Self-Propagating High-Temperature Reduetive Synthesis of TiB2-Al2O3 Composite Powders

TiB2-Al2O3 composite powders were produced by self-propagating high-temperature synthesis（SHS） method with reductive process from B2O3-TiO2-AI system. X-ray diffraction（XRD） and scanning electron microscopy（SEM） analyses show the presence of TiB2 and Al2O3 only in the composite powders produced by SHS. The powders are uniform and free-agglomerate. Transmission electron microscopy （TEM） and high resolution electron microscopy （HREM） observation of microstructure of the composite powders indicate that the interfaces of the TiB2-Al2O3 bond well, without any interfacial reaction products. It is proposed that the good interfacial bonding of the composite powders can be resulted from the TiB2 particles crystallizing and growing on the Al2O3 particles surface with surface defects acting as nucleation centers.     

Synthesis of Ti3SiC2/TiB2 Composite by In-situ Hot Pressing （HP） Method

Ti3SiC2/TiB2 composite was successfully obtained by hot pressing Ti/TiC/Si/B4C power mixtures.Volume fraction of TiB2 in Ti3SiC2/TiB2 composite can not exceed 10%.Incorporation of excessive TiB2 will affect the reactions process.TiC and Ti5Si3 were two important intermediate phases during the whole reactions.The microstructure characteristics of the Ti3SiC2/TiB2 composites were analyzed using scanning electron microscopy （SEM） and transmission electron microscopy （TEM）.The experimental results show that the grains of Ti3SiC2/TiB2 composite are structured in a layered form,and the formation of TiB2 particles as reinforcements with elongated or equiaxed shape distributes in Ti3SiC2 matrix.     

Fabrication of homogenous dispersion TiB<Subscript>2</Subscript>-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> composites

In order to get a homogenous mixture and compact of TiB2-Al2O3, hybridization as a surface modification method was used to prepare nano-scale Al2O3 coated TiB2 particles. PE-wax particles were first coated onto TiB2 particles by hybridization, and then the nano-scale Al2O3 particles were coated onto the surface of TiB2 coated by PE-wax particles again. SEM, TEM and EDS were used to characterize the microstructure of as-received core/shell particles and its compacts. The experimental results show that a particle-scale homogenous dispersion of TiB2 and Al2O3 can be formed not only in mixed powder but also in dewaxed compacts. The compacts then were sintered by gas-pressing sintering (GPS). Finial products show improved mechanic properties comparing with reference samples fabricated by normal ways.     

Direct synthesis of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-modified Li(Ni<Subscript>0.5</Subscript>Co<Subscript>0.2</Subscript>Mn<Subscript>0.3</Subscript>)O<Subscript>2</Subscript> cathode materials for lithium ion batteries

To improve the cyclic stability at high temperature and thermal stability, the spherical Al₂O₃-modified Li(Ni_0.5Co_0.2Mn_0.3)O₂ was synthesized by a modified co-precipitation method, and the physical and electrochemical properties were studied. The TEM images showed that Li(Ni_0.5Co_0.2Mn_0.3)O₂ was modified successfully with nano-Al₂O₃. The discharge capacity retention of Al₂O₃-modified Li(Ni_0.5Co_0.2Mn_0.3)O₂ maintained about 99% after 200 cycles at high temperature (55 °C), while that of the bare one was only 86%. Also, unlike bare Li(Ni_0.5Co_0.2Mn_0.3)O₂, the Al₂O₃-modified material cathode exhibited good thermal stability.     

Microstructure and mechanical properties of TiB<Subscript>2</Subscript>-Al<Subscript>2</Subscript>O<Subscript>3</Subscript> composites

Effects of Al2O3 and Ni as the additives on the sinterability, microstructure and mechanical properties were systematic studied. The experimental results show that only a relative density about 96.2% of hot-pressing TiB2-30%Al2O3 can be attained due to the plate-like TiB2 particle and its random orientation and excessive Al2O3 grain growth. When sintering temperature is higher than 1 700 ℃, TiB2 grain growth can be found, which obvious improves flexural strength of TiB2 matrix but decreases toughness. It seems that mechanical properties of TiB2-Al2O3 composites are mainly depended on relative density besides grain growth. otherwise, they will be determined by relative density and TiB2 matrix strength together. Anyway, Al2O3 addition can weaken the grain boundary and thus improve the toughness of the materials. A flexural strength of 529 MPa, Vickers hardness of 24.8 GPa and indentation toughness of 4.56 MPa·m1/2 can be achieved inTiB2-30vol% Al2O3.     

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.     

Synthesis and electrochemical properties of Cr-doped Li<Subscript>3</Subscript>V<Subscript>2</Subscript>(PO<Subscript>4</Subscript>)<Subscript>3</Subscript> cathode materials for lithium-ion batteries

Cr-doped Li₃V₂(PO₄)₃ cathode materials Li₃V_2−x Cr _x (PO₄)₃ were prepared by a carbothermal reduction(CTR) process. The properties of the Cr-doped Li₃V₂(PO₄)₃ were investigated by X-ray diffraction (XRD), scanning electron microscopic (SEM), and electrochemical measurements. Results show that the Cr-doped Li₃V₂(PO₄)₃ has the same monoclinic structure as the undoped Li₃V₂(PO₄)₃, and the particle size of Cr-doped Li₃V₂(PO₄)₃ is smaller than that of the undoped Li₃V₂(PO₄)₃ and the smallest particle size is only about 1 μm. The Cr-doped Li₃V₂(PO₄)₃ samples were investigated on the Li extraction/insertion performances through charge/discharge, cyclic voltammogram (CV), and electrochemical impedance spectra(EIS). The optimal doping content of Cr was that x=0.04 in the Li₃V_2−x Cr _x (PO₄)₃ samples to achieve high discharge capacity and good cyclic stability. The electrode reaction reversibility was enhanced, and the charge transfer resistance was decreased through the Cr-doping. The improved electrochemical performances of the Cr-doped Li₃V₂(PO₄)₃ cathode materials are attributed to the addition of Cr³⁺ ion by stabilizing the monoclinic structure. Funded by the Guangxi Natural Science Foundation(No. 0832259) and the National Basic Research Program of China (No. 2007CB613607)     

Influence of Fe/Ni/Al additive on the sintering behaviors of TiB<Subscript>2</Subscript> cermets

Fe-Ni-Al mixtures as hot-pressing sintering additive to Titanium diboride (TiB₂) were studied. It is found that liquid alloy formed under high temperature hardly has effects on the densification behaviors of TiB₂-independent. Fe-Ni-Al additive just works as filler between TiB₂ particles and does not change the TiB₂-independent sintering behaviors. Pressing mode has a great effect on the liquid flowing between TiB₂ particles. Multiple-steps pressing mode will give more time and space for the liquid flowing and improve the relative density of TiB₂-Fe-Ni-Al cermet.     

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）.     

Fabrication of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-NaCl composite heat storage materials by one-step synthesis method

Thermal energy storage is an attractive option for effectiveness since it gives flexibility and reduces energy consumption and costs. New composite materials for storage and transformation of heat of NaCl-Al₂O₃ composite materials were synthesized by one-step synthesis method. The chemical composition, morphology, structure, and thermal properties were investigated by XRD, EDS, SEM, and DSC. The results show that NaCl can be absorbed by Al₂O₃ particle from 800 to 900 °C for Al₂O₃ particle surface is rich active structure. The results also indicate that the leakage of NaCl when the phase change can be prevented by Al₂O₃ particles and the enthalpy of phase change of NaCl-Al₂O₃ material is 362 J/g. The composites have an excellent heat storage capacity. Therefore, this study contributes to one new thought and method to prepare high temperature heat storage material and this material can be applied in future thermal engineering.     

Optimization of<Emphasis Type="Italic">p</Emphasis>-type segmented Bi<Subscript>2</Subscript>Te<Subscript>3</Subscript>/CoSb<Subscript>3</Subscript> thermoelectric material prepared by spark plasma sintering

1 IntroductionIt is well known that the performance of monolithicthermoelectric materials can be characterized as figure-of-meritZ,Z=α2σ/κ, where ,α,σandκare the See-beck coefficients ,the electrical conductivity andthe ther-mal conductivity,respectively.In the past years , greatefforts have been made inlookingforthermoelectric mate-rials with a higher Seebeck coefficient ,electrical conduc-tivity and alowerthermal conductivity[1-9].Butfor monol-ithic thermoelectric materials , their f…     

Effect of water soluble PVA on the microstructure characteristics of C-S-H formed in Na<Subscript>2</Subscript>SiO<Subscript>3</Subscript>-Ca(NO<Subscript>3</Subscript>)<Subscript>2</Subscript> solution system

The structure characteristics of hydrated calcium silicate synthesized by solution reaction method with the existing of water soluble polymer polyvinyl alcohol(PVA)are investigated.Using Na 2 SO 3 and Ca(NO 3 ) 2 as the main raw materials,in the condition of 2%(in weight)addition of PVA and the water to solid ratio of 20,hydrated calcium silicate samples(Ca/Si=1.0 and 1.5)were prepared with 60℃water bath.IR,BET,XRD and SEM methods were used to study the microstructure of the hydration products.The results s...     

Structure and Electrical Properties of （Na0.5Bi0.5）0.94Ba0.06TiO3 Ceramicwith0.5wt% of MnO

The structure and electrical properties of （Na0.5Bi0.5）0.94Ba0.06TiO3 ceramic doped with 0.5 wt% of MnO were investigated in comparison with those of （Na0.5Bi0.5）0.94Ba0.06TiO3 ceramic. It was ascertained that the MnO addition did not cause remarkable change in crystal structure and microstructure. The MnO addition mainly displayed a hard effect on the electrical properties, an increase of coercive field （E） and mechanical quality factor （Qm） together with a decrease of dielectric constant （εr） and piezoelectric constant （d33）. An enhancement of electromechanical coupling factor （kp） with the MnO addition was obtained too. An essential relation between the piezoelectric properties and ferroelectric nature of the ceramics was detected. It was found that the piezoelectric properties of the ceramics highly depended on the corporative contribution of remanent polarization （Pt） and coercive field.     

Improved Breakdown Strength in (Ba<Subscript>0.6</Subscript>Sr<Subscript>0.4</Subscript>)<Subscript>0.85</Subscript>Bi<Subscript>0.1</Subscript>TiO<Subscript>3</Subscript> Ceramics with Addition of CaZrO<Subscript>3</Subscript> for Energy Storage Application

(Ba_0.6Sr_0.4)_0.85Bi_0.1TiO₃ ceramics doped with x wt%CaZrO₃ (x= 0-10) were synthesized by solid-state reaction method. The effects of CaZrO₃ amount on the dielectric properties and structure of (Ba_0.6Sr_0.4)_0.85Bi_0.1TiO₃ ceramics were investigated. X-ray diffraction results indicated a pure cubic perovskite structure for all samples and that the lattice parameter increased till x=5 and then slightly decreased. A homogenous microstructure was observed with the addition of CaZrO₃. Dielectric measurements revealed a relaxor-like characteristic for all samples and that the diffusivity γ reached the maximum value of 1.78 at x=5. With the addition of CaZrO₃, the dielectric constant dependence on electric field was weakened, insulation resistivity enhanced and dielectric breakdown strength improved obviously and reached 19.9 kV/mm at x=7.5. In virtue of low dielectric loss (tan δ<0.001 5), moderate dielectric constant (ε_r >1 500) and high breakdown strength (E_b >17.5 kV/mm), the CaZrO₃ doped (Ba_0.6Sr_0.4)_0.85Bi_0.1TiO₃ ceramic is a potential candidate material for high power electric applications.     

Thermal stability of LiFePO<Subscript>4</Subscript>/C-LiMn<Subscript>2</Subscript>O<Subscript>4</Subscript> blended cathode materials

Safety is important to lithium ion battery materials. The thermal stability of LiFePO₄/C-LiMn₂O₄ blended cathode materials is characterized by using TG, XRD, and SEM etc. The results show that LiFePO₄/C-LiMn₂O₄ possesses a worse thermal stability than pure spinel LiMn₂O₄ and pure olivine LiFePO₄/C. When LiFePO₄/C-LiMn₂O₄ blended cathode materials are sintered at 500°C under Ar atmosphere, the sintered cathode materials emit O₂, and appear impurity phases (Li₃PO₄, Fe₂O₃, Mn₃O₄). It is deduced that some chemical reactions take place between different materials, which leads to a worse discharge specific capacity. LiFePO₄/C-LiMn₂O₄ blended cathode materials, therefore, need to be managed and controlled strictly for the sake of thermal stability and safety.     

Two-step synthesis of TiC<Subscript>0.7</Subscript>N<Subscript>0.3</Subscript>@WC-MoC<Subscript>2</Subscript> core-shell microspheres and fabrication of TiC<Subscript>0.7</Subscript>N<Subscript>0.3</Subscript>@WC-MoC<Subscript>2</Subscript>-based cermets by SPS

The precursor with TiC0.7N0.3@WO3-MO3 microspheres were prepared by a novel method from the WO3-MoO3 sol dipping. Subsequently, TiC0.7N0.3@WC-MoC2 core-shell structural microspheres were successfully obtained by carburizing the precursor at 900 °C in a flowing mixture of CH4 (20 ml·min-1) and H2 (200 ml·min-1) for 2 h. Then TiC0.7N0.3@WC-MoC2-15Co cermets were prepared utilizing the core-shell powders by spark plasma sintering (SPS). Powders of the precursors with TiC0.7N0.3@WO3-MO3 microspheres, TiC0.7N0.3@WC-MoC2 microspheres and TiC0.7N0.3@WC-MoC2-15Co cermets were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray diffraction (XRD). The obtained TiC0.7N0.3@WC-MoC2 microspheres have a dense WC-MoC2 coatings shell. The thickness of the shell could be easily controlled by adjusting the number of sol dipping cycles. It was found that the TiC0.7N0.3@WC-MoC2 microspheres were more beneficial to fabricate the "core-rim" structures by SPS.     

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)     

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）.     

Microstructure and AMR Properties of Permalloy Films Sputtered on （Ni0.81Fe0. 19 ）0.66Cr0.34 Buffer

(Ni_0.81 Fe_0.19)_0.66 Cr_0.34 has a high resistivity and a crystal structure close to that of Ni_0.81 Fe_0.19. The electrical and X-ray diffraction measurements prove that a thin NiFeCr seed layer induces a well (111)-orented Ni_0.81 Fe_0.19 film. Post-annealing treatment improves the magnetic properties of (Ni_0.81Fe_0.19)_0.66 Cr_0.34(45Å)/Ni_0.81Fe_0.19 (150Å)/Ta(55Å) thin film prepared under a deposition field, whereas the inter-diffusion of NiFe/Ta deteriorates the magnetoresistance properties of the film.     

Synthesis and characterization of (PEO)<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>−(V<Subscript>0.85</Subscript>Mo<Subscript>0.15</Subscript>)<Subscript>2</Subscript>O<Subscript>5</Subscript> nanocomposite films

(PEO) _x −(V_0.85Mo_0.15)₂O₅(x=0,0.5,1.0) nanocomposite films were prepared by a modified sol-gel method. The structure of the films was analyzed by XRD, and the DC electrical conductivity. Cyclic voltammogram and optical spectral transmittance were investigated. The results show that the (V_0.85Mo_0.15)₂O₅ xerogel has a layered structure and its interlayer space increased from 1.3181 nm at x=0 to 1.7897 nm at x=1.0. The introduction of MoO₃ improved the DC electrical conductivities of the films due to the generation of V₄₊ to maintain the electrical neutrality of the oxides. PEO intercalated in the interlayer of (V_0.85Mo_0.15)₂O₅ oxides has interaction with the oxides, enhancing the amount of Li⁺ ions inserted into the interlayer of the oxides. Moreover, the intercalation of PEO into the interlayer of (V_0.85Mo_0.15)₂O₅ oxides improved the cathodic electrochromic property in near ultraviolet region and anodic electrochromic property in visible range. JIANG Cong-sheng: Born in 1963 Supported by the Science Foundation of Hubei Province (Grant No. 2001ABB083)