RESEARCH AND PRODUCTION OF GLASS-CERAMIC DECORATED MATERIAL CONTAINING CHROMIUM

In this paper, the influences of catch-color agent content on glass-ceramic decorated material in the system of CaO-Al_2O_3-SiO_2 were studied. By ladder temperature furnace and sintering shrinkage curve measurement, the influence of catch-color agent content on sintering and crystallization temperature was discussed. By means of XRD, three point bending strength and density measurement, the properties of the decorated material were investigated.     

Na_2O对微晶玻璃装饰板烧结和析晶的影响

研究了Na_2O含量对CaO-Al_2O_3-SiO_2系统微晶玻璃装饰板析晶温度、析晶相,烧结收缩及表面气泡的影响。确定了合适的Na_2O含量及烧结温度范围。     

热处理对CaO-Al2O3-SiO2系微晶玻璃性能影响

以CaO-A l2O3-SiO2为主要原料,采用烧结法制备出微晶玻璃.利用DSC确定了核化温度和晶化温度.利用XRD和SEM研究微晶玻璃的物相组成和显微结构.通过研究热处理温度对微晶玻璃性能的影响,可得出在780℃核化1h、948℃晶化2h时,微晶玻璃的性能最好.     

烧结法制MgO-SiO2-Al2O3-B2O3-KF玻璃陶瓷成分设计优化及显微析晶研究

通过烧结与水淬相结合的方法制备并系统探讨了MgO- SiO2-Al2O3-B2O3-KF玻璃陶瓷的显微析晶.研究表明:MgO-SiO2-Al2O3-B2O3-KF玻璃陶瓷的烧结收缩率与玻璃化及组分的析晶程度相关;析晶程度愈高,烧结坯愈致密;试样中成分配比愈接近云母晶体成分的原子比,玻璃陶瓷的显微析晶程度愈高;在烧结温度为1 000℃时,即开始出现析晶,到1 050℃时,析晶程度达到最高,继续提高烧结温度,显微析晶又发生重熔.     

Effect of nucleating agents on microstructure and mechanical properties of SiO2-Al2O3-ZrO2 glass-ceramics

SiO2-Al2O3-ZrO2 glasses with different nucleating agents were crystallized under special processing schedule. The microstructure and mechanical properties of the glass-ceramics in SiO2-Al2O3-ZrO2 system were investigated by differential scanning calorimetry, scanning electron microscopy, X-ray diffraction and three-point bending method. The results show that ZrO2 is not an effective nucleating agent in SiO2-Al2O3-ZrO2 system, while TiO2 is effective for the separation of spinel, and P2O5 facilitates solubility of ZrO2 in glass and crystallization. The main crystalline phases of the glass-ceramics are spinel, anorthite and tetragonal zirconia. With the increase of ZrO2 content in the glass, glass-ceramics show higher bending strength （120 MPa） than others.     

INFLUENCE OF ZnO AND BaO CONTENTS ON SINTERING AND CRYSTALLIZATION OF GLASSCERAMIC DECORATIVE MATERIALS

In this paper,the influence of ZnO and BaOcontents on sintering and crystallization of decorative materi-al in the system of CaO-Al_2O_3-SiO_2 was studied. The opti-mum ZnO, BaO contents and sintering or crystallization tem-perature for the glass-ceramic were determined.     

氧化铝对微晶玻璃装饰板烧结及晶化影响

研究了Al2O3含量的变化对CaO-Al2O3－SiO2系统微晶玻璃的烧结和析晶的影响规律。结合工业化生产,确定了合适的Al2O3含量范围。     

水热法合成条件对氧化锆晶相影响的光谱研究

以硝酸锆为前驱物,用水热法分别合成了纯单斜相、四方相以及四方和单斜混合相的氧化锆纳米粒子.应用XRD、拉曼光谱和TEM探讨了水热过程中前驱体浓度、晶化温度和晶化时间对ZrO2晶粒尺寸和相变的影响.结果表明,水热制备过程中上述合成条件均影响ZrO2晶粒尺寸,其中晶化温度对其影响最大,但是晶化温度对ZrO2的形貌影响不大.延长晶化时间有利于单斜晶相的形成,而且随着晶化时间延长,ZrO2的晶化程度增加.在水热合成过程中采用较低的前驱体浓度、较高晶化温度及延长晶化时间有利于控制合成单斜相ZrO2.     

琥珀色微晶玻璃装饰板材的研制

研究了着色剂舍量对CaO－Al2O3－SiO2系统微晶玻璃装饰板材颜色的影响。采用样温炉和高温粘度计确定合理的核化温度，晶化温度。并通过X衍射等手段分析其主晶相。     

Effect of heat treatment method on microstructure of tailings glass ceramics

A Cao-Mgo-Al2O3-SiO2 quaternary system was established with the main crystal phase design based on Diopside, and the effect of once-through sintering heat treatment on microstructure of iron railings glass ceramics was studied by using DTA, SEM along with measurement of microhardness and volume density. The experimental results show that, when the total amount of FeO and Fe2O3 exceeds 10wt%, a large number of fine nuclei are produced in the annealing process, and the phenomenon of nucleus resorption happens during the process of nucleation heat treatment, which is unfavorable for preparing iron tailings glass ceramics through once-through sintering method. When the annealing temperature from 1250 ℃ to 830 ℃, setting crystallization time for 4h, without heat treatment, crystals are well grown with arrangement and interlocking in glass phase. At 830 ℃ the crystals are well developed, well distributed and of good size; with crystallization time of 4 h the crystals with radial shape have high content and regular arrangement.     

Structure of Bi2O3-ZnO-B2O3 system low-melting sealing glass

Bi_2O_3-ZnO-B_2O_3 system glass is a kind of lead-free low melting sealing glasses. The structure of Bi_2O_3-ZnO-B_2O_3 system low-melting sealing glass was investigated by DSC, FT-IR, XRD and SEM. The results show that with the increase of B_2O_3 content, the transition temperature Tg and softening temperature T_f of Bi_2O_3-ZnO-B_2O_3 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 [BO_3] pyramidal and [BiO_6] octahedral units and B-O from [BO_3] and [BO_4] units. With the decrease of B_2O_3 content, the crystallization tendency of the glass increases. In glass samples B_1 and B_2, crystallization starts at 460 ℃ and 540 ℃, respectively. Both of them precipitate Bi-(24)B_2O_(39) phases.     

烧结法建筑装饰微晶玻璃冲蚀磨损研究

利用冲蚀磨损实验研究了影响CaO-Al2O3-SiO2系统烧结法微晶玻璃装饰板材冲蚀行为，通过正交实验，讨论了磨粒种类、冲蚀角、冲蚀时间，磨粒粒径等因素对CaO-Al2O3-SiO2系统微晶玻璃的冲蚀性的影响。     

Transformation toughening of Al2O3/ZrO2 laminated ceramics with residual compressive stress

With the help of scanning electronic microscopy and X-ray diffraction, the relationships of microstructure characteristics, phase assemblage, and fracture micrograph of Al2O3/ZrO2 laminated ceramics were studied. Compared with monolithic Al2O3/ZrO2 ceramics, the existence of surface compressive stresses greatly restrained the growth of ZrO2 and Al2O3 grains at high sinter tem- perature, fined the grain size, and increased the content of metastable t-ZrO2, which made the fracture transformation energy quantity 70% higher than that of the monolithic ceramics. The trans-granular and inter-granular fracture features were observed in the surface and center layers, which further verified that transformation toughening is the main mechanism, whereas, micro-crack toughening is helpful for enhancing fracture toughness.     

温度及Y_2O_3对SG法制备ZrO_2相结构及粒度的影响

针对纳米ZrO2粉体粒径较小、比表面积大、极易发生团聚问题,以纳米ZrO2为研究对象,采用溶胶-凝胶(SG)法,以氧氯化锆为锆源,水为溶剂,Y2O3为稳定剂,PEG-6000为分散剂,主要研究烧结温度及Y2O3对制成的纳米ZrO2相结构及其粒度的影响.实验结果表明:经XRD分析,所制得的ZrO2试样主要为四方相结构,随着煅烧温度的升高,粉体粒径增大;SEM测试结果表明,在一定ZrO2陶瓷粉体粒度范围内,随着稳定剂Y2O3加入量的增加,粉体颗粒间的分散性有所改善.综合考虑对纳米ZrO2相结构及粒度的影响,确定最佳烧结温度为650℃,稳定剂Y的最佳加入量为7.5mol%,制备的ZrO2纳米粉体粒径尺度最佳,晶型稳定性好且分散性得到改善.     

MnO2对磷渣微晶玻璃显微结构和性能的影响

烧结法CaO-Al2O3-SiO2微晶玻璃具有结构致密均匀,抗冲击、耐磨、耐腐蚀、无放射性、色泽丰富、纹理美观等特性,是一种新型绿色环保型装饰材料。以磷渣为主要原料,以Fe2O3和MnO2为着色剂,制备了米黄色微晶玻璃。利用X射线衍射和扫描电子显微镜等测试技术,研究了不同MnO2含量对微晶玻璃显微结构、晶相种类的影响,测定了微晶玻璃的化学稳定性。研究结果表明:当MnO2质量含量小于5.5%时,微晶玻璃主晶相为β-硅灰石,随着MnO2含量的增加析晶量减少,晶粒尺寸由0.42μm减小到0.3μm;当MnO2质量分数为6%时,主晶相变为钠长石且析晶量增加、晶体尺寸增大。当MnO2质量分数大于4%时,MnO2质量分数每增加0.5%其摊平温度约降低10℃,适量加入MnO2使其化学稳定性提高。     

烧结法制MgO-SiO_2-Al_2O_3-B_2O_3-KF玻璃陶瓷成分设计优化及显微析晶研究

通过烧结与水淬相结合的方法制备并系统探讨了MgO-SiO2-Al2O3-B2O3-KF玻璃陶瓷的显微析晶.研究表明：MgO-SiO2-Al2O3-B2O3-KF玻璃陶瓷的烧结收缩率与玻璃化及组分的析晶程度相关;析晶程度愈高,烧结坯愈致密;试样中成分配比愈接近云母晶体成分的原子比,玻璃陶瓷的显微析晶程度愈高;在烧结温度为1 000℃时,即开始出现析晶,到1 050℃时,析晶程度达到最高,继续提高烧结温度,显微析晶又发生重熔.     

Crystallization Mechanism of Na2O-CaO-Al2O3-SiO2-F Glass Containing Cr2O3

The effect of Cr2O3 on the nucleation and crystallization of Na2O-CaO-Al2O3-SiO2-F- glass has been investigated by means of ESR(Electron Spin Resonance), SEM(Scanning Electron Microscope), EDS(Energy Dispersive Specrometer) and so on. Computer pattern recognition is applied to optimize the heat-treatment schedules. The experimental results show that the base glass containing more than 1 .5 % (mass fraction) Cr2O3 can be nucleated internally and converted to spheroidal crystal glass materials. The spheroidal crystal consisted of fibrous wollastonite crystals radiating from a center. The residual glass phase filled in the interstices between the fibers and between the spherulites. During heat treatment process, the valence states ofchromium changed from Cr6- to Cr3-, and the Cr-spinel solidsolution [CaCr2O4] precipitated followed this valence change. At the primary stage of crystallization, the Cr-spinel could act as a nucleating center on which the principal or}stalline phase β-CaSiO3 grew epitaxially.     

Effects of nucleating additives on crystallization and properties of CaO-B2O3-SiO2 glass-ceramics

ZrO₂, TiO₂ and P₂O₅ were doped in CaO-B₂O₃-SiO₂ glass-ceramics as nucleating additives. Effects of different nucleating additives on the phase separation and crystalline behaviors were investigated by using gradient temperature furnace, DTA and XRD. Then, sintering process of the glass-ceramics was investigated by testing sintering shrinkage, dielectric constant and loss. The experimental results shows that the glass-ceramics doped with nucleating additives represents higher crystallization, with ZrO₂ as an exceptional effective dopant to promote the precipitation of wollastonite crystal. Finally, ZrO₂ containing glass-ceramics was chosen to study the influence of sintering temperature and soaking time with the help of X-ray diffraction analysis and density measurement. The glass-ceramics can be well consolidated at 850 °C for 10 min, with low dielectric constant (5.87) and loss (3.21 × 10⁻⁴), which is desirable for LTCC application.     

Stress Analysis of CaO-Al2O3-SiO2 System Glass-ceramic with Different Thickness

In order to study the relationship between thickness and residual stress in CaO-Al2O3-SiO2 glass-ceramics.The residual stress was measured in CaO-Al2O3-SiO2 system glass-ceramic with different thickness,and the formation mechanism and characterization of residual stress in CAS system Glass-ceramic were analyzed by the X-ray diffraction analysis.The experimental results show the compressive residual stress increass with thickness of glass-ceramic increasing.     

CaO-Al_2O_3-SiO_2系统微晶玻璃的振动光谱研究

通过红外光谱及拉曼光谱,研究了CaO－Al2O3－SiO2系统微晶玻璃的微观结构．系统分析TCaO、Al2O3、B2O3取代SiO2后成分变化对微晶玻璃结构的影响．从振动光谱研究及理论分析两个角度讨论了Al3 、B3 的配位状态变化,并得到一致结论。