Microstructure and microwave dielectric properties of lead borosilicate glass ceramics with Al_2O_3

The effects of Al2O3 addition on both the sintering behavior and microwave dielectric properties of PbO-B203-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 Tg and softening temperature Tf 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℃ have better properties of density p=2.72 g/cm3, dielectric constant Er=6.78, dielectric loss tan8=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.

Effect of Different Forms of Silica on Sintering, Microstructure and Properties of Borosilicate Glass/Al_2O_3 Composites

The effects of the introduction of silica glass and silica ceramic into Ca-Al-B-Si-O glass/ Al2O3 composites on decreasing the shrinkage and the dielectric constant of samples were investigated by FTIR, DSC, XRD and SEM. The results show that silica ceramic filler can better improve the formation of Si- O-Si network in the composites under high temperature, which leads to increased continuity of glass network at high temperature, and deduces the increase of viscosity of composites and further results in the decrease in the shrinkage of samples. Densification, three-point strength, and dielectric constant of samples decrease with the increase of silica glass or silica ceramic content. By contrast, Ca-Al-B-Si-O glass/Al2O3 composites with 4 wt% silica ceramic exhibit better properties of a bulk density of 2.81 g.cm-3, a porosity of 0.3%, a 3dp value of 202 MPa, a er value of 7.41 , a tan d value of 8.3 ×10^-4 at 10 MHz and a well matching with Ag electrodes. This material is suitable to be used as the LTCC material for the application in wireless communications.

The Effect of Sm_2O_3 on the Chemical Stability of Borosilicate Glass and Glass Ceramics

Sm2O3 containing zinc-borosilicate glass and glass ceramics were prepared by melt quenching method, and the effect of Sm2O3 and micro-crystallization on the chemical stability of borosilicate glass was explored. DTA analysis showed that the endothermic peak and exothermic peak of basic glass changed from 635 ℃ and 834 ℃ to 630 ℃ and 828 ℃ respectively as a result of the doping of Sm2O3. XRD analysis showed the promoting effect of Sm2O3 on crystallization ability of this glass. The cumulative mass loss of base glass, Sm2O3 containing glass, glass ceramic and Sm2O3 containing glass ceramic was 0.289, 0.253, 0.329, 0.269 mg/mm2 respectively after 26 days corrosion in alkali solution, and 1.293, 1.290, 0.999, 1.040 mg/mm2 respectively in acidic erosion medium. Micro-crystallization decreased and improved the alkali and acid resistance of borosilicate glass respectively, the addition of Sm2O3 increased the alkali resistance of base glass and glass ceramics, and the slight effect of Sm2O3 on the acid resistance of borosilicate glass was also observed.

Preparation and Optical Properties of Er^(3+)-Doped Gadolinium Borosilicate Glasses

Er^(3+)-doped Gd_2O_3 -SiO_2 -B_2O_3 -Na_2O glasses were prepared, and formation range of glass of Gd_2O_3 -SiO_2 -B_2O_3 system was experimentally obtained. It is found that the glass phase can be formed only when the content of SiO_2 is 0～50%(molar fraction), Gd_2O_3 is 0～30%(molar fraction) and B_2O_3 is above 20%(molar fraction) in this glass system. The glass can also be obtained but becomes translucent at the contents of 60%(molar fraction) SiO_2 and 30% Gd_2O_3 , or at the contents of 60%(molar fraction) SiO_2 and 30%(molar fraction) B_2O_3. There is no glass phase formed in other glass components. Glass forming ability for Gd_2O_3 content of 10%, was characterized by the value of β, the parameter of crystallization tendency, which is 0.32～1.76, obtained from the differential thermal analysis. The absorption and emission cross section, the J-O parameters Ωt_((2,4,6)) and radiative transition probabilities were calculated by using the theory of McCumber and Judd-Ofelt. The emission properties at 1.5 μm of the samples are discussed with the product of full width at half maximum and stimulated emission cross section. It can be seen that the value of the FWHM×σ_e^(peak) product in the prepared glass is more than those of germanate, silicate and phosphate glasses. Furthermore, the maximum value of the product among these glasses reported in this work is close to that of oxyfluoride silicate glass. Therefore, the Er^(3+)-doped gadolinium borosilicate glass in this paper is a candidate for broadband erbium doped fiber amplifiers.

Effect of Fe_2O_3 on non-isothermal crystallization of CaO-MgO-Al_2O_3-SiO_2 glass

The crystallization behavior and kinetics of CaO-MgO-Al2O3 SiO2（CMAS） glass with the Fe2O3 content ranging from zero to 5%were investigated by differential scanning calorimetry（DSC）.The structure and phase analyses were made by Fourier transform infrared spectroscopy（FT-IR） and X-ray diffraction（XRD）.The experiment results show that the endothermic peak temperature about 760℃ is associated with transition and the exothermic peak temperature about 1000℃ is associated with crystallization.The crystallization peak temperature decreases with increasing the Fe203 content.The crystallization mechanism is changed from two-dimensional crystallization to one-dimensional growth,and the intensity of diopside peaks becomes stronger gradually.There is a saltation for the crystallization temperature with the addition of 0.5%Fe2O3 due to the decomposition of Fe2O3.Si-O-Si,O-Si-O and T-O-T（T=Si,Fe,Al） linkages are observed in Fe2O3-CaO-MgO-Al2O3-SiO2 glass.

Al_(2)O_(3)在储能材料中的应用研究进展

Al_(2)O_(3)作为陶瓷材料、催化剂、催化剂载体及研磨磨料等有广泛的应用。因氧化铝具有优良的抗酸碱腐蚀性和力学等性能且热稳定性好、来源丰富,所以近年来逐渐开始应用在储能材料领域,进一步拓展了氧化铝的应用范围。主要针对氧化铝包覆后的二次储能电池正极材料、负极材料,以及改进隔膜的力学性能等方面进行研究。报道了近年来氧化铝在锂离子电池、钠离子电池、锂硫电池、电解液、隔膜方面的应用研究进展。

Modification of Nano-α-Al2O3 and Its Influence on the Surface Properties of Waterborne Polyurethane Resin Composite Passivation Films

Silane coupling agent KH560 was used to modify the surface of nano-α-Al2O3 in ethanol-aqueous solution with different proportions. The particle size of nano-α-Al2O3 was determined by nano-particle size analyzer, and the effects of nano-α-Al2O3 content, ethanol-aqueous solution ratio and KH560 dosage on the dispersion and particle size of nano-α-Al2O3 were investigated. The material structure before and after modification was determined by Fourier transform infrared spectroscopy (FTIR). Aqueous polyurethane resin and inorganic components are combined with modified nano-α-Al2O3 dispersion to form chromium-free passivation solution. The solution is coated on the galvanized sheet, the adhesion and surface hardness are tested, the bonding strength of the coating and the surface hardness of the substrate are discussed. The corrosion resistance and surface morphology of the matrix were investigated by electrochemical test, neutral salt spray test and scanning electron microscope test. The chromium-free passivation film formed after the modification of nano-α-Al2O3 increases the surface hardness of galvanized sheet by about 85%. The corrosion resistance of the film is better than that of a single polyurethane film. The results show that the surface hardness and corrosion resistance of polyurethane resin composite passivation film are significantly improved by the introduction of nano-α-Al2O3.

Preparation and Spectra Properties of BaO-Al_2O_3-P_2O_5-Sm_2O_3 System Protection Glasses

The forming-regions of phosphate glasses doped with high Sm2O3 contents were studied by two step melting method. The relationship between absorption spectrum and rare earth contents was also discussed. The spectra of BASP glasses were measured by spectrophotometer. The results show that the forming regions will shrink with the increase of Al2O3 and it is difficult to form glass when [PO4]/[AlO4] < 2. The forming regions tend to be a closed elliptical, and the intensity of characteristic absorption peak increases gradually with the increase of Sm2O3, the absorption lines broadens non-uniformly and there is approximate linear relation between optical density at the 1064 nm wavelength and Sm2O3 content.

Structure of Bi_2O_3-ZnO-B_2O_3 system low-melting sealing glass

Bi2O3-ZnO-B2O3 system glass is a kind of lead-free low melting sealing glasses. The structure of Bi2O3-ZnO-B2O3 system low-melting sealing glass was investigated by DSC, FT-IR, XRD and SEM. The results show that with the increase of B2O3 content, the transition temperature Tg and softening temperature Tf of Bi2O3-ZnO-B2O3 system low-melting sealing glasses increase, which leads to the liquid phase precipitation temperature increasing and promotes the structure stability in the glass. With increasing the heat treatment temperature, a large number of liquid phases appear in samples and the sinter efficiency of the samples increases. The FT-IR spectra of the glasses show the presence of some bands that are assigned to vibrations of Bi--O bond from [BO3] pyramidal and [BiO6] octahedral units and B--O from [BO3] and [BO4] units. With the decrease of B203 content, the crystallization tendency of the glass increases. In glass samples Bl and B〉 crystallization starts at 460 ℃ and 540 ℃, respectively. Both of them precipitate Bi24B2O39 phases.

THE STRUCTURE AND PROPERTIES OF Li_2O-Al_2O_3-SiO_2LOW EXPANSION GLASS CERAMICS CONTAINING B_2O_3

Through measuring the coefficient of linear expansion, the structure and properties of the Li2O-Al2O3-SiO2 low expansion glass ceramics containing B2O3 are studied by JR and XRD. It is shoutn that the IR method is efficient in the study of the glass-ceramics structure. There is a " Boron abnormality" in the system which has an important influence on the properties of the glass-ceramics.

Effect of SrO Content on Structure,Thermal Properties and Chemical Stability of Bi2O3-B2O3-ZnO-SrO Low-melting Glass for Si-Al Alloy Package

The 40Bi2O3-30B2O3-(30-x)ZnO-xSrO (x=0-15mol%,BBZSr) glass system was prepared by the conventional melt quenching method.The effect of SrO addition on structure,thermal properties,chemical stability and sealing performance of BBZSr glass were investigated thoroughly.The experimental results show that the total proportions of [BO3] group and [BO4] group decrease and the vibrations of [BiO3] group and [BiO6] group become weaker with the increase of SrO addition content,suggesting the glass network structure is strengthened owing to the SrO addition.Hence,both the thermal and chemical stability were significantly improved as the SrO content was increased.When the SrO content increased from 0 to 15mol%,the glass transition temperature and softening temperature slightly increased from 380 to 388 ℃ and from 392.7 to 402.2 ℃,respectively,meanwhile the coefficient of thermal expansion also increased from 10.49×10^-6 to 11.16×10^-6/℃ (30-300 ℃).The BBZSr glass with 15mol% SrO exhibited excellent comprehensive properties with low glass transition temperature(384.9 ℃),low softening temperature(400.3 ℃),high coefficient of thermal expansion (11.14×10^-6 ℃,30-300 ℃),good thermal and chemical stability.Besides,the glass had the good wetting behavior and sealing performance for Al-50%Si alloy.

Sintering,crystallization and dielectric properties of CaO-B_2O_3-SiO_2 system glass ceramics

CaO-B203-SiO2 （CBS） glass powders are prepared by conventional glass melting method at different melting temperatures whose properties and microstructures are characterized by X-ray diffraction （XRD） and scanning electron microscopy （SEM）. It is found that there are SiO2 and some unknown phases in CBS glass melting liquid from 1 300 ℃ to 1 500 ℃ and the amount of these phases decreases with the increase of the melting temperature. The CBS glass melted at 1 450 ℃ could be sintered from 830 ℃ to 930 ℃ and the bulk densities of the samples are all higher than 2.4 g/cm^3. From the points of the properties and energy conservation, the melting temperature of 1 450 ℃ is the optimal melting temperature. The glass ceramic sintered at 850 ℃ exhibits better dielectric properties： er=6.33, tan6=2.2×10^-3 at 10 GHz, and the major phases of the samples are CaSiO3, CaB2O4 and SiO2.

Three-photon-excited fluorescence of Tb^(3+)-doped CaO-Al_2O_3-SiO_2 glass by femtosecond laser irradiation

A near infrared to visible blue, green, and red upconversion luminescence in a Tb^3＋-doped CaO-Al2O3-SiO2 glass was studied, which was excited using 800 nm femtosecond laser irradiation. The upconversion luminescence was attributed to ^5D3→^7F5, ^5D3→^7F4, ^5D3→^7F3, ^5D4→^7F6, ^5D4→^7F5, ^5D4→^7F4, and ^5D4→^7F3 transitions of Tb^3＋. The relationship between upconversion luminescence intensity and the pump power indicated that a three-photon simultaneous absorption process was dominant in this upconversion luminescence. The intense red, green, and blue upconversion luminescence of Tb^3＋-doped CaO-Al2O3-SiO2 glass may be potentially useful in developing three-dimensional display applications.

Microstructure and dielectric properties of Ca-Al-B-Si-O glass/Al_2O_3 composites with various alkali oxides contents

The effects of alkali oxides （Na2O and K2O addition on both the sintering behavior and dielectric properties of Ca-AI-B-Si-O glass/Al2O3 composites were investigated by Fourier transform infrared spectroscopy （FTIR）, differential scanning calorimeter （DSC）, X-ray diffractometry （XRD） and scanning electron microscopy （SEM）. The results show that the increasing amount of alkali oxides in the glass causes the decrease of [SiO4], which results in the decrease of the continuity of glass network, and leads to the decrease of the softening temperature Tf of the samples and the increasing trend of crystallization. And that deduces corresponding rise of densification, dielectric constant, dielectric loss of the low temperature co-fired ceramic （LTCC） materials and the decrease of its thermal conductivity. By contrast, the borosilicate glass/A1203 composites with 1.5% （mass fraction） alkali oxides sintered at 875 ℃ for 30 rain exhibit better properties of a bulk density of 2.79 g/cm3, a porosity of 0.48%, a 2 value of 2.28 W/（m.K）, a er value of 7.82 and a tand value of 9.1 × 10-4 （measured at 10 MHz）.

JOINING MECHANISMS OF β"-Al_2O_3 CERAMIC AND PYREX GLASS TO Al MATRIX COMPOSITE

The bonding of β″-Al2O3 and pyrex glass to A1 matrix composites by anodic bonding process is achieved. The microstructure of the bonded interface and the joining mechanisms are analyzed with scanning electron microscope （SEM）, energy dispersive X-ray fluorescence spectrometer （EDX）. It is observed that the bonding region across the interface consists of the metal layer, oxide transitional layer and the ceramic layer, with the transitional layer composed of surface region and sub-surface region. The bonding process can mainly be categorized into anodic bonding process and solid state diffusing process. The pile-up of the ions and its drift in the interface area are the main reasons for anode oxidation and joining of the interface. The temperature, voltage and the drift ions in the ceramic or glass during the bonding process are the essential conditions to solid state diffusing and oxide bonding at the interface. The voltages, temperature, pressure as well as the surface state are the main factors that influence the anodic bonding.

BRIGHT LONG AFTERGLOW PHOSPHORESCENCE GLASS MADE OF SrAl_(2)O_(4): Eu^(2+), Dy^(3+) AND GLASS FRITS

Bright long afterglow phosphorescence glasses were prepared by using SrAl2O4： Eu^2＋, Dy^3＋ phosphors and suitable glass frits together. The SrAl2O4： Eu^2＋, Dy^3＋ phosphors were initially prepared by the solid reaction method. Three kinds of glass frits were prepared to match the SrAl2O4： Eu^2＋, Dy^3＋ phosphors. Effects of the compositions of the glass frits, the ratios of the phosphors to the frits us well us the firing temperature and firing times on the properties of the samples were discussed. XRD analysis indicated the samples exhibited the typical diffraction peaks of SrAlwO4： Eu^2＋, Dy^3＋. The emission spectra of the samples showed broad bands peaking at 510nm.The excitation spectra of the samples showed broad bands ranging from 300 to 480hm. These are believed due to the 5d4f-4f transitions of Eu^2＋ in the SrAl2O4： Eu^2＋, Dy^3＋ phosphors. The afterglow luminescence of the samples excited by a 40W fluorescence lamp for 30min can be observed in the dark for more lOh with the naked eyes. It can find wide applications in many fields.

Preparation,Structures,Thermal Properties and Sintering Behaviors of B_2O_3-SiO_2-ZnO-BaO-Al_2O_3 Glass

B_2O_3-SiO_2-ZnO-BaO-Al_2O_3 glass with different Al_2O_3 contents（1mol%, 3mol%, 5mol%, and 7mol%） was prepared, and it was intended to be used as lead-free and low-melting glass sealants for solid oxide fuel cells. The effects of Al_2O_3 content on the structures, thermal properties, and sintering behaviors of the B_2O_3-SiO_2-ZnO-BaO-Al_2O_3 glass were investigated in detail. The Al_2O_3 content largely influenced the structures and thermal properties of the glass. When the Al_2O_3 content 5mol%, the transition temperature of the glass decreased with the Al_2O_3 content, while the crystallization temperature increased with the Al_2O_3 content. However, higher Al_2O_3 content degraded the stability of the glass. The B_2O_3-SiO_2-ZnO-BaO-Al_2O_3 glass with 5 mol% Al_2O_3 content exhibits the optimal sintering densification characteristics and can be used as glass sealants for solid oxide fuel cells.

Melting, sintering and wetting properties of ZnO–Bi_2O_3–B_2O_3 sealing glass

Glasses based on ZnO-Bi_2O_3-B_2O_3 system are expected to be a new kind of sealing glasses because of their low melting temperature and other properties.In order to reveal the effect of B_2O_3 on the rheological behavior of ZnO-Bi_2O_3-B_2O_3 system glass melt,the properties of viscosity,thermal expansion,fluxion property and wetting process between cylinder samples and stainless steel were investigated with the rotating crucible viscometer,dilato meter and high-temperature microscope.The structure of sintered glass samples was investigated with scanning electron microscope.The results show that the B_2O_3 content increasing in B_1-B_3 at the given temperature between 400 ℃ and 500 ℃ leads to the increasing of the sample viscosity.When the amount of B_2O_3 increases from 5.24%to 9.24%(mass fraction),the coefficients of thermal expansion of glass samples decrease smoothly from 10.94×10^(-6) to10.71×10^(-6) and 10.38×10^(-6) ℃^(-1) respectively.In the case of sealing temperature,its value increases from 453 ℃ to 494 ℃.ZnO-Bi_2O_3-B_2O_3 system low-melting glass powder sintering was with viscous liquid to participate,which could make the densification of glass sample more effective and more efficient.With the content of B_2O_3 increasing,the wetting angle between the glasses samples and stainless steel could also increase,and the resulting appropriate sealing temperature range is 460-490 ℃.

激光清洗硅片表面Al_2O_3颗粒的试验和理论分析

以KrF准分子激光器为激光源,对目前工业上常用的硅片研磨抛光液的主要成分Al2O3颗粒进行激光清洗的试验和理论分析。建立一维热传导模型,利用有限元分析软件MSC.MarC模拟硅片表面的温度随激光作用时间和能量密度的分布。通过理论计算,量化了颗粒所受到的清洗力以及其与硅片表面之间的粘附力,理论预测出1μm Al2O3颗粒的激光清洗阈值为60 mJ/cm2。在理论分析的指导下,利用248 nm3、0 ns的KrF准分子激光进行单因素试验,研究激光能量密度、脉冲个数、激光束入射角度对激光干法清洗效率的影响,并且实验验证了清洗模型以及场增强效应对激光清洗结果的影响。

纳米Al_2O_3改性变压器绝缘纸性能的研究

为了研究纳米Al2O3改性绝缘纸的绝缘性能,实验室制备了含不同质量分数的纳米Al2O3绝缘纸手抄片,并对真空浸油后的绝缘纸性能进行了测试。结果表明在一定的质量分数内纳米Al2O3改性后的绝缘纸的工频击穿场强得到较大的提高,在质量分数为1%时,工频击穿场强提高了12.75%,绝缘纸的抗张强度增加了14.13%;在1%的添加量内绝缘纸的介电常数、介电损耗都随纳米Al2O3含量的增加而减小。