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Progress of Biomineralization Process of Calcium Phosphate in Bone and Teeth
OUYANG Jian-Ming,ZHENG Hui
2005 Vol. 20 (4): 0778
Abstract(
2218 )
PDF(1393KB)(
1786
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Calcium phosphates are the main biominerals in organism. The biomineralization process of various calcium phosphates in bone and teeth in vivo and in vitro was reviewed in this paper. The composition, structure, organic matrix and formation mechanisms of bone and teeth were introduced and compared. The modulation of organic matrix on the growth of calcium phosphate was discussed about the molecular recognition, lattice matching and electrostatic interaction at the organic/inorganic interface.
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Synthesis and Structure Characterization of Coal -based Nano-structured Onion-like Fullerenes
DU Ai-Bing,LIU Xu-Guang,XU Bing-She
2005 Vol. 20 (4): 779784
Abstract(
2345 )
PDF(656KB)(
1437
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Nano-structured onion-like fullerenes (NSOFs) was synthesized from coal by radio frequency plasma. High resolution transmission electron microscope (HRTEM) and X-ray diffraction(XRD) techniques were used to characterize the morphologies and structures of the products. Results indicate that NSOFs can be prepared from coal with high yield. The highly graphitized products contain no carbon nanotubes, the particles display a clear polyhedral or quasi-spherical morphology with hollow center and the method described here might be used to synthesize pure NBOFs at low costs.
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Simple and Effective Preparation of N-doped TiO2 Nanocrystallites with Visible-light Activities
YANG Song-Wang,GAO Lian
2005 Vol. 20 (4): 785788
Abstract(
2391 )
PDF(279KB)(
1322
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N-doped Ti02 nanocrystallites were prepared by mixing tetrabutyl titanate and urea in ethanol, then calcined at a certain temperature and time. The prepared powders were characterized by XRD, XPS and UV-Vis absorbance spectra and their photocatalytic activities under visible-light irradiation were also investigated. N-doped TiO2 prepared by this method could make its absorbance shoulder evidently shift into visible-light region. Also it has high photocatalytic activities in the degradation of methylene blue under visible-light irradiation.
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Preparation and Characterization of La Doped TiO2 Nanoparticles by Sol-hydrothermal Method
JING Li-Qiang,SUN Zhi-Hua,WANG Bai-Qi,QU Yi-Chun,FU Hong-Gang
2005 Vol. 20 (4): 789793
Abstract(
2208 )
PDF(250KB)(
1157
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TiO2 nanoparticles doped with different content of La were prepared by a sol-hydrothermal method, and also characterized by surface photovoltage spectroscopy (SPS) and photoluminescence (PL) spectra. The effect of La dopant content and calcination temperature on surface photoelectrical and photoluminescence performance was investigated, and their inherent relationships discussed. The results show that an appropriate content of La dopant could effectively enhance the photocatalytic activity of TiO2 calcined at appropriate temperature. Moreover, there are certain relationships among SPS and PL and the activity, i.e., the stronger the SPS and PL signals, the larger the separation rate of photoinduced electron-hole pairs, the higher the photocatalytic activity of La doped TiO2 nanoparticles.
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Microwave Synthesis and Characterization of Size-controlled Platinum Nanoparticles Supported on Carbon Supports
ZHAO Jie,CHEN Wei-Xiang,LI Xiang,ZHENG Yi-Fan,XU Zhu-De
2005 Vol. 20 (4): 794800
Abstract(
2041 )
PDF(793KB)(
1620
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Carbon supported platinum nanoparticles were synthesized by microwave assisted heating ethylene glycol solution of H2PtCl6 with different pH values in the presence of XC-72 carbon or carbon nanotubes supports. The products were characterized by EDX, TEM and XRD. The effects of pH values of ethylene glycol solutions on the sizes and uniformity of Pt nanoparticles and their dispersion on carbon supports surfaces were investigated. TEM images show that the average diameter of platinum nanoparticles decreases from 5.5nm to 2.7nm with the increase of pH values from 3.4 to 9.5 for Pt/XC-72, and the average diameter from 5.3nm to 2.8nm with the increase of pH values from 3.5 to 9.4 for Pt/CNTs. In addition, increasing pH values of ethylene glycol solution can improve the size uniformity and dispersity of platinum nanoparticles on carbon surfaces.
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Preparation of Barium Sulfate Submicro-particles with High Purity by Solventing-out Process
WANG Xiao-Hui,JIANG Bin-Bo,CHEN Ji-Zhong
2005 Vol. 20 (4): 801807
Abstract(
1905 )
PDF(421KB)(
1229
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A novel micronization technique using solventing-out crystallization was described for the preparation of submicron BaSO4 particles. The submicron BaSO4 particles were characterized by transmission electron microscope (TEM), scanning electron microscope (SEM), laser diffraction-based particle size analyzer and X-ray diffraction (XRD). The product was obtained as spherical particles with mean sizes from 160--750 nm. The effects of feed mode, feed concentration, feed rate, agitation intensity and crystallization temperature in the solventing-out process were investigated. A well-efficiency dispersant was selected. The experimental results indicate that lower crystallization temperature, reversed feed mode, higher feed rate, controlling solution concentration to a certain extent and faster agitation rate will lead to producing smaller BaSO4 particles. Furthermore, the purity of submicron BaSO4 particles prepared by solventing-out crystallization is upon to 99.7%, and it indicates that the solventing-out crystallization is not only a micronization technique but also an excellent purification process.
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Synthesis of Sodium Titanate Nanotubes by Microwave Hydrothermal Method
FU Min,JIANG Zhi-Dong,MA Zi-Feng,SHANGGUAN Wen-Feng
2005 Vol. 20 (4): 808814
Abstract(
2538 )
PDF(757KB)(
1427
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The effects of raw material, reaction time, NaOH concentration were studied on the synthesis of sodium titanate nanotubes via a microwave hydrothermal method. Sodium titanate nanotubes with a uniform morphology were synthesized in NaOH solution (8--12mol/L), heated by a microwave power of 195W over 70min. The samples were investigated by means of TEM, XRD, BET, EDAX and N2 adsorption/desorption technique. The nanotubes derived from the microwave hydrothermal method features shortened reaction time and higher thermal stability, with the tube structure collapsed at a temperature over 500℃, 100℃ higher than that synthesized by the ordinary hydrothermal method. Furthermore, the samples after calcination at 300℃ will convert into single crystalline sodium titanate nanotubes.
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Synthesis of Tungsten Oxide Nanorods Doped with Transition Metal Molybdenum
CAO Guang-Sheng,YU Qing-Sen,DONG Xi-Gui,SONG Xu-Chun,TAN Fei
2005 Vol. 20 (4): 815820
Abstract(
2379 )
PDF(616KB)(
1202
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Tungsten oxide nanorods doped with molybdenum were synthesized by a facile hy-drothermal method using tungstenic acid precipitate doped with molybdenum as precursor, which was prepared by the reaction between HC1 solution and Na2WO4 solution immingled different percentages of (NH4)6Mo7O24·4H20 respectively. The samples of the products were characterized by XRD, SEM, EDX, TEM and PL. The results show that the dimensions of as-synthesized tungsten oxide nanorods gradually decrease with the increase of the percentage of doped molybdenum, the photoluminescence emission peak intensities of them weaken down accordingly.
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Preparation of Micrometer Fibres by the Organic-gel Method
SHEN Xiang-Qian,JING Mao-Xiang,WANG Tao-Ping,ZHOU Jian-Xin
2005 Vol. 20 (4): 821826
Abstract(
1874 )
PDF(657KB)(
1258
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Metallic nickel, alumina, magnesia fibres were prepared respectively by the organic-gel method from the raw materials of citric or lactic acid and their metal salts. The fibres featured with diameters of less than 1μm and fine crystalline particles of less than 100nm were obtained. The structure, thermo-decomposition process and surface morphologies of the fibres derived from thermal decomposition of the gel precursors were characterized by FTIR,XRD,DSC and SEM. The designability of fibrous textures was discussed as well. The experimental results indicate that the organic-gel method can be a promising process for preparation of micrometer fibres composed of nano-structured crystalline particles.
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Cage-like Structure of Amorphous ZnO
WANG Zhi-Jian,JIA Wei-Min
2005 Vol. 20 (4): 827830
Abstract(
2247 )
PDF(251KB)(
1101
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The octahedral cage-like structure of amorphous ZnO was deduced from the experimental results given by PL spectra, X-ray powder diffraction, Infrared adsorption spectroscopy and combining with corresponding Raman spectra. The octahedral cage-like structure can explain the UV emission character of amorphous ZnO.
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Er3+-doped Tungsten-Tellurite Glass and Planar Waveguide
ZHAO Shi-Long,CHEN Bao-Yu,HU Li-Li
2005 Vol. 20 (4): 831836
Abstract(
1973 )
PDF(255KB)(
1186
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Er3+-doped tungsten-tellurite glass for broadband waveguide amplifier application was fabricated and characterized by the thermal stability, spectroscopic properties and ion exchange property. The glass transition temperature Tg and crystallization onset temperature Tx are 377.1 and 488.5℃, respectively. The fluorescence spectrum indicates that the fluorescence width at half maximum (FWHM) is 52nm. Calculated by McCumber theory the peak stimulated emission cross section of Er3+ from the upper level 4I13/2 to the ground level 4I15/2 is 0.91×10-20cm2. Multi modes at 632.8nm were detected in Er3+-doped tungsten-tellurite glass, and the fitting effective diffusion coefficient De of Ag+ ion at 300℃ and the activation energy Q were calculated to be 2.82×10-16μm2 and 149.7kJ/mol, respectively. The results show that Er3+ doped tungsten-tellurite glass is a prospective candidate for broadband integrated optical amplifier materials.
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Influence of P2O5 on Thermal Behavior and Bioactivity of Sol-Gel Glasses
WANG Chuan-Hui,LI He-Jun,HUANG Feng-Ping,YANG Quan-Zu
2005 Vol. 20 (4): 837841
Abstract(
1857 )
PDF(496KB)(
1006
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Two bioactive glasses in the system CaO-P2O5-SiO2 were prepared by sol-gel process, from tetraethylorthosilicate (TEOS), triethylphosphate (TEP) and hydrated calcium nitrate (one with P2O5 and the other P2O5 free). Thermal behavior and reaction mechanism of xerogels were analyzed by TG-DTA methods. The in~ vitro bioactivity of both glasses was assessed by soaking them in simulated body fluid. The results reveal that the presence of P2O5 in the glass composition gives rise to the change of thermal behavior: the organic groups of triethyl phosphate are decomposed in the temperature range 300--420℃ and the residual OH groups are removed at 570℃ or so. The crystal of hydroxyl carbonate apatite formed on the surface of the glass containing P2O5 is larger and, relatively, the bioactivity is improved.
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Effect of Cr2O3 on the HLW Iron Phosphate Glass Wasteforms
HUANG Wen-Hai,ZHOU Nai,DAY Delbcrt E,RAY Chandra S
2005 Vol. 20 (4): 842850
Abstract(
1855 )
PDF(546KB)(
1438
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The chemical durability, and structure of iron phosphate glasses containing 70wt% of a simulated high level nuclear waste (HLW), doped with different amounts of Cr2O3 were investigated. All of these iron phosphate glassy and crystallized wasteforms possess an outstanding chemical durability as measured by their small dissolution rate (10-9g/(cm2·min)) in deionized water at 90℃ for 128 days, their low normalized mass release as determined by the Product Consistency Test (PCT) and a barely measurable corrosion rate of <0.1 g/(m2·d) after 7 days at 200℃ by the Vapor Hydration Test (VHT) can meet all current DOE requirements for chemical durability. The PCT results show that the Cr2O3 doping into IP70W samples can suppress the element release from both the glassy and crystallized samples and improve the chemical durability. The solubility limit for Cr2O3 in the iron phosphate melts estimated at 4.1 wt%, is at least 3 times larger than that for borosilicate glasses. The results from FTIR and DTA show that the structure of IP glass wasteforms has no significant changes when Cr2O3 doped into IP70W samples. Mossbauer spectra show that there is a redox reaction between Fe and Cr ions during the melting process and that the ratio of Fe2+/Fe3+ increases with the increase of Cr2O3 amount in the compositions. These Cr6+ ions formed can improve the chemical durability of the glass wasteforms.
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SPS Sintering and Magnetic Properties of Fe-based Amorphous/Nanocrystalline Powder
LU Bin,YI Dan-Qing,LIU Yan,LIU Hui-Qun,WU Biao-Li
2005 Vol. 20 (4): 851858
Abstract(
1932 )
PDF(675KB)(
1298
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The influence of SPS sintering temperature on microstructure and magnetic properties of the sintering bulk alloy of melt quenching Fe70Cr8Mo2Si5B15 powders by ball milling and MA Fe73.5Cu1Nb3Si13.5B9 and Fe80Co4Nb7B9 nanocrystalline powders was studied. The results show that (1) under 30MPa/5min conditions, the relative densities of bulk alloys increase with the increase of sintering temperatures. When Fe70Cr8Mo2Si5B15 bulk alloy sintered at 1000℃, its relative density reaches above 99%, and when Fe73.5Cu1Nb3Si13.5B9 and Fe80Co4Nb7B9 bulk alloys sintered at 1050℃, their relative densities reach to 99%; (2) the main phase of sintering bulk alloys is α-Fe phase, and a little second phase intermetallic compound. The grain size of α-Fe phase in bulk alloys is in nanometer range, Fe70Cr8Mo2Si5B15 bulk alloy has the finest grain size, its average grain size is about 50nm; (3) with the sintering temperature increasing, the specific saturate magnetization Bs of these bulk alloys increases and coercive force Hc decreases, respectively. Fe70Cr8Mo2Si5B15 bulk alloy has the lowest Hc, 4.1kA·m-1.
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Crystallite Size and Electrochemical Performance of Metal Hydrides Based on LaNi5 Prepared by Twin-Roll Process
LU Dong-Sheng,LI Wei-Shan,TANG Ren-Heng,XIAO Fang-Ming
2005 Vol. 20 (4): 859863
Abstract(
1864 )
PDF(386KB)(
1114
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AB_5-type hydrogen storage alloy La0.65Ce0.28Pr0.02Nd0.05Ni3.8Co0.7Mn0.3Al0.2 was prepared by twin-roll process, and the microstructure, capacity and cyclic stability of the alloy were characterized by SEM, XRD and constant current charge and discharge. The alloy has a uniform nano-scale crystallite size of about 40nm. Its discharge capacity is 336mAh/g at 0.2C rate (64mA/g), and 312mAh/g at 2C rate (640mA/g) and retains 80% of the initial capacity after 400 cycles. The influence of La content on electrochemical capacity and cyclic stability of the alloy was also studied. It is found that discharge capacity of the alloy increases with the increase of La content when La less than 60wt% and keeps unchanging from 60% to 80%. However, cyclic stability of the alloy decreases with the increase of La content.
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Growth of Composite Sapphire/Ti:Sapphire by Hydrothermal Method
SONG Ci,ZHANG Chang-Long,XIA Chang-Tai,HANG Yin,XU Jun
2005 Vol. 20 (4): 864868
Abstract(
2005 )
PDF(275KB)(
1148
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Composite sapphire/Ti:sapphire crystals for high power applications were grown by the hydrothermal method. The X-ray diffraction pattern of omega scan indicates that the coating Al2O3 is of high quality. The strong bonding between the coating Al2O3 and Ti:Al2O3 is suitable for the strong thermal stresses present with intense pumping. The optical loss at the boundary of the composite crystal is considerably low.
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Defect Study of Tm:YAG Crystal
SONG Ping-Xin,ZHAO Zhi-Wei,XU Xiao-Dong,DENG Pei-Zhen,XU Jun
2005 Vol. 20 (4): 869874
Abstract(
1996 )
PDF(837KB)(
1223
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Tm:YAG crystal with high quality was grown by the Czochralski method. Some of the samples were annealed at 1000℃ for 25h in the air. Chemical corrosion was used to the slices of Tm:YAG crystal before and after air annealing. The etch pits in (111) plane were observed by Leitz optical microscope and scanning electron microscope (SEM). The shapes of etch pits located in (111) plane exhibit as a triangle structure. Stress birefringence of Tm:YAG slices as grown and after air annealing was investigated by polarization microscope. The lattice integrality of Tm:YAG crystal was investigated by high-resolution X-ray diffraction. The air annealing on slices for long time in high temperature can reduce the total density of the dislocations, and improve the quality of the crystals.
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Growth and Spectrum Characteristics of LiNbO3:Cr Crystal
YOU Zhen-Yu,TU Chao-Yang,ZHU Zhao-Jie,LI Jian-Pu,ALAIN Brenicr
2005 Vol. 20 (4): 875882
Abstract(
1604 )
PDF(555KB)(
1290
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The LiNbO3:Cr crystals with the sizes up to φ20mm×60mm were grown by the Czochralski technique. The absorption spectrum shows that there are two strong absorption wideband peaks and one weak
absorption peak belonging to Cr3+ ion in the crystal. The peak values of two strong absorption wideband peaks are 481nm and 657nm, which correspond to 4A2→4T1 and 4A2→4T2
transitions, respectively. The weak absorption peak at 727nm corresponds to 4A2→2E (R line) transition; The fluorescence spectrum shows that one emission wideband peak ranging from
800nm to 982nm coexists with one weak emission peak at 750nm corresponding to ^4T_2→2E transition. The peak value of emission wideband is 870nm, which corresponds to 4T2→4A2
transition. The crystal field and Racah parameters were calculated, the values of Dq, B and C are 1522.1, 542.5 and 3218.7cm-1, Dq/B=2.81 indicates that it has an stronger crystal
field. The result shows that the wideband tunable laser can be gotten from this crystal because it not only has the necessary spectra characteristics required for tunable laser crystal but also has the good
physics chemical properties. Furthermore, the UV laser at about 410nm can also be gotten from the crystal by its self-frequency doubling because it has a higher frequency-doubling coefficient.
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Effects of Preparation Conditions on the Microstructure and Properties of Hot Pressed SiC/SiC Composites
DONG Shao-Ming,DING Yu-Sheng,JIANG Dong-Liang,KOHYAMA Akira
2005 Vol. 20 (4): 883888
Abstract(
1908 )
PDF(625KB)(
1761
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SiC/SiC composites were prepared by hot pressing using nano-SiC and sub-micrometer SiC powders for matrix formation. The effects of preparation conditions, such as particle size, sintering temperature and sintering pressure, on the microstructural evolution and mechanical properties were characterized. The composite using nano-SiC for matrix formation could promote densification at a relatively lower temperature. At 1780℃, 20MPa, a high performance composite, N-SiC/SiC, could be obtained. While using sub-micrometer SiC for matrix formation, fiber and matrix interaction was enhanced with the increasing of eityer sintering temperature or pressure, which would disbenifit for the performances of the composite.
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Internal Friction of Continuous Fiber-reinforced SiC-matrix Composites
ZHANG Jun,XU Yong-Dong,ZHANG Li-Tong,CHENG Lai-Fei
2005 Vol. 20 (4): 889894
Abstract(
2006 )
PDF(481KB)(
1086
)
The internal friction of C/SiC and SiC/SiC composites was investigated by means of forced vibration from room temperature to 600℃ under different strain amplitude, and the internal friction mechanism was also discussed. The results show that the internal friction of C/SiC composites decreases at first and then increases with increasing temperature, and the minimum of internal friction occurs at about 120℃. While the internal friction of SiC/SiC composites increases monotonically with the increase of temperature. C/SiC composites have a higher internal friction value and lower dynamic modulus than SiC/SiC composites. The internal friction of both C/SiC and SiC/SiC composites decreases when the strain amplitude is increased, while the dynamic modulus of both the composites is independent of the strain amplitude.
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Preparation and Performance of High Thermal-stable Alumina-substrate Materials
WANG Xiao-Hong,GUO Yun,GUO Yang-Long,WANG Yun-Song,LU Guan-Zhong
2005 Vol. 20 (4): 895901
Abstract(
2101 )
PDF(808KB)(
1038
)
High thermal-stable alumina-substrate materials were prepared by the reverse microemulsion method and characterized by XRD, nitrogen adsorption at low temperature, TEM and so on. The results indicate that the samples prepared by the reverse microemulsion method have higher thermal stability. After calcination at 1100℃ for 10h, the surface area of alumina, Ba-doped alumina and Si-doped alumina is 51, 90 and 175m2·g-1 respectively, which is much higher than that of the same samples prepared by the sol-gel method. Besides this, the phase structures and the pore diameter distribution of the sample derived from the reverse microemulsion method are also more different to those of the sample derived from the sol-gel method. The former shows transition alumina structure and uniform nanometer particles even calcined at 1100℃ for 10h. The presence of Ba or Si can increase the phase transformation temperature of alumina and restrict its grain growth at high temperature.
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Preparation and Photocatalytic Activity of Pt-modified TiO2 Pillared Bentonite
LI Yi-Min,LU Yue-Qing,QIU Huan-Huan,LIU Ying,LI Hai-Yang
2005 Vol. 20 (4): 902906
Abstract(
2198 )
PDF(254KB)(
1008
)
TiO2 pillared bentonite (TiO2-PILC) was prepared with an intercalation of polynuclear titanium complex formed by reaction of Ti(i-C3H7O)4 and acetic acid. TiO2 pillared bentonites modified with platinum (Pt-TiO2-PILCs) were carried out via the photodeposition method. Characteristics of the pillared bentonites were examined by XRD, BET, TEM. TiO2-PILC and Pt-TiO2-PILCs were used as composite photocatalysts in photocatalytic degradation of sodium pentachlorophenate(PCP-Na). The results indicate that all the pillared bentonites contain TiO2 in the anatase phase and with a mean crystallite size of TiO2 about 5nm. The photocatalytic activities of Pt-TiO2-PILCs are superior to that of TiO2-PILC. In addition, the experiments also illustrate that the composite photocatalysts can be easily recovered, regenerated and reused.
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Preparation and Antibacterial Performance of Zeolite Loaded Silver Antibacterial Agent
HOU Wen-Sheng,WEI Li-Qiao,DAI Jin-Ming,JIA Hu-Sheng,XU Bing-She
2005 Vol. 20 (4): 907913
Abstract(
2368 )
PDF(292KB)(
1079
)
The silver-supporting antibacterial zeolite was prepared by the ion exchanging method with zeolite as the carrier and AgNO3 solution as the exchanging solution. The influence of preparation process on exchanging ability of zeolite was studied and the optimum preparation process was determined. The structure was characterized by X-ray diffraction (XRD) and the antibacterial ability was tested. The results show that the exchanging ability is greatly influenced by the concentration of exchanging solution, temperature, time and pH values. The suitable concentration of exchanging solution is 0.1mol/L. The pH value should be controlled between 6--8. In view of energy consumption, ambient temperature is appropriate, but in view of reaction time, the reaction should be heated. The silver-supporting antibacterial zeolite has an excellent antibacterial performance against E. coli and S. faecalis.
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Study on in vitro Bioactivity and Cytotoxicity of γ-Ca2SiO4 Ceramic
GOU Zhong-Ru,CHANG Jiang,ZHAI Wan-Yin,LIN Kai-Li,ZENG Yi
2005 Vol. 20 (4): 914920
Abstract(
2163 )
PDF(794KB)(
1065
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In this study, the in vitro bioactivity and cytotoxicity of gamma-dicalcium silicate (γ-Ca2SiO4) ceramic were evaluated systematically. The surface physicochemical changes of the ceramic soaked in a simulated physiological fluid (Kokubo’s SBF) for various periods were determined by means of XRD, FT-IR, SEM and EDS analysis. The results indicated that the ceramic surface transformed to a carbonated hydroxyapatite (CHA) within 72h and a silica-rich layer occurred between the CHA layer and ceramic matrix after 240h. In addition, the ionic products of the material dissolution had no cytotoxicity to fibroblasts compared with the negative control. This ceramic supported the bone mesenchymal stem cells (BMSCs) adhesion and spreading, and the BMSCs established close contacts with the ceramics after 24h of culture. This combination of properties indicates that the novel γ-Ca2SiO4 ceramic might be suitable for potential application in the biomedical field, preferentially as materials for bone repair.
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Preparation and Study on Composite Metal Ion Antibacterial Zeolites
YU Bo,WANG Fang
2005 Vol. 20 (4): 921926
Abstract(
2094 )
PDF(385KB)(
1268
)
The four categories of antibacterial zeolites were prepared by different methods with 13X zeolite as their carrier, and their structures and properties were characterized by WAXD, EDS, AAS and bacteriostasis circle tests. The results show that the basic structure of 13X does not change in the process of the cation exchange, and the cations absorbed by 13X can be slowly released into medium. The composite metal zeolites contained Ag+ cations prepared by the method of composite cations exchange are optimum in antibacterial performance and superior to AGZ-330 antibacterial agent in their bacteriostasis and cost. The composite metal ions zeolites have better slowly release effect and high content of cations killing bacterials more effectly due to their synergistic effect and broad spectrum antibacterial properties.
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Efficiency of the FCVI Process for Fabricating C/C Composites
ZHANG Shou-Yang,LI He-Jun,HAN Hong-Mei
2005 Vol. 20 (4): 927932
Abstract(
1911 )
PDF(323KB)(
975
)
In order to deeply understand the forced-flow-thermal-gradient chemical vapor infiltration (FCVI) process for fabricating carbon-carbon composites, the model concerning pores in preforms was established in this paper, the pores in preforms were composed of opened pores and closed pores, the CVI process is the closing process of opened pores. On the basis of the chemical reaction dynamics and the heat and mass transmission theory, a new concept, the residual time of densification (RTD), was put forward, from which a theoretical method was deduced to predict the densification efficiency of the process and control the technique qualifications, based on this theory, the highest densification efficiency of FCVI process can be acquired when the density distribution of performs accord with a certain mathematical relationship during CVI process. As a result, the relationship between the density distribution of preforms and the process efficiency was analyzed comprehensively, and a variable factor, ψ, was defined to evaluate the efficiency of FCVI process. The practical experiments showed that, if the ψ valued around 0 in any stage of the process, the highest densification efficiency of FCVI process can be acquired. Guided by the presented method, the densification efficiency was improved to a satisfactory level in practical FCVI processes.
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Preparation and Performance of Novel Al3+ Modified Silica Gel Adsorptive Materials
FANG Yu-Tang,DING Jing,FAN Juan,YANG Jian-Ping,YANG Xiao-Xi
2005 Vol. 20 (4): 933939
Abstract(
1928 )
PDF(488KB)(
1217
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Al3+ modified silica gel adsorptive materials were prepared by treating ceramic fiber matrix with sequential impregnation of aqueous solution of sodium silicate(Na2SiO3), acidic aluminium salt. The results show that the optimal reaction condition is 26.67% Na2SiO3, 10% aluminium salt and 1.8 solution pH value. 29Si and27AlMAS NMR spectra show that some Al is incorporated in SiO4 tetrahedral framework structure which is not influenced by the replacement of Al for Si atoms. The Al3+ modification results in symmetric stretching vibration shifting from 968cm-1 of Si--OH to 954cm-1 of Si (Al)--OH. SEM imagine reveals Al3+ modified silica gel is well scattered on the surface corrugated ceramic paper and in the apertures between fibers of paper. EDS analysis indicates the existence and percentage of modified Al3+ in the adsorptive materials surface micro zone. Porous medium surface area analysis shows that the mesopore is dominant for adsorption in Al3+ modified silica gel. For the Al3+ modification, the humidity adsorbing ability, heat resistance property and tensile strength and burst of Al3+ modified silica gel adsorptive materials are superior to those of silica gel.
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Electrochemical Corrosion of Nano-multilayered Ti/TiN Films on 316L Stainless Steel in the Simulated Bodily Fluid
LIU Cheng-Long,LIN Guo-Qiang,YANG Da-Zhi,ZHAO Yan-Hui,DENG Xin-Lu
2005 Vol. 20 (4): 940946
Abstract(
1964 )
PDF(552KB)(
1016
)
Nano-multilayered Ti/TiN films were synthesized on biomedical 316L stainless steel through the Bulat-6 arc ion plating system. The anti-corrosion performances of different films were studied elementarily in Troyde’s simulated bodily fluid. The results show that it is about 5 and 2 times, for the breakdown potential of 316L+Ti/TiN in neutral and acidic Troyde’s simulated bodily fluid, higher than that of 316L stainless steel, and one eighth and one third of the corrosion current density of the substrate, respectively, which indicates that the sensitivity of local corrosion for the substrate is depressed greatly. However, the delay in reverse cathodic scanning is caused by the worse self-repairable property of Ti/TiN film. The anti-corrosion performance of 316L+Ti/TiN, in Troyde’s simulated bodily fluid, is improved effectively by the existence of the nano-multilayered structure and pure titanium layer.
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Formation and Microstructure of Zeolite Silicalite-1 Membranes on α-Al2O3 Supports with Different Pore Sizes
ZHANG Xiong-Fu,LIU Hai-Ou,WANG Jin-Qu
2005 Vol. 20 (4): 947954
Abstract(
1969 )
PDF(951KB)(
1055
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The formation and microstructure of zeolite silicalite-1 membranes on the α-alumina supports with different pore sizes by secondary growth synthesis from clear solutions were studied. The deposition of the seeds with 100nm and 600nm sizes and growth of the membranes on the different supports were investigated, respectively. SEM and XRD characterization of the samples shows that a continuous uniform seed layer and dense, intergrown membrane on the support with the pore size of 0.1μm can be obtained by using both 100nm and 600nm size seeds, whereas, on the support with the pore size of 4μm, a continuous seed layer can not be formed by using the same seeding time for either 100nm or 600nm seeds. On the support with the pore size of 4μm, a seed layer can only be obtained by using 100nm seeds in a longer contact time, however, 600nm seeds cannot be deposited to form a seed layer. The seed layers and membranes grown from the smaller seeds are better intergrown and possess smooth surfaces, whereas the seed layers and membranes grown from the larger seeds display coarse surfaces and poorer intergrowth.
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Effects of NO and N2O Flow Rates on Electronic Properties of p-type ZnO Thin Films
ZHOU Ting,YE Zhi-Zhen,ZHAO Bing-Hui,XU Wei-Zhong,ZHU Li-Ping
2005 Vol. 20 (4): 955958
Abstract(
2098 )
PDF(253KB)(
890
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Nitrogen-doped p-type zinc oxide (ZnO) thin films were deposited on glass substrates by metalorganic chemical vapor deposition (MOCVD). The p-type ZnO, with the lowest resistivity of 5.52Ω·cm and the highest hole concentration of 2.17×1018cm-3, can be achieved at the NO and N20 flow rates of 40 and 25sccm, respectively, and the sample was most stable. Four months later, all samples still showed p-type conduction, but the resistivities were increased.
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Growth Mechanism for N-doped ZnO Films Grown by Spray Pyrolysis Method
ZHAO Jun-Liang,LI Xiao-Min,BIAN Ji-Ming,ZHANG Can-Yun,YU Wei-Dong,GAO Xiang-Dong
2005 Vol. 20 (4): 959964
Abstract(
2571 )
PDF(491KB)(
1097
)
N-doped ZnO films were grown at Si(100) substrates by ultrasonic spray pyrolysis with the precursor of zinc acetate and ammonium acetate. Thermal-mass spectrometric analysis (TG-DSC-MS), X-ray diffraction (XRD), and field emission scanning electron microscope (FESEM) were employed to analyze the growth mechanism, crystal structure and electrical properties of films. Results show that the films grown at different substrate temperatures show different growth mechanisms, which could influence crystal structure and electrical properties of films. The successful p-type doping can be realized at an optimized substrate temperature. The p-type ZnO film shows excellent electrical properties such as a hole concentration of 3.70×1018cm-3, hole mobility of 110cm2·-1s-1 and resistivity of 1.4×10-2Ω·cm.
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Growth and Optical Properties of Nanocrystalline ZnO Porous Film by Ultrasonic Assisted Successive Ionic Layer Adsorption and Reaction (UA-SILAR) Method
GAO Xiang-Dong,LI Xiao-Min,YU Wei-Dong
2005 Vol. 20 (4): 965970
Abstract(
1926 )
PDF(646KB)(
1032
)
Ultrasonic irradiation technique was introduced to the traditional successive ionic layer adsorption and reaction (SILAR) method to modify the microstructure and crystallinity of ZnO films. ZnO nanocrystalline porous films were successfully deposited on glass substrates from aqueous solution at 90℃ by using the precursor of [Zn(NH3)4]2+. Results show that as-deposited ZnO films exhibit excellent crystallinity with the preferential orientation of (002) plane. A porous feature with interconnected particles of 200~400 nm in ZnO films was observed, and each ZnO particle formed is by the aggregation of many crystallites in the size of 30~50nm. Because of the intense scattering function of the porous structure on the incident light, the films exhibit low transmittance in the visible band (~20%). With the excitation of photon of 340 nm, an intense UV emission at 390 nm was observed in the PL spectra for as-deposited samples, indicating its good optical properties. The introduction of ultrasonic irradiation in the film deposition process can exert significant effects on the structure and crystallinity of ZnO films.
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Microstructure of LiNbO3 Thin Films Grown on Silicon Substrates by Pulsed Laser Deposition
LU Huan-Ming,YE Zhi-Zhen,HUANG Jing-Yun,WANG Lei,ZHAO Bing-Hui
2005 Vol. 20 (4): 971975
Abstract(
1989 )
PDF(473KB)(
977
)
A lithium niobate (LiNbO3) thin film was fabricated by a pulsed laser deposition method on Si(001) substrate with about 5nm-thick amorphous silicon oxide surface layer, under the conditions of 600℃ substrate temperature and 30 Pa oxygen pressure. The film was investigated by transmission electron microscope and X-ray diffraction. The factors influencing on the evolution and preferred orientation of the LiNbO3 were discussed. The results obtained show that the LiNbO3 thin film is highly c-axis oriented perpendicularly to the substrate under the optimized deposition conditions above mentioned.
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Investigation on the Mechanism of the Pechini Process for LiCoO2
FENG Sheng-Lei,LIANG Hui,WANG Ke-Wei,LI Wei-Ke
2005 Vol. 20 (4): 976980
Abstract(
2616 )
PDF(304KB)(
1096
)
LiCoO2 powders were prepared by the Pechini method with cobalt nitrate and lithium hydrate as raw materials, citric acid as complexing agent and ethylene alcohol as cross-linking agent. The optimal pH for the Pechini process was studied. Two key steps, complexation and esterification, were explored with infrared spectra. The results show that in the solution of pH=5, citric acid exists mostly in the form of HCit2-. During the process of complexation, complex compound is generated by Co2+ and HCit2-, while Li+ is homogenously dispersed in the citric acid solution. During the process of fat polymerization, different complexed molecules are polymerized together by ethylene alcohol. After dehydration, gels with space structure are formed.
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Transport Properties in La0.7-xDyxSr0.3MnO3 System
LI Hong,ZHANG Ming-Yu,CAI Zhi-Rang,GUO Huan-Yin,PENG Zhen-Sheng,YAN Guo-Qing
2005 Vol. 20 (4): 981987
Abstract(
2115 )
PDF(434KB)(
991
)
The influence of Dy doping at La-site on transport properties of La0.7-xDyxSr0.3MnO3 (x=0.00, 0.10, 0.15, 0.20, 0.30, 0.40, 0.50, 0.60, and 0.70) was studied. The experimental results indicate that with increasing Dy doping, the system undergoes a transition from long range ferromagnetic order to the cluster-spin glass state and further to antiferromagnetic order. The transport properties exhibit abnormal behaviour at high doping condition. For x=0.50, a transition from metal to insulator occurs after the occurrence of insulator-metal transition near Tc, which seldom occurs in ABO3 structure. The samples of x=0.60 and 0.70, exhibit insulator behavior far above Tc.
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Piezoelectric Properties of Morphotropic Phase Boundary for PNW-PMS-PZT Piezoelectric Ceramics
PEI Zhi-Bin,DU Hong-Liang,JU Jun,WEI Xiao-Yong,QU Shao-Bo
2005 Vol. 20 (4): 988992
Abstract(
2228 )
PDF(222KB)(
1121
)
The piezoelectric ceramics (PNW-PMS-PZT) were prepared by traditional ceramics process. The phase structure of all ceramics samples was analyzed. Results show that the pure perovskite phase is in all ceramics specimens researched. The effect of the content of PMS, PNW and Zr/Ti ratio on the region of morphotropic phase boundary for PNW-PMS-PZT piezoelectric ceramics was studied. Results show that the phase structure of PNW-PMS-PZT piezoelectric ceramics changes from tetragonal to rhombohedral with the increase of the amount of PMS, PNW and the ratio of Zr/Ti in the system. The composition of PNW-PMS-PZT piezoelectric ceramics near the morphotropic phase boundary obtained is the content of PMS: 5~6mol%; the content of PNW: 2~3mol%; the content of PZT: 91~93mol%; the ratio of Zr/Ti: 50/50. At the same time, there is high piezoelectricity near the morphotropic phase boundary.
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Sintering Behavior of PMnN-PZT Ceramics
LI Bao-Shan,ZHU Zhi-Gang,LI Guo-Rong,YIN Qing-Rui,DING Ai-Li
2005 Vol. 20 (4): 993999
Abstract(
2197 )
PDF(622KB)(
1092
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The microstructure and the piezoelectric properties as well as the valency of Mn in Pb[(Zr0.52Ti0.48)0.95(Mn1/3Nb2/3)0.05]O3 (PMnN-PZT) ceramics sintered at different temperatures from 1070℃ to 1280℃ were investigated by XRD, SEM, TEM, XPS. The experimental results suggest that grain sizes, tetragonality and kp of the ceramics increase with the increase of sintering temperature, and Qm fluctuates with the increase of sintering temperature. The obtained results by X-ray photoelectron spectrum and TEM suggest that there exist apparently the liquid phase of PbO and stoichiometric composition departure during the sintering. Low temperature induces the existence of the Mn2+, producing more oxygen vacancies, and therefore the fluctuation of mechanical quality factor (Qm) with the sintering temperature occurs.
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Sintering Temperature Influence on the Dielectric and Piezoelectric Properties of Pb(Mn1/3Sb2/3)O3-PbZrO3-PbTiO3 Ceramics
ZHU Zhi-Gang,LI Bao-Shan,LI Guo-Rong,ZHANG Wang-Zhong,YIN Qing-Rui
2005 Vol. 20 (4): 10001006
Abstract(
2063 )
PDF(457KB)(
1002
)
The effects of sintering temperature on the microstructure and piezoelectric properties of Pb(Mn1/3Sb2/3)O3-PbZrO3-PbTiO3 (PMS-PZT) ceramic were investigated. Results show that the optimized properties of εr=1530, d33=374pC/N, Kp=0.6, tanδ=0.41%, Qm=1250 can be obtained when the ceramic sintered at 1240℃ for 2h, which suit for high-power applications. Meanwhile, the ceramic also possesses superior characteristics (εr=1370, d33=348pC/N, Kp=0.57, tanδ=0.62% and Qm=1620) for multilayer components and thick-film devices when it sintered at 1150℃. Results also indicate that PMS-PZT ceramic can be sintered in a wide temperature range. High temperature microscope, SEM, TEM, and EDS investigation confirm that PbO and Sb_2O_5 can form a liquid phase acting as a secondary phase on grain boundaries at lower sintering temperature, and then enter the crystal lattice to form perovskite structure at higher sintering temperature.
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Low Distortion Dielectric Ceramics for Base-Metal-Electrode MLCC
OU Yi-Cheng,LU Zhen-Ya,CHEN Xu-Ming
2005 Vol. 20 (4): 10071012
Abstract(
1875 )
PDF(407KB)(
1044
)
A dielectric ceramic with the main phase of (Ca,Sr,Ba)(Zr,Ti)O3 was successfully sintered in reducing atmosphere. The crystal phases were analyzed by the XRD method. A proper synthesis process was used to obtain the dielectric material without ferroelectric BaTiO3 phase. With high dielectric constant(εr: 300~400), low dielectric loss (tgδ ≤30×10-4), low capacitance changes under DC bias (about 0.03% when the dc bias is 2.5kV/mm), the dielectric material is applicable for low distortion base-metal-electrode MLCC
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Dielectric Properties of BSTO/Mg2SiO4/MgO Ceramic Composites
CHEN Ying,DONG Xian-Lin,GAO Min,LIANG Rui-Hong,CAO Fei
2005 Vol. 20 (4): 10131018
Abstract(
2046 )
PDF(531KB)(
1109
)
BSTO/Mg2SiO4/MgO ceramic composites were fabricated by conventional ceramic processing. The microstructures and dielectric properties of the samples were measured and investigated systemically. The effects of the doping of Mg2SiO4/MgO on the microstructures and dielectric properties of BSTO/Mg2SiO4/MgO ceramic composites were investigated. The results show that compared with the other BSTO ceramic composites, BSTO/Mg2SiO4/MgO ceramic composites not only can be sintered at a lower temperature but also keep a higher tunability while the dielectric constant decreases. The typical composition of BSTO/39wt/% Mg2SiO4/17wt% MgO has a dielectric constant of ~80.21, a dielectric loss of ~0.003 and a tunability of ~12% under applying 2kV/mm dc bias field.
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Influence of Grain Size on Breakdown Voltage of PZT95/5 Ferroelectric Ceramics under Shock Compression
ZHANG Fu-Ping,HE Hong-Liang,DU Jin-Mei,WANG Hai-Yan,LIU Gao-Min
2005 Vol. 20 (4): 10191024
Abstract(
2410 )
PDF(280KB)(
1062
)
Breakdown voltages of two kinds of PZT95/5 ferroelectric ceramics with different grain sizes were investigated under shock compression. Weibull distribution model was used to analyze the experimental data. The results show that the breakdown voltage of PZT95/5 samples can be described by two parameter Weibull distribution. According to the density function and failure probability function of the Weibull distribution, PZT95/5 ceramics with fine grains possess more optimum breakdown voltage distribution than PZT95/5 ceramics with coarse grains.
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