal substrate stably.
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Preparation of TiO2 Aerogels by Ambient Pressure Drying
HU Jiu-Gang,CHEN Qi-Yuan,LI Jie,LU Bin,LI Peng-Ju
2009 Vol. 24 (4): 685689
Abstract(
2931 )
PDF(2281KB)(
2014
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TiO2 aerogels were prepared by sol-gel method at ambient pressure using tetrabutyl titanate as raw material, formamide as drying control chemical additive, tetralthyl orthosilcate(TEOS)/ethanol as pore fluids extractant. The structural properties of aerogel samples were characterized by means of XRD, BET, TEM, SEM, EDS and FT-IR, etc. Experimental results show that asprepared TiO2 aerogel is in amorphous state with the apparent density of 0.375g/cm3, the specific surface area of 523m2/g and the average pore size of about 9.9nm. After calcinated at 850℃ in air for 4h, the sampletransforms from amorphous state to anatasetype crystal, while its’ pore volume shrinks and average pore size increases to 16.3nm, the specific surface area reduces to 208m2/g. TiO2 aerogel prepared by the above method presents excellent thermal stability and high specific surface area.
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Synthesis and Structure of Carbon/Silica Hybrid Aerogels
CHEN Liang,ZHANG Rui,LONG Dong-Hui,LING Li-Cheng
2009 Vol. 24 (4): 690694
Abstract(
2959 )
PDF(3112KB)(
1827
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Hybrid hydrogels were synthesized by sol-gel polymerization of resorcinol and formaldehyde added by colloidal silica solutions. Carbon/silica hybrid aerogels were prepared from the hydrogels by supercritical drying and carbonization. Carbon aerogels and silica aerogels were obtained by removing silica with HF etching and carbon with air burning from the hybrid aerogels respectively. Carbon xerogels were prepared by ambient drying, carbonization and HF etching from the hydrogels. The microstructures of the four kinds of gels were characterized by TEM and N2 adsorption. It is found that the carbon and silica frameworks are continuous and interpenetrated each other. The silica framework can improve the strength of hybrid gels, which can decrease the volume shrinkages by preventing collapse of the hybrid framework during supercritical drying and carbonization, resulting in carbon aerogels with high specific surface area of 934m2/g and large total pore volume of 3.9cm3/g.
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Characterization and Antibacterial Ability of Copper-Modified Hexagonal Mesoporous Silica in situ
CHEN Jun-Hua,WANG Fei,CHENG Nian-Shou,DING Zhi-Jie,FU Zhai-Hui,YIN Dong-Hong
2009 Vol. 24 (4): 695701
Abstract(
3290 )
PDF(2502KB)(
1781
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Coppermodified hexagonal mesoporous silica (Cu-HMS) was in situ prepared with sol-gel method. The structure and the performance of Cu-HMS were characterized by XRD, TG-DTA, ESR, UV-Vis, FT-IR, ESEM, EDS and N2 adsorptiondesorption isotherms. Based on bacteriostasis experiments of E. coil, S. aureus, B. subtilis and G. bacillus, the antibacterial ability of the sample was also investigated. The results show that the particles of Cu-HMS look like regular thallus, the specific surface area is 533m2/g, the average pore size is 3.6nm, and the copper ions are presented in framework of the sample, especially. The sample has favorable mesoporous structure, thermal stability and ultraviolet-visible-light absorption ability. Furthermore, The bacteriostasis experimental results show that Cu-HMS has favourable and steady antibacterial ability. When the dosage of Cu-HMS is 20mg/L, the bacteriostasis ability may be visibly detected in 12h, while the dosage is up to 200mg/L, E. coil, S. aureus and B. subtilis may be killed after 24h.
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Immobilization of Papain on Siliceous Mesocellular Foam
ZOU Ze-Chang,WEI Qi,NA Wei,SUN Hui,NIE Zuo-Ren
2009 Vol. 24 (4): 702706
Abstract(
2750 )
PDF(1998KB)(
1641
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Siliceous mesocellular foam (MCF) was employed as carriers in the immobilization of papain, and the properties and the stabilities of the immobilized enzyme were investigated in detail. The results show that the amount of papain immobilized on MCF material reaches 334 mg/g MCF. The optimal pH and reaction temperature of the immobilized papain are 7.5 and 50℃, respectively. The Michaelis constant (Km) of immobilized papain is disclosed as 6.99×10-3mol/L by the Lineweaver-Burk plot at 37℃. The immobilized papain with 65.1% of the activity remaines after repeating the catalysis of casein for 8 times. After stored at 4℃ for 60d, the immobilized papain retaines 75% of the activity, while the free papain only retains 53.6%.The pH, thermal, operational, storage stabilities of the immobilized enzyme are improved due to the large pore microenvironment and the shield of the mesopores of MCF, which can be considered as excellent supports for papain immobilization.
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Surface Modification of Amorphous Calcium Phosphates by Stearic Acid and Their Stability
LI Yan-Bao,LI Huai-Dong,CHENG Xin,LIU Wen-Hao,LI Dong-Xu,XU Zhong-Zi
2009 Vol. 24 (4): 707711
Abstract(
3477 )
PDF(1727KB)(
1832
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The precipitated amorphous calcium phosphates (ACP) were modified by stearic acid (SA) at about 78℃ for different times, using ethanol as reaction medium in a reflux setup. Modification effects of SA were investigated by activation ratio, contact angle, FTIR and TGA/DTA. The stability of the ACP powders before and after modification was examined by FTIR, XRD and TGA/DTA. The results show that the optimal adding amount of SA is 5 wt%, there are about 4 wt% SA on the surface of the ACP powders, and SA reacts with ACP to form -COOCa and HPO42- groups which leads to a hydrophobic coating form on the ACP surface containing the long alkyl chain of SA. The ethanol mediated reflux method does not induce phase conversion of ACP at about 78℃ for 24h, and the modified ACP powders are still amorphous even after stored in air at room temperature for more than one year. It is proposed that SA existing on the surface of the ACP powders has higher ability to retard conversion of ACP into its crystalline polymorphous than β-CD due to the strong steric hindrance of the long alkyl chain of SA.
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Sintering and Phase Transition of 0.25CuO-0.75MoO3 Doped ZnO-TiO2 Microwave Dielectric Ceramics
LIU Zhong-Chi,ZHOU Dong-Xiang,GONG Shu-Ping,HU Yun-Xiang
2009 Vol. 24 (4): 712716
Abstract(
2925 )
PDF(2469KB)(
1934
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The effects of 0.25CuO-0.75MoO3 (in mole ratio, abbreviated to CM) addition on the sintering behavior, phase transition and microwave dielectric properties of ZnO-TiO2 (ZT) ceramics were investigated. CM-doped ZT ceramics were prepared by conventional solid-state reaction method and sintered at temperatures ranging from 900℃ to 1050℃. The micrographs, elemental composition, phase structures and microwave dielectric properties of the samples prepared were characterized or measured by field-emission scanning electron microscopy (FE-SEM) equipped with an energy dispersive spectroscopy (EDS), X-ray diffraction (XRD) and a network analyzer, respectively. It is demonstrated that both Cu2+ and Mo6+ are introduced into the lattice of the main phase which lower the decomposition temperature of ZnTiO3 and the onset temperature at which Zn2TiO4 and rutile could form solid solution (Zn2Ti3O8). Meanwhile, it is confirmed that, the doping of CM can effectively enhance the densification of ZT ceramics at relatively low sintering temperatures. The ZT ceramic sample with 4wt% CM addition sintered at 975℃ for 4h reaches a density value of 94% theoretical density, and exhibited microwave dielectric properties as follows: dielectric constant εr=28.6, quality factor Qf=12150GHz and temperature coefficient of resonant frequency τf=+17.8×10-6/℃.
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Preparation of Superior Magnetic SrFe12O19 Microtubules with Template Method
LI Qiao-Ling,ZHANG Cun-Rui,JING Hong-Xia
2009 Vol. 24 (4): 717720
Abstract(
2810 )
PDF(2425KB)(
1606
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The strontium ferrite microtubules were prepared by the solgel method using the absorbent cotton as template and calcined at different temperatures.And the hexagonal nano-SrFe12O19 was prepared by prime sol-gel method. The phase, morphology and particle diameter of samples were studied by XRD, SEM and TEM. The magnetic properties of samples were tested by VSM. It is found that the strontium ferrite microtubules are obtained through the absorbent cotton template. The microtubules is fabricated with the external diameter of 8μm to 13μm and the wall thickness of 1μm to 2μm. The coercive force and magnetization of the strontium ferrite microtubules are improved by 30%, 20%, respectively. The coercive force, the specific saturation magnetization and residual magnetization of the microtubules are 547.2kA/m, 70.1A·m2/kg and 42.4A·m2/kg, respectively. The formation mechanism of the microtubules are dicussed.
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Preparation and Characterization of M-type Strontium Ferrite Hollow Fibers
SONG Fu-Zhan,LIU Jin-Yong,MENG Xian-Feng,SHEN Xiang-Qian,XIANG Jun
2009 Vol. 24 (4): 721726
Abstract(
3117 )
PDF(2626KB)(
1673
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The Mtype strontium ferrite (SrFe12O19) hollow fibers were prepared by the organic gel-precursor transformation method using citric acid and metal salts as raw materials. The gel-precursors and the as-prepared fibers were characterized by FTIR, XRD, TG/DSC, SEM and VSM. The results show that the gel spinnability is related with the chemical composition and pH value. The gel exhibits an appropriate spinning performance when the molar ratio of citric acid to the total metal ions is 1.5∶1.0 and the pH value is around 4.2. The M-type strontium ferrite hollow fibers obtained are characterized with high aspect ratio, thin diameters and ratio of the hollow diameter to the fiber diameter being about 1/2.The fibers calcined at 1100℃ are composed of SrFe12O19 nanoparticles with hexagonal plate morphology and average particle size of about several hundred nanometers. At room temperature, the saturation magnetization and coercivity of the M-type strontium ferrite hollow fibers calcined at 1100℃ are 53.5A·m2/kg and 386.96kA/m, respectively. These M-type strontium ferrite hollow fibers possess a shape anisotropy characteristic and the coercivity for the aligned hollow fibers parallel and parpendicular to the applied field is correspondingly 391.66kA/m and 358.72kA/m.
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Study on the Synthesis and Properties of Superparamagnetic Monodisperse Fe3O4 Nanoparticles
JIANG Wen,WEN Xian-Tao,WANG Wei,WU Yao,GU Zhong-Wei
2009 Vol. 24 (4): 727731
Abstract(
3308 )
PDF(2154KB)(
2188
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There are extensive applications for superparamagnetic Fe3O4 nanoparticles in the field of biomaterials. Superparamagnetic magnetite nanoparticles coated with oleic acid were prepared in the refluxing mixed system of water, ethanol alcohol and toluene at 74℃. The effect of the OH- concentration on the surface properties, size, dispersion and magnetic properties of magnetite nanoparticles was studied systematically. The properties of magnetite nanoparticles were tested by X-ray diffraction (XRD), fourier transform infrared (FTIR), dynamic light scattering (DLS), transmission electron microscopy (TEM) and vibrating sample magnetometer (VSM). The results show that when the molar ratio of NaOH to Fe(Ⅱ) is less than 8, magnetite nanoparticles coated with oleic acid can be dispersed easily in nonpolar solvents. The addition of NaOH has no obvious influence on the size and the saturation magnetization of magnetite nanoparticles. While the molar ratio of NaOH to Fe(Ⅱ) is more than 8, magnetite nanoparticles can only be dispersed in polar solvents, such as water. Although the saturation magnetization increases to 40A·m2/kg, magnetite nanoparticles are polydisperse and easy to agglomerate in water.
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Microwave Absorbing Property and Modification of Ferrite-encapsulated Cenosphere Powders
ZHANG Yan-Qing,ZHANG Xiong
2009 Vol. 24 (4): 732736
Abstract(
2784 )
PDF(2393KB)(
2041
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Ferrite-encapsulated cenosphere powders were prepared by citrate sol-gel method. The additive was used to improve the performance of ferrite coating. Microstructure of the products was tested by SEM and EDS. It was found that the coating was independent of the type of ferrite. Adding glycol or polyethylene glycol into the precursors can help the ferrite encapsulation. Microwave reflection loss of the coatings with thickness of 1.8mm made from ferrite-encapsulated cenosphere powders was tested in the frequency range from 5GHz to 18GHz. It was found that the ferrite-encapsulated cenosphere coating exhibited better microwave absorbing property than the pure ferrite. More, adding glycol can improve the microwave absorbing property of the coatings.
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Effect of Forming Gas on Properties of SrBi2Ta2O9 Ferroelectric Thin Film and Powder
WANG Dong-Sheng,YU Tao,HU An,WU Di,LI Ai-Dong,LIU Zhi-Guo
2009 Vol. 24 (4): 737740
Abstract(
2641 )
PDF(2105KB)(
1885
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SrBi2Ta2O9 (SBT) ferroelectric thin film and powder samples were fabricated by using metalorganic decomposition (MOD) method. XRD and SEM results show that SBT powders still remain polycrystalline perovskite structure and amounts of Bi and δ-Bi2O3 are reduced from SBT annealed in the forming gas at 400℃. Spherical and needle structures form on the surface of SBT thin films annealed in the forming gas at 500℃. Bi element in powders is more easily reduced at lower temperature compared with that of thin films and form needle structures on SBT surface. Bi deficiency derived from forming gas annealing causes serious ferroelectricity degradation on the SBT capacitors. Annealed in the forming gas ambient at 400℃ for 5.5min, the remnant polarization of SBT films drop about 43%. If annealing time is longer than 8.5min, films are breakdown and ferroelectricity disappears totally. However, no obvious polarization fatigue with 109 electric field cycling could be observed.
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Preparation and Characterization of Ferroelectric Composite Ultrathin Film by Electrostatic Self-assembly
YE Yun,JIANG Ya-Dong
2009 Vol. 24 (4): 741744
Abstract(
2791 )
PDF(1572KB)(
1636
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The ferroelectric ultrathin multilayer of PDDA/PVDF-BT were fabricated on the pretreated quartz substrates between cationic electrolyte of poly (diallyldimethyl ammonium chloride) (PDDA) and anion reagent by electrostatic self-assembly method. Negatively charged poly (vinylidene fluoride) (PVDF) dispersed with inorganic BaTiO3 nano-granules in organic solvent was using as anion reagent. The thickness of the 12-layer ferroelectric composite ultrathin films characterized by quartz crystal microbalance (QCM) is about 82nm, and there exists a nearly linear relationship between the thickness and layer number of ultrathin films. The results of SEM and XRD show that the composite ultrathin films are deposited on the quartz surface smoothly and densely with uniform distribution of BaTiO3 nano-granules, and excellent crystalline performance. The hysteresis loop of ferroelectric composite ultrathin films shows that the electric polarization of the composite ultrathin films is increased to 3μC/cm2.
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Structure and Ferroelectric Properties of Ti4+-doped BiFeO3 Ceramics
ZHENG Chao-Dan,ZHANG Duan-Ming,LIU Xin-Ming,LIU Chao-Jun,YU Chun-Rong,YU Jun
2009 Vol. 24 (4): 745748
Abstract(
2845 )
PDF(2250KB)(
1832
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BiFe1-xTixO3 (x=0,0.05,0.10,0.15 and 0.20) (BFTxO) ceramics were prepared by the solid-state reaction technology. The effects of Ti doping on the microstructure, morphology, the ferroelectric properties and ferroelectric-paraelectric phase transition were investigated. The result of X-ray diffraction pattern implies that the rhombohedral structure is distorted to an orthorhombic structure by Ti doping. The measured Raman scattering spectra also show that Ti doping modifies the ceramic structure from rhombohedral to orthorhombic. Compared with the pure counterparts, the average grain sizes of the BiFe1-xTixO3 (x=0.05、0.10) ceramics decrease with the increase of Ti4+ concentration. The leakage current density and the remnant polarization of the BiFe1-xTixO3 (x=0.05,0.10) are improved due to the decreased oxygen vacancies by Ti4+ doping. The current density values for the pure BiFeO3 and BiFe0.95Ti0.05O3 ceramics are 1.4×10-4A/cm2 and 7.3×10-6A/cm2 at 100V, respectively. The remnant polarization (2Pr) of BiFe0.95Ti0.05O3 ceramic is 2.78μC/cm2 at 8kV/mm. DTA and Raman scattering spectra results indicate that the ferroelectric transition temperature (Tc) of the BFTxO crystal is influenced by the content of Ti ions. With the increase of Ti content, the ferroelectric transition temperature decreases.
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Preparation and Characterization of Tetragonal BaTiO3 Thin Film with Self-assembled Monolayers Technique
TAN Guo-Qiang,LIU Jian,MIAO Hong-Yan,HE Zhong-Liang,XIA Ao
2009 Vol. 24 (4): 749754
Abstract(
3144 )
PDF(2365KB)(
1907
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Self-assembled monolayers (SAMs) technique based on traditional liquid phase deposition and bio-inspired theory is one of the most promising processes for preparing inorganic thin films. Using octadecyl-trichloro-silane (OTS) as stencil, tetragonal BaTiO3 thin film was successfully prepared on glass wafers in the solution consisting of (NH4)2TiF6, Ba(NO3)2 and H3BO3 with SAMs technique. Hydrophilic characteristic mensuration of glass wafers and photographs of atomic force microscopy (AFM) indicate that the hydrophobe substrate changes into hydrophile by UV iradiation, and a modification of OTS-SAM is changed by UV light. Photographs of metallographic microscope indicate that the surface of BaTiO3 thin film deposited on OTS-SAM is smooth and homogeneous, and an induction of BaTiO3 thin film deposition is directed by OTS-SAM. X-ray diffraction (XRD) and field-emission scanning electron microscope (FE-SEM) results show that the BaTiO3 thin film with well-crystalline tetragonal phase is successfully prepared after annealing at 600℃ in air for 2h. BaTiO3 thin film grows on glass substrate with a rod-like morphology, the length of the nanowire is in the range from 500nm to 1000nm, which is composed of nanosized grains of around 100nm. The formation mechanism of OTS-SAM and BaTiO3 thin film is carefully discussed.
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Preparation of AlN Powder by Microwave Carbon Thermal Reduction
XIAO Jin,ZHOU Feng,CHEN Yan-Bin
2009 Vol. 24 (4): 755758
Abstract(
3486 )
PDF(1805KB)(
1619
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Aluminium nitride powders were prepared by microwave carbon thermal reduction method. The effects of aluminium sources, carbon sources and additives on AlN powder structure and morphology were studied. XRD analysis shows that most suitable aluminum source and carbon source are selected to be as aluminum hydroxide and acetylene black, respectively. The catalysis effect of additive A on nitridation is most obvious. Industry aluminum hydroxide and acetylene black are completely converted into AlN by adding additive A and heating at 1300℃ for 1h in nitrogen atmosphere. The results show that microwave carbon thermal reduction can reduce the reaction temperate and shortened the reaction time for the preparation of nitride powder.
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Study on Reaction Mechanism of Reactive Ball Milling of Ti with Urea to Prepare TiN Powder
SUN Jin-Feng,LI Xiao-Pu,LIANG Bao-Yan,ZHAO Yu-Cheng,WANG Ming-Zhi
2009 Vol. 24 (4): 759763
Abstract(
3339 )
PDF(2578KB)(
1803
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Titanium nitride (TiN) powders were synthesized by reactive ball milling titanium (Ti) and urea at room temperature. The structure of the as-synthesized powders were analyzed by XRD, the urea decomposed temperature and the decomposed products were characterized by TG-FTIR, the morphology and the microstructure were observed by TEM and the component of the powders were analyzed by EELS. The powders milled for 70h were annealed at 800℃ in vacuum for 5h. The results show that TiN powders with grain size of 6-7nm can be synthesized by reactive ball milling Ti and urea for 70h. The XRD patterns of the annealed powders prove that the powders are single phase of TiN. In the milling progress, titanium reacts with the decomposed products of urea, ammonia gas (NH3) and cyanic acid (HNCO) to form TiN. With the milling time increasing, the activity and the defect energy of titanium increase, so the diffusion activation energy for nitrogen diffusing in titanium decreases. The diffusion distance also decreases because the new TiN layer between Ti and nitrogen can be brought by milling. With the content of TiN increasing, the nucleus of TiN are formed which grow to nano-crystalline.
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Effects of Precipitants on the Properties of Nd3+∶Lu2O3 Nano-powders
ZHOU Ding,SHI Ying,YUN Ping,XIE Jian-Jun
2009 Vol. 24 (4): 764768
Abstract(
3042 )
PDF(2082KB)(
1574
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Neodymium doped lutetia nanocrystalline powders were synthesized by a wet chemical processing using three different precipitants, i.e. ammonium hydroxide (NH4OH), ammonium hydrogen carbonate (NH4HCO3) and the mixed solution of NH4OH+NH4HCO3, respectively. Compared with the other two precipitants, the Nd-doped Lu2O3 powder synthesized by mixed solution of NH4OH+NH4HCO3 had the advantages of higher specific surface area, smaller particle size (30nm) and narrower particle size distribution (from 60nm to 160nm). Green compacts were formed from as-synthesized Nd3+∶Lu2O3 powders by dry-pressing followed by a cold isostatic pressing. The green compact made from powders synthesized by mixed precipitants acheived the highest linear thermal shrinkage of about 17% at 1400℃, demonstrating more superior sinterbility than the other two powders. Highly transparent samples were obtained after being sintered in flowing H2 atmosphere at 1880℃ for 8h. The linear optical transmittance of the polished transparent samples reached 75.5% at the wavelength of 1080nm.
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Femtosecond Laser Induced Ba2TiSi2O8 Crystal Precipitation in Glass
LU Bo,DAI Ye,MA Hong-Liang
2009 Vol. 24 (4): 769772
Abstract(
3110 )
PDF(1442KB)(
1639
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Ba2TiSi2O8 crystal was space-selectively precipitated in a 33.3BaO-16.7TiO2-50.0SiO2 glass sample by using a high repetition femtosecond laser with 800nm, 150fs and 250kHz. After the femtosecond laser irradiated for a period of time, the luminescence of the focused point could chang from 800nm red light to 400nm blue one due to second-order optical nonlinearity of the precipitated crystal. Raman spectra show Ba2TiSi2O8 crystal is formed. During the femtosecond laser irradiation, heat accumulation effect occurs in the irradiated region by continuously absorbing pulse energy, and the glass would be heated to its crystallization temperature, therefore Ba2TiSi2O8 may grow or precipitate in the crystallized region. Furthermore, the Raman spectra at different positions of the irradiated region demonstrate that Ba2TiSi2O8 crystal grows more effectively in the center compared with that in the outers. This result is agreeable with the femtosecond laserinduced temperature distribution because the temperature increases more quickly in the focused region.
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Gd3+-sensitized Tb3+-doped Scintillating Silicate Glasses
WANG Sheng,QIAN Qi,ZHANG Qin-Yuan,YANG Zhong-Min,JIANG Zhong-Hong
2009 Vol. 24 (4): 773777
Abstract(
2730 )
PDF(1795KB)(
1741
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Gd3+-sensitized Tb3+-doped scintillating silicate glasses with Gd2O3 and Tb2O3 concentrations up to 45wt% were prepared. Effects of different Gd2O3 and Tb2O3 concentrations on the density, refractive index and luminescence properties under UV and X-ray excitations were investigated and the energy transfer mechanisms between Gd3+ and Tb3+ analyzed and discussed. The results show that, with the increasing concentrations of Tb3+ and Gd3+, a monotonic increase in the energy transfer efficiencies from Gd3+∶6P7/2 to Tb3+∶5H7 is observed followed by enhanced emissions centered at 620, 583, 541 and 496nm under 273nm UV excitation. However, with X-ray excitation, the incorporation of a large amount of Tb3+ weakens the luminescence emission due to the increase of point defects in glass.
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Lowcost Preparation and Photoelectric Property Study of PbSe Nanocrystalline Films
ZHOU Feng-Ling,LI Xiao-Min,GAO Xiang-Dong,Qiu Ji-Jun
2009 Vol. 24 (4): 778782
Abstract(
3212 )
PDF(2167KB)(
2021
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PbSe nanocrystalline films were deposited on glass substrates by chemical bath using the Pb(Ac)2 solution and Na2SeSO3 solution as the reactants. Effect of the concentration of complexing agent ([OH-]) in the chemical bath on the crystal structure, morphology and electricoptical property of the film were investigated. The results indicate that crystal size of the film is about 10nm which is correlated with the complexing agent concentration. With low concentration of [OH-], the film is uniform and compact, whereas it becomes loose and discontinuous with high concentration of [OH-]. Optical transmission spectra show a blue shift of the absorption edge from 5μm to 1μm in the asgrown films, and the absorption edge moves to longer wavelength after annealing at 300℃. The as-grown film shows a huge sheet resistant (>10GΩ), and the sheet resistant obviously decrease to 10kΩ~100MΩ after annealing in air and in oxygen. Electro-optical performance is studied by measuring the current vs time (i-t) curve at a signal of light pulse. The i-t curves indicate an obvious photoelectrical response in nanocrystalline films at the presence of light. The film annealed in air has a slow-electro-optical performance, whereas the film annealed in oxygen has a fast response.
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R-plane Sapphire Substrate for Non-polar GaN Film
YANG Xin-Bo,XU Jun,LI Hong-Jun,BI Qun-Yu,CHENG Yan,SU Liang-Bi,ZHOU Guo-Qing
2009 Vol. 24 (4): 783786
Abstract(
3021 )
PDF(2107KB)(
1990
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R-plane sapphire used for epitaxial growth of non-polar GaN film was grown by the temperature gradient technique (TGT) method and chemical mechanical method was used to polish the r-plane sapphire substrate. The crystallization quality, optical property and surface roughness of as-obtained r-plane sapphire substrate were investigated. The average full width at half maximum (FWHM) of the substrate is 19.4arcsec and the dislocation density is 5.6×103cm-2. The transmission of the substrate is higher than 80% when the wavelength is longer than 300nm and the optical homogeneity is 6.6×10-5. The average surface roughness of the r-plane sapphire substrate is 0.49nm. The results indicate that as-obtained r-plane sapphire substrate meets the basic standard of GaN substrate.
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Synthesis and Characterizations of Lithium Vanadium Oxide Nanotubes
CUI Chao-Jun,WU Guang-Ming,ZHANG Ming-Xia,SUN Juan-Ping,YANG Hui-Yu,SHEN Jun
2009 Vol. 24 (4): 787792
Abstract(
3273 )
PDF(2358KB)(
1948
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Lithium vanadium oxide nanotubes as cathode materials for rechargeable lithium batteries were prepared via a sol-gel reaction followed by hydrothermal treatment, in which V2O5 and LiOH·H2O were used as raw materials and C16H33NH2 as structure-directing template. Structure and morphology of the nanotubes were investigated by SEM, TEM, XRD, FT-IR and XPS.Meantime, electrochemical behavior of the materials was researched by cyclic voltammetry. The results show that the inner and the outer diameters of the obtained nanotubes are of about 30nm and 70nm with length between 1μm to 3μm, respectively. It is also confirmed by XPS that the elements of the products are made up of various chemical states. The electrochemical performance indicates that the obtained nanotubes as cathode materials for rechargeable lithium batteries have good lithium-ion insertion/deinsertion reversibility.
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Properties of CeB6 Cathode Fabricated by Spark Plasma Reactive Liquid Phase Sintering Method
ZHOU Shen-Lin,ZHANG Jiu-Xing,LIU Dan-Min,BAO Li-Hong
2009 Vol. 24 (4): 793797
Abstract(
3055 )
PDF(2653KB)(
1425
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CeHx nano-powders were prepared by hydrogen arc plasma method, and then the mixed powders of nano-CeHx and micron boron were sintered by Spark Plasma Reactive Liquid Phase Sintering (SPS) method to fabricate high-properties polycrystalline bulk CeB6 cathodes. The reaction equation of sintering CeB6 and reactive liquid phase sintering mechanism were studied. The optimum process parameters are listed as follows, pressure of 50MPa, temperature of 1500℃, and holding time of 5min. The experimental results show that the CeB6 sintered body with purity of 99.89% and relative density of 99.61% is single-phase of cerium hexaboride. The hardness and bend strength of the sintered CeB6 reach 2051kg/mm2 and 254.2MPa. The electron emitting density of the CeB6 sintered by SPS is 20.38A/cm2 at 1600℃, the work function is 2.42eV. In contrast to traditional preparation method, SPS method obviously reduces the sintering temperature and shortens the sintering time of CeB6, and improves the mechanics and emission properties.
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Characteristics of Carbon Paper as Electrode for Vanadium Redox Flow Battery
LIU Su-Qin,SHI Xiao-Hu,HUANG Ke-Long,LI Xiao-Gang
2009 Vol. 24 (4): 798802
Abstract(
3326 )
PDF(1652KB)(
1784
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The carbon paper (CP) heat-treated at 435℃ for 10h were characterized by FTIR spectroscopy and BET, and their electrochemical behaviors were investigated by cyclic voltammograms, impedance spectroscopy and charge-discharge techniques. The results show that -COOH functional groups form after heattreated for 10h and specific surface area increases significantly. The vanadium redox battery with modified CP electrode exhibits excellent performance at current density of 50mA/cm2. The average current efficiency reaches 95% and average voltage efficiency reaches 89%. The improvement of electrochemical performance for the electrode is ascribed to the -COOH group and the special surface of CP.
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Effect of Te Doping on Thermoelectric Property of SryCo4Sb12-xTex Compounds
ZHAO Xue-Ying,BAI Sheng-Qiang,LI Xiao-Ya,ZHOU Yan-Fei,CHEN Li-Dong
2009 Vol. 24 (4): 803807
Abstract(
2703 )
PDF(1382KB)(
1719
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Skutterudite compounds, SryCo4Sb12-xTex, were synthesized by melting method and SPS method, the thermal and electrical properties were measured in the temperature range from 300K to 850K. Both carrier concentration and electrical conductivity of SryCo4Sb12-xTex compounds are higher than those of the matrix with similar Sr filling fraction. The magnitude of Seebeck coefficient is increased in comparison with that of matrix with similar carrier concentration, especially at high temperature. Lattice thermal conductivity is further decreased due to the extra electron-phonon scattering mode introduced by Te doping. The maximum ZT value of 1.0 is obtained for Sr0.18Co4Sb11.95Te0.05 at 850K, which is improved by 35% compared with that of Sr0.17Co4Sb12.
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Novel Preparation, Characterization, Property of Lithium Bis(oxalate) Borate
LIU Jian-Wen,LI Xin-Hai,WANG Zhi-Ying,GUO Hua-Jun,HU Qi-Yang
2009 Vol. 24 (4): 808812
Abstract(
3663 )
PDF(1723KB)(
1881
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A novel preparation method of lithium bis(oxalato)borate (LiBOB) called acetonitrile solution method was introduced. Lithium source was firstly pretreated by P204 extraction resin. Then Li2CO3 was reacted with H3BO3 and H2C2O4 directly in acetonitrile solution. As-prepared LiBOB was finally purified in ethylene glycol di-methyl ether (C4H10O2). The synthesized LiBOB was characterized by infrared spectrum, X-ray diffraction (XRD) pattern, atomic absorption and ion chromatography. Thermal stability capability of as-synthesized LiBOB was analyzed by differential thermal analysis and thermogravimetry. The results indicate that the as-synthesized LiBOB has higher purity, lower impurity contents and better thermal stability than commercialized LiBOB, the purity of the as-synthesized LiBOB reaches 99.95%.
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Effects of B and C on Hydrogen Storage Properties of Li-N-H Complex Hydrides
LIU Yi-Xin,YANG Shu-Quan,ZHANG Dan-Dan,LI Guang-Xu,WEI Wen-Lou,GUO Jin
2009 Vol. 24 (4): 813816
Abstract(
3034 )
PDF(1960KB)(
1701
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LiNH complex hydrides were prepared by mechanical alloying and the effects of B and C as catalyst on hydrogen storage properties were investigated. The results show that LiNH2 and Li2NH are the main phases in Li-N-H complex hydrides and the amorphous degree of the main phases increase with B element added. Although the hydrogen storage capacity decrease with B and C element added, the effective hydrogen storage capacity increase and the kinetic properties of hydrogen absorption/desorption can be improved when the adding n(B)∶n(C)=1∶2. The hydrogen absorption/desorption temperature can be decreased effectively with adding B. The reversible hydrogen absorption/desorption capacity can also be improved with milling time prolonging.
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Brazing of SiC Ceramics Using Ag-Cu-In-Ti Filler Metal
LIU Yan,HUANG Zheng-Ren,LIU Xue-Jian,YUAN Ming
2009 Vol. 24 (4): 817820
Abstract(
2891 )
PDF(1282KB)(
1629
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Sintered silicon carbide was jointed with itself using Ag-Cu-In-Ti filler metal successfully. Interfacial microstructure was investigated by electron probe microanalysis (EPMA) and transmission electron microscope (TEM). Joining strength of SiC/SiC joints was measured by four-point flexural strength. The experimental results indicate that joining strength has a peak value with the joining temperature increasing, and the max flexural strength reaches 234MPa, however joining strength decreases monotonously with the holding time increasing. The interface of joints is composed of three parts: SiC substrate, reaction layer and filler metal. The continuous and compact reaction layer which is composed of strip layer, TiC layer and Ti5Si3 layer, combines the SiC substrate and filler metal tightly. The strip layer consisting of Ag, In, Si, Cu, Ti and C elements is about 20nm in thickness. The elemental linescanning result shows that nearly all the active element Ti concentrate in the reaction layer and the main reason for the joining is the reaction between Ti and SiC.
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High Temperature Oxidation Mechanism of Ti3SiC2-64vol%SiC Ceramics
TANG Hui-Yi,ZHU De-Gui,LIU Bo,SUN Hong-Liang
2009 Vol. 24 (4): 821826
Abstract(
2958 )
PDF(2518KB)(
1721
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Full dense Ti3SiC2-64vol%SiC ceramics were successfully fabricated by in situ synthesis under hot isostatic pressing (HIP). The high temperature oxidation behaviors and mechanisms of the ceramics were studied by thermogravimetry tests (TG) at 1100-1450℃ in air. Testing results indicate the curves of isothermal kinetics of the ceramics obey parabolic oxidized law or paraboliclinear oxidized law. The addition of SiC (64vol%) efficiently improves the oxidation resistance of Ti3SiC2-SiC ceramics. According to XRD and SEM-EDS results, the oxidized layers are composed of an outer layer of TiO2 (rutile) and SiO2 (glass),and a transition layer of mixture of TiO2 and SiO2. At high temperature (1400℃), the growth morphology of TiO2 layer can be influenced by the formation of glassy SiO2. The continuous and dense TiO2 films which can efficiently prevent the diffusion of oxygen are formed. The parabolic rate constants decrease about one order of being oxidized at 1400℃ for long time compared with that oxidized at 1200℃. The oxidation resistance of Ti3SiC2-64vol% SiC ceramics at 1400℃ is better than that oxidized at 1200℃.
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Crystallization of Amorphous SiCN Ceramic Annealed in Vacuum
XIA Yi,QIAO Sheng-Ru,WANG Qiang-Qiang,ZHANG Cheng-Yu,HAN Dong,LI Mei
2009 Vol. 24 (4): 827830
Abstract(
3323 )
PDF(1590KB)(
1917
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SiCN ceramic was fabricated by electro-thermal pyrolysis using hexamethyldisilazane as precursor. X-ray diffraction and transmission electron microscope were employed to study crystallization process of amorphous SiCN after annealing at temperature from 1700℃ to 1900℃ in vacuum. Decomposition-crystallization mechanism was used to characterize its crystallization process. Amorphous SiCN begin to decompose below 1300℃ in vacuum and Si-C-enriched districts are formed and then changes to form β-SiC crystal. Crystallinity degree increases as treated temperature rises. Phase transition from β-SiC to α-SiC occurs after annealing at 1700℃. The nitrogen is released in the form of N2 and Si3N4 crystal is not detected though it often exists in the SiCN annealed in N2 atmosphere.
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Slip Casting and Pressureless Sintering of ZrB2-SiC Ceramics
WANG Xin-Gang,LIU Ji-Xuan,KAN Yan-Mei,ZHANG Guo-Jun,WANG Pei-Ling
2009 Vol. 24 (4): 831835
Abstract(
3137 )
PDF(2033KB)(
1815
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The dispersion of ZrB2 particles in water was investigated using polyethyleneimine (PEI) as a dispersant. Results showed that the ZrB2 slurry had a isoelectric point of pH=5.7. The application of PEI changed the isoelectric point of the ZrB2 slurry to pH=11.5. High solids loading (45vol%) ZrB2-20vol% SiC slurries were prepared at pH=8.0 by adding 1.0wt% PEI. The green body prepared by slip casting had a relative density of 53%. The effects of boron as a sintering aid on the pressureless sintering process of the ZrB2-20vol% SiC ceramics were investigated. Nearly fully dense ZrB2- SiC composites were obtained by sintering at 2100℃ for 3 h. The sintered ceramics demonstrated a Vickers hardness of (17.5±0.5)GPa, a flexure strength of (406±41)MPa,and a fracture toughness of (4.6±0.4)MPa·m1/2.
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Preparation and Property of SiC/(ZrB2-SiC/SiC)4 Anti-oxidation Coatings for Cf/SiC Composites
WU Ding-Xing,DONG Shao-Ming,DING Yu-Sheng,ZHANG Xiang-Yu,WANG Zheng,ZHOU Hai-Jun
2009 Vol. 24 (4): 836840
Abstract(
3143 )
PDF(2702KB)(
1825
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A SiC/(ZrB2-SiC/SiC)4 coating was prepared by slurry painting and pulse CVD. The composition and structure of the coating were studied by using XRD,SEM and EDS analysis, then the anti-oxidation property of the coating was investigated. The results show that the thickness of obtained coating is about 100μm, ZrB2-SiC layer and Pulse CVD SiC layer are bonded to each other alternately. After oxidation at 1500℃ in air for 25h, the weight loss of the Pulse CVD coating is 5.1%, while weight gain of the SiC/(ZrB2-SiC/SiC)4 coating is about 2.5%. The SiC/(ZrB2-SiC/SiC)4 coating shows excellent antioxidation property.
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Densification and Surge Current Performance of SnO2-Sb2O3 Based Varistor Ceramics
LU Zhen-Ya,HUANG Huan,WU Jian-Qing
2009 Vol. 24 (4): 841844
Abstract(
3002 )
PDF(1353KB)(
1655
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Influence of TiO2, Co3O4, Cr2O3, Ni2O3 and MnO dopings on the microstructure and electrical properties of SnO2-Sb2O3 based varistor ceramic materials was investigated. It is found that TiO2 and Co3O4 are effective dopants for improving densification of SnO2 ceramics. According to XRD analysis, Co2SnO4 crystal phase are formed by the reaction between Co3O4 and SnO2, and TiO2 is dissolved into the SnO2 phase. Doping of Sb2O3 can improve the semiconducting processes of SnO2 grains. Co-doping Cr2O3, Ni2O3 and MnO is efficient to improve the nonlinear property and surge current withstanding performance of the materials. The samples with a diameter of 14mm have a nonlinear coefficient (α) of about 50, a breakdown electric filed of about 350V/mm and a leakage current of less than 5μA, and the withstanding surge peak current of 8/20μs waveshape is about 2kA, which meet practical requirement.
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Fabrication of Agglomerate-free ZnO Nanoparticles by Electrospraying and Subsequent Two-step Heat Treatment
ZHANG Pan,LI Jian-Lin
2009 Vol. 24 (4): 845847
Abstract(
3027 )
PDF(1512KB)(
1734
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Agglomerate-free ZnO nanoparticles were prepared by electrospraying and subsequent two-step heat treatment, providing a novel way for the fabrication of agglomeratefree oxide nanopowders. Using Zn(CH3COO)2·2H2O ethanol solution added proper polyvinylpyrrolidone as electrosprayed liquid, a cone-jet was successfully formed that produced symmetrical micron droplets. The electrosprayed products were dried then. Agglomerate-free ZnO nanoparticles were derived after annealing the dried electrosprayed products in nitrogen at 600℃ for 1h followed by annealing in air at 400℃ for 1h. Results of SEM and XRD tests demonstrate that the as-prepared ZnO nanoparticles are well developed with a uniform size, and a hexagonal wurtzite structure.
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Polycrystalline Mullite Fibers Prepared by Sol-Gel Method
LI Cheng-Shun,ZHANG Yu-Jun,ZHANG Jing-De
2009 Vol. 24 (4): 848852
Abstract(
3385 )
PDF(1914KB)(
1846
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Polycrystalline mullite fibers were prepared by sol-gel method, using aluminum powders, hydrochloric acid and silica sol as raw materials, water as solvent. The aggregation state of Al3+ was measured by 27Al NMR. The pyrolytic decomposition patterns of mullite fibers were assessed by heating samples to different temperatures and characterizing the products by thermogravimetric analysis (TG), differential thermal analysis (DTA), X-ray diffractometry (XRD), and Fourier transform infrared spectroscopy (FT-IR). The micrograph of mullite fibers were observed by means of Scanning Electron Microscope (SEM). The results of 27Al NMR show that Al3+ ions aggregate in the PAC sol in the form of Al13 with Keggin structure. TG/DTA analyses show the exotherm at 970℃ can be attributed to the formation of mullite phase and weight loss of the mullite fibers in the heat treatment reaches 48.24%. XRD and FT-IR analyses show that phasepure mullite can be formed at 1000℃ with no other intermediate. After heat-treated at 1250℃, the mullite crystalline fibers with diameter of 3-5μm, grain size of 240nm and tensile strength of 1.1GPa are obtained.
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Modification Mechanism of the Surfacetreated PANbased Carbon Fiber by Electrochemical Oxidation
GUO Yun-Xia,LIU Jie,LIANG Jie-Ying
2009 Vol. 24 (4): 853858
Abstract(
3508 )
PDF(2904KB)(
2065
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Surface treatment is one of the most important procedures for the preparation of the high performance carbon fiber. The morphology of the surface-treated PAN carbon fiber was characterized in terms of AFM, SEM, XPS and XRD. And the modification mechanism of the electrochemical oxidation method was also discussed. Results show that the weaker layer of carbon fiber surface is removed by the electrochemistrical etching. As compared with the untreated carbon fiber, the grooves after treatment become widened and deepened, and the surface roughness is also increased one-fold. The functional groups on the carbon fiber surface are increased after the chemical oxidation of electrochemistry, as confirmed by that the (O1s+N1s)/C1s atomic ratio is increased by 9.7%. The physical and chemical double effectiveness mechanism is put forward that the physical and chemical state of the carbon fiber surface can be improved simultaneously by the electrochemical oxidation.
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Study on the Radical Grafting Polymerization of MMA onto Basic Magnesium Chloride Whisker Surface
ZHANG Lu,CHEN Xue-Gang,YAO Zhi-Tong,YE Ying,XIA Mei-Sheng
2009 Vol. 24 (4): 859863
Abstract(
2929 )
PDF(2137KB)(
1684
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The composite material nano-BMC/γ-MPS/PMMA was prepared using nano-BMC as raw material, which was obtained by brine method. The nano-BMC whisker was pretreated by silane coupling agent 3-(trimethoxysilyl) propyl methacrylate (γ-MPS) and then conducted to surface radical grafting polymerization which is initiated by water-soluble initiator K2S2O8 in ethanol/water mixture. The structure and morphology of nano-BMC/γ-MPS/PMMA was characterized by Fourier Transformed Infrared Spectroscope (FT-IR), Scanning Electron Microscope (SEM) and X-ray Diffraction (XRD) analysis. The influences of reaction conditions on the conservation of whisker morphology and grafting polymerization were investigated. The result shows that the reaction conditions have a significant effect on the morphology of nano-BMC whisker. The grafting efficiency reaches 56.1% and the morphology of nano-BMC whisker is well conserved when the reaction is kept at 82℃ for 6h in the ethanol-water solution with the 8∶2 ratio of ethanol to water.
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Numerical Analysis of Heattransfer Model of Mircrowave Sintering for Ceramics Composites with Heat Conduction Phases
HAO Hong-Shun,XU Li-Hua,HUANG Yong,XIE Zhi-Peng,ZHANG Xiao-Meng,LI Xing-Wang
2009 Vol. 24 (4): 864868
Abstract(
2664 )
PDF(2397KB)(
1547
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Based on the characteristic of microwave heating, the numerical heat-transfer model of two-dimensional stable-state heat conduction of microwave sintering for ceramics composites with heat conduction phases was built up and validated by the experiment of microwave sintering densification for SiCw/TZP ceramics. The prediction of the newly-established model is in accord with experimental results of composite ceramics such as SiCw/TZP ceramics. The influencing factors about two-dimensional stable-state temperature field distribution such as concentration and distribution of heat conduction phases, category of matrix and mode of thermal insulation are analyzed. The results indicate that matrix with high coefficient of thermal conductivity, heat conduction phases with high concentration, uniform distribution of heat conduction phases in matrix and appropriate thermal insulation equipment should be considered in the design of composite ceramics with heat conduction phases.
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Nanoscale Elastic Response of Grain Boundaries in ZnO Varistors by Acoustic Mode AFM
ZHAO Kun-Yu,ZENG Hua-Rong,SONG Hong-Zhang,CHENG Li-Hong,ZENG Jiang-Tao,CAI Wen-Jie,HUI Sen-Xing,LI Guo-Rong,YIN Qing-Rui
2009 Vol. 24 (4): 869872
Abstract(
3165 )
PDF(1229KB)(
1440
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Low-frequency acoustic mode atomic force microscopy was successfully developed based on the commercial AFM. The experimental results on nanometer scale elastic response at the grain boundaries in ZnO varistors assessed by the technique were presented. Different acoustic contrast of the individual micro-grains at grain boundaries were examined which reflected the distribution of additives. The acoustic contrasts enhanced at the grain boundaries can be observed clearly, which present possibility of crystal lattice expanding of Bi-rich phase caused by phase transition in the heat treatment. The lateral resolution of acoustic image is down to nanometer scale. The results show the application perspective of low-frequency scanning probe acoustic microscopy in functional materials at submicro- or nanometer scale.
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