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Research and Development Status of Calcium Fluoride Crystals Used in Lithography System
DONG Yong-Jun,ZHOU Guo-Qing,YANG Wei-Qiao,SU Liang-Bi,XU Jun
2004 Vol. 19 (3): 449455
Abstract(
2186 )
PDF(422KB)(
1238
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The reasons why calcium fluoride crystals can be used in lithography system were explaned. The research and development status of calcium fluoride crystals was summarized. Meanwhile the important problems need to be resolved in the process and measures that should be taken into consideration were pointed out. In the end the development foreground was expected.
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Research and Development of Reaction Sintered Silicon Carbide
WANG Yan-Xiang,TAN Shou-Hong,JIANG Dong-Liang
2004 Vol. 19 (3): 456462
Abstract(
2232 )
PDF(497KB)(
2037
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Reaction sintered silicon carbides are getting more and more attention because of their proper mechanical strength, oxidation resistance and low cost. In this paper, the type, the focus of current research about reaction sintered silicon carbide and the reaction mechanism of carbon with molten silicon were reported.
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Influence of Al Content on the Structure and Electrochemical Performance of Al-substituted α-Ni(OH)2
XIAO Hui-Ming,WANG Jian-Ming
2004 Vol. 19 (3): 463470
Abstract(
2003 )
PDF(353KB)(
1030
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Nano-sized Al-substituted α-Ni(OH)2 with high electrochemical performance was synthesized through a chemical co-precipitation method in organic solvent and characterized by means of X-ray diffraction and infrared spectroscopy. Sample’s structure stability in concentrated alkaline solution was investigated and the relationship between structure and electrochemical performance was studied. The experimental results show that the mean crystal sizes of samples containing 7.5%,13.2%and 17.2%(molar ratio)Al are 5.4, 6.9 and 11.0 nm respectively. The structure of the sample with 7.5% Al is of the mixture of α-Ni(OH)2 and β-Ni(OH)2, whereas the structurers of the samples respectively with 13.2% and 17.2% Al are of pure α-Ni(OH)2. Structure stability increases with Al content increasing due to gradually increased crystallinity and so do its discharge mediate potential and specific electrochemical capacity.
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Preparation of Nanometer Mullite by Sol-Gel-SCFD Method
ZHAO Hui-Zhong,LEI Zhong-Xing2,WANG Hou-Zhi,ZHANG Wen-Jie
2004 Vol. 19 (3): 471476
Abstract(
2127 )
PDF(589KB)(
1194
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Nanometer mullite was prepared through Sol-Gel-SCFD and middle temperature calcination by using aluminium-isopropoxde and tetraethyl orthosilicate as starting materials, the alumina-silica binary aerogel and calcined nanosized materials were investigated by using thermogravimetry-differential scanning calorimeter (TG-DSC), transmission electron microscope (TEM), X-Ray diffractometer (XRD) and specific surface area and porosimetry. TG-DSC indicated the removal of most of the volatiles, i.e. 15.98% up to about 700℃, and in the DSC curve, the existence of two exothermic peaks at about 445 and 1015℃ may be due to the crystallization of Si-O-Al-O in diphasic gels and mullitization, and a small endothermic peak at about 805℃ indicated the decomposition of structural water molecules. The beginning temperature of mullitization of the Al2O3-SiO2 at about 1015℃ in gel was confirmed by TG-DSC, XRD and TEM, XRD results which also showed the formation of mullite at the range 1100-120℃. TEM and surface area and porosimetry results showed that the nanosized mullite calcinated at 1100 and 1200℃ exhibited the sizes of 30nm and 50nm, specific surface area 138.91m2/g and 95.81m2/g respectively.
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Synthesis of CdS Nanorods in Sol Template
ZHAO Qi-Tao,HOU Li-Song,HUANG Rui-An,GU Si-Peng
2004 Vol. 19 (3): 477480
Abstract(
1792 )
PDF(526KB)(
949
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CdS nanorods were synthesized by a soft chemistry method using cadmium nitrate and thioacetamide as starting compounds and DMF as solvent at low temperature(~50℃). The CdS nanorods have diameters of 7~20nm and lengths up to 500nm. Measurements including transmission electron microscopy (TEM), X-Ray diffraction(XRD) and energy-dispersive spec- troscopy(EDS) were carried out to study the microstructure of the samples. The nanoporous sol templates formed by the controlled hydrolysis and condensation of Ti(OC4H9)4 in the presence of AcAc provide an effective matrix for the growth of CdS nanorods.
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Fabrication of Multimetal Disulfide Nanotube and Its Structural Characteristics
LI Guo-Hua,ZENG Yue-Wu,SONG Xu-Chun,XIA Jun-Bao,CHEN Wei-Xiang,XU Zhu-De
2004 Vol. 19 (3): 481486
Abstract(
2016 )
PDF(1186KB)(
1047
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The fabrication and structure controlling of inorganic fullerene-like nanocompounds have attracted wide interests in recent years. A new approach of exfoliating-restacking-structure controlling was applied to overcome some technological problems in present preparation approaches. MoS2 and WS_2 powders were used as precursor materials and exfoliated into single layers by butyllithium. The sample was treated by MnCl2 solution at 80℃ to introduce Mn2+ cations into the reactive system. In this way, the single layer was restacked and the structure of product could be controlled. The products were characterized by XRD, TEM and HRTEM respectively. XRD results indicate that multimetal disulfide compounds can be fabricated by this new approach. TEM results show that the morphology of the multimetal disulfide compounds exhibits hollow-like nanotubes. HRTEM results show that the structure of the hollow-like nanotubes is of double layers. And the substructure of the inner layer exhibits multi-wall shape. Based on the above results, a possible formation mechanism of hollow multi-wall nanotubes was discussed.
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Fabrication of Cu7S4 Nano-crystals with Supported Liquid Membrane
SUN Dong-Mei,WU Qing-Sheng,DING Ya-Ping
2004 Vol. 19 (3): 487491
Abstract(
2088 )
PDF(829KB)(
1158
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A novel fabrication method of Cu7S4 nano-crystals by supported liquid membrane (SLM) system was investigated. SLM consists of CHCl3 as solvent, o-phenanthroline as a mobile carrier and polymer membrane as supported template. The results indicated that Cu7S4 which has hexagonal structure with cell constant of a=15.475Aand c=13.356Acan be prepared at room temperature with 0.2mol/L CuCl2 and 0.2mol/L Na2S as reactants. The average size of Cu7S4 is about 7nm. In addition, the forming mechanism and optical properties of Cu7S4 were discussed.
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Electrorheological Effect of Titania-Coated Kaolinite Nanocomposite Particles
WANG Bao-Xiang,ZUO Zhao-Yang,ZHAO Xiao-Peng
2004 Vol. 19 (3): 492496
Abstract(
2047 )
PDF(488KB)(
991
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Kaolinite/TiO2 nanocomposite particles were prepared by sol-gel technique. The analysis of XRD,FT-IR and SEM shows that the surface of kaolinite is coated by nano-TiO2 crystal. Furthermore the electrorheological effect is associated with the TiO2 mass percent in the nanocomposite particle. When the content of TiO2 in the composite is 34%, E=3kV/mm, and volume fraction is 25%, the yield stress of kaolinite/TiO2 nanocomposite ERF is 3.4 kPa, which is 5 times of that of kaolinite.
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Structure and Electrochemical Properties of LiCo0.3Ni0.7O2 Prepared by the Rheological Phase and Spray Drying Method
XU Hui,ZHONG Hui
2004 Vol. 19 (3): 497502
Abstract(
2162 )
PDF(643KB)(
1036
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The cathode materials LiCo0.3Ni0.7O2 were prepared from Co0.3Ni0.7(OH)2 and LiOH·H2O dispersed in the organic solution by the rheological phase and spray drying method in air at different sintering temperature for 16h. The TG-DTA analysis, XRD analysis, SEM and electrochemical tests were used to study the physical and the electrochemical performances of the materials. The results indicate that molecular level completely mixing of the raw materials of samples made by our method makes the sintering temperature drop to a lower temperature and the resulted sample has an excellent layered structure and the cation mixing and nonstoichiometric products are effectively restrained when sintered at 700℃. The material(sintered at 700℃) cycled between 2.80~4.25V shows a high initial capacity of 172mAh/g with an efficiency of 90.8% and its irreversible capacity only 16mAh/g. 91% of the initial discharge capacity remains after 40 cycles.
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Surface Modification Mechanism of Spinel Structure LiMxMn2-xO4 as Cathode Materials for Lithium Ion Batteries
ZHAO Shi-Xi,LIU Han-Xing,ZHANG Ren-Gang,LI Qiang,OUYANG Shi-Xi
2004 Vol. 19 (3): 503509
Abstract(
2103 )
PDF(374KB)(
1196
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The grains of LiMn2O4 and LiMxMn2-xO4 (M=Li, Ni) were coated with LiCoO2 by using sol-gel process. XRD and EPMA studies confirme the presence of a Co-rich spinel LiMn2-xCoxO4 layer on the surface of LixMn2-xO4 grains and the content of Co decreases gradually from the surface to the core of spinel grains. Furthermore, the amount of Mn3+ in the surface layer is less than in the core, so the possibility of Mn dissolution decreases. The surface treatment is effective in reducing the rate of Mn dissolution into electrolyte and improving cyclability of spinel LiMxMn2-xO4 cathode materials. After bulk Ni-doped spinel LiNi0.1Mn1.9O4 coated with LiCoO2, the cyclability of the material is better than that of pure spinel LiMn2O4and just only cations doped.
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Preparation and Sintering Densification of Nanocrystalline NASICON Solid Material
ZHU Qi-Feng,QIU Fa-Bin,QUAN Yu-Jun1,WANG Yong-Wei,QUAN Bao-Fu,XU Bao-Kun
2004 Vol. 19 (3): 510516
Abstract(
2256 )
PDF(814KB)(
1212
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Nanocrystalline solid material of NASICON (sodium super ionic conductor) was synthesized by the sol-gel and high-temperature sintering process, in which normal inorganic reagents and silicon organic reagent were used as the raw materials. The temperature range of 750~890℃ for the formation of NASICON phase was recognized through the analysis of TG-DTA result conducted for NASICON xerogel. Thus, the sintering process was carried out in the temperature range of 800~1000℃. As shown from the results of some analytical methods such as XRD, FT-IR, FE-SEM, impedance spectrum and the measurement of Archemede density, the solid-electrolyte NASICON with grain size of nanometer, good crystallinity and high relative density was synthesized successfully by adopting appropriate sintering temperature and period. A linear Arrhenius plot for the resulted NASICON material was achieved and a reasonable active energy was got based on the complex impedance measurement conducted at different temperatures. The solid material possessed an ideal ionic conductivity. Moreover, highly crystallized NASICON showed higher ionic conductivity.
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Electrochemical Assembled p-type Bi2Te3 Thermoelectric Materials with Nanowire Array Structure
WANG Wei,JIA Fa-Long,HUANG Qing-Hua,ZHANG Wei-Ling,GUO He-Tong,SHEN Yu-Tian
2004 Vol. 19 (3): 517522
Abstract(
2112 )
PDF(696KB)(
1028
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he electrodeposition process of p-type Bi2Te3 thermoelectric materials in the solution containing Bi+3 and HTeO2+1 was investigated. During the electrodeposition prosess, Bi+3 can promote the reduction of HTeO2+1. The addition of glycerin in the electrodepositing solution can decrease the solving rate of alumina templates in the solution, but glycerin also decreases the electrodeposition rate remarkably. The p-type Bi2Te3 thermoelectric materials with nanowire array structure were electrochemically assembled into the nano-pores of the alumina template. The performance measurements show that the Seebeck coefficient α of the nanowire array is much higher than that of the bulk thermoelectric materials with the same composition.
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Effect of Dopants on Long Afterglow Properties of Y2O2S:Eu Phosphor and Its Long Afterglow Mechanism
YUAN Shuang-Long,YANG Yun-Xia,XU Zhi-Zhen,FANG Bin
2004 Vol. 19 (3): 523528
Abstract(
2453 )
PDF(388KB)(
1246
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Y2O2S:Eu phosphors doped with Mg2+, Ca2+, Sr2+, Ba2+, Ti4+ were studied by PL spectra, XRD, decay curve, relative brightness and TL spectra. The results show that those dopants do not change crystal structure of the host, but influence afterglow properties and relative brightness, and the decay curve comprised of a fast and a slow part is well exponential. Codopants of Mg and Ti suggest the longer afterglow duration than single ion doping, being dependent on their contents. The long afterglow mechanism of Y2O2S:Eu host materials was discussed on the basis of experimental results.
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Prediction of Immiscibility Boundaries of Binary Glass System
LUO Zhong-Kuan,JIANG Zhong-Hong,LIU Jian-Hong,CAI Hong-Hua,HONG Wei-Liang,XU Hong
2004 Vol. 19 (3): 529535
Abstract(
2040 )
PDF(392KB)(
1012
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The assumption of molecules group of glass network was made, and the relation of immiscibility boundary was derived and established. The immiscibility boundary curve of some glass system was calculated and estimated by using the new theory relation, and the results are closely agreed with the experimental immiscibility boundaries. This relation first solved the non-symmetry curve of immiscibility for the binary oxides glass system theoretically. It can be considered that this new theory and the equation can be applied in the more glass phase separation systems, and mutual interaction between different molecules can be calculated further.
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Modified CZ. Growth and the Properties of Nd3+:KGd(WO4)2 Crystal
TU Chao-Yang,LI Jian-Fu,YOU Zheng-Yu,ZHU Zhao-Jie,WU Bai-Chang,LUO TaO,LAI Hong-Zhang
2004 Vol. 19 (3): 536640
Abstract(
1687 )
PDF(539KB)(
1222
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The crystal of Nd3+:KGd(WO4)2 with the size of φ20mm×35mm was grown by using the modified CZ.
method. The absorption and emission spectra in the directions of a, b and c axes were measured, the result shows that the intensity of absorption
and emission spectra in the direction of a axis is the strongest. Therefore, the direction of a axis is the most suitable for laser experiment. A laser
output of 125.5 mJ at 1.067μm was obtained when a laser crystal with the size of φ3.5mm×26mm was pumped by a Xe lamp. Compared with the
YAG:Nd3+ laser crystal, which was performed the same laser experiment at the same conditions, Nd3+:KGd(WO4)2 has the advantages of lower
laser threshold and higher efficiency as well as the polarized laser output. Therefore, it is expected that Nd3+:KGd(WO4)2 crystal will be very
useful in the miniature laser.
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Structure and Grain Growth Habit of Directional Solidification Ceramics of (1-x)Pb(Mg1/3Nb2/3)O3 - xPbTiO3 (x=0.30, 0.33, 0.38) Relaxor Ferroelectric Solid Solutions
SUN Shi-Wen,PAN Xiao-Ming,LI Dong-Lin,LI Hong-Jun,ZHU Li-Hui,HUANG Qing-Wei,WANG Ping-Chu
2004 Vol. 19 (3): 541545
Abstract(
1511 )
PDF(610KB)(
1009
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This work describes the grain growth habit of the (1-x)Pb(Mg1/3Nb2/3)O3-xPbTiO3 (PMN-PT or PMNT) system ferroelectric solid solutions prepared by a directional solidification technique. The results show that the preferential direction of the grain growth depends not only on the composition of the melts, but also on the crucible pulling-down speed. For a fixed PMN/PT ratio, e.g. 62/38, higher speed of crucible pulling-down leads to a preferential grain growth orientation of [110], rather than the [111], which is usually reported in single crystal growth studies, whereas lower crucible pulling-down speed tends to produce [111] grain-orientation ceramics. When the crucible is pulled down at a certain rate, the preferential grain-growth orientation changes from [111] to [110] with reducing PbTiO3 molar contents.
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Microstructure and Mechanical Properties of Al2O3/Ni Cermet
LI Guo-Jun,HUANG Xiao-Xian,GUO Jing-Kun
2004 Vol. 19 (3): 546552
Abstract(
1853 )
PDF(2253KB)(
1258
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Ni-coated Al2O3 powders with different Ni content were prepared by the coating technique. The powders were sintered by hot-pressing, and Al2O3/Ni cermet obtained. Results show that the densification is enhanced with the increase of temperature, and when temperature is more than 1400℃, the densification is decreased with the increase of Ni content. Ni particles introduced in Al2O3 ceramic matrix can reduce grain sizes, enhance strength and toughness. Compared with single phase Al2O3 material, Al2O3/4vol% Ni cermet has flexural strength of 19% and fracture toughness of 35% enhanced. SEM photos of fracture surface show that the fracture model of the cermet changes from intergranular fracture to transgranular fracture with the increase of Ni content.
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Preparation and Thermal Shock Property of Si3N4 Ceramic Reinforced by Orientation SiC Whiskers
LUO Xue-Tao,CHEN Xian-Jun,HUANG Qian-Jun,CHEN Li-Fu
2004 Vol. 19 (3): 553558
Abstract(
2021 )
PDF(877KB)(
1242
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A highly orientation SiC whisker reinforced Si3N4 composite was fabricated by fiber extrusion and hot-pressing technique, which SiC whiskers were unidirectional oriented in the extruded carrier fiber. Microstructure of the composites was observed by SEM. Whisker directions were image-processed to quantify SiC whisker orientation in the extruded fibers and the composites. Effects of sintering temperature and SiC whisker content on the flexural strength and fracture toughness of the composites were investigated. The experimental results show that the flexural strength and fracture toughness of the orientation SiC whisker toughened Si3N4 composites are higher than that of the random SiC whisker toughened Si3N4 composites after thermal shock experiment, in temperature difference of 1000℃ and 500℃.
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Ordered Oxynitrides Mesoporous Materials with High Nitrogen Content
ZHANG Cun-Man,XU Zheng,WAN Ke-Shu,LIU Qian
2004 Vol. 19 (3): 559565
Abstract(
2070 )
PDF(497KB)(
1146
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The ordered oxynitrides mesoporous materials were successfully prepared by the ni- tridation of Al-MCM-41 and SBA-15 mesoporous materials (containing template) in flowing NH3 environment. The composition and structure of the synthesized materials were analyzed by CNH analysis, IR spectrum, Si MAS NMR, N_2 sorption, low-angle XRD, and HRTEM. The results of analysis show that the obtained oxnitrides mesoporous materials by nitriding at higher tempera- ture (1273~1323K) and long soaking time (8~24h) still possess good order, high nitrogen content (10~21wt%), high surface area (700~900m2g-1), and narrow pore distribution.
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Preparation of PLZST with Complex Perovskite Structure by Coprecipitation
XUE Li-Hong,ZHANG Yi-Ling,LI Qiang,GUO Quan-Yong,LIU Rui
2004 Vol. 19 (3): 566570
Abstract(
2266 )
PDF(226KB)(
1202
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A modified chemical coprecipitation route to synthesize homogeneous lead lanthanum zirconate stannate titanate (PLZST) precursors was described. The formation process of PLZST from the precursors was monitored by thermal analysis, and the phases were characterized by X-ray diffraction. Compared with the solid-state reaction of constituent oxides, the PLZST powders prepared by coprecipitation have high purity, homogeneous and low synthesis temperature. The formation temperature of single perovskite PLZST is as low as 700℃ in this method of preparation. Pb content analyzed by chemical methods indicates that the loss of Pb in PLZST synthesized at low temperature is minimal.
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Grain-Boundary Chemistry of BaTiO3 based PTCR Ceramics as CO Gas Sensors
ZHOU Zhi-Gang,TANG Zi-Long,ZHANG Zhong-Tai
2004 Vol. 19 (3): 571578
Abstract(
2158 )
PDF(483KB)(
1100
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The sensing phenomena and mechanism of doped BaTiO3 based PTCR ceramics for chemical sensors are close related to the variation of chemical defect structure in the grain boundaries with environmental atmospheres. The surfaces and grain boundaries are act as a uniform source and sink for vacancies, and the lattice defects play a positive role for the sensing effect in the ceramics. The grain boundary chemistry, specially, formation and distribution of defects, defect changes in adsorption and desorption process with surrounding CO gas, redistribution of electrons on quenching to room temperature for high dopant concentrations as well as potential barrier in grain boundary were discussed.
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Dielectric Behavior and Piezoelectric Properties of La3+-doping 0.94(Na1/2Bi1/2)TiO3-0.06BaTiO3 Ceramics
LI Hui-Dong,FENG Chu-De,XIANG Ping-Hua
2004 Vol. 19 (3): 579585
Abstract(
2236 )
PDF(998KB)(
1153
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(1-x)(Na1/2Bi1/2)TiO3-xBaTiO3 (x=0.06) with 1-5 at% lanthanum was prepared by the conventional mixed oxide method. The effect of La3+ doping on dielectric behavior and piezoelectric properties of the ceramics was studied. The relaxor behavior of the La3+ doped ceramics is more evident. At room temperature, the dielectric constant is increased. When the La content is less than 1.5 at%, the piezoelectric properties are enhanced. But in the meantime the dielectric loss of the ceramics is also increased. When the content of La3+ is up to 3 at%, the ceramics’ piezoelectric properties are remarkably debased.
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Temperature Stability of Nb-doped PMS-PZ-PT Ceramics
ZHOU Fei,LONG Ji-Wen,MENG Zhong-Yan
2004 Vol. 19 (3): 586592
Abstract(
2291 )
PDF(318KB)(
1087
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The influences of Nb-doping on the temperature stability of PMS-PZ-PT ternary system ceramics were investigated. The stable temperature dependence of resonance frequency, electromechanical coupling coefficient K31 and piezoelectric constant d31 were measured. Results show that the donor dopants can not only optimize piezoelectric properties of the system, but also improve the temperature stability. So the modified PMS-PZ-PT ceramics can achieve the requirements for high-power piezoelectric devices such as ultrasonic motors.
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Electrochemical Properties of Carbon Aerogels Electrode for Super-capacitor
MENG Qing-Han,LIU Ling,SONG Huai-He,ZHANG Rui,LING Li-Cheng
2004 Vol. 19 (3): 593398
Abstract(
2583 )
PDF(635KB)(
1458
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The electrochemical measurement of carbon aerogel electrods show that carbon aerogels exhibit excellent properties of high efficiency, good electrochemical behavior as electrode materials. Both surface area and pore volume of carbon aerogels determine their specific capacitance. High pore volume and wide pore distribution contribute to increasing the capacitance. Activated carbon mixed with different ratio of carbon aerogels increases the capacitance of the electrode, while the capacitance is the highest when the content of carbon aerogels in the composites is 15 percent。
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Morphology Control of Vapor Grown Carbon Nanofibers
ZHU Chun-Ye,XIE Zi-Li,GUO Kun-Min
2004 Vol. 19 (3): 599604
Abstract(
2136 )
PDF(1061KB)(
1593
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The influences of catalyst precursor, promoter and benzene to hydrogen mole ratio on the morphology of carbon filaments and selective preparation of carbon filaments by the floating catalyst method were reported. By controlling the contents of ferrocene (catalyst precursor), thiophene (promoter) and benzene to hydrogen mole ratio, straight carbon nanotubes (S-CNTs), curving carbon nanotubes (C-CNTs), beaded carbon nanofibers (B-CNF) and carbon nanofibers (CNF) were synthesized. Effects of different parameters, especially, critical role of catalyst, promoter and benzene to hydrogen mole ratio were discussed. From TEM, Raman spectroscopy, HRTEM and TG-DSC analysis, it can be concluded that controllable growth of carbon filaments with different morphologies can be realized in the floating catalyst system by simply controlling such parameters as catalyst, promoter and benzene to hydrogen mole ratio.
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Field Activated Combustion Synthesis of Tungsten Carbide (Ⅰ)——Field Activated Combustion Synthesis
JIANG Guo-Jian,ZHUANG Han-Rui,LI Wen-Lan,SHON In-Jin
2004 Vol. 19 (3): 605609
Abstract(
1920 )
PDF(337KB)(
929
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The activation of self-propagating combustion reactions in the W-C system was achieved by using an electric field. Self-propagating combustion in elemental reactants with the composition corresponding to WC can be activated only when the imposed field is above the threshold value of 1V·cm-1. The nature of the combustion products depends on the field strength. The strength of diffraction peak of WC in XRD pattern increases with the increase of field strength. The product is WC and W2C. The effects of tungsten particle sizes and the relative densities of the reactant compacts on the synthesis of tungsten carbide were also investigated. The results show that the combustion temperature and combustion wave propagation velocity increase with the decrease of the size of tungsten particles. At the optimum relative density, the combustion temperature and wave velocity attain the maximum value.
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Deposition of Polycrystalline ZnO Thin Films by Successive Ionic Layer Adsorption and Reaction Process (SILAR)
GAO Xiang-Dong,LI Xiao-Min,YU Wei-Dong
2004 Vol. 19 (3): 610616
Abstract(
2466 )
PDF(966KB)(
1289
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ZnO thin films were grown on glass substrates by a relatively new and simple chemical deposition method, successive ionic layer adsorption and reaction (SILAR), with the precursor of zinc-ammonia complex ([Zn(NH3)4]2+. XRD and SEM were applied to analyze the crystalline structure and the morphology. The effects of annealing process in air on the crystalline structure and the morphology of ZnO films were discussed. Further, the growing mechanism of ZnO films by SILAR technique was probed. Results show that, the obtained ZnO films after 200 deposition cycles are the zincite structure with the orientation of <002>. The as-deposited films are dense, smooth and uniform, with the film thickness of 800nm. The annealing process in air results in the decrease in oxygen vacancy of ZnO films and the increase in the degree of orientation along c-axis. The amount of interstitial zinc also increases with the augment of the annealing temperature. The re-crystallization resulted from the air annealing at 500℃ affects the micro structure and morphology of ZnO films significantly. The decrease in the ratio of NH3·H2O to Zn2+ in precursor will improve the growth rate of ZnO films.
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Properties of Aluminium Alloy Ceramic Coating Prepared by Microarc Oxidation
WU Han-Hua,YU Feng-Rong,LI Jun-Jie,Lü Xian-Yi,JIN Zeng-Shun
2004 Vol. 19 (3): 617622
Abstract(
2515 )
PDF(889KB)(
36586
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Under the condition of keeping impulse amplitude of alternating voltage constant, microarc oxidation of aluminium alloy in aqueous solution containing sodium silicate and sodium hydroxide was carried by means of alternating current power supply. It is found that the current passing through the sample is divided obviously into five different stages with the oxidation time. The ceramic coatings prepared in the different stages were studied by scanning electron microscopy (SEM) and X-ray diffraction (XRD), respectively. The result shows that the ceramic coatings mainly contain γ-Al2O3, α-Al2O3 phases; the γ-Al2O3 and α-Al2O3 contents are close relative to oxidation time. The difference of γ-Al2O3 and α-Al2O3 contents between external layer and internal layer of the coating is mainly caused by the change of cooling rate of molten alumina in microarc zone.
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Electrical Properties of Nanostructured Al2O3-3wt% TiO2 Coating Deposited by Plasma Spraying Deposited by Plasma Spraying
LIN Xin-Hua,ZHOU Xia-Ming,HUANG Jing-Qi,DING Chuan-Xian
2004 Vol. 19 (3): 623628
Abstract(
2188 )
PDF(1073KB)(
989
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Conventional and nanostructured Al2O3-3wt%TiO2 coatings were deposited by plasma spraying with conventional and nanostructured powders, respectively. The phase compositions and microstructure of the as-spraying coatings were characterized by XRD, SEM and TEM. The electrical resistivity, dielectric constant and dielectric loss of coatings were measured. In both conventional and nanostructured Al2O3-3wt%TiO2 coatings, alumina mainly existed in the form of γ-Al2O3 with some α-Al2O3. Non-stoichiometric Ti2O3 was found in the conventional coating; while in the nanostructured coating, titania reacted with alumina to form solid solution. The conventional Al2O3-3wt%TiO2 coating exhibited a typical splat microstructure. For the nanostructured Al2O3-3wt%TiO2 coating, many equiaxed α-Al2O3 grains besides splat lamellae were also observed. The size of equiaxed α-Al2O3 grains was about 150~800nm. Compared to the conventional Al2O3-3wt%TiO2 coating, electrical resistivity of the nanostructured Al2O3-3wt%TiO2 coating increased. But the nanostructured coating exhibited lower dielectric constant and dielectric loss.
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Effect of Pt/Ru Supported by Carbon Nanotubes on the Ability of PEMFC to Resist CO Poisoning
LI Yan-Hui,CHEN Jun-Feng,DING Jun,MAO Zong-Qiang,XU Cai-Lu,WU De-Hai
2004 Vol. 19 (3): 629633
Abstract(
2111 )
PDF(967KB)(
1092
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Carbon nanotubes prepared by a catalytic pyrolysis method were oxidized and homogeneously deposited with Pt and Pt/Ru nanoparticles on their surfaces. The experimental results show that the catalysts of Pt deposited on carbon nanotubes of the proton exchange membrane fuel cell are easily poisoned by CO and lose their activity, which make the fuel cell voltage decrease sharply with decreasing of current density. But their ability to resist CO poisoning improves when Pt/Ru deposited on carbon nanotubes as catalysts, this suggests that Ru can oxidize CO adsorbed on the surfaces of Pt into CO2, so the catalyst ability to resist CO poisoning increases.
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Preparation and Properties of Washcoats for Three Way Catalyst
JIANG Ping-Ping,ZHANG Shun-Hai,GUO Yang-Long,GUO Yun,WANG Xing-Yi,LU Guan-Zhong
2004 Vol. 19 (3): 634640
Abstract(
2112 )
PDF(542KB)(
1774
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The washcoats deposited on a ceramic honeycomb were prepared with pseudoboehmite as γ-Al2O3 precursor, CeO2-ZrO2-La2O3, pore enlarger and other additives. The relations of apparent viscosity and solid content in the coating gel to the loading of coating, and the effect of the particle size distribution in the coating gel on the properties of washcoats were studied. The microstructures and surface performances of the washcoats deposited on a ceramic honeycomb were characterized by scanning electron microcopy (SEM), BET surface area, vibration by ultrasonic and hot impact simulation. The results show that the solid content of 30%~40% in the coating gel should be used propositionally, the loading of coating in the first impregnation > that in the second impregnation > that in the third impregnation, the feasible loading of coating is 8%~15%. The viscosity in the coating gel affects the performance of washcoats on a ceramic honeycomb. When an apparent viscosity of the gel is lower, an arrow particle size distribution and smaller particles in the coating gel can be obtained, and the prepared coating has excellent properties of the vibration-resistant by ultrasonic, heat-resistant and so on; when an apparent viscosity is higher, there are a wide particle size distribution and mainly micron-meter particles in the coating gel, which is available to form the higher loading of the coating on a ceramic support, but its performance is poorer. After supporting the washcoats, the BET surface area of the ceramic honeycomb can reach 50m2/g.
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Effect of Substrate Temperature on the Deposition Process and Microstructure of ZnO Films Grown by Ultrasonic Spray Pyrolysis Method
BIAN Ji-Ming,LI Xiao-Min,GAO Xiang-Dong,YU Wei-Dong
2004 Vol. 19 (3): 641646
Abstract(
1898 )
PDF(729KB)(
1908
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ZnO thin films were grown on Si (100) substrate by the modified ultrasonic spray pyrolysis (USP). X-ray diffraction (XRD) and scanning electron microscopy (SEM) were employed to analyze the crystalline and microscopic structure of the films. The effect of the substrate temperature on the growth mechanism and the microstructure of ZnO films were studied. Results show that the as-deposited ZnO films are dense, smooth and homogeneous with uniform spherical crystallites, consistent with the hexagonal wurtzite polycrystalline structure. The preferential orientation of (002) is for all deposited films. The minimum crystallite size of ZnO films under the optimal growth condition is 40 to 50 nm. The temperature of the substrate has significant effects on the deposition process. With the increase of the temperature of the substrate, there lies a maximum deposition rate of ZnO films, which can be interpreted by different growing mechanism, and the preferential orientation along $c$ axis is augmented in a marked degree and the crystalline grain size is refined as well.
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Electroless Ni-P-SiC Composite Coating
YU Shi-Jun,SONG Li-Xin,HUANG Yin-Song,ZHAO Rong-Gen,HU Xing-Fang
2004 Vol. 19 (3): 647652
Abstract(
2367 )
PDF(846KB)(
1120
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A series of Ni-P-SiC composite coatings were successfully prepared by electroless plat- ing process. Up to 22vol% SiC particles can be uniformly distributed in Ni-P matrix. It was found that hardness linearly increases with the SiC particles co-deposition in the as-deposited coatings. Heat-treatment can improve the coating properties, i.e. in the conditions 400℃ with 1h treated, Ni-P-SiC coating shows the highest hardness of HV501435. Wear tests show that electroless Ni-P- SiC exhibits good wear resistant property. The wear rate is only 30% of that of Ni-P coating and 10% of mild steel substrate, respectively.
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Preparation and Mechanism of Nesting Spherical Layered Closed-cage Structured Nano WS2
ZHENG Yi-Fan,SONG Xu-Chun,LIU Bo,HAN Gui,XU Zhu-De
2004 Vol. 19 (3): 653656
Abstract(
2198 )
PDF(1008KB)(
1014
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WS3 precursors were fabricated by a simple precipitation method. The nano-WS2 particles with nesting spherical layered closed-cage structure were obtaincd by WS3 precursors heated at high temperature in hydrogen atmosphere. The samples were identified and characterized by high-resolution transmission electron microscopy (HRTEM), powder X-ray diffraction (XRD) and energy dispersive X-ray (EDX), and the mechanism of formation was researched.
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Preparing Process and Sintering Behavior of Nano LaAlO3 Powders
LI Wei,ZHUO Ming-Wen,SHI Jian-Lin,WANG Yi-Lin,KAN Yan-Mei,WANG Ling
2004 Vol. 19 (3): 657660
Abstract(
1995 )
PDF(373KB)(
912
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Preparing process and sintering behavior of nano LaAlO3 powders were investigated. The coprecipitation method was applied to synthesize nano LaAlO3 powders. By using La(NO3)3 and Al(NO3)3 as raw materials and keeping pH≈9, the coprecipitation process can be finished at room temperature. Pure LaAlO3 nano powders with a size of about 50nm can be obtained after calcining at 800℃ for 2h. After dry pressing with a pressure of 300MPa, the nano LaAlO3 powders can be sintered at 1500℃ for 4h, and a high density of about 6.2g/cm3 reached.
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Preparation of Ultrafine Ce-Zr-Ba Mixed Oxide Powder with High Surface Area
CHEN Min,ZHENG Pei-Zhuang,HANG Zhi-Bin,ZHENG Xiao-Ming
2004 Vol. 19 (3): 661665
Abstract(
2035 )
PDF(461KB)(
926
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Ultrafine powder of Ce-Zr-Ba mixed oxide was prepared with a macromolecule surface modified method. The typical structure, particle size, surface area and pore structure of the powder were investigated by TEM, XRD, BET and TG-DTA technologies. The results show that the Ce-Zr-Ba mixed oxide powder is nano-sized with the particle size of 50nm, and a high surface area of 119.0m2/g at the calcination of 600℃ for 4h. The surface area of the powder remains 87.4m2/g even calcination at 800℃ for 4h. After calcination at 1000℃ for 4h, it will keep good particle distribution and in nano-sized properties. This powder can be used as the material in three way catalyst (TWC) for its novel character of resistance high temperature and high surface area.
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Metal/Dielectric Multilayers Filter to Suppress the Slow Component of the Scintillation Light in BaF2 Crystal
MA Xiao-Hui,GU Mu,XU Rong-Kun,WU Yong-Gang,CAO Er-Hua
2004 Vol. 19 (3): 666670
Abstract(
2047 )
PDF(204KB)(
1017
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On the basis of the difference of the emission bands between the fast and slow components in BaF2 crystal, the metal/dielectric multilayers filter with several periods of Al2O3/MgF2/Al/MgF2… was designed and developed in order to suppress the slow component of the scintillation light in BaF2. The results from transmission, emission and decay time spectrum show that the film can increase about 80 times of the ratio of the intensities of the fast emission to the slow one and can widen the application field of BaF2 scintillation crystal in high count rate experiments.
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High-Temperature Phase Transformation of Er3+-doped Boehmite (γ-AlOOH) Gels during Sintering
YANG Tao,WANG Xing-Jun,WANG Hui,LEI Ming-Kai
2004 Vol. 19 (3): 671675
Abstract(
1938 )
PDF(218KB)(
911
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The 0~20mol%Er3+-doped γ-AlOOH gels were prepared by using sol-gel methods from the aluminium isopropoxide [Al(OC3H7)3]-derived Al2O3 sols. The phase structures and these transformation processes of Er3+-doped γ-AlOOH gels sintered at 950~1400℃ were investigated by using X-ray diffraction (XRD) and differential thermal analysis (DTA). The experimental results show that Er3+ doping lead to restraining the phase transformation of θ→α for alumina, and decreasing the growth rate of α phase with an increase of 50~70℃ for the completed transformation temperature. The precipitation of the two Er-Al-O compounds, i.e. Al10Er6O24 and ErAlO3 phases, is dependent on the Er3+ doping concentration and the sintering temperature. The ErAlO3 phase precipitates in the 1~5mol%Er3+-doped Al2O3 sintered at 1100~1200℃. The Al_{10Er_6O_{24 phase precipitates in the 5~20mol%Er3+-doped Al2O3 sintered at 1000~1100℃, and is in all Er3+-doped Al2O3 with further increasing the sintering temperature. The nucleation of phase transformation for θ→α is accelerated due to the presence of ErAlO3 phase, resulting in a decrease of 30~50℃ for the beginning temperature of phase transformation correspondingly. It has no greatly influence on the growth rate of α phase. The Al10Er6O24 phase does not affect the phase transformation for θ→α
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Research on Slipcasting Process for BaTiO3-based Chip PTCR
LIU Huan,GONG Shu-Ping,CHEN Yan,ZHENG Zhi-Ping,ZHOU Dong-Xiang
2004 Vol. 19 (3): 676680
Abstract(
2011 )
PDF(341KB)(
1222
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In order to acquire highly concentrated BaTiO3 slurry suitable for slipcasting process, the factors, that may influence the property of slurry, were investigated. The results obtained show that when pH=9 and the weight concentration of PVA and dispersant is 0.8% and 0.4% respectively, the solids loading as high as 80wt%(55vol%) can be achieved. In addition, The PTCR effect of chip PTCR formed by this slipcasting process was examined.
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Ba0.5Sr0.5TiO3 Dielectric Materials Prepared by Citrate-nitrate Combustion
SHEN Cai,LIU Qing-Feng,LIU Qian
2004 Vol. 19 (3): 681685
Abstract(
2185 )
PDF(583KB)(
1167
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Ultra-fine Ba0.5Sr0.5TiO3 (BST) powder was prepared by using barium nitrate, strontium nitrate, tetra-n-butyl titanate, and ammonium hydroxide via citrate-nitrate combustion process. The pH value and dispersant, strongly influencing on the particle distribution of BST powder, were investigated in detail. The precursor powders were pressed into tablets(φ=20.0mm, d=5.0 mm)and then fully sintered at 1300℃ for 2h.At 25℃, the dielectric constant and dissipation factor of the sintered sample were 1470 and 0.006 at 10kHz, respectively, measured by a HP4192A Impedance.
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Effects of Alumina on the Sintering and Conductivity of Yttria-Stabilized Zirconia
LI Ming,HE Li-Ping,CHEN Zong-Zhang,LI Su-Fang,XIANG Lan-Xiang,LUO Shang-Geng,ZOU Chang-Gui,LIANG Xue-Yuan
2004 Vol. 19 (3): 686690
Abstract(
2293 )
PDF(605KB)(
1047
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The effects of the alumina doped through the normal co-precipitation on the sintering and conductivity of Yttria-stabilized zirconia were studied. The study shows that proper addition of alumina can accelerate the process of sintering and improve the sintering density of zirconia, but it does harm to the sintering density of YSZ if the content of alumina is too high; the grain-boundary conductivity increases at first and then decreases with increasing content of added alumina. The reason why grain-boundary conductivity changes with the content of alumina is that alumina segregated to the grain boundary has two opposite effects on the grain boundary: at one side it can scavenge silicon dioxide which blocks ionic transport at the grain boundary, at the other side it decreases the free oxygen ion vacancy concentration.
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Preparation of CdS Thin Films by SILAR Method
LIU Xiao-Xin,JIN Zheng-Guo,BU Shao-Jing,ZHAO Juan,CHENG Zhi-Jie
2004 Vol. 19 (3): 691695
Abstract(
2950 )
PDF(575KB)(
1228
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The SILAR method was applied to prepare cadmium sulfide thin films on a glass substrate at room temperature. The growth rate and surface morphology of the films with cycle times were characterized. The effect of annealing on crystal structure and resistivity of the films was studied. In addition, the growth mechanism of heterogeneous reaction of the thin film was discussed. The results show that the film as-deposited is amorphous and compact, the growth rate is about 2nm/cycle and the size of the particles is increased from 60nm to 100nm with the increase of the cycle times. The crystallinity is increased and the resistivity is decreased with the increase of annealing temperature from RT to 673K.
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Experimental Study on Biomimetic Synthesizing Silica Films at the Air-water Interface
ZHU Li,WANG Yi-Ping,HU Tong-Yu,LI Wei
2004 Vol. 19 (3): 696700
Abstract(
2332 )
PDF(646KB)(
1143
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Free-standing silica films were prepared repeatedly at the air-water interface by the biomimetic synthesis technology, during which the hydrolysis of tetraethyoxysilane (TEOS) was directed by cetyltrimethylammonium bromide (CTAB) supra-molecules assemblies. The effects of material ratio, calcining conditions and DCCA(drying control chemical agent) on the qualities of silica films were investigated. The various characterization results showed that the biomimetic synthesized silica film has a modal pore diameter of 1.8nm and thickness of about 2μm, its upper surface is smooth and integral.
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Effect of Substrate Bias on Crystallization Temperature and Dielectric Properties of Sputtered Ta2O5 Films
XU Shi-Long,ZHU Man-Kang,HUANG An-Ping,WANG Bo,YAN Hui
2004 Vol. 19 (3): 701704
Abstract(
2010 )
PDF(275KB)(
1041
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At the substrate temperature of 620℃, crystalline Ta2O5 films were sputtered by introducing suitable negative substrate bias of 100~200V. It was thought that the ion bombardment to the substrate was enhanced with introducing the negative substrate bias. The diffusion and looseness of deposited particles on the surface of substrate were accelerated. Consequently, the crystallization of Ta2O5 films was improved and the crystallization temperature was lowered. Meanwhile, the C-V result indicated that the dielectric properties of Ta2O5 films were further improved by introducing negative substrate bias.
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