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Low Melting Temperature Machinable Bioactive Glass-ceramic
QIN Xiao-Mei,XIU Zhi-Meng,ZUO Liang,LI Song
2003 Vol. 18 (6): 11581162
Abstract(
2386 )
PDF(1306KB)(
1285
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A basic composition of SiO2-MgO-Al2O3-K2O-CaO-P2O5-F glass system was selected,
and different contents of ZnO were added. The melting results show that the addition of ZnO can reduce the melting temperature of the glass
from 1450℃ to 1300℃. Thus, the transparent as-cast glasses of the machinable bioactive glass ceramic can be obtained at the lower temperature.
The main phases of the glass ceramic are mainly mica phase and apatite phase after crystallization. Microstructure of the glass ceramic is petaloid-like.
The fracture of the glass ceramic is transgranular and some crystals are drawn and this feature makes the glass ceramic show high strength. The glass ceramic
also has good machinability due to the existence of mica phase.
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Effect of Fluorine on the Crystallization of Li2O-Al2O3-SiO2 Glasses
HU An-Min,LIANG Xai-Ming,GU Shou-Ren
2003 Vol. 18 (6): 11631168
Abstract(
2012 )
PDF(672KB)(
1504
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The nucleation and crystallization behavior of Li2O-Al2O3-SiO2 glasses with varied amounts of Fluorine content were investigated by the differential thermal analysis (DTA), X-ray diffraction (XRD) and the scanning electron microscopy (SEM). The results show that with the increase of the fluorine concentration, the crystallization peak temperature (Tp) decreases, the crystallization activation energy (E) decreases, the Avrami exponent (n) increases. The onset of the precipitation of LixAlxSi1-xO2 crystal and its transformation to β-spodumene all shift to lower temperature and the grain size increases with the fluorine added. The values of the Avrami exponent (n) and the crystallization activation energy (E) agree well with the scanning electron microscopy observation of equivalent axis grain crystal. The results suggest that the fluorine promotes the initial crystallization and ion diffusion in the glass system.
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Thermodynamic Analysis on the Post-crystallization for Calcium Titanium Phosphate Glass Ceramics
WANG De-Ping,HUANG Wen-Hai,ZHOU Nai
2003 Vol. 18 (6): 11691176
Abstract(
1923 )
PDF(489KB)(
1475
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Porous glass ceramics with CaTi4(PO4)6 as the main crystalline phase could be produced by heat-treating the 5Na2O-20TiO2-32P2O5-43CaO glass system at 690℃ and 735℃ separatively and then by acid-leaching the crystallization product Ca3(PO4)2. In this paper, a method of enlarging the size of pores was introduced. A high temperature heat-treatment (880℃), that called post-crystallization, could be inserted into the processes between crystallization and acid-leaching. In the post-crystallization, there was a solid reaction where the CaTi4(PO4)6 and 5Ca3(PO4)2 reacted and then products TiO2 and Ca2P2O7 produced. The later phase could be easily leached from the glass-ceramic. The pores became larger, since more Ca and P were leached. In the present study, the change in free enthalpy of the solid reaction was estimated as --333Kcal/mol by applying the approximate first thermodynamic equation. The phase analysis, XRD before and after post-crystallization, confirmed that this solid reaction could happen spontaneously. The dynamic parameters for crystallization activation energy and reaction index were calculated as 584.7kJ/mol and 3.2 respectively by applying Johnson-Arirami-Mehl equation while implied that the sample was crystallized in bulk. This calculation was also confirmed by the observation under SEM, that the pore size enlarged in the whole area of the sample after post-crystallization.
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On the Structure and Nature of Glass
ZHU Pei-Nan
2003 Vol. 18 (6): 11771180
Abstract(
2098 )
PDF(275KB)(
1285
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The author reveiws the works on study of the structure and nature of glass, done by the author and his colleagues,
in the past 20 years. Some important conclusions indicated that glass as the non-crystalline solid, its structure may contain two types of agglomerated
atoms or atomic groups, i.e., disorder groups and ordered orientated (one dimensionally prefered) groups. In addition, a little quantity (negligible)
of nano-crystals may appear as a particular role in real glass and this characteristic may distinguish it from ideal glass. A table is shown for
interpretating more briefly. A schematic diagram of fused silica glass structure is designed by the author and provided here, so, it may express the stucture and nature of
glass with its reasonable scientific recognition.
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Optical Characteristics of C/0.5Al2O3-0.5P2O5-100SiO2 Gel Glasses Prepared at Different Temperatures
YANG He-Qing,WANG Xuan,ZHANG Bang-Lao,LI Yong-Fang,FANG Yu,ZHANG Liang-Ying,YAO Xi
2003 Vol. 18 (6): 11811186
Abstract(
2314 )
PDF(448KB)(
1086
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0.5Al2O3-0.5P2O5-100SiO2 gels containing organic group (OC2H5) were synthesized through partial hydrolysis of alkoxide. The gels were calcined at 300~700℃ in N2 atmosphere, in which-OC2H5 was carbonized to form carbon nanoparticles with various sizes. Their absorption and photoluminescence spectra were measured. The absorption edge shifts to the higher-energy side as the size of the carbon particle decreases. This phenomenon was interpreted in terms of a quantum confinement effect of electron and hole in the carbon nanoparticles. The gel glasses doped with carbon nanoparticles show a strong and broad room-temperature photoluminescence with a peak located around 586nm under the excitation of 532nm line of a Nd:YAG laser. The position of photoluminescence peaks shifts hardly with changing the size of carbon nanoparticles. The photoluminescence spectra are originated from the surface of carbon nanoparticles or interfacial layer between it and gel matrix. The carbon nanoparticles are amorphous carbon nanoparticle in the gel glasses by the X-ray diffraction, high-resolution transmission electron microscopy and Raman spectra.
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Effect of Composition on the Tendency of Forming BAS (Barium Aluminosilicate) Sintered Glass by Sol-Gel Process
YANG Jue-Ming,ZHOU Wan-Cheng,BAO Xiao-Ping,CHEN Ping
2003 Vol. 18 (6): 11871191
Abstract(
2046 )
PDF(449KB)(
1197
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The effect of composition on the tendency of forming BAS (barium aluminosilicate) sintered glass with compositions near the theoretical composition of
barium feldspar by sol-gel process was studied by XRD, SEM and Raman spectrum. Results indicated that, in the experimental range, larger SiO2 content and larger
BaO/Al2O3 ratio were advantageous to glass formation. Increasing BaO/Al2O3 ratio causes an increase in the amount of alumina with [AlO4] structure. The
relationship between [AlO4]/Al3+ and BaO/Al2O3 can be expressed as a linear equation. A criterion for glass formation in the studied system was established. The
criteron showed good fitness with the experimental results.
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Low Temperature Sintering of Bimodal Alumina Powder Mixtures with Nanocrystalline Component
LI Jiang,PAN Yu-Bai,NING Jin-Wei,HUANG Li-Ping,GUO Jing-Kun
2003 Vol. 18 (6): 11921198
Abstract(
2360 )
PDF(992KB)(
1623
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Nanocrystalline α-Al2O3 powder was prepared by a wet-chemical method calcining the dry NH4Al(OH)2CO3 precursor synthesized from NH4Al(SO4)2 and NH4HCO3. Alumina ceramics were fabricated by pressureless sintering process at 1450℃ from bimodal alumina powder mixtures with the prepared nanocrystalline component using MgO and SiO2 as additives. The effect of nanocrystalline α-Al2O3 component on alumina ceramics was also studied. The materials fabricated have better mechanical properties.
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Optimization Study on the Rheological Behavior of Alumina Suspensions
LIU Yang-Qiao,GAO Lian
2003 Vol. 18 (6): 11991204
Abstract(
2299 )
PDF(630KB)(
1486
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The influence of various polyelectrolyte dispersants on the rheological properties of sub-micron alumina suspensions was investigated. Stable 58vol% alumina suspensions suitable for casting was prepared by optimizing the factors including pH, dispersant type and amount, etc. Green compacts with homogeneous microstructures were obtained by the gel casting method. Finally, Al2O3 bodies sintered at 1600℃for 2h, with a relative dencity more then 98% were fabricated.
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Application of Silica Sol-Gel in Colloidal Forming of Ceramics
LUO Jie-Sheng,XIE Zhi-Peng,MA Jing-Tao,HUANG Yong,CHENG Yi-Bing
2003 Vol. 18 (6): 12051209
Abstract(
2447 )
PDF(474KB)(
1700
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A novel colloidal forming processing of ceramics was investigated. The characteristic of silica sol-gel was applied successfully to colloidal forming of ceramics. The process is based on the casting of the slurry, containing powder and silica sol prepared by hydrolysis of tetraethoxysilane (TEOS) at pH 12.8. Then the mixture forms gelled parts through silica sol-gel. Ceramic green parts with strength of 5MPa can be obtained by this method. The forming process has advantages of low toxicity and high consolidation rate.
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Preparation of Nano-TI(C,N) Reinforced Ti(C,N)-based Cermets
XU Zhi-Mou,YI Xin-Jian,HU Mao-Zhong,XU Shang-Zhi
2003 Vol. 18 (6): 12101216
Abstract(
2179 )
PDF(745KB)(
1390
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Ti(C,N)-based cermets were produced by using nanopowders of Ti(C,N). The effects of sintering temperature, holding time and rate of raising temperature on the properties of Ti(C,N)-based cermets containing 10wt% nanopowders of Ti(C,N) were studied. An optimum process of preparating cermets was obtained. It was the sintering temperature of 1450℃, holding time of 75min and rate of raising temperature of 3℃/min. The tensile strength was improved about 36.7% by using the process. The reinforcing mechanisms were considered chiefly to be grains refining, distributing and solution.
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Research on Ternary Boride Based Cermet
WANG Yong-Guo,LI Zhao-Qian,ZHANG Di
2003 Vol. 18 (6): 12171221
Abstract(
1860 )
PDF(459KB)(
1354
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Ternary boride based cermet (TBBC) was produced successfully by using the reaction liquid sintering method under 1280℃ and vacuum. The hardness, density and coefficient of thermal expansion of TBBC are 92.4HRA, 8.2g/cm3 and 8.0×10-6/K respectively. The microstructure of TBBC was studied by using SEM, XRD and EDS. Results show that the main composition of TBBC is ternary-boride-based hard phase and ferrous-base binder phase. TBBC has excellent wear resistance performance.
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Fabricating Transparent Yttria Ceramics at Low Temperature
WANG Jie-Qiang,ZHENG Shao-Hua,YUE Yun-Long,TAO Zhen-Dong,SUN Xu-Dong
2003 Vol. 18 (6): 12221228
Abstract(
1936 )
PDF(682KB)(
1339
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A new method for obtaining highly sinterable Y2O3 powders was developed. Those powders were used to prepare transparent bodies with conventional sintering at relatively low temperature. Yttrium nitrate was used as a mother salt, and ammonia as a precipitant reagent, the fine and dendritic precursor crystal was prepared by controlling the content of sulfate ions in the reaction system. The highly pure and low-agglomerated Y2O3 powders were obtained by calcinating the precursor at 1100℃, the primary particles were spherical and about 60nm in diameter. The powder compact pressed in steel die could be sintered to transparency without additives under vacuum at 1700℃. The sintered transparent Y2O3 polycrystalline exhibited a homogeneous microstructure and its transmittance was up to 70% in the near infrared wavelength region.
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Synthesis and Electrochemical Performance of Li1+xV3O8 as Cathode Material for Lithium Secondary Batteries
GAO Jian,JIANG Chang-Yin,YING Jie-Rong,WAN Chun-Rong
2003 Vol. 18 (6): 12291234
Abstract(
1785 )
PDF(778KB)(
1213
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A novel technique was studied to prepare Li1+xV3O8 as cathode material for lithium secondary batteries. V2O5 sol was prepared via a “quencher” method by NH4VO3 as raw material. Then it was mixed with LiOH solution. The spherical precursor was obtained by a spray drying method. The Li1+xV3O8 powders were synthesized by sintering the spherical precursor. DTA/TGA were employed to analyze the precursor. The investigation of XRD, SEM and the determination of the electrochemical properties show the particles obtained by sintering at 350℃ for 24h are fine, spherical, narrowly distributed and well crystallized. The resultant material also has excellent electrochemical properties with an initial discharge specific capacity of 378 mAh·g-1, and the discharge specific capacity of the 10th cycle is 312mAh·g-1.
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Defect State in Grain Boundary of Ba0.92Ca0.08Ti1.02O3 Ceramics with Low Room Temperature Resistivity
CAO Ming-He,YUAN Jun,ZHOU Dong-Xiang,GONG Shu-Ping
2003 Vol. 18 (6): 12351239
Abstract(
1974 )
PDF(397KB)(
1322
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The distribution of elements on the grain boundaries of Ba0.92Ca0.08Ti1.02O3 ceramics with low room temperature resistivity was studied by TEM combined with EDS. The point defects in the grain boundaries were also analyzed. The results show that the point defects in the grain boudaries of Ba0.92Ca0.08Ti1.02O3 ceramics with low room temperature resistivity mainly include Mn"Ti, Mn'Ti or Al'Ti, and V"Ba.
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Microstructure and Dielectric Tunable Properties of Al_2O_3-doped Barium Strontium Titanate in the Paraelectric State
LIANG Xiao-Feng,WU Wen-Biao,MENG Zhong-Yan
2003 Vol. 18 (6): 12401244
Abstract(
1974 )
PDF(690KB)(
1225
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Al2O3-doped Ba0.6Sr0.4TiO3(BST) ceramics were prepared by using conventional ceramic technology. The samples were analysed by SEM and XRD. The results indicate that Al3+ behaves as a grain-growth helper below a certain doping level and also the dopants have entered the unit-cell maintaining the perovskite structure of the solid solution. The dielectric constant and dissipation factor decrease and the tunability increases by addition of Al2O3. The specimen at doping level of 0.8wt% has the optimal overall dielectric properties.
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Preparation of Superionic Conducting Amorphous Materials with High Concentration of Silver Ions
PENG Hui-Fen,GU Nan-Ju,MACHIDA Nobuya,SHIGEMATSU Toshihiko
2003 Vol. 18 (6): 12451249
Abstract(
1978 )
PDF(327KB)(
1250
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High-energy ball-milling process is a powerful method for the preparation of amorphous phases, nanocrystalline materials, and so on. In this paper, we applied the high-energy ball-milling process to the synthesis of superionic conducting amorphous materials with Ag2S content of 80 mol%. Ball milling of 12h to 20h led to the formation of amorphous phases in the composition. The amorphous samples showed very high ionic conductivities, among which the 20h-ball-milled sample presented the maximum conductivity of 2.96×100Sm-1 at 298 K. Further ball milling resulted in partial precipitation of Ag8SiS6 crystalline phase, therefore, a decrease in ionic conductivity was observed for the samples ball-milled for longer than 27h. DC polarization measurements suggested that the ion transport number of the amorphous samples and the ball-milled samples containing some Ag8SiS6 crystalline phase, together with that of the Ag8SiS6 crystal, was practically unity.
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Surface Modification and Characterization of Al2O3 Micropowder
YU Zhi-Qiang,WU Gao-Hui,SUN Dong-Li,JIANG Long-Tao
2003 Vol. 18 (6): 12501254
Abstract(
1922 )
PDF(660KB)(
1493
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α-Al2O3 micropowder with the even coating of Y2O3 was obtained in such an experiment by using α-Al2O3 powder as base material and Y(NO3)3 solution as coating phase through the liquid phase coating method. The aluminium matrix composite reinforced by α-Al2O3 particles modified by Y2O3 was fabricated. The microstructure of the composite is more even. The mechanical properties testing indicates that the strengthening effect of the modified-Al2O3 porticles on the Al alloy is improved obviously and the tensile strength of the composites increases by 27.2%, yield strength increases by 33.1%, and the elongation increases by 10.3%.
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Sb-doped ZnO Nanoparticles Prepared by Vapor-phase Oxidation
ZHU Bai-Lin,ZENG Da-Wen,XIE Chang-Sheng,HU Mu-Lin,SONG Wu-Lin
2003 Vol. 18 (6): 12551260
Abstract(
2133 )
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1232
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Pure and Sb-doped ZnO nanoparticles were obtained by vapor-phase oxidation from Zn-Sb alloy with different mole ratios as the raw material at the same experimental condition. The morphology, structure and chemical state were investigated by TEM, XRD, HRTEM and XPS. With an increase in content of Sb in raw materials, the shape of nanoparticles varying from tetrapod-shaped whisker, rod-liked, quadrangle to hexagon was observed by TEM. HRTEM image of the regularly hexagonal nanoparticles indicates the distance between (1100) planes neighbouring in the Sb-doped ZnO nanoparticles with wurtzite structure is larger than that of the undoped ZnO nanoparticles reported in literature. The XPS result clearly shows that Sb element has been doped into the ZnO nanoparticles, although the XRD patterns of the as-synthesized nanoparticles reveal that there is not second phase except ZnO. The forming mechanism of tetrapod-shaped ZnO nanoparticles and the effects of Sb on morphology of nanoparticles were discussed.
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Surface Morphology, Spectra and Photocatalytic Bactericidal Effect of Chlorophyll-Sensitizing TiO2 Crystalline Phases
LI Min,WANG Zhen-Ling,SHI Heng-Zhen,ZENG Yi
2003 Vol. 18 (6): 12611266
Abstract(
1886 )
PDF(421KB)(
1297
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Different crystalline TiO2 films prepared by the sol-gel method were modified by employing chlorophyll as the sensitizer, and characterized by XRD, AFM, UV-vis absorption spectra and Fluorescence emission spectra. The activity of killing the pathogenic bacteria of cabbage soft rot on chlorophyll-sensitized TiO2 film was investigated. The results show that three TiO2 nanocrystalline particles of anatase, mixed-crystalline and rutile sensitized by natural chlorophyll can effectively kill pathogenic cabbage-soft-rot bacteria under visible light.
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Preparation of NiO/SiO2 Composite Catalysts by Hydrothermal Methods and Its Application to Carbon Nanotubes Synthesis
ZHU Yan-Juan,DENG Shu-Hua,YI Shuang-Ping,ZHONG Shao,CHEN Yu-Lian,HE Yan-Yang,ZHANG Hai-Yan
2003 Vol. 18 (6): 12671272
Abstract(
2592 )
PDF(876KB)(
1250
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The binary colloid (Ni(OH)2/SiO2) was prepared by using Ni(NO3)2(6H2O) and (C2H5O)4SiO4 as starting materials. Then a part of the colloid was dried in open air and the other part was used to form NiO/SiO2 composite powders at hydrothermal conditions. Carbon nanotubes (CNTs) were systhesized respectively by using these two kinds of powders as catalysts,with acetylene as the source of carbon. The phase and morphology of the both catalysts and the morphology, output and yield of the two kinds of CNTs were compared by using XRD and TEM. The results show that the catalyst powders synthesized by the hydrothermal method, compared with those synthesized in open air, are with smaller diameters (10~20nm), better dispersion and have stronger catalytic activities, so that the pure CNTs with smaller tube diameters of 10~16nm can be obtained at a high yield. The differences of the carbon nanotubes prepared by using the catalysts synthesized by the hydrothermal method at different temperatures were also studied.
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Micro-structural Features of Co-filled Carbon Nanotubes
MA Xi-Cheng,ZHENG Guo-Bin,FENG Jing-Wei,LI Feng-Zhao,WEN Shu-Lin
2003 Vol. 18 (6): 12731279
Abstract(
2206 )
PDF(1808KB)(
1148
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Cobalt-filled carbon nanotubes were prepared in situ in the decomposition of benzene over Co/silica-gel catalysts. Transmission electron microscopy (TEM) investigation showed that the products contained abundance of carbon nanotubes (CNTs) and most of them were filled with metallic nanoparticles or nanorods. High-resolution TEM (HRTEM), selected area electron diffraction (SAED) patterns and energy dispersive X-ray spectroscopy (EDS) confirmed the presence of Co inside the nanotubes. The encapsulated Co was further identified as alpha-Co with fcc structure, which frequently consists of twinned boundaries. Based on the experimental results, a possible growth mechanism of the Co-filled nanotubes was proposed.
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Microstructure and Formation of HCA on the Surface of Bioactive Ceramics
ZHAO Li,LIN Kai-Li,CHANG Jiang
2003 Vol. 18 (6): 12801286
Abstract(
2519 )
PDF(2310KB)(
1273
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Hydroxyapatite (HAP), bioactive glass, wollastonite and composites of hydroxyapatite and wollastonite were prepared. These different bioactive ceramics were soaked in the simulated body fluid (SBF) under the same condition and characterized by Fourier Transform Infrared Spectrometry (FTIR) and Field Emission Scanning Electron Microscope (FESEM). The results showed that the surfaces of these bioactive ceramics were covered with a layer of carbonate hydroxyapatite (HCA) when soaked in SBF. The speed of HCA deposition and the microstructure of the HCA were different between different materials. HCA formed on the surfaces of the above bioactive ceramics was spherical, and the HCA layer formed on the surfaces of HAP and wollastonite was slightly loose as compared with that on bioactive glass. When wollastonite was added into HAP, both the speed of HCA deposition and the microstructure of HCA formed on the surfaces of the composites were clearly affected. The results show that the speed of the HCA deposition and the microstructure of HCA in SBF can be used to estimate the in vitro bioactivity of inorganic biomaterials, and the bioactivity of the composites can be regulated by the ratio of the wollastonite/hydroxyapatite.
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Thermal Conductivity of Fine-grain Doped Graphite at Elevated Temperatures
FAN Zhuang-Jun,LIU Lang,LI Jian-Gang,SONG Jin-Ren
2003 Vol. 18 (6): 12871292
Abstract(
2188 )
PDF(1665KB)(
1275
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Fine-grain doped graphites, which possess excellent thermal-mechanical properties, were prepared by the ball-milling dispersion method. At the same time, the correlation between microstructure observed by SEM, EDX and XRD and the properties of the doped graphite was discussed. Such materials had dense and homogeneous structure with carbides dispersed uniformly in the carbon substrate, and showed an excellent thermal conductivity at elevated temperatures and thermal shock resistance.
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Preparation of Core-Shell Polystyrene/ Silica Composite Microspheres and Hollow Silica Spheres
YANG Xiao-Ling,ZHU Yi-Hua,ZHU Meng-Qin,LI Chun-Zhong
2003 Vol. 18 (6): 12931298
Abstract(
2491 )
PDF(1158KB)(
1500
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The core-shell polystyrene/silica composite microspheres with tailored dimensions and compositions were prepared by layer-by-layer self-assembling. The polymer cores were removed by calcination and hollow silica spheres with tailored wall thickness were produced. TEM photographs showed that silica nanoparticles formed a uniform shell round the core, which turned into a clear-cut hollow sphere after calcination. TG revealed that silica content within the composite microspheres increased with the assembled nano silica diameter. Both the successful assembly of SiO2 and the complete removal of PS can be verified by FIIR comparison of PS, SiO2, composite microspheres and the powders after heating treatment. With the same number layers of nanoparticles adsorpted on the latex cores, the larger the selected SiO2 nanoparticles diameter (10nm, 20nm, 40nm), the larger the composite microspheres diameter, and the thicker the hollow spheres’ wall.
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Synthesis of Novel Porous Silica/Montmorillonite Composites by Gallery-Template Structure-Directing Method
ZHOU Chun-Hui,LI Qing-Wei,GE Zhong-Hua,NI Zhe-Ming,LI Xiao-Nian
2003 Vol. 18 (6): 12991305
Abstract(
2471 )
PDF(451KB)(
1069
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The purified natural montmorillonites were modified by cetyltrimethylammonium bromide (CTAB) and octadecyltrimethylammonium chloride respectively. Mixtures of the modified montmorillonites, neutral amine and tetraethylorthosilicate (TEOS) at a molar ratio of 1:20:150 were allowed to react for 8h. The resulting intercalates were centrifuged, dried in air and calcined at 540℃ for 4h to burn off the organic templates, a series of novel porous silica/montmorillonites composites were successfully synthesized by the gallery-template structure-directing process. The structure of the samples was characterized by XRD, TG, FT-IR, N2 adsorption-desorption isotherms and acid-catalyzed alkylation probe reaction. The results show that the samples synthesized have a narrowly pore distribution and super-gallery height, a large BET specific area. With the increasing of chain length of neutral amine, the pore size and gallery height increase accordingly. The synthetic materials are potentially effective solid acid catalysts for the Friedel-Crafts alkylation of catechol with tert-butyl alcohol to synthesize butyl 4-tert-butylcatechol (4-TBC). Over synthetic porous material by using CTAB and hexylamine as template, the selectivity to 4-TBC of 78.5% and catechol conversion of 45.5% can be obtained under experimental condition.
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Synthesis Regularity of NaA Zeolite Membrane in Microwave Field
CHENG Zhi-Lin,CHAO Zi-Sheng,FANG Wei-Ping,WAN Hui-Lin
2003 Vol. 18 (6): 13061312
Abstract(
1874 )
PDF(2402KB)(
963
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Zeolite membrane has the potential advantages in a number of applications such as separation and catalysis, chemical sensors, electrode, acoustic wave devices and optics devices. The paper reports a novel method for continuous NaA zeolite membrane deposited on porous aluminum substrate by microwave heating at ambient pressure and under reflux. The effects of placement manners, alkalinity, Na+ concentration and synthesis times on zeolite membrane formation were investigated. XRD and SEM results show that high alkalinity and high Na+ concentration don’t benefit to form continuous membrane, whereas dissolve membrane layer. Among three placement manners, vertical placement and horizontal placement manners show better effects on zeolite membrane formation. In order to improve membrane quality, employing multi-stage synthesis is necessarily, which is prone to restrain transformation of NaA zeolite and increases intergrown degree of membrane in gel reactant system for short synthesis time.
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Preparation and Characteristics of Beta-alumina Films on α-Alumina and Its Composite Substrate
WEN Zhao-Yin,LIN Zu-Xiang,GU Zhong-Hua,XU Xiao-He,JIANG Dong-Liang
2003 Vol. 18 (6): 13131319
Abstract(
2420 )
PDF(1930KB)(
1001
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Beta-Al2O3 structured ionic conductors, involving β- and β’’-Al2O3 phases, are among the most favorable solid electrolyte materials for electrochemical sensors because of their excellent ionic conductivity and chemical stability. Usually they are used in tube or disc forms. Microcrack-free beta-Al2O3 films on α-Al2O3 or its composite ceramic substrates were obtained by the surface reaction of the substrate with lithium and sodium component from beta-Al2O3 atmosphere. SEM results show heterogeneous microstructures of the beta-Al2O3 film, with some overgrown grains as large as 15μm. The addition of MgAl_2O_4 spinel phase in the α-Al2O3 substrate effectively improves the morphology of the films with maximum grain size of 2~3μm. The kinetic processes of the Na-beta-Al2O3 (Li,Mg) film formation on composite substrate are controlled by both the lithium transportation velocity and the rearrangement of α-Al2O3 to spinel structure of beta-Al2O3. Impedance analyses indicate that the beta-Al2O3 films obtained possess comparable electrical properties to those of ceramic blocks and depend on the relative contents of β- and β’’-Al2O3, and obey the Arrehnius relationship.
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Tribological Behavior of Electroless Ni-P-Carbon Nanotube Comoposite Coating
CHEN Xiao-Hua,ZHANG Gang,CHEN Chuan-Sheng,YI Guo-Jun,JIANG Wen-Zhong
2003 Vol. 18 (6): 13201324
Abstract(
2178 )
PDF(2121KB)(
1107
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Carbon nanotube was used as a reinforcement agent to prepare Ni-P matrix composite coating. The tribological behaviour of the composite coating was examined on a reciprocating wear test machine. The surface morphologies before and after wear test were analyzed by scanning electron microscopy. The results show that the carbon nanotubes are uniformly embedded in the matrix and one end protruded from the surface. The Ni-P-carbon nanotube composite coating has high wear resistance and self-lubrication. The CNTs layer in the matrix protects the surface of the matrix from wearing. Meanwhile the incorporation of the CNTs suppresses the plastic deformation and enhances the mechanical properties of the coating.
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Effects of Electrical Parameters on the Microstructure of Microarc Oxidation Ceramic Coatings on Ti6Al4V Alloy
WANG Ya-Ming,JIANG Bai-Ling,LEI Ting-Quan,GUO Li-Xin,CAO Yue-Ping
2003 Vol. 18 (6): 13251330
Abstract(
2172 )
PDF(1188KB)(
1387
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Ceramic oxide coatings were formed on Ti6Al4V alloy surface by Microarc Oxidation(MAO) in Na2SiO3-KOH-(NaPO3)6 solution using an AC power supply. The effects of voltage and frequency of the power on growth kinetics, microstructure and phase constitute of the coatings were studied. The results show: with voltage increasing or frequency decreasing, the growth rate of the coatings increases, but the surface morphology becomes coarser. The as-deposited coatings are relatively dense and uniform, mainly composed of anatase and rutile TiO2. The phase constitute in the coatings depends on electrical parameters of voltage and frequency. With voltage increasing or frequency decreasing, the content of anatase TiO2 decreases, while rutile TiO2 increases and becomes the predominant phase.
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Super-hydrophilicity of TiO2/SnO2 Composite Film
LIU Qing-Ju,YANG Xi-Kun,LIU Qiang,WANG Bao-Ling,WU Xing-Hui
2003 Vol. 18 (6): 13311336
Abstract(
2021 )
PDF(419KB)(
1165
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TiO2/SnO2 composite thin films were prepared on soda-lime glass with the sol-gel method. The influence of SnO2 doping concentration, heat-treatment temperature and film thickness on the super-hydrophilicity and photocatalytic activity of the composite films was studied by XRD, XPS, UV-spectra, measuring the contact angle and the degradation of methyl orange. The results indicate that the doping of SnO2 into TiO2 can improve their hydrophilicity and photocatalytic activity, and the composite film with 1%-5% SnO2 and heat-treated at 450℃ is of super-hydrophilicity. The optimal SnO2 concentration for the photocatalytic activity is 10% and larger film thickness is helpful to reduce the contact angle of the composite films.
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Effects of HNO3 Treatment on Photocatalytic Activity and Surface Microstructures of Sol-gel Derived TiO2 Nanometer Thin Films
ZHANG Xie-Qun,YU Jia-Guo,ZHAO Xiu-Jian,ZHAO Li,MO Shao-Bo,LIU Ying
2003 Vol. 18 (6): 13371344
Abstract(
2112 )
PDF(1109KB)(
1082
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TiO2 nanometer thin films were prepared on soda-lime glass and pre-coated SiO2 soda lime glass via a sol-gel method, respectively. The as-calcined TiO2 nanometer thin films were then treated by dipping them in 1mol/L HNO3 aqueous solution. The TiO2 nanometer films before and after surface acid treatment were characterized by UV-VIS spectrophotometry, X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM), and photocatalytic activity of the thin films were evaluated by photocatalytic decoloration of methyl orange aqueous solution. The results show that SiO2 layer can effectively retard the diffusion of Na ions from glass substrates to TiO2 films. The photocatalytic activity of TiO2 thin films is significantly enhanced after treated with HNO3 solution. The enhancement of the activity is ascribed to the reduction of sodium ions and the increase of the surfacehydroxyl content in the TiO2 films.
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Preparation of Iron-Nitride Magnetic Fluid
LI Xue-Hui,AN Hong,QI Rui,ZHANG Xiu-Ling,LIU Zhong-Fan,LIU Zong-Ming
2003 Vol. 18 (6): 13451350
Abstract(
2111 )
PDF(243KB)(
1338
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The gas-liquid reaction method was used to prepare iron-nitride magnetic fluids, and the optimum conditions of prepartion were found out. The specific magnetization intensity of iron-nitride magnetic fluid prepared reached 0.05T(before being condensed), and the iron-nitride magnetic fluids obtained were applied in static sealing valves made by our group.
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Synthesis of Composite AIN Powder Mixed with Sintering Additives by the Lanxide Method
LIN Zhi-Lang,ZHENG Xin-He,WANG Qun,ZHOU Mei-Ling
2003 Vol. 18 (6): 13511356
Abstract(
2280 )
PDF(865KB)(
995
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Composite AlN powder, mixed with the sintering additive Y_2O_3, was synthesized by the direct nitridation of molten Al-Mg-Y alloys. The character of products was determined by means of electron microscopy, X-ray diffraction, granularmetric analysis and chemical composition analysis etc. The results show that the nitridation rate of the raw alloys is higher, and the nitridation products are porous enough to be easily crushed. Composite AlN powder, obtained by the Lanxide method, has excellent characters such as high purity, especially low oxygen content, and narrow well-distributed grain size and so on.
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Preparation, Characterization and Influential Parameters of ZnO Nanoparticles Synthesized by Precipitation Method
WANG Jin-Min,GAO Lian
2003 Vol. 18 (6): 13571360
Abstract(
2139 )
PDF(1171KB)(
1312
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ZnO nanoparticles were synthesized by a precipitation method with Zn(NO3)2·6H2O as the starting material and Na2CO3 as the precipitant. When the concentration of the reactants reduced from 2.0 to 0.5mol·L-1, the particle size hardly changed but the agglomeration was weaker. TG-DSC curves of the precursor show that the precursor decomposes at about 253℃. XRD pattern of the powder indicates that the hexagonal wurtzite ZnO nanocrystals can be obtained when the precursor calcinated at 300℃ for 2h. TEM micrographs show that the ZnO nanoparticles are well dispersed and the average particle size is 15~20nm. The specific surface area of the obtained powder is 64.12m2·g-1. There is no obvious difference whether to wash the precipitate by distilled water or ammonia before to wash by ethanol.
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Preparation of Zinc Sulfide Nano-particles by High-Gravity Method
LI Ya-Ling,WANG Yu-Hong,CHEN Jian-Feng,Jimmy Yun
2003 Vol. 18 (6): 13621366
Abstract(
2004 )
PDF(587KB)(
1175
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By using zinc nitrate and hydrogen sulfide as source materials, nanometer zinc sulfide was synthesized by a high gravity method in a rotating packed bed. The effect of aging time on product sizes was investigated and 48h was chosen. Well-dispersed nanometer zinc sulfide particles with a sphalerite crystal phase were prepared. The crystal structure, optical properties, size and morphology of the product were also characterized by XRD, UV-Vis spectrophotometer and TEM. The results show that the average particle size of ZnS obtained is about 30nm and the conversion rate is 97.5 percent.
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以NH4HCO3为沉淀剂通过共沉淀法制备2Y-TZP纳米粉体
TANG Jiao-Ning,JIN Xi-Hai,GAO Lian
2003 Vol. 18 (6): 13671371
Abstract(
2161 )
PDF(661KB)(
1214
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2Y-TZP nanopowder was prepared by a coprecipitation method, using NH4HCO3, ZrOCl2·9H2O and Y(NO3)3 as the starting materials. During the precipitating process, (NH4)3ZrOH(CO3)3·2H2O was formed through a two-step reaction. First, NH4HCO3 reacted with ZrOCl2·9H2O to form Zr(OH)4, then NH4HCO3 further reacted with Zr(OH)4 to form (NH4)3ZrOH(CO3)3·2H2O. The resulting (NH4)3ZrOH(CO3)3·2H2O was unstable and decomposed into ZrO2, NH3, H2O and CO2 at about 130℃. The 2Y-TZP powders obtained by calcining the precipitate mixture at 300℃ and 450℃ showed very fine particle sizes and were almost free of large hard aggregates. Furthermore, these powders showed good sinterability and could be highly densified at a low temperature of 1225℃.
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Properties of La0.7 Pb0.3 MnO3 Colossal Magnetoresistance Material Studied by the Internal Friction Technology
LI He-Qin,HE Xiao-Xiong,FANG Qian-Feng
2003 Vol. 18 (6): 13721376
Abstract(
2005 )
PDF(325KB)(
1028
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The internal frictions and elastic moduli of colossal magnetoresistance material La0.7Pb0.3MnO3 were measured on multi-function internal friction apparatus with the low frequency torsion pendulum. The inverse proportionality of the peak height against the measurement frequency and the invariance of the peak position by changing frequencies are typical features of phase transition. The corresponding elastic modulus with a local minimum at internal friction peaks also characterizes the nature of phase transition. The relationships between double peaks of internal friction and the double peaks of electric resistance versus temperature were explaned by studying the colossal magnetoresistance effect and the susceptibility. The internal friction peak and resistance peak at higher temperatures correspond well with Curie temperature, ascribed to a transition from PMI to FMM. The internal friction peak at lower temperatures and the monotony descending of susceptibility may be interpreted as the phase separation originated from an inhomogeneous distributing of electric and magnetic phase, whereas the high resistance peak at lower temperatures may be partly from the phase separation.
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Structural and Electrical Properties of Bi3NbTiO9 Solid Solution
ZHANG Zhen,YAN Hai-Xue,DONG Xian-Lin,WANG Yong-Ling
2003 Vol. 18 (6): 13771380
Abstract(
1914 )
PDF(534KB)(
947
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Bi3NbTiO9 (BNT) ceramic material with 95%~97% of the theoretical density was prepared by the conventional mixed-oxide method. Its Curie temperature (Tc) of 914℃ was measured to be almost the highest one among those of all the ceramics known up to date. And obviously, the piezoelectric ceramic can be used at higher temperatures. The crystal structure of the ceramic was examined by XRD method. Anisometric plate-like crystalline grains were observed by SEM, which revealed the layered structure of the material. Furthermore, the hysteresis (P-E) loop measurement showed a typical hard ferroelectricity in the Bi3NbTiO9 ceramics, and the piezoelectric constant (d33) measured was 7pC/N.
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Conductivity of Magnetron-sputtered Nanometer TiO2 Thin Films
GU Guang-Rui,LI Ying-Ai,TAO Yan-Chun,HE Zhi,ZHAO Yong-Nian
2003 Vol. 18 (6): 13811384
Abstract(
2200 )
PDF(306KB)(
1316
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The conductivity of nanometer TiO2 thin films was studied. The dependence of the conductivity of TiO2 thin films on the thickness of the film and the substrate materials were educed. The TiO2 films were deposited by reactive magnetron sputtering of Ti target in an Ar+O2 mixture in a conventional sputtering reactor. The thickness of the films varied in the range from 15nm to 225 nm. The electrical resistivity of the films was measured at room temperature in the air. The results show that the conductivity of TiO2 thin films varies from metal, semiconductor to nonconductor. This is attributed to the transfer of the electrons at the interface between the TiO2 and substrates, and the difference of work function determines the depth of the transfer of the electrons.
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Cubic MgxZn1-xO Films Grown on Si (111)
QIU Dong-Jiang,WU Hui-Zhen,CHEN Nai-Bo,TIAN Wei-Jian
2003 Vol. 18 (6): 13851388
Abstract(
1822 )
PDF(281KB)(
980
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Epitaxy of the cubic MgxZn1-xO thin films on Si (111) was achieved by the reactive electron beam evaporation for the first time. Energy dispersive x-ray detection (EDX) and x-ray diffraction (XRD) were employed to characterize the as-grown films. The orientation of cubic MgxZn1-xO films relies on the growth temperature and the highly (200) oriented MgxZn1-xO films are attainable only at the optimal growth temperature of about 200℃. Photoluminescence excitation (PLE) spectroscopic measurement demonstrates that the optical absorption band edge of the cubic MgxZn1-xO is at 4.20eV, which is 3.50eV lower than the band gap of MgO. Furthermore, XRD measurements indicate the lattice mismatch between cubic MgxZn1-xO and MgO is only 0.16%. The successful growth of high quality MgxZn1-xO renders the fabrication of cubic phase MgxZn1-xO/MgO multiple quantum wells possible.
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