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.     

Microstructure and microwave dielectric properties of CaO-B2O3-SiO2 glass ceramics with various B2O3 contents

The effects of B2O3 addition on both the sintering behavior and microwave dielectric properties of CaO-B2O3-SiO2 (CBS) glass ceramics were investigated by Fourier transform infrared spectroscopy (FTIR),X-ray diffractometry (XRD) and scanning electron microscopy (SEM).The results show that the increasing amount of B2O3 causes the increase of the contents of [BO3],[BO4] and [SiO4],which deduces the increase of CaB2O4 and α-SiO2 and the decrease of CaSiO3 correspondingly.No new phase is observed throughout the...     

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.     

Effect of nano-ZrO2 on microstructure and thermal shock behaviour of Al2O3/SiC composite ceramics used in solar thermal power

The Al2O3-ZrO2(3Y)-SiC composite ceramics used in solar thermal power were prepared by micrometric Al2O3,nano-ZrO2 and SiC powders under the condition of pressureless sintering.The bulk density and bending strength of samples with 10vol% nano-ZrO2 sintered at 1480℃ were 3.222 g/cm3 and 160.4MPa,respectively.The bending strength of samples after 7 times thermal shock tests (quenching from 1000℃ to 25℃ in air medium) is 132.0MPa,loss rate of bending strength is only 17%.The effect of nano-ZrO2 content on the microstructure and performance of Al2O3-ZrO2(3Y)-SiC composite ceramic was investigated.The experimental results show that the bending strength of samples with above 10vol% nano-ZrO2 content has decreased,because the volume expansion resulting from t-ZrO2 to m-ZrO2 phase transformation is excessive;Adding proper nano-ZrO2 would be contributed to improve the thermal shock resistance of the composite ceramics.The Al2O3-ZrO2(3Y)-SiC composite ceramic has promising potential application in solar thermal power.     

Microstructure and microwave dielectric properties of lead borosilicate glass ceramics with Al2O3

The effects of Al₂O₃ addition on both the sintering behavior and microwave dielectric properties of PbO-B₂O₃-SiO₂ glass ceramics were investigated by Fourier transform infrared spectroscope (FTIR), differential thermal analysis (DTA), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The results show that with the increase of Al₂O₃ content the bands assigned to [SiO₄] nearly disappear. Aluminum replaces silicon in the glass network, which is helpful for the formation of boron-oxygen rings. The increase of the transition temperature T _g and softening temperature T _f of PbO-B₂O₃-SiO₂ glass ceramics leads to the increase of liquid phase precipitation temperature and promotes the structure stability in the glasses, and consequently contributes to the decreasing trend of crystallization. Densification and dielectric constants increase with the increase of Al₂O₃ content, but the dielectric loss is worsened. By contrast, the 3% (mass fraction) Al₂O₃-doped glass ceramics sintered at 725 °C have better properties of density ρ=2.72 g/cm³, dielectric constant ɛ _r =6.78, dielectric loss tan δ=2.6×10⁻³ (measured at 9.8 GHz), which suggest that the glass ceramics can be applied in multilayer microwave devices requiring low sintering temperatures.     

Forming regularity and relation between composition and property of B2O3-BaO-ZnO glass

B2O3-BaO-ZnO glass was prepared by using conventional melt quenching technology. The forming regularity and the relationship between the composition and the property of B2O3-BaO-ZnO glass were investigated. The results show that the composition range for forming B2O3-BaO-ZnO glass is very wide, but the content of B2O3 has a limit within mole fraction of 25%-75%. When the content of B2O3 is over the limit, the melt will be divided into two phases with different compositions and structures, whereas too low content of B2O3 will result in the crystallization of the melt during the cooling process. The thermal expansion coefficient, the transition temperature and the resistivity of the glass at room temperature are (5-10)×10-6 ℃-1, 480-620 ℃ and (1.5-3.0)×1010 Ω·m, respectively.     

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.     

In-Situ Preparation and thermal shock resistance of mullite-cordierite heat tube material for solar thermal power

In order to improve the thermal shock resistance of solar thermal heat transfer tube material, the mullite-cordierite composite ceramic as solar thermal heat transfer tube material were fabricated by pressureless sintering using α-Al2O3 , Suzhou kaolin, talc, and feldspar as starting materials. The important parameter for solar thermal transfer tube such as water absorption (Wa ), bulk density (Db ), and the mechanical properties were investigated. The phase composition and microstructure of the composite ceramics were analyzed by XRD and SEM. The experimental results show that the B3 sintered at 1 300 ℃ and holding for 3 h has an optimum thermal shock resistance. The bending strength loss rate of B3 is only 2% at 1 100℃ by air quenching-strength test and the sample can endure 30 times thermal shock cycling, and the water absorption, the bulk density and the bending strength are 0.32%, 2.58 g·cm-3 , and 125.59 MPa respectively. The XRD analysis indicated that the phase compositions of the sample were mullite, cordierite, corundum, and spinel. The SEM images illustrate that the cordierite is prismatic grain and the mullite is nano rod, showing a good thermal shock resistance for composite ceramics as potential solar thermal power material.     

Luminescent properties of Ce3+ ions in zinc phosphate glass prepared in air

Glasses are prepared by sintering P2O5, ZnO and Ce2(C2O4)3 10H2O mixtures at 1 100 ℃ in air and then annealed at 400 ℃ for 10 hours. The obtained glasses are homogeneous, transparent and colorless. Emission and excitation spectra are measured for the samples and the results show that the glasses contain Ce3+ trivalent cerium ions. The parameters of glass preparation obtained here may be adapted to preparing this type of glasses doped with other lanthanide ions, so as to study energy transfer phenomena and variation of radiative lifetime with refractive index due to local field effect.     

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.     

Effects of rare earth oxides on viscosity,thermal expansion,and structure of alkali-free boro-aluminosilicate glass

Effects of rare earth oxides(Y_2O_3,La_2O_3,and Er_2O_3) on the viscosity,thermal expansion,and structure of alkali-free boro-aluminosilicate glasses were investigated by the rotating crucible viscometer,dilatometry and FT-IR absorption spectra.The results showed that the melting temperature of alkali-free boroaluminosilicate glasses decreased from 1 697.55 to 1 662.59,1 674.37 and 1 640.87 ℃ with the introduction of 1 mol%La_2O_3,Y_2O_3 and Er_2O_3,respectively.However,the glass transition temperature T_g,dilatometric softening temperature T_d and coefficient of thermal expansion of alkali-free boro-aluminosilicate glasses increased when adding the rare-earth oxides.At high temperatures,incorporating rare earth oxides into glass resulted in the peak at about 1 085 cm~(-1) towards lower wavenumber and the absorption band in the region of850-1 260 cm~(-1) broader,which indicated that rare earths acted as network modifiers and increased the numbers of non-bridging oxygen in the glass melts.However,the rare earths had an opposite effect and accumulated the glass structure at low temperatures near T_g.     

Low-temperature sintering and microwave dielectric properties of Li2MgTi3O8 ceramics doped with BaCu（B2O5）

The influences of BaCu(B₂O₅) (BCB) addition on sintering, microstructure and microwave dielectric properties of Li₂MgTi₃O₈ ceramics were investigated using X-ray diffractometry, scanning electron microscopy and microwave dielectric measurements. The experimental results show that a small amount of BaCu(B₂O₅) addition can effectively reduce the sintering temperature to 900 °C, and induce only a limited degradation of the microwave dielectric properties. Typically, the best microwave dielectric properties of ɛ _r=24.5, Q×f =24 622 GHz, τ _f=4.2×10⁻⁶ °C⁻¹ are obtained for 1.0% BCB-doped Li₂MgTi₃O₈ ceramics sintered at 900 °C for 3 h. The BCB-doped Li₂MgTi₃O₈ ceramics can be compatible with Ag electrode, which may be a strong candidate for low temperature co-fired ceramics applications.     

Relationship between Liquid Phase Content and the Orientation of PMNT Ceramics by TGG Method

The effects of glass frit on the sintering and electric properties of PMN-PT textured ceramics were investigated. The glass frits, including PbO, Bi2O3 and ZnO, were selected since liquid phase sintering lowered the PMN-PT sintering temperature. The piezoelectric properties of PMN-PT ceramics with glass frit addition are strongly dependent on the densification. The addition of glass frits into PMN-PT matrix reduced the sintering temperature to 1 100 ℃ instead of 1 150 ℃ for samples without glass. The piezoelectric coefficients (d33) of PMN-PT textured ceramics achieved 568 pc/N with 1 wt% excess PbO.     

Effects of heat treatment temperature on crystallization and thermal expansion coefficient of Li2O-Al2O3-SiO2

The basic glass of Li₂O-Al₂O₃-SiO₂ system using P₂O₅ as nucleator was prepared by means of conventional melt quenching technology, and the heat-treatment process was determined by using differential thermal analysis. The crystalline phases and the microstructure of the glass-ceramics were investigated by using X-ray diffraction and scanning electron microscopy. The results show that the glass based on Li₂O-Al₂O₃-SiO₂ oxides using P₂O₅ as nucleator can be prepared at lower melt temperature of 1450°C and the glass-ceramics with lower thermal expansion coefficient of 21.6 × 10⁻⁷°C⁻¹ can also be obtained at 750°C. The glass-ceramics contain a few crystal phases in which the main crystal phase is β-quartz solid solution and the second crystal phase is β-spodumene solid solution. When the heat treatment temperature is not higher than 650°C, the transparent glass-ceramics containing β-quartz solid solution can be prepared. β-quartz solid solution changes into β-spodumene solid solution at about 750°C. And the appearance of the glass-ceramics changes from translucent, part opaque to complete opaque with increasing temperature.     

The effect of Bi2O3 on the structure and properties of float glass

CaO-Al₂O₃-SiO₂ system float glasses were melted at an elevated temperature, and about 60% of the total energy was occupied by melting and clarification stage. In order to reduce the melting temperature of the float glasses, Bi₂O₃ was added as fluxing agent. The structure and some melting properties such as the influence of the addition of the oxidation bismuth on the properties of float glass melt, melting temperature, and the structure of glass were studied. The results showed that the basic structure was not changed with the addition of Bi₂O₃ from 0.5% to 2%. The viscosity of the glass melt decreased with the addition of Bi₂O₃ obviously, as the viscosity of the glass melt was 1.35 Pa·s, the temperature was reduced by about 30 °C from sample A₁ to sample A₅. With the increasing of Bi₂O₃, the bending strength of glass was reduced and the transmisivity of glass samples had no change in visible light range, and the transmissivity of the glass samples was more than 88%. The ultraviolet cut-off length showed red shift with the addition of Bi₂O₃. With the increasing of Bi₂O₃, the water resistance of the glass samples was improved.     

Effects of Substrate Temperatures on the Structure and UV-shielding Properties of TiO2-CeO2 Films Deposited on Glass by Radio-frequency Magnetron Sputtering

TiO2-CeO2 films were deposited on soda-lime glass substrates at varied substrate temperatures by rf magnetron sputtering using 40% molar TiO2-60% molar CeO2 ceramic target in Ar：O2=95：5 atmosphere.The structure,surface composition,UV-visible spectra of the films were measured by scanning electron microscopy and X-ray diffraction,and X-ray photoelectron spectroscopy,respectively.The experimental results show that the films are amorphous,there are only Ti^4＋ and Ce^4＋ on the surface of the films,the obtained TiO2-CeO2 films shou a good uniformity and high densification,and the films deposited on the glass can shield ultraviolet light without significant absorpition of visible light,the films deposited on substrates at room temperature and 220℃ absorb UV effectively.     

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.     

Effect of annealing on microstructure and properties of Si_3N_4-AlN composite ceramics

Aiming at developing novel microwave-transparent ceramics with low dielectric loss,high thermal conductivity and high strength,Si3N4-AlN(30%,mass fraction) composite ceramics with La2O3 as sintering additive were prepared by hot-pressing at 1 800 °C and subsequently annealed at 1 450 °C and 1 850 °C for 2 h and 4 h,respectively.The materials were characterized by XRD and SEM.The effect of annealing process on the phase composition,sintering performance,microstructure,bending strength,dielectric loss and the...     

Fabrication and characterization of composite YSZ-La9.33Si6O26 oxygen-ion conductor

To improve the conductivity of Y₂O₃-stabilized ZrO₂ (YSZ) based oxygen-ion conductor, Zr_0.85Y_0.15O_1.925-La_9.33Si₆O₂₆ (YSZ-LSO) composite ceramics with the mass fraction of La_9.33Si₆O₂₆ (LSO) of 15% were prepared by using a modified coprecipitation method. The phases, microstructures and conductivities of the YSZ, LSO and YSZ-LSO were investigated by X-ray diffraction, electron microscopy and complex impedance, respectively. The results show that the as-calcined powder of YSZ-LSO composite has the grain size less than 10 nm, and the as-sintered composite ceramics are composed of YSZ and LSO phases. The conductivity can be enhanced obviously by composite method. At 700 °C, the conductivity of the composite ceramic is 0.125 S/cm, which is one order in magnitude higher than that of the YSZ ceramic and two orders in magnitude higher than that of LSO ceramic. By analyzing the impedance spectra and modulus spectra, the interfacial effect on the conductivity improvement was proposed.     

Effect of nucleating agent on the crystallization of tailings glass ceramics prepared by one-time sintering

Glass ceramics was made by the one-time sintering method using the main raw material of iron tailings. On the basis of quaternary system of CaO-MgO-Al₂O₃-SiO₂, using DTA, XRD and SEM, the effects of different nucleating agents and mixing amounts as well as heat treatment on the crystallization of tailings glass ceramics were studied. The experimental results show that, nucleating agent and heat treatment are two necessary conditions for one-time sintering preparation of tailings glass ceramics namely, only adding nucleating agent or experiencing heat treatment, the quaternary system can not crystallize. The composite nucleating agent consisting of Cr₂O₃ and TiO₂ can further lead to the crystallization of the CaO-MgO-Al₂O₃-SiO₂ quaternary system at the lower temperature, with the major phase of diopside. In the range of mass content, 0%–4%, crystal intensity and crystal content grow. But when mass content is more than 4%, the crystal size will become coarser and the crystal distribution will be less regular. Different heat treatment regimes do not change the composition of the crystalline major phase in the glass ceramics crystallization of CaO-MgO-Al₂O₃-SiO₂ system. In the range of 30–60 minutes, with the extension of nucleation and crystallization, crystallization degree enhanced, but if the holding time surpasses 60 minutes, the crystallization is worse. Funded by The National Key Technology R & D Program of China for the 11^th Five-Year Plan(2006BAJ04A04)