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Review of Cathode Material LiMn2O4 for Lithium Ion Batteries
ZHENG Zi-Shan,TANG Zi-Long,ZHANG Zhong-Tai,SHEN Wan-Ci
2003 Vol. 18 (2): 257263
Abstract(
2335 )
PDF(684KB)(
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Spinel LiMn2O4 has been considered to be the most promising alternative cathode material for the new generation of lithium ion batteries in terms of its low cost, non-toxicity and easy manufacture. However, the capacity fading rapidly upon charge/ discharge cycling, especially at the high working temperature (>55℃), hinders its commercial application. Over the past decade much work has been devoted to the spinel LiMn2O4 and its several fading mechanisms have been proposed such as Jahn-Teller distortion, dissolution of Mn2+ into electrolyte, electrolyte decomposition and transformation of cubic to unstable tetragonal phase, etc. Its capacity retention could be improved much by doping, surface coating and improving preparation technique. The recent developments in cathode material LiMn2O4 have been reviewed in this paper based on the recent results in our research group.
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Growth and Electric Properties of Relaxor Ferroelectric Single Crystal PZNT93/7
XU Jia-Yue,TONG Jian,SHI Min-Li,LU Bao-Liang,ZHANG Ai-Qiong,FAN Shi-Ji
2003 Vol. 18 (2): 264268
Abstract(
1970 )
PDF(645KB)(
1088
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Relaxor ferroelectric single crystal Pb[(Zn1/3Nb2/3)0.93Ti0.07]O3 (PZNT93/7) was grown by a flux-Bridgman method using 50mol% PbO as the flux. Nucleation was modified by O2 gas cooling system at the bottom of Pt crucible. The size of the crucible was 40mm×40mm×300mm. The rate of pulling-down was 0.5mm/h and the rate of oxygen fluid was 1~1.6L/min. The maximum size of the obtained crystals was φ30mm×25mm. The as-grown PZNT crystal exhibits an obvious growth morphology and the largest revealed face is (001) determined by X-ray diffraction. Due to unstability of O2 fluid and slow mass transport, red PbO inclusions are easily formed in the crystal. The measurements of dielectric and ferroelectric properties show that the crystal can satisfy the requirements of array-type transducers in a new type of medical diagnostic equipment.
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Growth and Scintillation Properties of Cerium-doped Lutetium Oxyorthosilicate(Lu2SiO5:Ce) Crystals
REN Guo-Hao,WANG Shao-Hua,LI Huan-Ying,LU Sheng
2003 Vol. 18 (2): 269274
Abstract(
2189 )
PDF(497KB)(
1458
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Cerium-doped lutetium oxyorthosilicate (LSO) crystal with the dimension of φ35mm×40mm was grown by using the Czochralsky method. Due to cerium ion doping, its absorption edge shifts from 195nm of undoped LSO crystal to 380nm. The intensities of ultraviolet excitation wavelength of LSO:Ce decrease by degrees of 380,332,319 and 216nm. The emission of LSO:Ce crystals has the characteristic of band emission and the emission wavelength spans from 390nm to 560nm. The X-ray excited emission also has band characteristics with two peaks of 390 and 426nm. These luminescence properties are related to the electronic transition of Ce3+ ion from its excited 5d levels to two split ground state levels of 4f as well as the existence of two luminescence centers of Ce3+ ion in LSO lattice.
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Phase Formation and Physical Properties of MnxCd1-XIn2Te4 Ingots Grown by the Bridgman Method
CHANG Yong-Qin,AN Wei-Jun,GUO Xi-Ping,JIE Wan-Qi
2003 Vol. 18 (2): 275282
Abstract(
2005 )
PDF(880KB)(
1009
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Diluted magnetic semiconductor MnxCd1-xIn2Te4(x=0.1, 0.22 and 0.4) ingots were grown by the Bridgman method. The structure and composition of different phases and the compositional distribution along the axis and radius of the MnxCd1-xIn2Te4 ingot were analyzed. α+β+β1 structures are formed at the tip of the MnxCd1-xIn2Te4 ingots. Among them, α and β phases are crystallized from the melt while β1 is precipitated from α phase when temperature is below solidus. The content of β phase increases with the growth process, and finally, a pure β phase-region is formed. At the end of the ingots, an In2Te3-type phase with a fcc structure is crystallized. There exist two distinct interfaces between the different neighbouring phase-regions. The band gap of MnxCd1-xIn2Te4 shifts towards the high energy side with the increase of x. At higher temperatures(50~300K) the variation of magnetic susceptibility χ with T in MnxCd1-xIn2Te4 follows the Curie-Weiss (C-W) law. However, a paramagnetic behavior exists at lower temperature (<50K). The antiferromagnetic exchange of Mn2+ increases with the composition, x.
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Empirical Calculations of the Formation Energies of Point Defects in Lithium Niobate
FENG Shao-Xin,LI Bao-Hui,YANG Zhi,JIN Qing-Hua,GUO Zhen-Ya,DING Da-Tong
2003 Vol. 18 (2): 283288
Abstract(
2150 )
PDF(255KB)(
1992
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The formation energies of point defects in lithium niobate crystals were calculated in terms of the inter-ionic potential parameters and shell model parameters, determined by empirical parameterization. The results show that Li Frenkel disorders are the intrinsic defects in stoichio-metric lithium niobate crystals and Li vacancy model is the dominant defect species in congruent lithium niobate crystals.
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Raman Spectra of the Inclusions in KDP Crystals
WANG Sheng-Lai,GAO Zhang-Shou,KONG Yong-Fa,ZHANG Cun-Zhou,FU You-Jun,SUN Xun,LI Yi-Ping,ZENG Hong
2003 Vol. 18 (2): 289294
Abstract(
2106 )
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1209
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The inclusions in KDP crystals were studied by using laser microscope Raman spectrum technique. Water solution was found in the spherical inclusions between pyramid sectors, while CO2 and H2S in the prolate inclusions in expanded prismatic sectors besides water solutions. These impurities were also found in the crystals with dense scatters. The results show that the compositions differences in above inclusions are related to different growth mechanisms on the prismatic and the pyramidal faces of the crystal. The existence of these impurities in growing solution is one of the factors to generate the inclusions as well as scatters in crystals.
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Adaptability of Glass Properties Estimating Model for GRIN Optic Elements
HAO Yin-Lei
2003 Vol. 18 (2): 295300
Abstract(
2485 )
PDF(362KB)(
1106
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Glass properties estimating models based on uniform and stress free glasses encounter certain discrepancy from measured value when being used for refractive index change (ΔN) estimation in gradient index (GRIN) optic element prepared by ion exchange. A comparison was made between HSD model and Gan Fuxi model in this paper. Result shows that Gan Fuxi model generates relatively low aberration when being used to calculate in lightly stressed GRIN optic element, but becomes invalid in heavily stressed GRIN optic element; While HSD model is much more adaptive on estimating in heavily stressed GRIN optic element, for involving polarizability factor and volume factor of glass composition separately.
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Structure and Electrochemical Properties of Nd-doped LiMn2O4 Spinel
YANG Shu-Ting,JIA Jun-Hua,CHEN Hong-Jun
2003 Vol. 18 (2): 301306
Abstract(
2067 )
PDF(250KB)(
1103
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LiMn2-xNdxO4 spinels doped with a wide range (x=0.005~0.1) of rare earth element (Nd) were synthesized. The result of the specific capacity dependence on x value shows that the sample with x=0.01 has the highest capacity among the samples. The structural change during cycles of LiMn2-xNdxO4(x=0.01) spinel was studied by X-ray powder diffraction which shows that the samples maintain spinel structure and after 100 cycles the symmetry of the unit cell increases. The charge-discharge curves of the obtained spinel show that after 100 cycles the capacity loss is only 14.9% which shows that the structure of LiMn2-xNdxO4(x=0.01) is stable. The FTIR spectra of LiMn1.99Nd0.01O4 samples indicate that there is no intense reaction between positive material and the electrolyte, but the trace of the H+/Li+ exchange may be the cause of the little capacity loss.
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Electrochemical Characteristic of SEI in Secondary Lithium Batteries
LIU Yu,WANG Bao-Feng,XIE Jing-Ying,YANG Jun,CHEN Jian
2003 Vol. 18 (2): 307312
Abstract(
2885 )
PDF(459KB)(
2087
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The SEI (solid electrolyte interphase) film on the surface of three kinds of carbonous materials: Mesocarbon Microbead (MCMB); Porous Carbon (PC) and Synthetic Graphite (SG), which can electrochemically insert and extract lithium reversibly, was investigated in the appointed electrolyte. The formation of SEI is related to the structure and BET surface of the carbonous materials. This causes the main irreversible capacity of carbonous electrode at the first charge and discharge cycle. It will play an active role for the cycle stability after the first charge and discharge cycle when the stable film is forming on the surface of the electrode.
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Application of the Low-heating Solid-state Reaction Method in Preparation of Multi-metal Oxides Composite -Synthesis, Structure and Electrochemical Properties of Rhombohedral LiMnO2 Cathode Material for Lithium-ion Batteries
TANG Xin-Cun,HE Li-Ping,CHEN Zong-Zhang,JIA Dian-Zeng
2003 Vol. 18 (2): 313319
Abstract(
2181 )
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1250
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LiMnO2 compounds with rhombohedral structure were prepared by the low-heating solid-state reaction method at the temperature range of 350~700℃. The powder X-ray diffraction technique was applied to investigate the structures of the obtained samples. XRD result shows that the structures of these samples are the same as that of LiCoO2. Compared with LiCoO2 and LiCo0.8Ni0.2O2 prepared by the same method, the lattice parameter of r-LiMnO2, c/a, is relatively smaller due to the Jahn-Teller deformation. Selected-area electron diffraction and XRD results indicate the existence of the cubic spinel impurities in the r-LiMnO2 samples sintered at 600℃ and 700℃. The tests of charge/discharge show that the samples prepared above 600℃ have two voltage plateaus of 3V and 4V, of which the plateau at 4V is related to the cubic spinel impurities. Whereas, the samples obtained below 500℃ present only one plateau of 3V. Especially, the sample obtained at 500℃ exhibits good structural stability in lithium-ion intercalation/deintercalation processes.
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Study on Modified PZT95/5 Ferroelectric Ceramics
DU Hui,SUN Da-Zhi,ZHONG Ni,QU Cui-Feng,YAO Chun-Hua,JIN Qi-Hua,LIN Sheng-Wei
2003 Vol. 18 (2): 320324
Abstract(
2057 )
PDF(343KB)(
1314
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PZT95/5 samples were prepared with the conventional ceramic process. Based on the principle of “the same valance, different ionic radius; similar ionic radius, different valances”, the additives such as alkali-metal carbonates, alkali-earth-metal carbonates, Fe2O3, SiO2, Nb2O5 and WO3 were doped into the PZT95/5 separately. The dielectric properties, polarization properties and FRL-FRH phase transition behavior were studied. The acceptor additives make dielectric constant of the material decrease, and the donor additives demonstrate the opposite effect; The remnant polarization in the material climes up with the increase of the cationic valances of additives; The pure PZT95/5 ferroelectric material obtained possesses FRL-FRH phase transition temperature at 15℃ , this is significant for its application.
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Structure and Dielectric Properties of (Sr,Ca)TiO3 Ceramics
LIU Yue-Hui,CHEN Xu-Ming
2003 Vol. 18 (2): 325330
Abstract(
1817 )
PDF(546KB)(
1348
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The phase component, structure and dielectric properties of (Sr,Ca)TiO3 systems were studied. When ST/CT ratio is 7:3, a main crystalline phase (Sr0.7Ca0.3)TiO3 complete solid solution with the ABO_3 perovskite structure is formed, the dielectric properties are improved by a microscale next crystalline phase BNT(Ba6Ti2Nb8O30) with the tungsten bronze structure in the system. The new ceramic materials with excellent dielectric properties (ε(20℃ 1MHZ)≥250, αc(-55~+125℃)=-1150ppm/℃, tgδ(20℃ 1MHZ)<5×10-4, ρv(20℃ 100VDC)≥1013Ω·cm) do not contain lead or bismuth , and can be used for Q group multilayer ceramic capacitors.
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Electrochemical Capacitor Using Nickel Oxide/Carbon Nanotube Composites Electrode
WANG Xiao-Feng,WANG Da-Zhi,LIANG Ji
2003 Vol. 18 (2): 331336
Abstract(
2264 )
PDF(422KB)(
1664
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Carbon nanotubes prepared by a catalytic pyrolysis method were considered as active electrode materials for the storage of energy in supercapacitors. Due to their unique mesoporosity, this material has a high ability for the accumulation of charges in the electrode/electrolyte interface. Electrochemical capacitors based on carbon nanotube/nickel oxide composite electrodes were developed through the electrochemical deposition of nickel oxide on the nanotube electrode. The value of capacitance obtained from nanotubes modified by nickel oxide reaches 52F/g. The self-discharge rate of this supercapacitor is much lower than that of the supercapacitor composed of carbon nanotube electrode.
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Oxidation Behavior of Aluminium Nitride
XU Xin-Rui,YAN Wei-Lin,ZHUANG Han-Rui,LI Wen-Lan,XU Su-Ying
2003 Vol. 18 (2): 337342
Abstract(
1871 )
PDF(749KB)(
1268
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The effects of atmosphere and humidity at different temperatures on the behavior of aluminium nitride were investigated. The resules obtained show that the oxidation behavior was greatly affected by the humidity. The oxidation of aluminium nitride at 1225℃ in wet N2, wet N2:O2=10:1 and wet air follows a parabolic rate law, while the oxidation in dry air follows a linear rate law. On the other hand, the oxidation kinetics in dry air is linear between 1100℃and 1300℃ with an activation energy of 233kJ/mol, and then arabolic above 1300℃
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Gelcasting of Alumina with Low-toxicity HEMA System
CAT Kai,HUANG Yong,YANG Jin-Long
2003 Vol. 18 (2): 343347
Abstract(
2375 )
PDF(518KB)(
1019
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The industrialization of gelcasting technique based on the acrylamide system has been prevented to some extent because acrylamide is a neurotoxin monomer. In this paper another gelcasting based on the polymerization of low-toxicity 2-hydroxyethyl methacrylate (HEMA) was successfully developed. The rheological properties of alumina suspensions with two dispersants, JN281 and tri-ammonium citrite (TAC), in the new system were compared. The results show that JN281 is more effective for the new system than the frequently used TAC. High solids loading ceramic suspension with low viscosity can be prepared by addition of JN281. The green bodies made through the new system have smooth surface with a dried green strength of 18MPa. The SEM photos also indicate that the green bodies have a homogeneous microscopic structure. Dense complex-shape ceramic parts were successfully produced through the new gelcasting system.
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Preparation of Machinable Zirconia Ceramics as a Dental Prosthetic Material
RONG Tian-Jun,ZHAO Yun-Feng,WANG Shi-Wei,ZHANG Yu-Feng,HUNAG Xiao-Xian,GUO Jing-Kun
2003 Vol. 18 (2): 348352
Abstract(
2173 )
PDF(582KB)(
1992
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The zirconia ceramic as a dental prosthetic material was prepared by liquid-phase sintering with CaO2-Al2O3 -SiO2 glass as the sintering aid. And the bending strength, fracture toughness, thermal expansion and machinable property of the sintered bodies were valued. The results obtained show that (1) CaO2-Al2O3-SiO2 glass is effective to lower the sintering temperature of zirconia ceramic to 1300℃; (2) the machinability of the dental prosthetic zirconia ceramic is comparable to that of In-Ceram; (3) its thermal expansion coefficient is 8.15~ 7.19×10-6/℃, bending strength is 360~340MPa and fracture toughness is 3.5~2.7MPa·m1/2.
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Conductive Property of Recrystallized Graphite Doped with Titanium and Silicon
QIU Hai-Peng,SONG Yong-Zhong,SHI Jing-Li,ZHAI Geng-Tai,LIU Lang
2003 Vol. 18 (2): 353360
Abstract(
2161 )
PDF(889KB)(
1108
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The bi-element doped recrystallized graphite was prepared from calcined coke, coal-tar pitch, titanium and silicon by a hot-pressing process in order to investigate the effects of the amount of dopants on the thermal conductivity, electrical resistivity, bending strength and microstructure. Experimental results show that the basic physical properties of recrystallized graphite with 15wt% of dopant titanium are improved greatly, compared with pure graphite prepared by the same process. The thermal conductivity of recrystallized graphite with 15wt% of titanium and less than 2wt% silicon increases with increasing the amount of silicon at ambient temperature. The thermal conductivity of RG-TiSi-152 with 15wt% titanium and 2wt% silicon is 494W/m·K. The thermal conductivity of bi-element doped recrystallized graphite with 15wt% titanium and more than 2wt% silicon decreases with increasing the amount of silicon at ambient temperature. The electrical conductivity and bending strength of silicon and titanium doped recrystallized graphite decrease with increasing the amount of silicon. XRD analysis indicates that titanium added to carbon substrates exists in the form of TiC precipitates and much of silicon added to carbon substrates will escape from the material at last. The layers spacing d002 and coherence length La of RG-TiSi-152 are 0.3355 nm and 864nm, respectively.
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Charaterization of Graphitization Degree of C/C Composites by Laser Raman Microspectroscopy
ZHANG Fu-Qin,HUANG Qi-Zhong,HUANG Bai-Yun,GONG Qian-Ming,CHEN Teng-Fei,XIONG Xiang
2003 Vol. 18 (2): 361366
Abstract(
2308 )
PDF(838KB)(
2022
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The structural parameters of carbon fiber, pitch-derived carbon and pyrolytic carbon in C/C composites were charaterized by laser Raman microspectroscopy and XRD. In Raman spectra of these carbons, two bands named D and G were observed near 1336.73cm-1 and 1581.00cm-1 respectively, the peak positions do not but the relative intensities of the two bands change with heat treatment temperatures. The relationship between the XRD data of graphitization degree g and R-1 where R is the relative intensity of band D to band G was plotted, the result shows that g increases with the increase of R-1, but the gradient of the R-1-g curve decreases and gradually tends to zero with the increase of R-1, and their relation can be written into the following equation: g=1-e-2.11(1/R-0.34). The foundation of the correlation between R-1 and g makes it possible to analyze the local distribution of graphitization degree in C/C composites.
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Preparation and Photoluminescence Properties of ZnO/BaTiO3 Nanocomposite System
YAO Li,YANG Bei-Fang
2003 Vol. 18 (2): 367372
Abstract(
1819 )
PDF(568KB)(
1083
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The ZnO/BaTiO3 nanocomposite system was prepared by a sol-gel method. The particle size, structure and phases of the nanocomposite were studied by XRD and TEM. In addition, enhanced photoluminescence of the nanocomposite under 370nm light excitation was observed at room temperature. The blue-green emission peak induced by oxygen vacancies of nano-ZnO particles, has blue-shift or red-shift with different heat-treatment temperatures, the blue-shift is assigned to quantum size effect, and the red-shift is attributed to the high dielectric environment effects of the BaTiO3 matrix.
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Microstructure Evolution of ZrO2-(Al2O3, Fe2O3) Materials Synthesized by Frozen-drying
LI Rui-Xing,YIN Shu,CHEN Lan,YU Ke-Ning,LI Shao-Hua,LIANG Huan-Zhen,SATO Tsugio
2003 Vol. 18 (2): 373378
Abstract(
2169 )
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1046
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Precursor powders of ZrO2-Al2O3, ZrO2-Fe2O3 and ZrO2-(Al2O3, Fe2O3) systems were produced by frozen-drying. Their phases transformation and microstructure were developed at deferent temperatures and sintering durations. Microstructure with fine grains was obtained in the ZrO2-(Al2O3, Fe2O3) system for the composition (ZrO2:Al2O3:Fe2O3=60:32:8 mol%) sintered at 1400℃ for 15h. The results obtained show that Fe2O3 has the effect of glomeration of grains in ZrO2 base ceramic materials.
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Formation of Cross-Linking Montmorillonite Nanocomposites by Adopting Chromium Compound
XIAO Zi-Jing,DAI Jing-Cao,YE Ling
2003 Vol. 18 (2): 379384
Abstract(
1843 )
PDF(251KB)(
1000
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The interlayered cross-linking of a 2:1 type montmorillonite with chromium cluster compound[Cr3O(OOCCH3)6(OH2)3]Cl·6H2O (namely CrC) was studied by X-ray diffraction, infrared analysis, differential thermal analysis, specific surface and ammonia adsorption measurement. Its preparation method, various influencing factors and some physical and chemical properties were also dealt with. As indicated by the results, the synthesis conditions such as species, size and Cr/Al molecular ratio of cross-linking agent greatly affect an interlayer space(d001); whereas an interlayer space of nanocomposite, CrC/clay ratio and Cr/Al molecular ratio of cross-linking agent play a very important role, influencing on surface properties and thermal stability of cross-linking montmorillonite nanocomposites.
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Interaction, Non-crystalline Structure and Catalysis Property on the Interface of Five Binary Transition Metal Oxides (I) Suggestion of Interface Non-crystalline Dispersion and Bulk Crystal Residual Ratio
WANG Zhi-Min,LI Li,HAN Ji-Xin,HAN Wei-Ping
2003 Vol. 18 (2): 385392
Abstract(
2116 )
PDF(511KB)(
1196
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The interaction and non-crystalline spontaneous dispersion at the interface of five systems of transition metal binary oxide, namely, TiO2(anatase)-MoO3, MoO3-V2O5, Fe2O3-MoO3, WO3-MoO3 and ZrO2-MoO3 containing 0~100wt% MoO3 respectively, were characterized by XRD, BET, FT-IR. The five systems were prepared by dry mixing and grinding up at room temperature, and then calcining at appropriate temperatures below melting point of two component oxides(500℃/5h). XRD quantitative analysis and extrapolation of crystal phase content indicate that each component oxide disperses spontaneously to form a non-crystalline phase at interface, and has a dispersed threshold value (the maximum dispersion capacity). BET measurements show the specific surface area of all samples are much smaller(3.71~11.3m2/g) than that of the supports such as γ-Al2O3 SiO2 and TiO2 gel etc. The dispersed threshold values of MoO2 (0.33~1.43g·10-2cm-2 determined by XRD and BET in the present paper are far greater than the monolayer dispersion capacity of MoO3 (0.117g·10-2cm-2) calculated from TANG’s model of O2- close-packed monolayer dispersion and also larger than MoO3 monolayer dispersion capacity(0.169g·10-2cm-2) calculated from the spherical octahedron model suggested in our ensuing paper. Such larger dispersed threshold value in the much smaller specific surface area signifies non-monolayer dispersion and/or chemical reaction at interface. By means of FT-IR spectra and its differential spectra, the new species of non-crystalline phase at interface and its characteristic absorption bands are discovered for the first time, and these bands are correlated to molecular structure, such as IR characteristic absorption bands of non-crystalline phase MoO3 appear at 960 and 826~828 cm-1.
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Effects of Annealing on the Optical Absorption of CdS/SiO2 Assembly
YANG Yi-Jun,KAN Cai-Xia,BI Hui-Juan,ZHANG Li-De
2003 Vol. 18 (2): 393399
Abstract(
1823 )
PDF(514KB)(
1297
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Monolithic mesoporous silica was prepared by sol-gel technique and the CdS/SiO2 assembly systems with different CdS loading were obtained by immersing followed by drying and thermal reaction. The effects of annealing temperature, ambiencent and loading on the optical absorption of CdS/SiO2 were investigated. It is found that the optical absorption edges of the CdS nanoparticles in mesoporous silica shift to the red as CdS loading concentration increases. The optical absorption edges red-shift along with the increase of annealing temperature under nitrogen and blue-shift under air were observed, which can be attributed to the quantum size effect.
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Synthesis and Characterization of Three-Dimensionally Ordered Macroporous (3DOM) Titania-Silica Mixed Oxides
SHEN Yong,WU Quan-Zhou,LIAO Ju-Fang,LI Yu-Guang
2003 Vol. 18 (2): 401406
Abstract(
2059 )
PDF(1131KB)(
1111
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Three-Dimentionally Ordered macroporous titanium-silica mixed oxides were successfully synthesized by using polystyren sphere colloid crystal as the template and the sol of tetraethyl silicate and tetrabutoxy-titane as the filling fluid. The sol filled in the voids among spheres by capillary forces, and then transformed into gel in situ. Latex spheres were removed by calcination(<5℃/min; 300℃,5h; 570℃, 5h). The macroporous samples show a beautiful iridescence in reflected light. SEM indicates that the pores are about 500nm in size and arrayed periodically in a face-centered cubic (fcc) structure and connected with each other by small windows. EDS indicates that the Si/Ti molar ratio is 2.7. XRD indicates the wall of the pores is amorphous.
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Preparation of SiO2 Aerogel by Rice Husk
HOU Gui-Hua
2003 Vol. 18 (2): 407412
Abstract(
2067 )
PDF(564KB)(
1350
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A SiO2 aerogel was prepared with rice husk, being cooked in boiling solution of diluent hydrochloric acid, then dried, and then pyrolyzed. The results show that the SiO2 mass content in aerogel is 99.99%, the average particle size is 20.77μm, and the specific surface area is 251m2/g determined by ICP-AES, particle size analyzer and surface area & pore size analyzer respectively. The structure transformation of rice husk during the aerogel preparation was investigated by XRD, IR and SEM.
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Electrical Properties of Pseudo-binary Alloys (PbTe)1-x(SnTe)x; Sintered at Different Temperatures
CUI Jiao-Lin,QIAN Xin,ZHAO Xin-Bing
2003 Vol. 18 (2): 413420
Abstract(
1835 )
PDF(794KB)(
1006
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Pseudo-binary alloys (PbTe)1-x(SnTe)x (x=0~1) were firstly prepared by the powder metallurgy method and their electrical properties were experimentally investigated. The results show that the grain size and pore size of the alloys sintered at higher temperature are larger than those sintered at lower one. The maximum Seebeck coefficients decrease with mole fraction x increasing, whereas the temperature, corresponding to the maximum Seebeck coefficients, shifts to higher temperature side when x ranges from 0 to 0.6, and remains almost unchanged when x>0.6. The electrical conductivity reaches the maximum when mole fraction x equals to 0.6. Besides, both Seebeck coefficients and electrical conductivities for all of the alloys sintered at high temperature reveal similar variation with the temperature to those sintered at lower one, not only the Seebeck coefficients but also the electrical resistivities for the alloys sintered at 550℃, however, are lower than those for the alloys with the same mole fraction but sintered at 725℃ when x≥0.2. It can be concluded, therefore, that the resultant electrical properties are little influenced by sintering temperature for the pseudo-binary alloys (PbTe)1-x(SnTe)x.
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Preparation and Optical Properties of Au/BaTiO3 Nanoparticle Composite Thin Films
DAI Shu-Gang,YANG Yong,HUANG Wei-Min,SHI Jian-Lin
2003 Vol. 18 (2): 421426
Abstract(
2001 )
PDF(489KB)(
1121
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High doping level of Au nanoparticles was successfully incorporated into sol-gel derived amorphous BaTiO3 thin films, and the optical properties of samples were studied. The characteristics of samples were investigated by using XRD, TEM, absorption spectra, and OKE(Optical Kerr Effect) techniques. Red shift of SPR (surface plasma resonance) absorption along with the increase of treat temperature was observed by absorption spectra. Films exhibited a larger third nonlinear susceptibility χ(3) and superfast response time in the nonlinear optical test.
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Formation Mechanism of Ternary Carbide Ti3AlC2 by Combustion Synthesis
GE Zhen-Bin,CHEN Ke-Xin,GUO Jun-Ming,ZHOU He-Ping,NING Xiao-Shan
2003 Vol. 18 (2): 427432
Abstract(
2018 )
PDF(889KB)(
1118
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The formation mechanism of Ti3AlC2 powders by the combustion synthesis was investigated by analyzing the microstructure and phase content of the quenched sample. The results show that the mechanism of the reaction is a solution- precipitation mechanism: at first previously formed TiC particles dissolve in the Ti-Al melt, followed by the precipitation of ternary phase Ti3AlC2 that will grow into a layered morphology. The model of combustion synthesis of Ti3AlC2 can be divided into four stages: unreacted stage, preheating and initial reacting stage, dissolution and precipitation stage, completely reacted stage.
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Effects of Paddle s Types on the Preparation of Ultrafine goethite Particles
FAN Hong-Lei,SONG Bao-Zhen,YANG Zhen-Qiu,LIU Ju-Hua,ZHANG Jian
2003 Vol. 18 (2): 433438
Abstract(
1754 )
PDF(616KB)(
1309
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Typical stirring paddles inducing radical flow and axial flow as well as axial and radical flow were selected in order to investigate their effects on the process of goethite preparation. Experimental results show that PBT (pitched blade turbine) inducing axial and radical flow reveals good dispersibility and complete mixing properties, and makes apparent reaction rate of the system larger. Moreover, with the increase of reaction time, the viscosity value of reaction system becomes large at first, and then amounts to a plateau, increases again at last. At the same time, ultrafine goethite particles prepared by PBT are with narrow particles’ size distribution, uniform morphology and few dendrities.
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Preparation of Nanocrystal Y2O3:Eu by the EDTA Complexing Sol-Gel Method
ZHAI Yong-Qing,YAO Zi-Hua,DING Shi-Wen,QIU Man-De,ZHANG Yi-Cao,AN Wei
2003 Vol. 18 (2): 439444
Abstract(
694 )
PDF(398KB)(
929
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Nanocrystal Y2O3:Eu was synthesized by the EDTA complexing sol-gel method at lower temperature using metal nitrate and EDTA as raw materials, the synthesis condition was optimized. The pyrolytic decomposition mechanism of the gel, formation process of Y2O3:Eu and the properties of the particles were investigated by TG-DTA, XRD, FTIR, SEM, Fluorescence Spectrophotometer. The results show that nitrate ions accelerate the decomposition of the EDTA-gel, and fine, homogenous, pure cubic phase Y2O3:Eu nanocrystal can be produced after the dry gel calcinated at 600℃ for 2h. The nanoparticles of the Y2O3:Eu are basically spherical in shape, about 20nm and 70nm in size respectively at 600℃ and 1000℃.
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Synthesis and Characterization of CdS Nanoparticles Modified with Organic
YAO Jian-Xi,ZHAO Gao-Ling,HAN Gao-Rong
2003 Vol. 18 (2): 445450
Abstract(
737 )
PDF(519KB)(
1011
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Surface-modified CdS nanoparticles were synthesized by using thiourea. PVP (poly N-vinyl-2-pyrrolidone) was used as the stabilizer. The structure and characterization of the nanoparticles were characterized by means of TEM, XRD, UV-absorption, FT-IR, and PL spectroscopies. The results demonstrate that the surface-modified CdS nanoparticles have excellent properties in the size distribution and optic qualities.
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Inorganic Sol-Gel Process of Preparing Long Afterglow Luminescent Powders
XIONG Yu-Hong,WANG Dong,LU Yi-Qing,LI Yong-Xiang,YIN Qing-Rui
2003 Vol. 18 (2): 451456
Abstract(
2145 )
PDF(613KB)(
1009
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The stable transparent sol of SrAl2O4 was successfully prepared by using cheap inorganic materials
as precursors. The uniform needle-like nano-powders were synthesized at low temperature and reduce atmosphere. The conditions and factors of preparing
the long afterglow powders of SrAl2O4:Eu2+,Dy3+ by sol-gel process were reported systematically. The microstructures and surface shapes
of samples were observed by the transmission electron microscope (TEM). The crystallization processes were determined by the X-ray diffractometer
(XRD). The luminescent properties were studied by the fluorescence spectrophotometer. The experimental results show that the luminescent features of samples
synthesized by the sol-gel process under the proper conditions are similar to those by solid-state reaction process, but the sintering temperature is reduced about 300℃.
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Influence of Ag Additive on the Microstructure of TiO2 Powders
HE Chao,YU Yun,ZHOU Cai-Hua,HU Xing-Fang,LARBOT Andre
2003 Vol. 18 (2): 457464
Abstract(
2068 )
PDF(722KB)(
989
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Ag-doped TiO2 powders were prepared by a sol-gel process. The influence of Ag doping on the microstructure and phase transformation behaviors of TiO2 powders was investigated by means of XRD, SEM, DSC-TG, SEM-EDX and N2 absorption. The results show that Ag dopant promotes TiO2 anatase to rutile transformation but depresses the growth of anatase grains, decreasing anatase grain sizes and increasing the specific surface area of TiO2 powder. The Ag doping therefore exhibits a great potential in improving the TiO2 photocatalytic activity.
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Elastic, Dielectric, Piezoelectric and Electromechanical Properties of Tetragonal Pb(Mg1/3Nb2/3)O3-PbTiO3 (PMN-PT)
CAO Hu,FANG Bi-Jun,XU Hai-Qing,LUO Hao-Su
2003 Vol. 18 (2): 465469
Abstract(
2030 )
PDF(215KB)(
1260
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Relaxor ferroelectric single crystal Pb(Mg1/3Nb2/3)O3-38%PbTiO3 (PMNT62/38) was grown directly from melt by a modified Bridgman technique. The XRD analysis confirms that PMNT62/38 single crystal has a tetragonal structure at room temperature. The εr-T peak at Tc and little dispersion over measured temperature range indicate that the PMNT62/38 single crystal is a normal ferroelectric. The full set of electromechanical properties was determined by using an impedance resonance technique, the Curie temperature being about 174℃, piezoelectric constant d33~300pC/N, and permittivity ε33~734 and ε11~4301. Electric-mechanical coupling coefficients measured are k33 84.6%, kt 60.8%, k31 44.5% and k15 45.9%.
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Influence of Temperature Gradient on Radiation Damage of BGO Crystals
XIAO Hai-Bin,HU Guan-Qin,XU Li
2003 Vol. 18 (2): 470474
Abstract(
1964 )
PDF(240KB)(
1134
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In this work, we grew two types of Bi4Ge3O12 (BGO) crystals in different temperature gradient by Bridgmen-Stockbarger technology and compared the optical transmissions and energy resolutions of the two types of BGO crystals before and after ultraviolet irradiation. It was found that the optical transmissions and energy resolutions of the two types of BGO crystals are similar before UV-irradiation. After UV-irradiation the optical transmissions at 480nm of the first type of BGO crystals which were grown in high temperature gradient cut down about 20% and their energy resolutions obviously changed bad from about 12% to 18%. But the optical transmissions and energy resolutions of the second type of BGO crystals which were grown in low temperature gradient keep unchanged on the whole. After 250℃/4h annealing, the optical transmissions and energy resolutions of the second type of BGO crystals can completely be recovered. Whereas the optical transmissions and energy resolutions of the first type of BGO crystals can’t completely be recovered until through 800℃/8h annealing. The thermoluminescence curves of the two types of BGO crystals show that there is a luminescence peak at 85℃ for second type of BGO crystal, whereas for the first type of BGO crystals, besides at 85℃, there are also two luminescence peaks at 130℃ and at 170℃ which may show that there exist defects with deeper traps in the first type of BGO crystals. The reason for the difference between the first and second type of BGO crystals may be that if the temperature drop dawn too fast during crystal growing, the defects in the melt can not spread out to the surface and so the defects easily exist in the first type of BGO crystals.
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Effect of the Substitution of Zinc on the Microstructure of β-Tricalcium Phosphate
FENG Zu-De,JIN Pu,MI Jin-Xiao,QIU Xing-Ping
2003 Vol. 18 (2): 475479
Abstract(
2093 )
PDF(310KB)(
1031
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X-ray diffraction and infrared absorption analysis were carried out on zinc-doped beta-tricalcium phosphate prepared by a liquid-phase reaction technique. Quantitative methods and regression analysis were used to calculate the variation of lattice constants of TCP, and the shift or degeneracy of the PO3-4 infrared absorption bands. X-ray diffraction analysis indicates that zinc can substitute calcium up to 20 atom %, inducing a statistically significant decrease of the lattice constants a and b. As the zinc content in TCP increases beyond 20 atom %, X-ray diffraction analysis shows the appearance of a new phase α-CaZn2(PO4)2. However, the effect of substitution of zinc on the lattice constant c is abnormal. The substitution of Zn up to 10 atom % results in a general decrease of the lattice constants c, while it increases as the content of zinc in TCP increases beyond 10%. FTIR spectra reveal that the substitution of Zn up to 10 atom% results in a statistically significant increase of the asymmetric P--O stretching vibration absorption band at 1045 and 1120cm-1 (P<0.05) and a statistically significant decrease of O--P--O bending vibration absorption band at 605cm-1 (P=0.00085), respectively.
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Properties of Long Afterglow SrAl2O4:Eu2+, Dy3+ Phosphor
GENG Jie,WU Zhao-Ping,CHEN Wei,LUO Lan
2003 Vol. 18 (2): 480484
Abstract(
2094 )
PDF(301KB)(
1202
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SrAl2O4:Eu2+, Dy3+ powder phosphors were synthesized by solid-state reaction process. Based on the XRD peaks, the powder phosphors were identified as SrAl2O4 phase, which is monoclinic(a=8.4428A, b=8.822A, c=5.1607A, β=93.415℃). These phosphors exhibited broadband peaks in both the excitation and emission spectra. The excitation peaks lied between 300nm and 450nm, and the main emission peaks lied around 518nm. The results indicate that the luminescence of these phosphors are due to 4f65d→4f7(8S7/2) transition of Eu2+. And its luminescence decay consists of the initial fast process and the later extremely slow process. The trap level of phosphors was analyzed through thermoluminescent spectra, which consists two peaks. This means that there are two electron traps in SrAl2O4: Eu2+, Dy3+, which can cause the long afterglow of the phosphors. The trap depths measured are 0.38eV and 1.34eV respectively.
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Synthesis and High Temperature Resistance Properties of Silver Loaded Fluorapatite Antibacterial
YE Bin,CUI Kai,FENG Qing-Ling,CHEN Guo-Qiang,CUI Fu-Zhai
2003 Vol. 18 (2): 485489
Abstract(
2155 )
PDF(674KB)(
1426
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Amorphous silver loaded fluorapatite powders with nano-sizes were prepared by the coprecipitation method. The silver loaded fluorapatite antibacterial was obtained after calcining the powders at 1000℃ for 3h. The antibacterial was characterized by TEM, XRD, AAS, SEM and antibacterial test. The results show that the antibacterial still has full antibacterial effect after calcining at 1350℃ for 3h.
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Study on the Texture of AIN Thin Films by Using the Pole-figure Method
XU Xiao-Hong,WU Hai-Shun,MA Wen-Jin,DUAN Jing-Fang,LI Zuo-Yi
2003 Vol. 18 (2): 490494
Abstract(
2180 )
PDF(290KB)(
1121
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Based on the X-ray diffraction results, the textures of aluminium nitride films were investigated by using the pole-figure method. Aluminium nitride thin films prepared have a high (002) plane texture, and most of the c-axis of particles are parallel with the normal of the substrate. Aluminium nitride thin films with (100) orientation are necessary, as they are applied to surface acoustic wave devices, and the pole-figure results are very useful for determining the c-axis of particles direction in the A1N (100) thin films.
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Preparation of Nanocrystalline TiN Film by Direct Nitridation of TiO2 Film
JIANG Hong-Bo,GAO Lian,LI Jing-Guo
2003 Vol. 18 (2): 495499
Abstract(
1787 )
PDF(588KB)(
1014
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At first, nanocrystalline TiO2 films were prepared by a sol-gel method on Al2O3 substrates. Then, nanocrystalline TiN films were successfully obtained by direct nitridation of the nano TiO2 films using NH3 as the reductant agent in a tube furnace. XRD, XPS and FE-SEM were used to study phase compositions and morphologies of the nanocrystalline TiN films. The results indicate that the best condition for preparing nanocrystalline TiN films by direct nitridation of films is nitridation temperature about 700℃ and nitridation duration of about 1h.
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Fabrication of LiCoO2 Thin-film Electrode by Soft Solution Processing
TAO Ying,CHEN Zhen-Hua,ZHU Bao-Jun,HUANG Wei-Zhuang
2003 Vol. 18 (2): 500504
Abstract(
1817 )
PDF(449KB)(
1286
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Thin films of lithium cobalt oxides were synthesized by the soft solution processing in a home-made solution. Films of LiCoO2 were deposited onto nickel substrates at 100℃ without any postsynthesis annealing. Their structure and chemical composition were checked by X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectrometry, cyclic voltammograms, and galvanostatic charge-discharge pattern analysis. The prepared LiCoO2 films show R3m crystallinity and preferred orientation of (101). the films grow layer by layer with homogenous grains, whose diameters are about 0.3μm. The thin-film electrode displays a good cyclic character and its first discharge capacity is 143mAh/g. LiCoO2 films made by soft solution processing can be used as cathode materials in lithium microbatteries.
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Influence of the TiCl4 Hydrolysis Condition on the Phase Transfer mation
SUN Jing,Gao Lian
2003 Vol. 18 (2): 505508
Abstract(
2624 )
PDF(0KB)(
3938
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Rutile titania powders were synthesized by directly hydrolysis of TiCl4 solutions at 70℃. The precipitates can be transformed into anatase phase without filtering and separation by varying pH of the system. Anatase titania can be transformed into rutile after calcination at 700℃. These phenomena were explained from the viewpoint of structure.
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Microwave-assisted Acid Dissolution of α-Al2O3
WU Xian-Xin,CHEN Tian-Yu
2003 Vol. 18 (2): 509512
Abstract(
2039 )
PDF(141KB)(
1094
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A method for the acid (HC1 or HNO3)dissolution ofα-Al2O3 by MARS-5 microwave digestion system was proposed. When the temperature of digestion system increased to 240℃,α-Al2O3 sample was dissolved by HC1 or HNO3. When the digestion reagent mass was constant, the digestion time was directly proportional to the sample mass. The digestion time was prolonged when the ratio of α-phase in Al2O3 sample was increased.
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