Fabrication and magnetic properties of Sm3(Fe,Ti)29Nx/α-Fe dual-phase nanocomposite permanent magnetic material

Sm3(Fe,Ti)29Nx/α-Fe dual-phase nanometer magnetic material was fabricated through rapid solidification, crystallization and nitridation of Sm-Fe (Ti) alloy. The effect of combination of rapid solidification and Ti alloy addition on the phase formation and microstructure of the Sm-Fe alloy is investigated in this paper. The microstructure of amorphous phase and dual-phase nano-grain crystals before and after crystallization annealing were observed using a high-resolution transmission electron microscope (HREM). The dual-phase nano-grains after annealing were compacted together with a clear interface with the direct exchange-coupling mechanism. Different annealing processes were used to examine the melt-spun alloy. Comparison of the images of SEM showed that annealing at 750℃ for 10 min was most suitable to get homogeneous and nano-grains. No obvious kink was detected in the second quadrant of the hysteresis loop like a single hard magnet, and strong exchange coupling was found between hard magnets and soft magnets.     

Synthesis and structure of NaNbO<Subscript>3</Subscript> ceramic powders in ultrahigh pressure field

The NaNbO3 powders were synthesized and their crystal structure changes were analyzed by ultrahigh pressure up to 6 GPa. The results indicate that the pure NaNbO3 powders can be synthesized at 300℃ under a pressure of 4 GPa, to significantly restrain the Na element volatilization compared with the traditional synthesis method. It is found that the crystal structure of synthesized NaNbO3 changes from low symmetry to high symmetry with the increase of the pressure.     

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     

Cu<Subscript>2</Subscript>ZnSnS<Subscript>4</Subscript> thin films prepared by sulfurizing different multilayer metal precursors

Cu₂ZnSnS₄ (CZTS) thin films were successfully fabricated on glass substrates by sulfurizing Cu-Sn-Zn multilayer precursors, which were deposited by ion beam sputtering and RF magnetron sputtering, respectively. The structural, electrical and optical properties of the prepared films under various processing conditions were investigated in detail. Results showed that the as-deposited CZTS thin films with the precursors by both ion beam sputtering and RF magnetron sputtering have a composition near stoichiometric. The crystallization of the samples, however, has a strong dependence on the atomic percent of constituents of the prepared CZTS films. A single phase stannite-type structure CZTS with a large absorption coefficient of 10₄/cm in the visible range could be obtained after sulfurization at 520°C for 2 h. The samples relative to the RF magnetron sputtering showed a low resistivity of 0.073 Ωcm and band gap energy of about 1.53 eV. The samples relative to the ion beam sputtering exhibited a resistivity of 0.36 Ωcm and the band gap energy is about 1.51 eV. Supported by the National Natural Science Foundation of China (Grant No. 10574106), the Planned Science and Technology Project of Guangdong Province (Grant No.2003C05005) and the Natural Science Fund of Zhanjiang Normal University (Grant No.200801)     

Effect of Electron Beam on the Structure and Crystallization Features of BaO-SrO-TiO2-SiO2 Glass

Glasses of BaO-SrO-TiO2-SiO2 after electronic radiation treatment of 50-1000 kgy were studied by means of IR spectra, DTA and visible light absorption method. The result shows that the glass structure is changed due to the formation of structue defect from oxygen vacancy and E‘color center, which resultsd in the crystallization process and new precursors, and decreasement of Tg temperature and crystallization peaks by 20 -50℃.     

Properties of Nano SiO2 Modified PVF Adhesive

Some properties of nano SiO2 modified PVF adhesive were studied .the experimental results show that nano SiO2 can inprope the properties of PVF adhesive very well.Meanwhile the modification mechanism of nano SiO2 to PVF adhesire and the applications of this adhesire in paper-plastic composite ,conctete and fireproof paint were discussed by using IR and XRD determination.     

Crystallization and Electrical Properties of （Ba0.4Pb0.3）Sr0.3TiO3 Thin Film by Pulsed Laser Deposition

（Ba0.4Pb0.3）Sr0.3TiO3 thin films were fabricated via pulsed laser deposition （PLD） technique on Pt/TiO2/SiO2/Si substrate. The crystallization of the films was characterized by XRD and FSEM, and the experimental results suggested deposition parameters, especially the deposition temperature was the key factor in forming the perovskite structure. The dielectric properties of the film deposited with optimized parameters were studied by an Agilent 4294A impedance analyzer at 1 MHz. The dielectric constant was 772, and the loss tangent was 0.006. In addition, the well-shaped hysteresis loop also showed that the film had a well performance in ferroelectric. The saturated polarization P, remnant polarization Pr and coercive field E were about 4.6 μC/cm2, 2.5 μC/cm2 and 23 kV/cm （the coercive voltage is 0.7 V）, respectively. It is suggested the film should be a promising candidate for microwave applications and nonvolatile ferroelectric random access memories （NvFeRAMs）.     

Microstructures and Properties of SiC／Al2O3 ／Al- Si Composites Prepared by Reactive Penetration

The composition, microstructures and properties of SiC/Al2O3/Al-Si composites formed by reactive penetration of the molten aluminum into the preforms of SiO2 and SiC were investigated. The composition of the composites was measured by X-ray diffraction ( XRD ). The microstructures of the composites were also measured by scanning electron microscopy (SEM) and optical microscopy. In addition, the factors affecting the properties of the composites were discussed. The experiments show that the mechanical properties of the composites depend on their relative densities and the sizes of the fillers“ SiC gains“. The denser the SiC/Al2O3/Al-Si composites, the higher their bending strength. As the filler “SiC gains“ become fine, the bending strength of the composites increases.     

Straight SiO<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript> nanorod Y junctions

Novel straight silicon oxide [SiO _x (1<x<2)] nanorod Y junctions have been synthesized on Si plate by thermal evaporation of mixed powders of silica and carbon nanofibers at 1300°C and condensation on a Si substrate without assistance of any catalyst. The synthesized samples were characterized by means of scanning electron microscopy, transmission electron microscopy, high resolution transmission electron microscopy, and energy dispersive X-ray spectroscopy. The results suggested that the straight nanorod Y junctions are amorphous and consist only of elements Si and O, and these rods with diameters about 50–200 nm have a neat smooth surface. The growth of such silicon oxide nanorods may be a result of the second nucleation on the surface of rods causing a change in the growth direction of silicon oxide nanorods developed. Supported by the Academic Human Resources Development in Institutions of Higher Learning under the Jurisdiction of Beijing, and the Program of Science & Technology Activity for Chinese Homecoming Fellow Abroad and Research Program of Beijing Key Laboratory for Sensor (Grant No. KM200810772009)     

Interface structure of Ag (111)/SnO<Subscript>2</Subscript> (200) composite material studied by density functional theory

Electric contact material of Ag/SnO₂ was successfully synthesized by in situ process method. The interface structure was characterized by high-resolution transmission electron microscopy (HTEM) and simulated at atomic scale on computer. The mean-square displacements of atoms near the interface were calculated, and the results showed that near the interface both Ag side and SnO₂ were mismatched and this effect decays rapidly far from the interface. By inspecting the calculated density of states (DOS), we found that the electric-conductivity of this composite material was decreased because of the localized 4d and 2p electrons of Ag and O near the Fermi surface, respectively. Electron density changed acutely across the interface, so that there was no extra compound precipitated. A micro-electric field also formed in the whole material due to the interface structure, and this may affect the electron conduction and the related electric-conductivity of the composite. It is found that the interface cohesive energy of Ag (111)/SnO₂ (200) was −3.50 J/m², which is higher than the experimental results. Supported by the National Natural Science Foundation of China (Grant No. 2008CB617609), the Natural Science Foundation of Yunnan Province (Grant No. 2006E003Z) and Science Innovation Foundation of Kunming University of Science and Technology     

Preparation of nanocrystalline BaTiO<Subscript>3</Subscript> ceramics

The high-dense nanocrystalline BaTiO₃ (BT) ceramics with grain size smaller than 100 nm have been successfully prepared by the two step sintering and the spark plasma sintering (SPS) process. The successive transitions in nanograin BT ceramics from rhombohedral to orthorhombic, tetragonal and cubic transitions, similar to those in coarse BT ceramics, were revealed by in-situ temperature dependent Raman spectrum. The multiphase coexistence and the diffused phase transition character were demonstrated in the 8 nm nanocrystalline BT ceramics. Supported by the National Basic Research Program of China (“973” Project) (Grant No. 2002CB613301) and the National Natural Science Foundation of China (Grant No. 50872093)     

Thermal-dynamical properties and pressure dependence of phonon spectrum of ordered Si<Subscript>50</Subscript>Ge<Subscript>50</Subscript> alloy based on <Emphasis Type="Italic">ab initio</Emphasis> methods

The phonon spectrum of ordered zincblende Si₅₀Ge₅₀ alloy is calculated by ab initio method. The energy band structure at zero pressure and the pressure dependence of phonon dispersion curves are shown up to 20 GPa. The calculation finds a pressure-induced softening of the transverse acoustic phonon mode and the mode frequency reaching zero at about 14 GPa, which indicate breaking of the symmetry and formation of a new phase under high pressure. Supported by the National Natural Science Foundation of China (Grant No. 50771090), the State Key Program for Basic Research of China (Grant No. 2005CB724404) and the Program for Changjiang Scholars and Innovative Team (Grant No. IRT0650)     

Photocatalytic performance of TiO<Subscript>2</Subscript> thin films connected with Cu micro-grid

Aiming at reducing the recombination of photo-induced carriers in semiconductor photocatalytic process, we prepared TiO₂ thin film with its surface modified by a connected Cu micro-grid via a microsphere lithography strategy, which showed higher photocatalytic activity than the pure TiO₂ film. The improvement of photocatalytic activity of Cu micro-grid to the TiO₂ film is due to the charge carrier separation and electron transfer by the conducting metal grid. The photocatalytic activity was improved as metal loading increased, which obtained the best performance at a certain loading amount, and then decreased at higher loading amount. This phenomenon was attributed to the metal’s bulk effect which could be explained by the relationship between the energetic positions and the metal cluster size. Supported by the National Natural Science Foundation of China (Grant Nos. 50672003, 50872005) and the National Basic Research Program of China (“973” Project) (Grant No. 2007CB613302) and the Fok Ying Tong Education Foundation (Grant No. 111050)     

Sensing characterization of Sn/In/Ti nanocomplex oxides for CO,CH<Subscript>4</Subscript> and NO<Subscript>2</Subscript>

The nanocomplex oxides of Sn-In and Sn-In-Ti were prepared by controlled co-precipitation method as sensing materials of semiconductor gas sensors for detection of CO, CH4 and NO2. Through manipulating the Sn/In cation ratio, metal salt total concentration, precipitation pH value and aging time, the nanocrystalline powders were successfully derived with chemical homogeneity and superior thermal stability, compared with the single component oxides. The particle size and morphology, surface area, and thermal and phase stabilities were characterized using TEM, TG-DTA, BET and XRD. The sensing tests showed that the Sn-In composites exhibit high sensitivity and selectivity for CO and NO2. The introduction of TiO2 enhanced CH4 sensitivity and selectivity, particularly, additives of Pd and Al2O3 as a dopant and surface modification greatly enhanced the sensing properties. The sensitivity depended on the composition of composites, calcination temperature and operating temperature. The optimal values were (25%In2O3- 75%SnO2)-20%TiO2 for ternary composite, 600 and 300℃, respectively. Temperature-programmed desorption (TPD) studies were employed to explain the gas adsorption behavior displayed by the surface of nanocomposites and X-ray photoelectron spectroscopic (XPS) analysis was used to confirm the electronic interactions existing between oxide components. The sensing mechanism of the nanocomposites was attributed to chemical and electronic synergistic effects.     

Conformation of Organic Chain in Phase Transition of Hybrid （Cl2H25NH3）2MnCl4

The structural change in phase transition of hybrid （Cl2H25NH3）2MnCl4 was investigated. The temperature and the structures of the phase transition is investigated by thermal gravimetry （TG） and differential scanning calorimetry （DSC）, infrared spectrum （IR） and X-ray diffraction （XRD）. The results suggest that the phase transition is reversible and the structural change arises from the conformation change of the organic chain. The interlayer distance increases when the hybrid transforms from low temperature phase to high temperature phase. This is explained by the diffusion of gauche-bond along the organic chains and they move away from each other when the phase transition occurs. Combining the experimental data with theoretical calculation, we propose that organic chain of the hybrid in high temperature phase is the conformation of gauche-bond alternating with trans bond （noted as GTG＇TGTG＇TGTG＇T）.     

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)     

Effect of the Cool System on Internal Stress of CaO-Al203-SiO2 Glass-ceramic System

The samples were attained through altering the cooling system of producing glass-ceramics. The X-ray diffraction was used to test the stress value of different samples. The relation of the cooling system and internal stress were also investigated. The experimental results show that the stress of glass-ceramic had a close relation with starting cool temperature. Above 800 ~C, glass-ceramic could be accelerated cooling and did not bring stress. Temperature between 500 ℃ and 800℃ was an important temperature range of the formation of stress in glass-ceramic, in which the glass-ceramic stress would change obviously. Cool system was the key on how to control and eliminate internal stress in order to reduce the destroy of materials crated by internal stress. In addition, glass particles size increase, glass-ceramic stress increase in consequent.     

Comparison of short period InAs/GaSb superlattices on GaSb and GaAs substrates

Type II superlattices (SLs) short period InAs(4ML)/GaSb(8ML) were grown by molecular-beam epitaxy on lattice-mismatched GaAs substrates and on GaSb substrates. A smooth GaSb epilayer was formed on GaAs substrates by inserting mulit-buffer layers including an interfacial misfit mode AlSb quantum dot layer and AlSb/GaSb superlattices smooth layer. SLs grown on GaAs substrates (GaAs-based SLs) showed well-resolved satellite peaks in XRD. GaSb-based SLs with better structural quality and smoother surface showed strong photoluminescence at 2.55 μm with a full width at half maximum (FWHM) of 20 meV, narrower than 31 meV of GaAs-based SLs. Inferior optical absorption of GaAs-based SL was observed in the range of 2―3 μm. Photoresponse of GaSb-based SLs showed the cut-off wavelength at 2.6 μm.     

Microstructures and fatigue-free properties of the La<Superscript>3+</Superscript> and Nd<Superscript>3+</Superscript> doped Bi<Subscript>4</Subscript>Ti<Subscript>3</Subscript>O<Subscript>12</Subscript> thin films prepared by modified sol-gel technique

Ferroelectric Bi_3.25La_0.75Ti₃O₁₂ (BLT) and Bi_3.15Nd_0.85Ti₃O₁₂ (BNT) thin films were fabricated on Pt/TiO₂/SiO₂/Si (100) substrates by a modified sol-gel technique. X-ray diffraction indicated that these films were of single phase with random polycrystalline orientations. The surface morphologies of the films were observed by scanning electron microscope, showing uniform, dense films with grain size of 50–100 nm. Well-saturated hysteresis loops of the films were obtained in metal-ferroelectric-metal type capacitors with Cu top electrodes at an applied voltage of 400 kV/cm, giving the remanent polarization (2P _r) and coercive field (2E _c) values of the films of 25.1 μC/cm² and 203 kV/cm for BLT, and 44.2 μC/cm² and 296 kV/cm for BNT, respectively. Moreover, these capacitors did not show fatigue behaviors after up to 1.75×10¹⁰ switching cycles at the test frequency of 1 MHz, suggesting a fatigue-free character. The influences of the La³⁺ and Nd³⁺ doping on the properties of the films were comparatively discussed. Supported by the National Key Basic Research and Development Program of China (Grant No. 2006CB932305) and the Natural Science Foundation of Hubei Province, China (Grant No. 2004ABA082)     

Study on BaTiO<Subscript>3</Subscript> films prepared by AC power microarc oxidation

BaTiO₃ films were prepared by microarc oxidation (MAO) with an in-house built alternating current (AC) power supply in Ba(OH)₂ solution in this study. The surface morphology, combinability with the substrate and phase composition of the films were investigated by XRD, SEM and TEM. The BaTiO₃ films were annealed at a temperature range of 900 to 1200°C and phase compositions were tested thereafter. The results showed that the BaTiO₃ films were mainly composed of the primitive hexagonal phase with relatively small amount of tetragonal and amorphous phases. Moreover, the amount of amorphous phase decreased with the time of annealing. The transformation of BaTiO₃ from hexagonal structure to tetragonal stucture became obvious until the annealing temperature reached 1200°C. The film consisted mainly of BaTiO₃ tetragonal structure with ferroelectric property. The influence of annealing on surface morphology and mechanism of phase transformation of the films were also discussed. Supported by Guangdong Natural Science Foundation (Grant No. 0500649)