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...     

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...     

Structure and dielectric properties of ZnO and Nb<Subscript>2</Subscript>O<Subscript>5</Subscript> doped BaO-TiO<Subscript>2</Subscript> system microwave ceramics

The microwave dielectric properties and microstructure of BaTi4.3ZnyO9.6＋y ＋0.02 mol% SnO2＋0.01 mol% MnCO3＋x mol% Nb2O5（x=0-0.05, y=0-0.08） system ceramics were studied as a function of the amount of ZnO and Nb2O5 doped. Addition of （y=0-0.05） ZnO and （x=0-0.025） Nb2O5 enhanced the reactivity and decreased the sintering temperature effectively. It also increased the dielectric constant ε r and quality factor Q（=1/tan 8） of the system due to the substitution of Ti^4＋ ions with incorporating Zn^2＋and Nb^5＋ ions, which was analyzed by the reaction ZnO＋Nb2O5＋ 3 TiTxTi →ZnTi＋ 2NbTi＋3TiO2. When the system doped with （y=0.05） ZnO and （x=0.025） Nb205 were sintered at 1 160 ℃ for 6 h, the εr. Qf0 value and rfwere 36.5, 42 000 GHz, and＋1.8 ppm/℃, respectively, at 5 GHz.     

Thermodynamic analysis of the formation of <Emphasis Type="Italic">In-situ</Emphasis> reinforced phases in cast Al-4.5Cu alloy

The thermodynamic analysis of the formation of in-situ reinforced phases in （TiB2＋Al3Ti）/Al-4.5Cu composites prepared by mixed salts reaction was conducted, and heat changes of mixed salts system were analyzed by differential thermal analysis（DTA）.The results show that although TiB2 possesses the strongest formation ability in Al-Ti-B ternary system, [Ti] is relatively excessive in the in-situ reaction and it combines with Al to form AlaTi phase. The reinforced phases are TiB2 and AlaTi in the produced composites due to the reaction taking place to form reinforced phase with the addition of mixed salts into Al-4.5Cu melt between 900 ℃ and 1 032 ℃.     

Synthesis and Dielectric Properties of New Niobate BiTi3Nb7O30

A new niobate Ba5 BiTi3Nb7O30 was synthesized by the solid-state reaction. It was characterized by X-ray diffraction and dielectric constant measurements. The results show that Ba5BiTi3Nb7O30 is paraelectric at room temperature and belongs to tetragonal 4/ mmm symmetry with unit cell parameters a = 1.25020 nm, c =0.39704 nm. Ba5BiTi3Nb7O30 has only one phase transition, paraelectric to ferroelectric, below 0℃.     

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.     

Preparation, Characterization and Dielectric Property of Sr5 LaTi3 Nb7O30 Ceramic

Sr5LaTi3Nb7O30 ceramic was prepared by the conventional high temperature solid-state reaction route. The sintered samples were characterized by X-ray diffraction, scanning electron microscopy ( SEM ), differential thermal calorimetry ( DSC ) and dielectric measurements. The results show Sr5LaTi3Nb7O30 belongs to paraclectric phase of filled tetrngonal TB structure at room temperature, and undergoes a diffuse phase transition in the temperature range of -54-34℃ . And Sr5LaTi3Nb7O30 ceramic shows a high dielectric constant of 479 with a low dielectric loss of 0.005 at 1MHz . In comparison with Ba-based ceramics with TB structure, the temperature coefficients of the dielectric constant ( τt ) is significantly reduced.     

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.     

Effect of Grain Size of CaCO3 and SiO2 on the Formation of C3S Under Different Conditions

The effect of grain size of CaCO3 and SiO2 on the formation of C3S under various conditions, such as rapid heating rate（800 ℃/min）, normal heating rate（30 ℃/min） and in the presence or absence of ZnO, was studied. The results show that the decomposition temperature of CaCO3, the temperature of appearance of liquid phase and the f-CaO content descend when the grain size of CaCO3 and SiO2 becomes smaller, which attributes to the reactive activity enhancement of powders due to the decrease of the particle size. When the grain size of CaCO3 and SiO2 is below 1 μm, the rate of the formation of C3S is greatly raised. A rapid sintering rate and the presence of ZnO have an important effect on the formation of C3S and can lower the temperature of the formation of C3S by about 50 ℃.     

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.     

Phase structure and electrical properties of La<Subscript>2</Subscript>O<Subscript>3</Subscript>-doped BiInO<Subscript>3</Subscript>-PbTiO<Subscript>3</Subscript> ceramics with high curie temperature

The phase structure and electrical properties of pure and La2O3-doped Bi-InO3-PbTiO3 （BI-PT） ceramics were studied respectively. In （1 -x）BI-xPT （x=0.72-0.80） ceramics, the stability of tetragonal phase increased with increasing x, and pure perovskite structure was obtained for x=-0.80 ceramics. The phase transition temperature range was between 575 ℃ and 600 ℃ for x=0.72-0.80 ceramics, higher than that of PT （-490 ℃）. The c/a ratio almost linearly decreased with increasing La2O3 content in x-0.80 ceramics. It is believed that Pb^2＋ vacancies were formed by La^3＋ substituting Pb^2＋ in La2O3-doped BI-PT ceramics. Tc shifted to lower temperature by 30 ℃/mol% La2O3. The maximum dielectric constant 8557 around 559 ℃ was exhibited in 0.5mol%-doped BI-0.80PT ceramics. La2O3-doped ceramics could be poled resulting from decreasing of c/a ratio and improving of dielectric loss and resistivity. The maximum piezoelectric coefficient d33 was 12 pC/N for 2mol%-doped BI-0.80PT ceramics.     

Structure and properties of Mg-doped SrBi<Subscript>4</Subscript>Ti<Subscript>4</Subscript>O<Subscript>15</Subscript> Bi-layered compounds

The structure and properties of Mg-doped SrBi4Ti4O15（SBT） were dicussed. Mg substitution into SBT had two possibilities states with the dopant amount variety. Mg cation substituted mostly into Sr^2＋ and the amount proportion was 68.11%.Mg ion will substitute into Ti ion site in perovskite layer when the doping amount increases. Polarization increases sharply when x=0.1 and then decreases becauses of the domain pinning. The Curie temperature of Mg-doped SBT is about 300 ℃ and there is a broad diffuse phase transition near Tc with a flat peak near the Ta of SBT.     

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.     

In-situ TEM Study on Mierostruetural Evolution of Nanostruetured TiO2

The effect of electron beam on the microstructures and phase transformation of nanostructured TiO2 heat treated at various temperatures for different time was studied by in-situ TEM and SAED. Anatase ex-situ heated at 250℃ and 360℃ transformed to rutile while irradiated by the electron beam. With the increasing sizes and distribution of the powders on the amorphous carbon, the process of phase transformation by the electron beam was encumbered. These evolutions may be due to the changes of vacuum atmosphere and the properties of powders.     

Stability of titanium-aluminium nitride (Ti<Subscript>2</Subscript>AlN) at high pressure and high temperatures

The stability of Ti2AlN at high pressure of 5 GPa and different temperatures of 700-1 600 ℃ was investigated using X-ray diffraction (XRD),scanning electron microscopy (SEM) equipped with an energy dispersive spectrometer (EDS).Ti2AlN was found to be stable at temperatures as high as 1 400 ℃under 5 GPa for 20 min,and was proved that it held better structure stability than Ti2AlC under 5 GPa through comparative experiments of Ti2AlN and Ti2AlC (representative compounds of M2AX phases (211 phase)).The reaction process at high pressure had some difference from that at ambient pressure/vacuum,and Ti2AlN directly decomposed to TiN and TiAl at 5 GPa and 1 500 ℃ for 20 min.Moreover,the mechanism of phase segregation was discussed.In addition,the behavior of Ti2AlN contacting with Zr at high pressure and high temperature (HPHT) was also studied.     

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.     

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.     

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.     

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.     

High-temperature oxidation behavior of Al<Subscript>2</Subscript>O<Subscript>3</Subscript>/TiAl matrix composite in air

The oxidation behavior of Al₂O₃/TiAl in situ composites fabricated by hot-pressing technology was investigated at 900° in static air. The results indicate that the mass gains of the composites samples decrease gradually with increasing Nb₂O₅ content and the inert Al₂O₃ dispersoids effectively increase the oxidation resistance of the composites. The higher the Al₂O₃ dispersoids content, the more pronounced the effect. The primary oxidation precesses obey approximately the linear laws, and the cyclic oxidation precesses follow the parabolic laws. The oxidized sample containing Ti₂AlN and TiAl phases in the scales exhibits excellent oxidation resistance. The oxide scale formed after exposure at 900°C for 120 h is multiple-layered, consisting mainly of an outer TiO₂ layer, an intermediate Al₂O₃ layer, and an inner TiO₂+Al₂O₃ mixed layer. From the outer layer to the inner layer, TiO₂+Al₂O₃ mixed layer presents the transit of Al-rich oxide to Ti-rich oxide mixed layer. Near the substrate, cross-section micrograph shows a relatively loose layer, and micro- and macro-pores remain on this layer, which is a transition layer and transferres from Al₂O₃+TiO₂ scale to substrate. The thickness of oxide layer is about 20 μm. It is also found that continuous protective alumina scales can not be observed on the surface of oxidation scales. Ti ions diffuse outwardly to form the outer TiO₂ layer, while oxygen ions transport inwardly to form the inner TiO₂+Al₂O₃ mixed layer. Under long-time intensive oxidation exposure, the internal Al₂O₃ scale has a good adhesiveness with the outer TiO₂ scale. No obvious spallation of the oxide scales occurs. The increased oxidation resistance by the presence of in situ Al₂O₃ particulates is attributed to the enhanced alumina-forming tendency and thin and dense scale formation. Al₂O₃ particulates enhance the potential barrier of Ti ions from M/MO interface to O/MO interface, thereby the TiO₂ growth rate decreases, which is also beneficial to improve the oxidation resistance. Moreover, the multi-structure of the TiO₂+Al₂O₃ mixed layer decreases the indiffusion of oxygen ions and also avails to improve the high temperature oxidation resistance of the as-sintered composites. Supported by the Special Program for Education Bureau of Shaanxi Province, China (Grant No. 08JK240) and Scientific Research Startup Program for Introduced Talents of Shaanxi University of Technology, China (Grant No. SLGQD0751)