Preparation and characterization of nanocomposite MgFe<Subscript>2</Subscript>O<Subscript>4</Subscript>/SiO<Subscript>2</Subscript>

Nanocomposites MgFe₂O₄/SiO₂ were successfully synthesized by the sol-gel method in the presence of N, N-dimethylformamide (DMF). The formation of pure MgFe₂O₄ was confirmed by powder X-ray diffraction (XRD) and electron diffraction. The structural evolution of MgFe₂O₄ nanocrystals was followed by powder X-ray diffraction and IR absorption spectroscopy. The formation of spinel structure of MgFe₂O₄ started at 800 °C, and completed at 900 °C. The transmission electron microscopy (TEM) measurements suggest that the particle sizes increase with the increasing annealing temperature, and the mean particle sizes of the spherical samples annealed at 800 °C, 900 °C and 1 050 °C are ca. 3 nm, 8 nm and 11 nm, respectively. Magnetization measurements at room temperature and 78 K indicate superparamagnetic nature of these MgFe₂O₄ nanocrystals. Funded by the National Natural Science Foundation of China(No. 30771676), the Natural Science Foundation of Jiangsu Province (No. BK20081842), and the Foundation of Nanjing Bureau of Personal for the Returned Overseas Chinese Excellent Scholars     

Microstructures and mechanism of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/Al composites fabricated by the reaction between SiO<Subscript>2</Subscript> and molten aluminum

Al₂ O₃/Al composite was fabricated by the reaction between SiO₂ and molten aluminum. The microstructures of the composite obtained under different reaction conditions were analyzed. The formation mechanism of the composite microstructure was discussed. Results show that the reaction kinetics is influenced remarkably by the reaction temperature, reaction time and the quantity of SiO₂. The morphologies of Al₂O₃ have different features, depending on the reaction temperature. The composite has equaxed Al₂O₃ grains when materials reacted below 1200°C, and the composite is composed of a large number of fine Al₂O₃ grains and aluninum. The composite has a frame-shaped Al₂O₃ microstructure at the reaction temperature of above 1250°C. CHENG Xiao-min: Born in 1964 Funded by the National Natural Science Foundation of China (No. 91522)     

Influences of heat treatments on crystallization in SiO<Subscript>2</Subscript>-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-MgO-K<Subscript>2</Subscript>O-F glass-ceramics

Five kinds of heating treatment processing were chosen according to the experiment result of differential scanning calorimeter to prepare SiO2-Al2O3-MgO-K2O-F glass ceramics samples.The effects of heat treatment processing on the crystallization of these samples were explored by X-ray diffraction and scanning electron microscopy techniques.The results indicate that phase separations can occur in the bulk regions of the glass sample when holding at 670 ℃ for 3 h.The phase separation can accelerate the precip...     

Manufacture Process of 8Y2O3 Stabilized ZrO2 from Nano Powders

The manufacture process of 8 mol% Y2O3 stabilized ZrO2 ( YSZ ) from nano powders, including the forming and sintering stages, was studied. During the forming process of YSZ powders, the relative density of YSZ increases lineally with the forming press, and the sintering linear shrinkage of YSZ to the forming press compiles to the parabola trend. When the forming press exceeding 500MPa, the samples with lower shrinkage and high density were obtained. The sintering temperature of YSZ decreases greatly because of the small size and high active surface of YSZ powders. As a result, the beginning sintering temperature of YSZ made in the experiment is as low as 825℃, and the end sintering temperature is 1300-1350℃ . The relative density of YSZ ceramic by solid sintering at 1300-1350℃ is more than 97% , with little and small pores in the uniform microstructure.     

Enhanced Low-field Magnetoresistence in the Absence of Mn Content in Polycrystalline La0.67Ca0.33MnO3

Magnetic and electrical transport properties of the La0.67Ca0.33Mn1-xO3 （x=0-0.16）, which were prepared by the sol-gel method followed by sintering treatment at 1 450, 1 100 and 900 ℃, respectively, were investigated. Experimental results show that, with the increase of x, the resistivity of samples increases and the insulator-metal transition temperature shifts towards lower temperature. Meanwhile, the intrinsic megnetoresistance effect is weakened and the extrinsic magnetoresistance is enhanced. For the samples with x=0.16 and 0.10 sintered at 1 100 ℃ and 900 ℃, respectively, low field magnetoresistance as high as about 50% can be observed. Furthermore, for the samples sintered at 1 100 ℃ and 900 ℃, the grain size is not only controlled by about sintering temperature, but also by the absence of Mn content x.     

Flux pinning effect of cubic equiaxed morphology and its Ti stabilizing in Nb<Subscript>3</Subscript>Sn superconductors

Two sets of internal-Sn Nb3Sn superconducting strands were fabricated through RRP method, one with 2 wt% of Ti alloyed in Sn core and the other just pure Sn. Four reaction temperatures of 650℃, 675℃, 700℃ and 725℃ and 128 h duration were applied for A15 phase formation heat treatment after Cu-Sn alloying procedure of 210℃/50 h + 340℃/25 h. For the heat-treated coil samples, transport non-Cu JC was examined through standard 4-probe technique and phase microstructure was observed by means of Field Emission Sc...     

Effect of aluminum addition on microstructure and properties of SiO<Subscript>2</Subscript>-B<Subscript>2</Subscript>O<Subscript>3</Subscript>-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-CaO vitrified bond

Influence of aluminum addition on the structures and properties of SiO₂-B₂O₃-Al₂O₃-CaO vitrified bond at low sintering temperature and high strength was discussed. FTIR and XRD analyses were used to characterize the structures of the basic vitrified bond with different contents of aluminum. The bending strength and the thermal expansion coefficients were also tested. Meanwhile, the microstructures of composite specimens at sintering temperature of 660 °C were observed by scanning electron microscope (SEM). The experimental results showed that the properties of vitrified bond with 1wt% aluminum were improved significantly, where the bending strength, Rockwell hardness, and thermal expansion coefficient of the vitrified bond reached 132 MPa, 63 HRB, and 6.73×10^-6 °C^-1, respectively.     

Composition Design for High C3S Cement Clinker and Its Mineral Formation

A new composition of Portland cement clinker was studied, in which KH, SM and IM was 0.98,2.4 and 2.4 respectively as well as its meal added 1%CuO （in mass）. Fired at 1 200℃,1 350℃,1 400℃ and 1 450℃ for 30 min, the resultant mineral phases component and mineral morphology were analyzed. The performances of the cement which was made of clinker burned at 1 450℃ and fly ash were determined. By means of QXRD, XRD and optical microscopy, it is shown that the clinker burnt at 1 450℃ has the larger size crystals and distinct crystal interface, in which the C3S content is 73.37% and the mineral phases is dominantly C3S, following by minor C2S, C3A and tetracalcium aluminoferrite. The results reveal that a new type of high C3S content clinker can completely be made by traditional temperature-time schedule. The performances of the cement produced from this clinker with addtion of 50% fly ash and 5% gupsum were in agreement with the 32.5 strength grade of Portland fly-ash cement. The results also show that the clinker has a significant effect of saving energy and utilizing waste slag.     

Preparation of Ti3SiC2 with Aluminum by Means of Spark Plasma Sintering

Polycrystalline bulk Ti3SiC2 material with a high purity and density was fabricated by spark plasma sintering from the elemental powder mixture with starting composition of Ti3Si3Si1-xAlxC2 , where x = 0. 05 -0.2. X-ray diffraction patterns and scanning electron microscopy photographs of the fully dense samples show that a proper addition of aluminum promotes the formation, and accelerates the crystal growth rate of Ti3SIC2, conse-quently results in a high purity of the prepared samples. The synthesized Ti3 SiC2 is in plane-shape with a size of about 10- 25μm in the elongated dimension. Solid solution of aluminum decreases the thermal stability of Ti3SiC2, and lowers the temperature of Ti3SiC2 decomposeing to be 1300 ℃ .     

Optical and magnetic properties of Fe<Subscript>2</Subscript>O<Subscript>3</Subscript>/SiO<Subscript>2</Subscript> nano-composite films

Fe₂O₃/SiO₂ nano-composite films were prepared by sol-gel technique combining heat treatment in the range of 100–900 °C. The particle size was observed by FE-SEM. Optical properties of the films were investigated by UV-visible spectra. Structural and magnetic characteristics were investigated through FT-IR and VSM. The transparency of the Fe₂O₃/SiO₂ nano-composite films decreased with the content of the Fe₂O₃. Water and organic solvent in the films were evaporated with heat treatment, so the transparency of the films was enhanced under high temperature. It is also found that the saturation magnetization (M _s) of the films increases with the temperature. As the content of the Fe₂O₃ increases, when the content of the Fe₂O₃ is around 30wt%, the M _s of the films has a maximum value.     

Dielectric properties of Bi<Subscript>4</Subscript>Ti<Subscript>3</Subscript>O<Subscript>12</Subscript> ceramics by impedance spectroscopic method

Various lead-free ceramics have been investigated in search for new high-temperature dielectrics. In particular, Bi₄Ti₃O₁₂ is a type of ferroelectric ceramics, which is supposed to replace leadcontaining ceramics for its outstanding dielectric properties in the near future. Ferroelectric ceramics of Bi₄Ti₃O₁₂ made by conventional mixed oxide route have been studied by impedance spectroscopy in a wide range of temperature. X-ray diffraction patterns show that Bi₄Ti₃O₁₂ ceramics are a single-phase of ferroelectric Bi-layered perovskite structure whether it is calcined at 800 °C or after sintering production. This study focused on the effect of the grain size on the electric properties of BIT ceramics. The BIT ceramics with different grain sizes were prepared at different sintering temperatures. Grain becomes coarser with the sintering temperature increasing by 50 °C, relative permittivity and dielectric loss also change a lot. When sintered at 1 100 °C, r values peak can reach 205.40 at a frequency of 100 kHz, the minimum dielectric losses of four different frequencies make no difference, all close to 0.027. The values of E _a range from 0.52 to 0.68 eV. The dielectric properties of the sample sintered at 1 100 °C are relatively better than those of the other samples by analyzing the relationship of the grain, the internal stresses, the homogeneity and the dielectric properties. SEM can better explain the results of the dielectric spectrum at different sintering temperatures. The results show that Bi₄Ti₃O₁₂ ceramics are a kind of dielectrics. Thus, Bi₄Ti₃O₁₂ can be used in high-temperature capacitors and microwave ceramics.     

Effect of Mg/Al ratios on hydration mechanism of tabular alumina carbon composites reinforced by Al<Subscript>4</Subscript>C<Subscript>3</Subscript> in situ reaction

Hydration mechanism of tabular alumina carbon composites reinforced by Al₄C₃ in situ reaction with Mg and Al was researched in water steam using super automatic thermostatic water bath from 25 °C to 85 °C. It is shown that hydration mechanism of the composites is chemical reaction control at 44.3 °C-84 °C in H₂O(g). The hydration was controlled by diffusion from 24.7 °C to 33 °C. The ratio of added Mg/Al influences the HMOR of the composites.The mechanism of HMOR of the composites with different ratios of Mg/Al can be discovered by means of SEM analysis. The active Mg/Al powder and flake graphite inside give the composites outstanding hot strength resulting from the interlocking structure of Al₄C₃ crystals at high temperature. Besides, the matrix changes into the Al₄C₃ with high refractoriness. The method of preventing the hydration of tabular alumina carbon composites reinforced by Al₄C₃ in situ reaction was immersed in the wax at suitable temperature or storing them below 33 °C in a dry place or storing them with paraffin-coating.     

Co-precipitation/hydrothermal synthesis of BiFeO<Subscript>3</Subscript> powder

A coprecipitation/hydrothermal route was utilized to fabricate pure phase BiFeO3 powders using FeCl3·6H2O and Bi（NO3）3·5H2O as starting materials, ammonia as precipitant and NaOH as mineralizer. The synthesized powders were characterized by XRD, SEM and DSC-TG analysis. In the process, single-phase BiFeO3 powders could be obtained at a hydrothermal reaction temperature of 180 ℃, with NaOH of 0.15 mol/L, in contrast to 200 ℃ and 4 mol/L for conventional hydrothermal route. Meanwhile, the micro-morphology of synthesized BiFeO3 powders changed with different reaction temperatures and concentrations of NaOH. The N6el temperature, Curie temperature and decomposition temperature of the synthesized BiFeO3 powders were detected to be 301 ℃, 828 ℃ and 964 ℃, respectively. The hydrothermal reactions mechanism to fabricate BiFeO3 powders were discussed based on the in-situ transformation process.     

Composite cathode Bi<Subscript>1.14</Subscript>Sr<Subscript>0.43</Subscript>O<Subscript>2.14</Subscript>-Ag for intermediate-temperature solid oxide fuel cells

Composites consisting of strontium stabilized bismuth oxide （Bi1.14Sr0.43O2.14, SSB） and silver were investigated as cathodes for intermediate-temperature solid oxide fuel cells with doped ceria electrolyte. There were no chemical reactions between the two components. The microstructure of the interfaces between composite cathodes and Ce0.8Sm0.2O1.9 （SDC） electrolytes was examined by scanning electron microscopy （SEM）. Impedance spectroscopy measurements show that the performance of cathode fired at 700 ℃ is the best. When the content of Ag2O is 70 wt%, polarization resistance values for the SSB-Ag cathodes are as low as 0.2 Ωcm^2 at 700℃ and 0.29 Ωcm^2 at 650℃. These results are much smaller than some of other reported composite cathodes on doped ceria electrolyte and indicate that SSB-Ag composite is a potential cathode material for intermediate temperature SOFCs.     

Molten Salt Synthesis of Ba（ Mgl／3Nb2／3 ）O3 Powder

The single-phrase Ba(Mgl/3Nb2/3)O3(BMN) powder was saccessfully prepared by the KCImolten salt synthesis(MSS) method. The temperature for single-phase BMN powders by MSS was about 400℃ lower than that by the solid-phase method. The average particle size (APS) was about 0.91,u.m at 900℃ and increased with increasing synhesis temperature. Based on the APS, the activation energy for particle growth in theMSS, whose value was 64. 1kJmol^-1.was attained. The sinterability of the powder prepared by MSS method wasbetter than that pretared by solid-phase method.     

Microwave sintering of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-ZrO<Subscript>2</Subscript>-WC-Co cermets

Composite powders of nanocrystalline WC-10Co (15wt%),Y2O3 (8mol%) stabilized nanocrystalline ZrO2 (30wt%),industrial cobalt powder (4.5wt%) and submicron Al2O3 (55wt%) composite powders were fabricated by high-energy ball-milling process.The nanocomposite powders were consolidated by microwave sintering process at temperature ranged 1300℃-1550℃ for 15min,respectively.The optimum consolidation conditions,such as temperature,were researched during microwave sintering process.Vickers Hardness of the consolidated cermets was measured by using a Vickers indentation test,and density of specimens was also determined by Archimedes’ principle.Microwave sintering process could not only increase the density of Al2O3-ZrO2-WC-Co cermets and reduce the porosity,but also inhibit abnormal grain growth.     

Erosion Resistance of CaO-AI203-SiO2 System Glass-Ceramics

The erosion resistance tests were used to research the erosion wear behavior of CaO-Al2O3-SiO2 system glass-ceramic. With the orthogonal test method, the factors thai affect the erosion wear of CaO-Al2O3-SiO2 system galss-ceramic such as pacticles property, impact angle, impact time, size of particles were discussed. The results show that erosion rate rises along a straight line at the early period of erosion wear. With the impact time increased, the erosion rate deviates from original staight line, tendency of the erosion rate increases, With the size of paricle increased , it will have more kinetic energy, the erosion rate of the surface of glass-ceramics ploate rises.     

Effect of SiO2 on the Preparation and Properties of Pure Carbon Reaction Bonded Silicon Carbide Ceramics

Effect of SiO₂ content and sintering process on the composition and properties of Pure Carbon Reaction Bonded Silicon Carbide (PCRBSC) ceramics prepared with C−SiO₂ green body by infiltrating silicon was presented. The infiltrating mechanism of C−SiO₂ preform was also explored. The experimental results indicate that the shaping pressure increases with the addition of SiO₂ to the preform, and the pore size of the body turned finer and distributed in a narrower range, which is beneficial to decreasing the residual silicon content in the sintered materials and to avoiding shock off, thus increasing the conversion rate of SiC. SiO₂ was deoxidized by carbon at a high temperature and the gaseous SiO and CO produced are the main reason to the crack of the body at an elevated temperature. If the green body is deposited at 1800°C in vacuum before infiltration crack will not be produced in the preform and fully dense RBSC can be obtained. The ultimate material has the following properties: a density of 3.05–3.12 g/cm³, a strength of 580±32MPa and a hardness of (HRA)91–92.3. WU Qi-de: Born in 1949 This work was financially supported by the Key Research Project of the China (No. 96-A10-01-07) and the Key Research Project of the Wuhan (20001001003)     

Effect of pre-heating temperature on structural and optical properties of sol-gel derived Zn<Subscript>0.8</Subscript>Cd<Subscript>0.2</Subscript>O thin films

Zn_0.8Cd_0.2O thin films prepared using the spin-coating method were investigated. X-ray diffraction, scanning electron microscopy, and UV-Vis spectrophotometry were employed to illustrate the effects of the pre-heating temperature on the crystalline structure, surface morphology and transmission spectra of Zn_0.8Cd_0.2O thin films. When the thin films were pre-heated at 150 °C, polycrystalline ZnO thin films were obtained. When the thin films were pre-heated at temperatures of 200 °C or higher, preferential growth of ZnO nanocrystals along the c-axis was observed. Transmission spectra showed that thin films with high transmission in the visible light range were prepared and effective bandgap energies of these thin films decreased from 3.19 eV to 3.08 eV when the pre-heating temperature increased from 150 °C to 300 °C.     

Investigation on phase evolution of the ZnO-B<Subscript>2</Subscript>O<Subscript>3</Subscript>-SiO<Subscript>2</Subscript> glass ceramics

ZnO-B₂O₃-SiO₂-Al₂O₃-Na₂O glass doped with nucleating agent TiO₂ was prepared with melting-quenching method and the effect of nucleating agent on the crystallization behavior and phase evolution of this glass was investigated by differential thermal analysis (DTA), X-ray diffraction (XRD), and scanning electron microscopy (SEM). The experimental results show that the glass transition temperature and the first crystallization temperature decrease from 630 °C and 765 °C to 595 °C and 740 °C, respectively, with introduction of TiO₂ into glass. There is no diffraction peaks in the XRD pattern but it is no longer transparent for the base glass without nucleating agent after heat treatment, which suggests the serious phase separation occurred, and the observation by SEM indicates that the phase separation is developed by nucleation and growth mechanism. However, there are two different crystals ZnAl₂O₄ and NaAlSiO₄ present in the glass containing TiO₂ after heat treating at 575 °C for 2 h and 740 °C for 6 h, respectively. What is interesting is that NaAlSiO₄ disappears as the crystallization time at 740 °C increases from 6 h to 12 h, and more ZnAl₂O₄ crystal is formed, namely, the further formation of ZnAl₂O₄ is at cost of NaAlSiO₄ with increasing crystallization time. And observation of the morphology of glass ceramics shows great difference with increasing crystallization time. Moreover, the ability of ZnO-B₂O₃-SiO₂-Al₂O₃-Na₂O glass ceramics against attacking of 1M HCl solution is increased by the crystals precipitated in heat treatment process.