Microstructure and Erosion Resistance of in-situ SiAlON Reinforced BN-SiO_2 Composite Ceramics

BN-SiO_2-SiAlON composite ceramics were successfully prepared by the means of hot pressed sintering.Xe plasma flow generated by HallThruster was used for sputtering the surface of the samples in order to evaluate the plasma erosion resistance.XRD,TEM,SEM,and LSCM were used to characterize the phase composition and morphologies of as-made composite ceramics before and after Xe plasma erosion.The ceramics were composed of h-BN,fused silica,and SiAlON,which maintained structuralstability during the process of Xe plasma sputtering.In conclusion,comparing with BN-SiO_2 composite ceramics,the plasma erosion rate of BN-SiO_2-SiAlON composite ceramics decreases significantly at first then rises with the increase of AlN addition.Erosion pits can be observed by using SEM on the surface after plasma sputtering,which demonstrates that the BN grains have dropped off the surface.In addition,mechanicaldenudation by high-speed Xe ions is recognized as the injury mechanism for the BN-matrix composite materials.     

Effect of MnO<Subscript>2</Subscript> on properties of SiC-mullite composite ceramics for solar sensible thermal storage

For improving the properties of SiC-mullite composite ceramics used for solar sensible thermal storage, MnO₂ was introduced as sintering additive when preparing. The composite ceramics were synthesized by using SiC, andalusite, α-Al₂O₃ as the starting materials with non-contact graphite-buried sintering method. Phase composition and microstructure of the composites were investigated by XRD and SEM, and the effect of MnO₂ on the properties of SiC composites was studied. Results indicated that samples SM1 with 0.2 wt% MnO₂ addition achieved the optimum properties: bending strength of 70.96 MPa, heat capacity of 1.02 J·(g·K)^-1, thermal conductivity of 9.05 W·(m·K)^-1. Proper addition of MnO₂ was found to weaken the volume effect of the composites and improve the thermal shock resistance with an increased rate of 27.84% for bending strength after 30 cycles of thermal shock (air cooling from 1 100 °C to RT).     

Solid Solution Characteristics of Pb（B1/3Nb2/3）O3-bascd Composite Ceramics

The solid solution characteristics of Pb（B1/3Nb2/3）O3-based （B=Zn^2＋, Mg^2＋, Ni^2＋） composite ceramics prepared by two-phase mixed-sintering method were developed based on dielectric measurements. Results show that there are double dielectric peaks for PZN-based composite ceramic, implying two phases coexist. However single dielectric peak was presented in PMN- and PNN-based composite ceramics, respectively. It is indicated that obvious solid solution reaction exists during the sintering process of these two systems. The effects of B-site ion difference on the solid solution characteristics were discussed by crystal chemistry. SEM was employed to investigated the microstructures of composite ceramics. The influences of solid solution reaction on grain growth were discussed.     

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.     

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.     

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 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.     

Preparation and piezoelectric properties of CuO-added (Ag<Subscript>0.75</Subscript>Li<Subscript>0.1</Subscript>Na<Subscript>0.1</Subscript>K<Subscript>0.05</Subscript>)NbO<Subscript>3</Subscript> lead-free ceramics

CuO-doped (Ag_0.75Li_0.1Na_0.1K_0.05)NbO₃ (ALNKN-xCuO, x = 0–2mol%) lead-free piezoelectric ceramics were prepared by the solid-state reaction method in air atmosphere. The effects of CuO addition on the phase structure, microstructure, and piezoelectric properties of the ceramics were investigated. The experimental results show that the ALNKN ceramics without doping CuO possess rhombohedral phase along with K2Nb6O16-type phase and metallic silver phase. For all of the CuO-doped ALNKN ceramics, a pure perovskite structure with the orthorhombic phase was obtained by enclosing the samples in a corundum tube. A homogeneous microstructure with the grain size of about 1 μm was formed for the ceramics with 0.5mol% CuO. The grain size increases with increasing amount of CuO. The temperature dependence of dielectric properties indicates that the ferroelectric phase of the ALNKN-xCuO ceramics becomes less stable with the addition of CuO. The ceramics with x = 1mol% exhibit relatively good electrical properties along with a high Curie temperature. These results will provide a helpful guidance to preparing other AN-based ceramics by solid-state reaction method in air atmosphere.     

Low-temperature sintering and microwave dielectric properties of Ba<Subscript>2</Subscript>Ti<Subscript>3</Subscript>Nb<Subscript>4</Subscript>O<Subscript>18</Subscript> ceramics

The effects of CuO and H3BO3 additions on the low-temperature sintering,microstructure,and microwave dielectric properties of Ba2Ti3Nb4O18 ceramics were investigated.The addition of less amount of CuO (< 1 wt%) considerably facilitated the densification of Ba2Ti3Nb4O18 ceramics.Appropriate addition of H3BO3 (< 3.5 wt%) remarkably improved the microwave dielectric properties of ceramics.The addition of H3BO3 and CuO successfully reduced the sintering temperature of Ba2Ti3Nb4O18 ceramics from 1300 to 1050 ℃.B...     

Effect of ZnO-B<Subscript>2</Subscript>O<Subscript>3</Subscript> glass addition on the microwave dielectric properties of BaO-Nd<Subscript>2</Subscript>O<Subscript>3</Subscript>-TiO<Subscript>2</Subscript>-Bi<Subscript>2</Subscript>O<Subscript>3</Subscript> system

The effect of ZnO-B₂O₃(ZB) glass addition on the sintering behavior, microstructures and microwave dielectric properties of BaO-Nd₂O₃-TiO₂-Bi₂O₃ (BNTB) system was investigated with the aid of X-ray diffraction, scanning electron microscopy and capacitance meter. It is found that the ZB glass addition, acting as a sintering aid, can effectively lower the sintering temperature of BNTB system to 850 °C. The dielectric constant of BNTB-ZB ceramics increases with the increase of soaking time and the value of dielectric loss decreased with increasing soak time. The optical dielectric properties at 1 GHz of ɛ=74, tan δ=4×10⁻⁴, and TCC=25 ppm/°c were obtained for the BNTB system doped with 25 wt% ZB glass sintered at 850 °C for 2 h, representing that the BNTB-ZB ceramics could be promising for multilayer low temperature co-fired ceramics applications.     

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.     

Effect of diatomite additive on the mechanical and dielectric properties of porous SiO<Subscript>2</Subscript>-Si<Subscript>3</Subscript>N<Subscript>4</Subscript> composite ceramics

Porous SiO₂-Si₃N₄ composite ceramics with high porosity and excellent mechanical properties were fabricated by pressureless-sintering at relatively low temperature of 1 500 °C using diatomite as pore forming agent. The effects of diatomite on flexural strength, fracture toughness, shrinkage, porosity and phase transformation of the porous ceramics were investigated in detail. Compared with that of the ceramic without adding diatomite, the porosity of the ceramic with 10% diatomite is increased by about 27.4%, the flexural strength and fracture toughness reaches 78.04 MPa and 1.25 MPa·m^1/2, respectively. As the porosity increases, the dielectric constant of porous SiO₂-Si₃N₄ ceramic decreases obviously from 3.65 to 2.95.     

Dielectric tunable properties of BaTi<Subscript>4</Subscript>O<Subscript>9</Subscript>-doped Ba<Subscript>0.6</Subscript>Sr<Subscript>0.4</Subscript>TiO<Subscript>3</Subscript> microwave composite ceramics

BaTi₄O₉-doped Ba_0.6Sr_0.4TiO₃ (BST) composite ceramics were prepared by the conventional solid-state reaction and their structure, dielectric nonlinear characteristics and microwave dielectric properties were investigated. The secondary phase of the orthorhombic structure Ba₄Ti₁₃O₃₀ is formed among BST composite ceramics with the increase of BaTi₄O₉. At the same time, a duplex or bimodal grains size distribution shows fine grains in a coarse grain matrix. The degree of frequency dispersion of dielectric permittivity below T _m is increased initially and then decreased with respect to BaTi₄O₉. As the BaTi₄O₉ content increases, the tunability of composite ceramics decreases, while the Q value increases. Interestingly, 70 wt% BaTi₄O₉-doped BST has a tunability ∼4.0% (under 30 kV/cm biasing) versus a permittivity ∼68 and quality factor ∼134.1 (at ∼3.2 GHz). Supported by the Ministry of Science and Technology of China through 973-project (Grant No. 2009CB623302), the Cultivation Fund of the Key Scientific and Technical Innovation Project, Ministry of Education of China (Grant No.707024), Shanghai Committee of Science and Technology (Grant No. 07DZ22302), and Shanghai Foundation Project under 06JC14070     

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.     

Dielectric Properties of B2O3 Doped MgTiO3-CaTiO3 System Ceramics

The dielectric ceramics with a main crystal phase of MGTiO3 and additional crystal phase of CaTiO3 were prepared by the conventional electronic ceramics technology .the strucures of MgTiO3 are ilmenitetype,and belong to hexagonal syngony.the ratio of MgTiO3 to Ca TiO3 doping on the dielectric properties of MGTiO3-CaTiO3(MCT)ceranics were inrestigated.the addition of B2O3 decreases the sintering temperatnre and results in rapid desification without obrious negative effect on the Q values of the system(Q=1/tan ).B2O3 exists as liquid phase in the sintering process,promoting the reactions as a singering agent.     

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)     

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.     

Preparation and properties of crystallizable Glass/Al<Subscript>2</Subscript>O<Subscript>3</Subscript> composites for LTCC material

The investigated low temperature Co fired ceramics(LTCC) composite of 60wt% CaO-Al2O3-B2O3-SiO2 glass and 40wt% α-Al2O3 as a filler is a non-reactive system, which is a critical part of the low temperature Co fired ceramics process. Through a study on densification process, the phase transformation and microstructure can be revealed. Its composites typically consist of CaO-Al2O3-B2O3-SiO2 glass and α-Al2O3 powders of average particle size (D50=3.49 mm). The sintering behavior, phase evaluation, sintered morphology, and microwave dielectric properties were investigated. In the fire range of 800 to 900 ℃, the composites were crystallized after completion of densification. It is found that the composites start to densify at 825 ℃, simultaneously, the dielectric constant (εr) reaches its maximum. With increasing heat-treatment temperatures, due to the loose microstructure of the material, tanδ increases slightly. The last of the sintered samples were identified as partly Anorthite at 850 ℃. At that temperature it has εr of 7.9 and tanδ less than 1×10-3, and can be used as a promising LTCC material.     

Microstrueturc and Mcehanieal Propcrtics of Heat-treated GeSb2Te4 Thin Films

The effect of annealing on microstructure, adhesive and frictional properties of GeSb2Te4 films were experimentally studied. The GeSb2Te4 films were prepared by radio frequency （RF） magnetron sputtering, and annealed at 200℃ and 340℃ under vacuum circumstance, respectively. The adhesion and friction experiments were mainly conducted with a lateral force microscope （LFM） for the GeSb2Te4 thin films before and after annealing. Their morphology and phase structure were analyzed by using atomic force microscopy （AFM） and X-ray Diffraction （XRD） techniques, and the nanoindention was employed to evaluate their hardness values. Moreover, an electric force microscope （EFM） was used to measure the surface potential. It is found that the deposited GeSb2Te4 thin film undergoes an amorphous-to-fcc and fcc-to-hex structure transition; the adhesion has a weaker dependence on the surface roughness, but a certain correlation with the surface potential of GeSb2Te4 thin films. And the friction behavior of GeSb2Te4 thin films follows their adhesion behavior under a lower applied load. However, such a relation is replaced by the mechanical behavior when the load is relatively higher. Moreover, the GeSb2Te4 thin film annealed at 340℃ presents a lubricative property.     

Preparation of MWNTs/Al<Subscript>2</Subscript>O<Subscript>3</Subscript> composites and their mechanical and electrical properties

Since their discovery by Iijima[1], carbon nanotubes (CNTs) have been the focus in novel materials research. Theoretical and experimental studies show[2-9] that CNTs have extraordinary mechanical and electrical properties. Krishnan et al.[2] have reported that the mean value of Young’s modulus of single-wall nanotubes (SWNTs) is 1.25 TPa. Yu et al.[3] measured Yang’s modulus of multi-wall nanotubes (MWNTs) between 270 and 950 GPa and breaking strength between 11 and 63 GPa. The ele…