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Influence of Interfaces on Mechanical Behavior of C/C Composites by CLVI Processing
SUN Wan-Chang,LI He-Jun,LU Jin-Hua,BAI Rui-Cheng,HUANG Yong
2005 Vol. 20 (6): 12571462
Abstract(
2139 )
PDF(1497KB)(
1395
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C/C composites were fabricated by a rapid chemical liquid-vaporized infiltration (CLVI) processing. The fractured surfaces were observed by scanning electron microscope (SEM). In this paper, three types of interfaces in the composites, the fiber-matrix interface within a tow, the interface between carbon cloths or bundles, as well as the interface between pyrocarbon laminar, were discussed. Moreover, their influences on mechanical behavior of the composites were analyzed. In order to obtain high strength and pseudoductility, it is necessary for C/C composites to have proper interface bond strength between fiber and matrix, smaller residual pores between carbon cloths or bundles, and proper gaps between pyrocarbon laminar within the matrix.
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Effect of in Inner Electrode Ag Diffusion on Electric Properties of Low Firing Multilayer Chip Zinc Oxide Varistor
ZHONG Ming-Feng,SU Da-Gen,ZHUANG Yan,CHEN Zhi-Xiong
2005 Vol. 20 (6): 12731378
Abstract(
2408 )
PDF(498KB)(
1342
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Effect of Ag diffusion of Pd-Ag inner electrode on electric properties of multilayer chip ZnO varistor was studied. The results show that Ag contents in inner electrode play a very important role in the electric properties of multilayer chip ZnO varsitor. When the Ag content is less than 90%, the properties are good, but when the Ag content is more than 90%, the properties deteriorate with the increase of the Ag content. And the properties of MLCV having pure Ag inner electrode are the worst. The capacitance reflecting the grain-boundary barrier capacitances decreases with the increase of Ag content. The analyses of V-I characteristic curves and complex impedances indicate that, during the co-firing process of the ceramic and inner electrode, with the increase of Ag content in inner electrode, the velocity of Ag diffusing in the ZnO lattice will speed, and the grain resistance increases excessively, and the electric properties of MLCV deteriorate.
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Template Preparation Techniques and Application of Hollow Micro- or Nano-Particles
HUANG Zhong-Mei,GUAN Jian-Guo,GAN Zhi-Ping,WANG Zhen-Jie
2005 Vol. 20 (6): 12811287
Abstract(
2325 )
PDF(706KB)(
1447
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The preparation techniques of hollow micro- or nano-particles by using either hard templates or soft templates were reviewed in terms of fabrication mechanism and structure controllability, and with emphasis on the recent progress of such preparation methods as layer-by-layer assembly, surface chemical reaction and coprecipitation, micro-encapsulation methods. The relationship between the structure and the performance, as well as the potential applications in areas of materials science, biomedicine, catalysts etc of the hollow micro- or nano-particles were also discussed.
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Observation of Ferroelectric Structures of Near-stoichiometric LiNbO3 Crystal and Its Mechanism
ZHENG Yan-Qing,CHEN Jian-Jun,LU Zhi-Ping,WANG Shao-Hua,SHI Er-Wei
2005 Vol. 20 (6): 12881294
Abstract(
2091 )
PDF(735KB)(
1328
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Near stoichiometric LiNbO3 crystals of varied composition were grown by a double crucible Czochralski method. An etching method was applied to observe the ferroelectric domain structures of the as-grown crystals. The results show that the congruent crystal grown along z-axis contains a domain structure consisting of concentric rings. The crystal with composition of 49.4mol% Li2O contains a special domain structure consisting of three fan-shape opposite domains with three-fold symmetry, which is consistent with the symmetry of the crystal structure. The crystal with composition of 49.7mol% Li2O has a single domain structure. The formation mechanism of the domain structures was discussed based on a thermoelectric field model. It is argued that the sign of the temperature gradient along z-axis in the front of para- ferroelectric interface is the critical factor that determines the polarity direction of the domain in development. Finally, the technological methods to control the domain structures were discussed.
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Structure and Vibration Spectrum of Laser Crystal Yb:KGd(WO4)2
WANG Ying-Wei,CHENG Hao-Bo,ZHU Zhong-Li,LI Jian-Li,LIU Jing-He
2005 Vol. 20 (6): 12951300
Abstract(
2313 )
PDF(521KB)(
1201
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The selection of the flux and the design of the proper processes are the key factor for the growth of Yb:KGd(WO4)2 laser crystal. Yb:KGd(WO4)2 crystal was grown by the Top Seeded Solvent Growth (TSSG) method using K2W2O7 as a suitable flux. On the base of TG-DTA, the crystal has two obvious absorption peaks at 1086℃ and 1021℃, its melting point is 1086℃, phase transition temperature from tetragonal to monoclinic is 1021℃. The Yb:KGd(WO4)2 crystal consists of WO6 octahedra which consists of WOOW double oxygen bridges and WOW single bridges. IR and Raman spectra show the atom group WO42- flex vibration at 436 cm-1 and atom group WO42- bend vibration at 740~925cm-1, WOOW double oxygen bridge vibration at 903, 765, 684, 438, 498 and 297cm-1, WOW single bridges vibration at 808, 526 and 232cm-1. Analyzing on the X-ray diffraction spectrum of Yb:KGd(WO4)2 crystal powder sample, we can conclude that the β-Yb:KGd(WO4)2 crystal is of a monoclinic system, and C2/c space group.
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Crystal Growth and Optical Characterization of Large-sized Cerium-doped Lu1.6Y0.4SiO5
YAN Cheng-Feng,ZHAO Guang-Jun,ZHANG Lian-Han,XU Jun
2005 Vol. 20 (6): 13011305
Abstract(
2160 )
PDF(387KB)(
1402
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Cerium-doped Lu1.6Y0.4SiO5 (LYSO) crystal with a dimension of φ60mm×110mm was grown by the Czochralski method. Advantages of LYSO Czochralski growth relative to LSO include reduced melting point, less propensity for formation of crystalline inclusions, lower cost of starting material. Its optical transmission, excitation and emission spectra of LYSO crystal were measured at room temperature. Results indicate that with the yttrium ion doping, absorption edge of LSO crystal is shifted towards short wavelength. Three absorption bands of LYSO are formed, which assign to the Ce3+ 4f1→5d1 transitions at room temperature. The Gaussian fits to the emission spectra of LYSO crystal excited with 358nm, show band characteristics with two peaks of 395 and 418nm, which assign to Ce1 site, and with the emission peak at 435nm, to Ce2 site.
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Surface Synthesis of CdSe Nanocrystals on Polystyrene Spheres
XIA Ming-Zhe,LI Dong-Sheng,YANG De-Ren,QUE Duan-Lin
2005 Vol. 20 (6): 13061310
Abstract(
2187 )
PDF(953KB)(
1254
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The CdSe nanocrystals were obtained by the chemical bath depostion on the surface of polystyrene (PS) served as the template. The transmission electron microscope (TEM) images show that the CdSe nanocrystals are coated on the surface of PS with the island morphology. The CdSe nanocrystals are cubic structure confirmed by XRD. Finally, according to the morphology changing with the reaction time, the formation of the morphologies is contributed to the PS electric double layer structure.
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Inhibiting Effect of Aluminosilicate Intermediate on Agglomeration and Phase Transition of TiO2 Nanoparticles
CHANG Jia-Zhong,LI Min,WANG Zhen-Ling,SHI Heng-Zhen
2005 Vol. 20 (6): 13111316
Abstract(
2109 )
PDF(402KB)(
1137
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By heating coal fly ash with hydroxide sodium solution, then hydrolysis, the aluminosilicate intermediate (ASI) was prepared. Through the addition of ASI into the titanium sol obtained by using the sol-gel method, titanium-aluminosilicate (TiO2/ASI) composites were prepared, and then heat-treated at different temperatures. The formation process and phase transition of TiO2 nanocrystalline in the TiO2/ASI composites were characterized by X-ray diffraction and UV-Vis diffuse reflectance spectra. The results indicate that the agglomeration of TiO2 nanoparticles and their phase transition from anatase to rutile can be inhibited efficiently. The adsorption activity of methylene blue of the synthesized TiO2/ASI composites is higher than that of only aluminosilicate intermediate or TiO2 particles.
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Preparation of Nano-scale Ni(OH)2 Based on Controlled Crystallization
HE Xiang-Ming,LI Jian-Jun,CHENG Hong-Wei,JIANG Chang-Yin,WAN Chun-Rong
2005 Vol. 20 (6): 13171321
Abstract(
2206 )
PDF(398KB)(
1118
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The dispersive nano-scale Ni(OH)2 was synthesized by a improved controlled crystallization process and dehydrated by azeotropic distillation with n-butanol. The pH value and temperature of controlled crystallization were optimized to be 11.0 and 45℃, respectively. As-prepared nano-scale Ni(OH)2 was dispersive, of 20nm size, and characterized by both TEM and XRD analysis. It had discharge capacity in excess of 258mAh·g-1.
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Synthesis and Photoelectric Property of Complexe C60Pd(Ph2PCH2CH2PPh2)
WU Zhen-Yi,YANG Sen-Gen,LIN Yong-Sheng,CHENG Da-Dian,ZHAN Meng-Xiong
2005 Vol. 20 (6): 13221328
Abstract(
2046 )
PDF(440KB)(
1108
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In the present work, the fullerene complexe C60Pd(Ph2PCH2CH2PPh2) was perpared by the method of ligand substitution via the reaction of C60 with Pd(Ph2PCH2CH2PPh2)2 in nitrogen atmosphere under refluxing, and the title compound was characterized by the methods of elemental analysis , FT-IR, UV-vis, XPS,XRD. The result shows that the structure of purposeful product is that the Ph2PCH2CH2PPh2 took up two coordination sites of the central metal, and C{60 took up another two sites in σ-π feedback pattern. Meanwhile the properties on redox and the thermostability were studied, the redox research indicates that the reduction potential of the complexe is more negative than that of the pure C{60. And the research on the photovoltaic effect for C60 Pd(Ph2PCH2CH2PPh2) complex which forming n+n heterojunction with GaAs electrode in photoelectrochemical cell shows that the photoelectric property of C60Pd(Ph2PCH2CH2PPh2) is excellent, especially in the Fe(CN)3-6/Fe(CN)4-6 redox couple mediator. The photovoltaic property of C60Pd(Ph2PCH2CH2PPh2) electrode at 1μm for thickness of C60Pd(Ph2PCH2CH2PPh2) is the best, the photopotential value is up to 367 mV.
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Synthesis and Characterization of MoS2 Composites Pillared by Hydroxy-Fe-Al Oligocations
PEI Xiao-Ke,LIN Bi-Zhou,ZHANG Jin-Fei,HAN Guo-Hua,LI Zhen
2005 Vol. 20 (6): 13291336
Abstract(
1971 )
PDF(747KB)(
1202
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Hydroxy-Fe-Al oligocations with a Keggin structure were prepared by a substitution reaction. Through the single-molecular-layer technology, the hydroxy oligocations are intercalated into the interlayers of molybdenum disulfide, which results in the pillared composites having the basal interlayer spacings from 1.394 to 1.513nm. With the increasing of Fe/Al molar ratio, the interlayer spacings and the surface areas of the pillared composites decrease, while their particle sizes increase. Catalyzed by the pillared composites, sulfide ions are oxidized into thiosulfate ions. It exhibits that their catalytic activities are 4 to 5 times higher than that of the pristine 2H-MoS$_2$, and that their catalytic activities are enhanced upon irradiation with visible light. Such catalytic behavior results from their more catalytically active sites, owing to their larger surface areas, and the generation of the photoinduced electron-hole pairs during the catalytically oxidization reaction process.
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Synthesis of FeS2 Nanowires and Effect of Sulfidation Parameters on the Formation
ZHANG Hui,YANG Gao-Qiang,ZHANG Ren-Gang,WANG Bao-Yi,WEI Long
2005 Vol. 20 (6): 13371342
Abstract(
2166 )
PDF(683KB)(
1389
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FeS2 nanowires array was prepared by the combination of anodic alumina menbrane technique and sulfidation procedure. Scanning electron microscope (SEM) observation shows the bundles of oriented nanowires with very high aspect ratio before and after sulfidation. The X-ray diffraction (XRD) patterns reveal that the nanowires crystallize well with the cubic pyrite phase at higher temperatures, and sulfidation time has a little influence on the grain size during crystallization. X-ray photoelectron spectroscope (XPS) spectra show that a sulphur surface component is found additionally to the known pyrite signals.
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Polyol Process Preparation and Characterization of Sb2Se3 Nanowires
CHEN Ming-Hai,GAO Lian
2005 Vol. 20 (6): 13431348
Abstract(
1952 )
PDF(1073KB)(
1390
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Sb2Se3 nanowires ([001] orientation) with a diameter of 100-200 nm and high aspect ratio were successfully synthesized at 180℃ for 10h by a facile non-aqueous polyol method, where home-prepared NaHSe alcohol solution was used as selenium source and PEG-400 served as an excellent solvent and structure director. The product was characterized by XRD, TEM, SAED, HRTEM, EDS and UV-Vis spectroscope, respectively. The effect of different polyols on the final product s morphologes was investigated. The results indicated that the PEG-400 played the key role in the crystal anisotropic growth and the non-aqueous polyol system provided a clean crystal growth condition.
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Preparation and Characterization of CaCO3 Nanowires
HAN Zhi-Hua,CAO Lin
2005 Vol. 20 (6): 13491352
Abstract(
2154 )
PDF(695KB)(
1270
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CaCO3 nanowires were synthesized from CaCO3 reagent by sol-gel process and thermal decomposition. The preparation of CaCO3 included two steps: In the first step, the wirelike intermediates containing Ca were synthesized by sol-gel process, which are with one dimension wire-like nanostructures; in the second step, the resulting samples were converted into CaCO3 nanowires by thermal decomposition. The diameter and length of the obtained nanowires are 50-80nm and up to 5μm separately. The nanowires are constited of self-assembled nanoparticles and they belong to the trigonal system.
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In Situ Coating Carbon Nanotubes with PbS Nanocrystals
SHAN Yan,GAO Lian
2005 Vol. 20 (6): 13531357
Abstract(
2241 )
PDF(556KB)(
1259
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A facile and effective method of in situ coating multi-walled carbon nanotubes (MWNTs) with PbS nanocrystals was introduced, which includes acid treatment of MWNTs, in situ introduction of sulfur precursor through the acid-base reaction between 2-mercatoethylamine and the -COOH groups on the surface of MWNTs and hydrothermal treatment in the following procedure. The samples were characterized by TEM, XRD and FTIR. TEM images showed that carbon nanotubes were nearly fully coated with a layer of PbS, and the coatine layer was 10~20nm in thickness. Atentative mechanism was proposed to explain the results.
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Synthesis and Characterization of Single-walled Carbon Nanotubes Using Catalysts Prepared by The Supercritical Drying Method
LUO Jun-Hang,ZHANG Xiao-Bin,LI Yu,CHEN Ji-Peng,LIU Fu
2005 Vol. 20 (6): 13581362
Abstract(
1957 )
PDF(510KB)(
1327
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The highly active Fe/Mo/Al2O3 catalyst with the large specific surface area was prepared by the supercritical drying method. The BET specific surface area of the as-prepared catalyst was increased from 294m2/g to 401m2/g. High quality single-walled carbon nanotubes (SWNTs) were synthesized by catalytic decomposition of CH4/H2 at 1000℃ using the catalyst. SEM, TEM, HRTEM, TGA and Raman spectroscopy were used to characterize the SWNTs. The content of SWNTs in the product propared is over 30wt%, which is much higher than that by using the conventional drying method, i.e. 2wt%. The mean diameter of the as-prepared SWNTs is in 0.8-1.0nm and they are usually bundles.
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Fabrication and Characterization of Highly Ordered Zinc Oxide Nanowire/Tube Arrays by Sol-Gel Template Method
YU Mei,LIU Jian-Hua,LI Song-Mei,WEI Wei
2005 Vol. 20 (6): 13631367
Abstract(
2518 )
PDF(888KB)(
1855
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Highly ordered zinc oxide nanowire/tube arrays were prepared by a sol-gel method in the pores of anodic alumina membranes (AAM). The morphology and crystalloid structure of zinc oxide nonawire/tube arrays were characterized by scanning electron microscope(SEM), transmission electron microscope (TEM) and X-ray diffraction (XRD). The results show that zinc oxide nonawires are very uniformly assembled and parallel to each other in the pores of the AAM template. The length and diameter of nanowires are dependen on the thickness and hole diameter of AAM. Zinc oxide nanotube arrays can be controlled by changing immersing time, temperature and concentration of the sol.
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Preparation of LiMn2O4 by Sol-Gel Method and Its Properties
LIU Su-Qin,LU Yan-Yan,HUANG Ke-Long
2005 Vol. 20 (6): 13681372
Abstract(
2232 )
PDF(487KB)(
1175
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Lithium manganese oxide, as a cathode material for Li-ion battery, was prepared by the sol-gel method with Ala as a chelating agent. The powder samples were confirmed to be a single phase LiMn2O4 by X-ray diffraction (XRD) studies. The textural properties of the powder samples were examined by scanning electron microscope (SEM), showing that the powders mainly consist of rod-shaped particles with uniform particle sizes. The synthesis mechanism of LiMn2O4 was preliminarily investigated by FT-IR and TG-DTA etc. Electrochemical properties of the sample were evaluated with charge and discharge tests. The results show that the samples have excellent electrochemical properties.
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Modified Small Punch Tests to Evaluate Ultimate Strength of PLZT Ceramics
XIONG Zhi,PENG Qing-Song,BAI Guang-Zhao,SHI Ying,JIANG Wan
2005 Vol. 20 (6): 13791384
Abstract(
2275 )
PDF(951KB)(
1266
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Modified small punch (MSP) tests were used to evaluate the ultimate strength of lanthanum-modified lead zirconate-titanate (PLZT) ceramics prepared by conventional mixed oxide (MO) method and mechanical alloying (MA) technique respectively. The MSP tests are very convenient for these two kinds of PLZT ceramics, poled or unpoled. Fracture surfaces were examined for the different MSP specimens; the dependence of mechanical and electrical properties of PLZT ceramics on microstructures was discussed in detail.
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Gas-sensing Properties of La0.68Pb0.32O3 Nano-materials under Low Operating Temperature
ZHANG Ling,HU Ji-Fan,QIN Hong-Wei,SONG Peng,JIANG Min-Hua
2005 Vol. 20 (6): 13851388
Abstract(
2063 )
PDF(169KB)(
1122
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The La0.68Pb0.32FeO3 sample with an orthogonal perovskite structure was prepared by using the sol-gel method. The gas-sensing properties were studied in CO gas. The experimental results reveal that the La0.68Pb0.32FeO3 sample shows smaller grain sizes, higher conductance and higher sensitivity to CO gas, especially the much lower operating temperature compared with LaFeO3 sample. The activation energy for La0.68Pb0.32FeO3 sample in CO gas is higher than that in air.
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Electrical Behavior of Nb-doped Bi4Ti3O12 Layer-structured Ferroelectric Ceramics
ZHANG Li-Na,LI Guo-Rong,ZHAO Su-Chuan,ZHENG Liao-Ying,YIN Qing-Rui
2005 Vol. 20 (6): 13891395
Abstract(
2086 )
PDF(680KB)(
1459
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Nb5+-doped Bi4Ti3O12 layer-structured ferroelectric ceramics were prepared by the solid-state reaction technology. Microstructures of Bi4Ti3-xNbxO12+x/2 materials were characterized by XRD and SEM. The results show that Bi4Ti3-xNbxO12+x/2 material has a single orthorhombic structure. The grains of polished and thermally etched surfaces reveal a needle-like structure. Electronic conductor mechanism of Bi4Ti3-xNbxO12+x/2 was analyzed by the Arrhe-nius fit of direct current conductivity vs temperature. Dielect constants of Bi4Ti3-xNbxO12+x/2 ceramics increase by Nb5+ doping. The Curie temperatures decrease linearly with the increase of Nb5+ concedntration. DSC results show that Bi4Ti3-xNbxO12+x/2 materials undergo the firstorder ferroelectric phase transition at the Curie point. Nb5+ doping Bi4Ti3O12 ceramics results in an increase remanent polarizatgion (Pr) according to ferroelectric test results. The reason is that Nb5+ substituting for Ti4+ decreases the concentration of oxygen vacancies. The effect of oxygen vacancies on domain pinning is reduced significantly.
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Structure and Photo Absorption Performance of Cu/WO3-TiO2 Photocatalyst
MEI Chang-Song,ZHONG Shun-He
2005 Vol. 20 (6): 13961402
Abstract(
2131 )
PDF(393KB)(
1384
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The solid material of coupled semiconductor WO3-TiO2, was prepared by a sol-gel method. The photocatalyst WO3-TiO2 supported metallic Cu was prepared by an isovolumic impregnation method. The surface structure, particle size and photo absorption performance of the materials were characterized by XRD, Raman, TPR, IR, TEM, XPS and UV-Vis. The experiment results show that 10wt%WO3 disperses on the surface of TiO2 support with one monolayer of non-crystalline phase, average particle size of 1wt%Cu/10wt%WO3-TiO2 is about 15nm. Blue shifting of photo absorption edges is observed clearly after the addition of WO3 on the surface of TiO2. The lattice WO3 forms and photo absorption performance decreases when the supporting amount of WO3 is more than that of the monolayer phase(>10wt%). The formation of bond W-O-Ti in the solid systems promotes the transfer of generating charge carriers between WO3 and TiO2. Loaded metalic Cu accelerates the transformation from the tetrahedrally coordinated W species to the octahedrally coordinated W species.
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Fabrication and Sustained Release Property of Nanostructured Hollow Silica Microspheres
YANG Xiao-Ling,YAO Ke,ZHU Yi-Hua
2005 Vol. 20 (6): 14031408
Abstract(
2419 )
PDF(691KB)(
2188
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Uniform hollow nanostructural hollow silica microsphers were produced by the layer-by-layer electrostatic self-assembly technique. The core-shell microspheres were constructed by alternately depositing positive polyelectrolyte PDDAMAC and silica nanoparticles (10nm, 20nm) onto the polystyrene PS microspheres which were used as the colloidal templates, then the templates were decomposed by calcination and hollow mesoporous silica microspheres come into being. TEM show monodispered silica microspheres have spherical void. XRD analyses indicate that crystallization degree of silica is nearly the same after heating treatment, which still maintain an amorphous from. The measurements of N2 adsorption-desorption isotherms yield the surface area of the hollow spheres assembled of silica with a diameter of 10 or 20nm are 282.71m2·g-1 and 158.17m2·g-1, and the average pore diameters of them are 11nm and 15nm respectively. The permeability and sustained release property of hollow silica sphere were also confirmed by the experiments of dye loaded and released.
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Batch Preparation of TiO2 Hollow Spheres by Templating Against PSA-A Latex
HAN Chun-Rui,LU Wei-Li,WU Xiu-Yong,FU Xun,HU Zheng-Shui
2005 Vol. 20 (6): 14091416
Abstract(
2123 )
PDF(1013KB)(
1232
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With Ti(SO4)2 as raw material, and water as dispersion medium, the PSA-A latex/titanium hydrolysis compounds core-shell microspheres were prepared by templating against PSA-A latex with carboxyl. The TiO2 hollow spheres of 450nm were obtained by calcining the as-prepared core-shell microspheres. TG-DSC, SEM, TEM, IR and XRD measurements were used to characterize the samples. The investigations of the core-shell formatting process and the effect of experimental conditions on pH value changes indicated that the varing rate of pH value was the determining factor for a successful coating. The optimum varing rate of pH value for core-shell microspheres formation was obtained and TiO2 hollow spheres were prepared in batches under the conditions of 230g/L PSA-A latex and 1mol/L Ti(SO4)2.
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Electro-chemical Detachment Process of Through-hole Porous Anodic Alumina Membrane
GAO Lu-Mei,WANG Pang-Pang,WU Xiao-Qing,SONG Xiao-Ping
2005 Vol. 20 (6): 14171422
Abstract(
2143 )
PDF(1035KB)(
1404
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A well-ordered porous anodic alumina (PAA) membrane was achieved by anodic oxidization of the aluminium electrode at constant voltages of 30-50V in a solution of 0.3mol·L-1 H2C2O4. A new electrical detachment process was carried out to detach the PAA membranes from aluminium base in the solution of HClO4 and CH3OH. The mechanism of the electrical detachment process and the factors of the pore diameter and thickness of the barrier layer were researched. A larger size of PAA (2cm×2cm) was obtained with thickness of 30-100μm and full-controlled open-hole pores. Compared with reported chemical process, the present method is nore simple and rapid and free of metal ions residuce. It is important for research of nanostructure assembling techniques.
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Synthesis of Mesostructured Material with Pore Wall Composed of the Primary Structure Units of Zeolite through the Dissolution of Zeolite
ZHANG Ying,DOU Tao,LI Yu-Ping,SHI De-Xian,ZHAO Zhen
2005 Vol. 20 (6): 14231430
Abstract(
2077 )
PDF(477KB)(
1387
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Mesostructured materials MSB and MSZ with the pore walls respectively composed of the structure units of zeolite β and ZSM-5, were successfully synthesized by a new method in which the silica-alumina precursors obtained through the dissolution of zeolites, assemble around the surfactant micelle of triblock copolymer EO20PO70EO20. Subsequently, the products are characterized by XRD, IR, TEM, N2-sorption, EDS and 29Si MAS NMR techniques. In the IR spectra of MSB and MSZ, the appearance of absorbance peaks characteristic of five-membered rings of zeolites in the range of 550~600cm-1 indicates that the primary structure units of zeolites are perhaps included in the pore walls of MSB and MSZ. N2 sorption data show that the pore walls of as-synthesized mesostructured materials are thicker than that of SBA-15. 29Si MAS NMR spectra of MSB and MSZ suggest the presence of Si-O-T(T=Si,Al) environments similar to those in zeolites. The hydrogenation dealkylation reaction of heavy aromatic on the MSB and MSZ shows higher conversion than the corresponding data on SBA-15, especially for MSB80 with the conversion difference as high as 9.78%. Thus, it is concluded that the pore walls of MSB and MSZ contain the primary structure units of zeolites.
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Development of Reticulated Porous Ceramics by Two-step Centrifuging Processing
PU Xi-Peng,QIU Fa-Gui,LIU Xue-Jian,HUANG Li-Ping
2005 Vol. 20 (6): 14311437
Abstract(
2287 )
PDF(765KB)(
1620
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Silicon nitride reticulated porous ceramics with controlled structure were fabricated by a two-step centrifuging processing, using polyurethane sponge as the template. According to the TG-DSC analysis of the template, the pyrolysis schedule was decided. Effects of centrifuging processing and viscosity on the loading content of slurry on the sponge and macrostructure of porous ceramics were studied. The structure and bond strength of the reticulated porous ceramics were also reported. Compared with the roll-press processing, the reticulated porous ceramics fabricated by the tqo-step centrifuging processing have higher slurry loading, more uniform structrue and higher bending strength.
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Preparation and Structure Characterization of Mesophase Pitch-based Carbon Foam
LI Tong-Qi,WANG Cheng-Yang
2005 Vol. 20 (6): 14381444
Abstract(
2215 )
PDF(1694KB)(
1969
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Green foams were prepared from a petroleum-derived mesophase pitch by using the size-restriction foaming method and the foams were further oxidized, carbonized and graphitized, consequently carbon foams with excellent cell structure were obtained. SEM and XRD were used to observe the morphologies and analyze the structures of foams. The results show that the cell size can be altered by controlling the free space in mold. During carbonization and consequently graphitization of foams, cell diameter reduces and the orientation of molecules in cell walls improves, approaching that of graphite. The walls of foam cells are built up by even ones and “Y” type junctions. The former has better molecular orientation than the latter. In is also found that the foam with large cells will have more close-grained molecular arrangement, but the crystallites in them are smaller.
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Microstructure and Properties of Al2O3-TiC Composites Fabricated by Combination of High-energy Ball Milling and Spark Plasma Sintering (SPS)
ZHANG Yan-Feng,WANG Lian-Jun,JIANG Wan,CHEN Li-Dong
2005 Vol. 20 (6): 14451449
Abstract(
2067 )
PDF(690KB)(
1352
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Aluminothermic reactive synthesis of Al2O3-TiC nanocomposite powders from a mixture of TiO2, Al, and C powders induced by high-energy ball milling and its consolidation through spark plasma sintering (SPS) were investigated. After being milled for 3h at ambient temperature, the powder mixtures reacted and homogeneous nanosized TiC and Al2O3 particles formed. The as-milled powders were consolidated by SPS technique in vacuum at 1450℃ for 4min under 50MPa, and the density of the as-sintered samples reached 99.6% of theoretical density. The final products showed fine microstructure, and most of the grain sizes of both Al2O3 and TiC nwere less than 1μm, and exhibited excellent properties: a flexural strength of 650±21MPa, a hardness of 19.1±0.2GPa, a fracture toughness of 4.5±0.2MPa·m1/2, and an electrical conductivity of 2.3828×105Ω-1·m-1.
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C/C Composites Fabricated by the Chemical Liquid Phase Vaporization Densification with the Catalyst
LI Jin,CHEN Zhen-Hua
2005 Vol. 20 (6): 14501456
Abstract(
2098 )
PDF(1066KB)(
1502
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This paper reported on an improved technique of the chemical liquid phase vaporization densification process for C/C composites preparation, based on the calefaction with the impulse inductive of the preform that was from the felt impregnated with the liquid phase pitch followed by carbonization. The pyrocarbon was yielded and deposited by the pyrolysis of the kerosene as the precursor at 800-1000℃ with ferrocene as the catalyst, and the density of the preform was increased from 0.3g/cm3 to 1.5-1.7g/cm3 in 3h. The relationship between the densification and the condition of the reaction process, the microstructures of the pyrocarbon and the function of the catalyst were examined by a metallography microscope.
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Influence of Interfaces on Mechanical Behavior of C/C Composites by CLVI Processing
SUN Wan-Chang,LI He-Jun,LU Jin-Hua,BAI Rui-Cheng,HUANG Yong
2005 Vol. 20 (6): 14571462
Abstract(
2795 )
PDF(1497KB)(
67318
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C/C composites were fabricated by a rapid chemical liquid-vaporized infiltration (CLVI) processing. The fractured surfaces were observed by scanning electron microscope (SEM). In this paper, three types of interfaces in the composites, the fiber-matrix interface within a tow, the interface between carbon cloths or bundles, as well as the interface between pyrocarbon laminar, were discussed. Moreover, their influences on mechanical behavior of the composites were analyzed. In order to obtain high strength and pseudoductility, it is necessary for C/C composites to have proper interface bond strength between fiber and matrix, smaller residual pores between carbon cloths or bundles, and proper gaps between pyrocarbon laminar within the matrix.
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Advances in the Synthesis of Large-area 3D Ordered Macroporous Titania Film Photonic Crystals by Silica Colloidal Crystal Templating
HU Xing-Fang,KUAI Su-Lan,YU Yun,TROUNG Vo-Van
2005 Vol. 20 (6): 14631466
Abstract(
2085 )
PDF(477KB)(
1663
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The recent advances of the authors’ study on the synthesis of large-area 3D ordered macroporous titania film photonic crystals by using silica colloidal crystals as templates were presented. The main procedure of the preparation was described as follows. Firstly, the silica colloidal crystal template was deposited onto a glass micro slide through a convective assembly process in which monodispersive silica spheres of 309nm were used. Secondly, after sintered at 600℃ for 1h the crystalline template was immersed vertically into a TiO2 sol for the infiltration of the template. Thirdly, the resulting titania-opal composite film was immersed in an aqueous NaOH solution for 24h to remove the silica template. By means of the systematical study of the processes and application of some innovative processing techniques such as silica colloidal crystal templating technique, alkali based template-etching technique, the highly ordered macroporous TiO2 film photonic crystals with sizes of centimeters were successfully fabricated. The results show that the shrinkage of the macroporous framework with a filling rate of 17.4% is less than 3%. The XRD pattern shows that the porous framework consists of nanocrystallites of anatase mixed with a magnéli phase (Ti5O9). The optical property measurements of the films indicate that the film photonic crystal has strong photonic bandgap behavior.
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Influence of Fe~3+ Doped on Phase Formation and the Oxygen Sensitivity of TiO2 Oxygen Sensitive Thin Films Prepared on Silicon Substrate by Sol-Gel Method
ZHANG Ai-Fang,DU Pi-Yi,HU Yue-Hua,WENG Wen-Jian,HAN Gao-Rong
2005 Vol. 20 (6): 14671474
Abstract(
1982 )
PDF(992KB)(
1356
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The Fe3+ doped TiO2 oxygen sensitive thin films deposited on single crystal silicon substrates were prepared by a sol-gel method. The phase structure of the thin films was measured by X-ray diffraction (XRD). The morphologies were observed by scanning electron microscope (SEM). The results showed that the anatase phase appeared with a small grain size dispersed homogeneously in the thin film. The rutile phase appeared with a morphology of special clustered grains and large sizes in the thin film. It was exhibited evidently that the formation of the rutile phase in the thin film on a single crystal substrate was dependent on Fe3+ doping in the system. The formation temperature was about 100℃ lower with 3mol% Fe3+ doped than that without Fe3+ doping. The largest content of the rutile phase appeared in the thin film while Fe3+ doping of about 6mol%. In addition, the crystal lattice of both the anatas phase and the rutile phase decreased with the substitution of a small size of Fe ions for a large size of Ti ions when doping Fe ions concentrantion below 6mol%. As Fe ions doped was above 6mol%, the c axis of the rutile phase increased while the c axis kept almost constant with the increase of Fe and thus both oxygen vacancy and structure distortion increased. The oxygen sensitivity of Fe doped TiO2 thin films was controled by the concentration of the oxygen vacancies and the content of the rutile phase in TiO2 thin films.The rutile phase and the sensitivity in the Fe doped TiO2 thin film showed maximum while Fe doping was 6mol%, and its oxygen sensitivity was 19 times more than that of the TiO2 thin film with 3mol% Fe doped.
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Pulsed Laser Deposition of MgO Films and Its Crystallinity
CHEN Tong-Lai,LI Xiao-Min,ZHANG Xia,GAO Xiang-Dong,YU Wei-Dong
2005 Vol. 20 (6): 14751480
Abstract(
2010 )
PDF(0KB)(
2306
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Systematic investigation of preparation-parameter dependence of MgO films’ crystallinity during pulsed-laser depositon of MgO films was carried out. It is found that MgO films’ crystallinity is mainly affected by substrate temperature and laser fluence, while the growth velocity of MgO films is dominated by pulse frequency, substrate-target distance and laser fluence. By comparison of the influence of metallic Mg target and sintered MgO target on the films’ cystallinity, it also found that, via inserting a TiN seed layer, the crystalline quality of MgO films can be greatly improved. Finally, under the optimal preparation-parameter conditions: TS=873K, DE=7J/cm2, DST=70mm, FL=5Hz, employing sintered MgO target and inserting a TiN seed layer, atomically smooth MgO films grown with layer-by-layer mode can be successfully obtained.
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Eifect of AIN on the Structure and Magnetic Properties of FePt Thin Films
LI Xiao-Li,XU Xiao-Hong,WU Hai-Shun
2005 Vol. 20 (6): 14811487
Abstract(
1951 )
PDF(322KB)(
1203
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FePt(50nm) and [FePt(2,3,5nm)/AlN(1nm)]n films were prepared by RF magnetron sputtering technique, then annealed at 550℃ for 30min. The effect of the number of bilayer repetitions (n) and AlN content on structure and magnetic properties of various FePt/AlN multilayers was studied. The highest coercivity and squareness of FePt/AlN multilayers annealed at 550℃ were obtained for n=8. The grain size of the FePt/AlN films by post-annealing increases with increasing n. Introducing the nonmagnetic AlN not only hinders the growth of FePt particles, but also reduces the intergrain exchange interactions of the FePt/AlN films. And the interactions are decreased as AlN content is increased. Grain size (Vgrain) has almost the same size as magnetic activation volume (V*) due to the addition of AlN in films by post-annealing.
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ZSM-5 Zeolite Membranes Prepared on Porous α-Al2O3 Tube from a Template-free Crystallization Gel
CHENG Yue,WANG Lian-Jun,LI Jian-Sheng,SUN Xiu-Yun,LIU Xiao-Dong
2005 Vol. 20 (6): 14881492
Abstract(
2067 )
PDF(593KB)(
1331
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ZSM-5 zeolite membranes synthesized on rough porous α-Al2O3 tubes with an average pore size of 2μm in the absence of organic template crystallization gel were investigated. The molar composition of nanosized ZSM-5 seeds was 9TPAOH: 25TEOS: 0.25 Al2O3: 480H2O. Porous α-Al2O3 tubes were seeded with these colloidal TPA-silicalite-1 crystals with a size of 90~100nm. The seeded supports were calcined in accordance with DTA/TG of nanosized ZSM-5 and treated in a synthesis sol-gel to grow the seed crystals into ZSM-5 membranes on the outer surface of porous α-Al2O3 tubes. The molar composition of the crystallization gel without organic templates was 67Na2O:Al2O3: 240SiO2: 6000H2O. XRD patterns show that the film consists of well-crystallized ZSM-5 zeolite. SEM investigation indicates that the zeolite films on the supports are defect free and that the film thickness is approximately 8μm. The permeability for H2 is 1.50×10-6mol$·m-2·s-1·Pa-1 and the ideal separation factor for H2/N2 is about 3.85.
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Preparation of Alumina Coatings on Titanium by Cathodic Micro-arc Electrodeposition
LI Xin-Mei,LI Yin-Suo,HAN Yong State
2005 Vol. 20 (6): 14931499
Abstract(
2112 )
PDF(679KB)(
1402
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An alumina coating with a thickness of 100μm on a titanium substrate was prepared by cathodic micro-arc electrodeposition. The microstructures and phase compositions of the coating at different voltages were studied, and the growth mechanism of the coating was analyzed. The results show that the coating grows by the following steps: the stage of no electric spark, micro-arc discharge and local arc light. In these courses Al(NO3)3 is dissociated and Al(OH)3 is deposited and dehydrated. The high temperature and pressure produced in micro-arc area are keys to the formation of the alumina coating. The coating is mainly composed of γ-Al2O3 and α-Al2O3. The content of α-Al2O3 is increased with increasing voltage, which amounts to 7% at 400V.
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Microstructure and Nanoindentation Mechanical Properties of Detonation Sprayed Coatings Derived from Al2O3/TiO2 Nanocomposite Powders
ZHAI Chang-Sheng,YANG Li,WANG Jun,ZHAO Wen-Ming,SUN Bao-De
2005 Vol. 20 (6): 15001508
Abstract(
2126 )
PDF(1268KB)(
1368
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This paper researched the microstructrue and nanoindentation mechanical properties of detonation sprayed coatings derived from Al2O3/TiO2 nanocomposite powders. The pores of the nanocomposite coating (NCC) appeared to be generally equal-sized and showed a very homogeneous distribution, while the conventional microcomposite coating (MCC) appears an inhomogeneous pore distribution. The results also indicate that NCC has better chimerism between splat interfaces than MCC and more homogeneous melting condition. A mass of grain boundaries, sub-boundaries and nanosized microcracks in NCC lead the matrix Al2O3 to be nanoparticulate, while a mass of unmelted particles can be detected in MCC. Both of Al2O3/3wt%TiO2 nanocompsite and conventional coatings exihibit apparently anisotropic nanoindentation mechanical behaviors, which are due to the anisotropic microstructure of the as-sprayed coatings. The mean values and distribution intervals of both nanoindentation hardness and Young’s modulus of NCC are higher than those of corresponding surface and cross section of MCC. Therefore, NCC exhibits better nanoindentation mechanical properties than MCC, which is due to the reinforcing effect of TiO2 nanoparticles on the matrix Al2O3 particles of NCC.
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Preparation and Laser Ablation Test of Vacuum Plasma Sprayed Boron Carbide Coatings
ZHENG Xue-Bin,JI Heng,HUANG Jing-Qi,ZENG Yi,DING Chuan-Xian
2005 Vol. 20 (6): 15091514
Abstract(
2271 )
PDF(859KB)(
1434
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Boron carbide coatings were deposited onto stainless steel via vacuum plasma spraying (VPS), and then their phase composition, microstructure, deposition efficiency, bonding strength and laser irradiation resistance were examined. Results obtained show that there is no distinct B2O3 in the VPS B4C coating, indicating that the oxidation of B4C can be avoided during VPS process. The denser B4C coating can be obtained by using the finer original powder. Deposition efficiencies and bonding strengths of coatings are higher in the cases of higher spray power and higher H2 flow due to the better melting condition of powders during spray process. Under appropriate spray parameters, the deposition efficiency and bonding strength of VPS B4C coating can be high to 72% and 49MPa respectively. Laser ablation test shows that the laser irradiation resistance is improved significantly for stainless steel after being deposited by B4C coating.
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