Effect of ZnO content on the physical,mechanical and chemical properties of glass-ceramics in the CaO–SiO2–Al2O3 system

The objective of this study was to evaluate the effect of ZnO content on the physical, mechanical and chemical properties of CaO–Al₂O₃–SiO₂ (CAS) glass-ceramics produced from Colombian wastes, such as fly ash, granulated blast furnace slag and glass cullet. The CaO/SiO₂ molar ratio of the mixtures was held constant (0.36). ZnO was added to the mixtures in proportions of 4, 7 and 10 wt%. The glass-ceramics were produced by the controlled crystallization of a parent glass. The values of crystallization temperature (T_p) show a fall up to 7 wt% and then shoots up with 10 wt% concentration of ZnO, but in general, ZnO addition lowers the temperature required for the formation of crystalline phases. In general, anorthite (CaAl₂Si₂O₈) is the main phase observed in all heat treated samples, in addition to albite (Na(AlSi₃O₈)) and labradorite (Na_0.45 Ca_0.55 Al_1.55 Si_2.45 O₈). The crystalline phases hardystonite (Ca₂ZnSi₂O₇) and willemite (Zn₂SiO₄) were also identified in the samples with 7 and 10 wt% ZnO. The densities of the glass-ceramics were between 2658 and 2848 kg/m³, and it was found that ZnO helps to increase the density of glass-ceramics. The elastic modulus was in the 100–105 GPa range, the fracture toughness was between 0.45 and 0.64 MPa m^1/2, and the Vickers microhardness was between 632 and 653 MPa. With regards to the durability, the weight loss of the glass-ceramics immersed in alkaline solution (NaOH) did not exceed 1.5 wt% after immersion for 6 h at 80 °C. The results of this study confirm that the vitrification process is a favorable option to utilize these industrial wastes.     

The effect of lithium fluoride on the thermal stability and thermoluminescence properties of borosilicate glass and glass-ceramics

The oxyfluoride glass and glass-ceramics from the LiF-B₂O₃-SiO₂ system are developed. The stable glass can be produced in the range of 20–40 mol% LiF. The effect of LiF admixture on the thermal stability of the glass as well as the thermoluminescence (TL) properties such as glow curves shape is studied. The results show that the increase of lithium fluoride content in the borosilicate glass causes efficiency enhancement of the thermoluminescence signal. We have clearly stated that the process of controlled crystallization of the oxyfluoride glasses can lead again to increased intensity of the TL process. The glass-ceramics with 40 mol% LiF reveals similar level of TL signal to commercially used doped LiF material and can be considered as active material for alpha and beta radiation detectors.     

Strengthening and toughening of a multi-component lithium disilicate glass-ceramic by ion-exchange

A multi-component lithium disilicate (LD) glass-ceramic with interlocking microstructure consisting of rod-like LD crystals and glassy matrix was ion-exchanged over wide temperature and time ranges in pure NaNO₃ or mixed NaNO₃ and KNO₃ baths below the glass transition temperature. Treatment temperature, time and salt bath dependences of surface characteristics and mechanical properties for the ion-exchanged glass-ceramic were investigated. It was found that the glass-ceramic with limited glassy matrix could be remarkably strengthened and toughened in NaNO₃ bath by adjusting the treatment temperature to a moderate level, at which Li⁺/Na⁺ exchange between the glassy matrix and the salt bath could form an ion-exchanged layer with larger depth and less stress relaxation. Furthermore, by using the mixed salt bath, the undesirable exchange of K⁺/Na⁺ in pure NaNO₃ bath could be limited; further enhanced strengthening effect was achieved. The results might renew the interest on strengthening LD glass-ceramics by traditional ion-exchange process.     

电解锰渣制备微晶玻璃正交实验研究

将煅烧后的电解锰渣作为单一的实验原料,采用烧结法,制备微晶玻璃,通过正交实验对锰渣微晶玻璃的热处理方案及性能进行探讨。实验通过DSC、XRD、SEM等方法对样品的性能进行表征,并测试了样品的体积密度、抗弯强度等性能。结果显示:不同的热处理条件下的锰渣微晶玻璃的主晶相均为透辉石(含铁),次晶相为普通辉石相。在800℃/0.5 h+980℃/1 h的热处理条件下得到的锰渣微晶玻璃的综合性能最优,其抗弯强度为106.82 MPa;体积密度为2.68 g/cm^3;维氏硬度为4.43 GPa;耐酸度为0.71%;耐碱度为0.07%。此外,锰渣微晶玻璃用作建筑材料,有非常大的应用潜力。     

烧结法制备微晶玻璃材料

微晶玻璃是由玻璃原位析晶而获得的一种结构均匀，致密，晶粒尺寸为纳米或亚微米级的新型陶瓷复合材料。本文介绍了烧结法制备徽晶玻璃复合材料的特征、工艺原理、微观结构、性能及应用。     

Torsional shear strength behavior of advanced glass-ceramic sealants for SOFC/SOEC applications

Since reliable long term operation of SOFC and SOEC devices depends critically on the mechanical behavior of the sealant material, the current work focuses on the characterization of the shear strength by a torsion test of two different glass-ceramic sealants that are used to join Crofer22APU substrates in an application relevant configuration. The two glass-ceramic sealants differ in terms of characteristic temperatures and crystalline phases with possible impications on the joining behavior. Statistically identical shear stress values were measured at room temperature for joined hourglasses of different size with both sealants, thus confirming a size independence of the measured strength values. Experimental post-test examination results confirm that the interfaces play a strong role regarding the measured shear strength and provide important insights with respect to integration of metallic and glass-ceramic components in SOFC/SOEC stacks.     

Crystallisation behaviour of the iron oxide-devoid BOF slag with adding SiO2

The current research attempted to investigate the crystallisation mechanism of iron oxide-devoid basic oxygen furnace (BOF) slag with adding SiO₂. First, the glass sample was prepared by adding 29?wt-% of SiO₂ to BOF slag, followed by eliminating iron oxide by reduction process. Non-isothermal DSC analysis together with confocal laser microscopy, XRD and EPMA mappings were carried out to observe the crystallisation process. The glass sample showed that the crystallisation process started from the surface where the main phases were identified to be akermanite, merwinite and wollastonite. In addition, the crystallisation process was affected by the nucleation temperature which was decided by the heating rate because of the difference in the nucleation rate between wollastonite and Mg-rich phases. The current results could be used to propose the feasibility of utilising BOF slag as glass-ceramics by chemical modification with heat treatment, which controls the crystallisation behaviour.     

Study of glasses/glass-ceramics in the SrO-ZnO-SiO2 system as high temperature sealant for SOFC applications

Glasses having composition (in wt.%) 51SrO-9ZnO-(40−x)SiO₂ (SZS), where x represents the additives like B₂O₃, Al₂O₃, V₂O₅, and Cr₂O₃, were prepared by melt-quench method and transformed into glass-ceramics by controlled crystallization based on differential thermal analysis (DTA) data. Glasses and glass-ceramics were characterized using dilatometry, X-ray diffraction (XRD), microhardness, and Raman spectroscopy. XRD revealed that glass-ceramics are composed of mainly Sr₂ZnSi₂O₇ and SrSiO₃ crystalline phases along with residual glassy phase. Raman spectroscopy showed that main constitutes of the glass network are the Q¹ and Q² silicate structural units. With the addition of B₂O₃ and other additives silicate glass network depolymerizes and concentration of Q¹ structural units increases at the expense of Q² units. Formation of phases during crystallization depends on the presence of different silicate structural units in the glass matrix. B₂O₃ goes into the glass network as triangular (BO₃) borate structural units and at higher concentration of B₂O₃, only a part of the B₂O₃ forms tetragonal (BO₄) structural units. Investigated glasses and glass-ceramics have thermal expansion coefficient (TEC) in the range of 105-120 × 10⁻⁷/°C which matches with TEC of other cell components. B₂O₃ containing SZS glasses show good adhesion/bonding with YSZ and Crofer 22 APU. Elemental line scans indicate that interdiffusion of Fe, Cr and Si across interface is responsible for good bonding with Crofer 22 APU and interdiffusion of Sr, Si, Y and Zr is responsible for good bonding with YSZ.     

利用硫铁矿尾矿制备微晶玻璃

以硫铁矿尾矿制备微晶玻璃,并用DTA、XRD、SEM等手段分析了微晶玻璃的相变、相组成及微观结构。结果表明,利用硫铁矿尾矿为主要原料,添加适量的其他原料,可获得主晶相为透辉石相的微晶玻璃。     

Crystallization and infrared radiation properties of iron ion doped cordierite glass-ceramics

Heterogeneous ion solution is an important method to improve the wanted property of polycrystalline materials. In this paper, for the purpose of infrared radiation property modification, different contents Fe₂O₃ were doped in MgO-Al₂O₃-SiO₂ system glasses. The effects of Fe₂O₃ doping on nucleation mechanism, crystallization behaviors and especially infrared radiation properties of this cordierite-crystalline based glass-ceramics were systematically investigated by means of differential thermal analysis (DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS). The results show that, the doping of iron ion can promote the phase separation of this magnesium aluminosilicate glass, and therefore change the crystallization mechanism of this glass from surface crystallization to bulk crystallization. The iron ion incorporates into the crystal structure of cordierite by mean of substituting Mg²⁺ in M site. The substitution of Fe³⁺ to Mg²⁺ can form the vacant site of Mg²⁺ cations. For the effects of lattice distortion, impurity and vacancy defects which caused by the incorporation of iron ion, the infrared radiation performance of cordierite based glass-ceramics can be improved effectively.