Iranian Journal of Materials Science and Engineering

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The effect of precipitation of ?.qss. and gahnite phases during heat treatment of glass frits in the ZnO-Al2O3-SiO2 system on the mechanical property of resulting glass-ceramic specimens were investigated. It was shown that gahnite glass-ceramics had higher bend strength and toughness values than ?.qss. ones. The results are attributed to the higher modulus of elasticity as well as higher thermal expansion coefficient of gahnite relative to the residual glass phase.

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Abstract: The application of inexpensive materials such as copper, zinc, lead, iron and steel slag in manufacturing of glass and glass-ceramic products in construction industry, lining materials as anti-corrosion and anti-abrasion coatings in metals and etc, has led to considerable progress in glass technology in recent years. The composition of slag glass-ceramics is mainly located in the SiO2-Al2O3-CaO-MgO system, in which one of the most important problems is the lack of bulk crystallization. To resolve the above-mentioned problem, the crystallization behavior of various compositions containing different nucleating agents Cr2O3 , Fe2O3 and TiO2 in the single, double and triple forms were studied by differential thermal analysis (DTA).The precipitated crystalline phases was determined by the X-ray diffractometry and the micro-structural analysis was studies using the SEM micrographs. The three point bending strength, micro-hardness and the chemical resistance of the best composition were determined. According to the results, the resulted glassceramic had a better specification than the stoneware floor tiles and the porcelain one, which are considered as the two important competitors for it.

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Abstract: Lead-containing glass borosilicate was synthesized by Sol-gel technique using metalalkoxids such as tetraethyleorthosilicate (TEOS), Al-sec-butoxide and trimethyl borate. The sol containing TEOS converts to gel during drop wise addition of Al-alkoxide while inorganic lead salt was added in the last stage of gelation to prepare the alcogels. The specimens were dried at room temperature to set then heated at 600°C quickly to avoid crystallization preparing a glass containing 63 wt% lead oxide. The influence of pH on absorption behavior of the sols studied by UV visible technique so the characteristic of the gel, alcogel and xerogel were studied in the different acidic concentrations. The UV spectrums show that the higher the acidity of the hydrolysis stages, the higher the absorbance. The results showed the sample with 63 wt% lead was found fully amorphous. Microstructure and phase analysis of the glass powders were investigated by X-ray diffraction (XRD), X-ray fluorescence (XRF) and scanning electron microscopy (SEM) equipped with EDS analysis.

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Oxynitride glasses are found as grain boundary phases in silicon nitride ceramics. They are effectively alumino-silicate glasses in which nitrogen substitutes for oxygen in the glass network, and this causes increases in glass transition and softening temperatures, viscosities (by two to three orders of magnitude), elastic moduli and microhardness. Calcium silicate-based glasses containing fluorine are known to have useful characteristics as potential bioactive materials. Therefore, the combination of both nitrogen and fluorine additions to these glasses may give useful glasses or glass-ceramics with enhanced mechanical stability for use in biomedical applications. This paper reports glass formation and evaluation of glass thermal properties in the Ca-Si-Al-O-N-F system. Within the previously defined Ca-Si-Al-O-N glass forming region at 20 eq.% N, homogeneous, dense glasses are formed. However, addition of fluorine affects glass formation and the reactivity of glass melts. This can lead to fluorine loss as SiF4, and also nitrogen loss, leading to bubble formation and porous glasses. The compositional limits for both dense
and porous glass formation at 20 eq.% N and 5 eq.% F have been mapped. At high fluorine contents under conditions when Ca-F bonding is favoured, CaF2 crystals precipitate in the glass. The role of the different cations on glass formation in these oxyfluoro-nitride glasses is discussed.

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Abstract: In the present work, effect of the nucleating agent such as TiO2, ZrO2, P2O5, Ye2O3 and CeO2 in single, double, triple and fourth systems on the crystallization behavior of various compositions was studied. Using differential thermal analysis (DTA), the composition of Li2O-Al2O3-SiO2 (LAS) was optimized and the coefficient of thermal expansion (CTE), three point flexural strength, hardness, thermal shock resistance, and chemical resistance of the most favorable composition were evaluated. The crystalline phase was determined by the x-ray diffractometry. Moreover, the micro-structure of the samples was studied by SEM technique. According to the results, -Eucryptites (high quartz solid solution) was the main crystalline phase and the CTE values of the optimized sample were determined as 1.65-1.93 10-6 in the temperature range of 20-500 oC. Furthermore, three point bending strength ranged from 139 to 155 MPa.

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Abstract: In this research work, crystallization kinetics of Fe55Cr18Mo7B16C4 alloy was evaluated by X-ray diffraction, TEM observations and differential scanning calorimetric tests. In practice, crystallization and growth mechanisms were investigated using DSC tests in four different heating rates. Results showed that a two -step crystallization process occurred in the alloy in which - Fe phase was crystallized in the first step after annealing treatments. Activation energy for the first step of crystallization i.e. - Fe was measured to be 276 (kj/mol) according to Kissinger model. Further, avrami exponent calculated from DSC curves was 2 and a three -dimensional diffusion controlled mechanism with decreasing nucleation rate was observed in the alloy. It is also known from the TEM observations that crystalline á – Fe phase nucleated in the structure of the alloy in an average size of 10 nm and completely mottled morphology.

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The effect of Y2O3, CeO2, P2O5, ZrO2 and TiO2 in single, double and triple form on crystallization mechanism of Li2OAl2O3- SiO2(LAS) glass-ceramic system was investigated .The nucleation and crystallization peak temperatures of optimized samples in each group were determined by Ray & Day method .The crystalline phase was determined by the X-ray diffractometery .The micro-structure of the samples was studied by SEM techniqe .Crystallization activation energy ,E, and kinetic constants(n ,m) were determined by differential thermal analysis (DTA) through Marotta and Augis-Bennet methods .According to the results ,the Avrami constants(m ,n) derived from the Marotta and Augis- Bennett, glasses containing both ZrO2 and TiO2 nuclei were showed bulk crystallization .The crystallization mechanism of specimens containing ZrO2, TiO2 and CeO2 in the triple nuclei series represent two-dimensional bulk crystallization .By comparison of Avrami constants and activation energy of crystallization of optimized samples with other results they gave much lower value of E(255.5 kJ/mol) and higher value of n in 4.38.The lattice constants of the main phase( -eucryptite solid solution)in samples were determined according to the XRD results

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Abstract: Glassy samples with xTiO2 .3SiO2 .Na2O composition that (8≤x≤40) (molar) were casted in refractory steel molds after melting at air as parallel palates. After polishing and getting to desire thickness, UV-VIS spectrometry in 200 -1100 nm was measured on samples. Glass density was measured by a sensitive micro balance and was found that by increasing titanium dioxide of glasses, glass density increases. Results from UV-VIS spectroscopy show that increase of titanium dioxide decreases light transmission and this value reaches zero for sample with 40 molar percent of titanium dioxide. One reason of this reduction is formation of crystalline phase in glass, in which, by increasing titanium content crystalline phase will be increased, results of X-ray diffraction and electron microscopy confirm this claim.

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ASTM F-75 Cobalt-base alloy castings are widely used for manufacturing orthopedic implants. This alloy needs both homogenization and solutionizing heat treatment after casting, as well as bioactivation of the surface to increase the ability of tissue bonding. In this study, ASTM F-75 Cobalt-base substrate was heat treated at 1220°C for 1 hour in contact with Hydroxyapatite-Bioglass powder in order to solutionize and homogenize the microstructure and promote surface bioactivation. For bioactivity evaluation, heat treated specimens were immersed in Simulated Body Fluid (SBF). Surface of specimens before and after the immersion was analyzed by Scanning Electron Microscopy (SEM), Energy Dispersive Spectroscopy (EDX) and X-Ray Diffraction (XRD). Results showed an appropriate microstructure with bioactive layer on the surface of specimens after heat treatment. In vitro result and formation of bone-like apatite layer on specimens indicated that heat treated samples were potentially suitable for bone replacement and tissue regeneration under highly loaded conditions.

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Abstract:Some types of glass and glass ceramics have a great potential for making bone tissue engineering scaffolds, drug carrier and bone cements as they can bond to host bone, stimulate bone cells toward osteogenesis, and resorb at the same time as the bone is repaired. Calcium phosphate glass ceramics have very attractive properties that allow them to use in bone tissue engineering. Calcium phosphate glasses could be used for the fabrication of resorbable constructs, with controlled biodegradability. This work was investigated crystallization and sinterability of biodegradable glass ceramics in the CaO–P2O5–Na2O–TiO2 system using differential thermal analysis (DTA), X-ray diffraction (XRD) and scanning electron microscopy (SEM). Sinterability of the glasses also was investigated by measurement of sintering parameters. Different thermal treatments were applied to control the degree of devitrification of glasses. In the developed glass ceramics Ca2P2O7 were the first phase to precipitate in the mother glass structure, followed by Ca(PO3)2 and TiP2O7 at elevated temperature. Ca2P2O7 and Ca(PO3)2 seem to have a very positive effect in bone formation in vivo. It is therefore expected that glass ceramics understudy have good potential to be used for bone regeneration applications

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Crystallization kinetics of Fe52Cr18Mo7B16C4Nb3 alloy was evaluated using X-ray diffraction, differential scanning calorimetric (DSC) tests and TEM observations in this research work. In effect, crystallization and growth mechanisms were investigated using DSC tests in four different heating rates (10, 20, 30, 40 K/min) and kinetic models (i.e. Kissinger- Starink, Ozawa, and Matusita methods). Results showed that a two -step crystallization process occurred in the alloy in which α - Fe and Fe3B phases were crystallized respectively in the structure after heat treatment. Activation energy for the first step of crystallization i.e., α - Fe was measured to be 421 (kj/mol) and 442 (kj/mol) according to both Kissinger- Starink and Ozawa models respectively. Further, Avrami exponent calculated from DSC curves was 1.6 and a two -dimensional diffusion controlled mechanism with decreasing nucleation rate was observed in the alloy. TEM observations reveal that crystalline α – Fe phase nucleated in the structure of the alloy in an average size of 10 nm and completely mottled morphology

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In this study, porous titanium composites containing 5, 10 and 15 wt. % nanobioglass were fabricated by space holder sintering process. The pore morphology and phase constituents of the porous samples were characterized by X-ray diffractometry (XRD) and scanning electron microscopy (SEM). The mechanical properties were determined by compression test. The porosity of the sintered samples showed an upward trend with an increase in bioglass content. As the bioglass content was increased, the compressive strength was first increased and then decreased. The results obtained in this work suggest that the fabricated porous compact with 10 wt. % bioglass with compressive strength value of about 76.7 MPa, high porosity and good biocompatibility has the potential application for bone tissue engineering.

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Crystallization of α – Fe phase during annealing process of Fe55Cr18Mo7B16C4 bulk amorphous alloy has been evaluated by X- ray diffraction, differential scanning calorimetric tests and TEM observations in this research. In effect, crystallization mechanism and activation energy of crystallization were evaluated using DSC tests in four different heating rates (10, 20, 30, 40 K/min). A two -step crystallization process was observed in the alloy in which α–Fe phases was crystallized in the first step after annealing process. Activation energy for the first step of crystallization process (i.e. α – Fe phase) was measured to be 276 (Kj/mole) according to Kissinger kinetic model. Furthermore, Avrami exponent calculated from DSC curves was two and a three -dimensional diffusion controlled mechanism with decreasing nucleation rate was observed in the alloy. It is also known from the TEM observations that crystalline α – Fe phase nucleated in the structure of the alloy in an average size of 10 nm and completely mottled morphology

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In the present study, the feasibility of α-Fe ferromagnetic phase formation in glass and glass-ceramic by reduction in hydrogen atmosphere have been investigated. The glass with the composition of 35Na 2 O–24Fe2O3–20B 2O3 – 20SiO 2 –1ZnO (mol %) was melted and quenched by using a twin roller technique. As quenched glass flakes were heat treated in the range of 400-675 °C for 1-2 h in hydrogen atmosphere, which resulted in reduction of iron cations to α-Fe and FeO. The reduction of iron cations in glass was not completely occurred. Saturation magnetization of these samples was 8-37 emu g -1 . For the formation of glass ceramic, As quenched glass flakes heat treated at 590 °C for 1 h. Heat treatment of glass ceramic containing magnetite at 675°C in hydrogen atmosphere for 1 h led to reduction of almost all of the iron cations to α-Fe. Saturation magnetization of this sample increased from 19.8 emu g -1 for glass ceramic to 67 emu g -1

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Porous hollow glass microspheres have many uses, including encapsulation of active materials. In this paper a fast and facile method for fabricating porous hollow glass-microspheres was demonstrated by etching them using dilute hydrofluoric acid. Then, a highly reactive amine was infiltrated into the etched glass microspheres. Scanning electron microscopy was conducted for the hollow glass microspheres prior and post etching process. With regards to the porous hollow glass spherical sample, the spherical nature, morphology, pore diameter and the porosity were studied using scanning electron microscopy. Formation of the intact hollow glass microspheres with an open through wall porosities following phase separation and etching of the boron oxide rich phase was demonstrated using reciprocating shaker as the most suitable agitation method. The BET results indicated that the surface of the porous microspheres contained nano-pores. It is believed that the simplicity of the reported fabrication technique of micro/nano porous structure has the potential to scaling up for large scale production

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In this study, the crystallization behavior of a 65GeO₂-15PbO-10MgF₂-10MgO glass (prepared by the conventional melt quenching technique) has been investigated. The microstructure and crystallization behaviors of this glass were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), non-isothermal differential thermal analysis (DTA) and Fourier transform infrared spectroscopy (FTIR). The results demonstrated that a fully glassy phase can successfully be prepared by the conventional melt quenching technique exhibiting one-stage crystallization on heating, i.e., the glassy phase transforms into crystalline MgGeO₃ and Pb₅GeO₇ phases. The activation energy for the crystallization, evaluated from the Kissinger equation, was approximately 202±5 kJ/mole using the peak temperature of the exothermic reaction. The Avrami exponent or reaction order, n, indicates the nucleation rate in this glass to increase with time and the crystallization to be governed by a three-dimensional interface-controlled growth.

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The construction sector is responsible for relevant environmental impacts and one of its most crucial points is the use of concrete. Geopolymers represent the most promising green and ecological alternative for common Portland cement and cementitious materials, due to its proven durability, mechanical and thermal properties. This work presents an experimental and comparative study of adhesion at the fiber-matrix interface between glass fibers and carbon fibers added to the geopolymer matrix. This analysis was performed by pull-out test, whereby it was found that the greatest efficiency was obtained by reinforcing with the glass fibers, incorporated at 2 mm in the geopolymer matrix. As results, the adhesion between the fibers and the geopolymer structure can be assessed, as well as the optimum length of application.

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Strong glass-ceramic foams with a compressive strength of 20 MPa were prepared by adding various amounts of Fe₂O₃ to a soda lime-based glass composition, and SiC as a foaming agent. The foams were prepared by firing the compacted samples in the range of 750–950°C for different soaking times. The crystallization behavior of the samples was investigated by Simultaneous Thermal Analysis (STA), Scanning Electron Microscope, and X-Ray Diffractometer (XRD). Based on the results, solid solutions of pyroxene groups were crystallized by the surface mechanism, between 730˚C and 900˚C during the firing of the specimens, and their amounts increases with increasing of the added iron oxide. Besides, we found that Fe₂O₃ neither acts as a nucleant for pyroxene nor as an oxidizer for SiC. The results also showed that the compressive strength as well as the crystallization behavior of the foams was influenced by the presence of the SiC particles.

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  As an alternative to conventional fertilizers, e.g. NPK (the Nitrogen-Phosphorous-Potassium containing chemical fertilizers) which release their nutrients in a short period of time, due to high solubility in irrigation water, glass fertilizers are ideal as they release macro- and micronutrients for crops and plant nourishment. Also, despite conventional ones, they have no ground-water pollution. In the present study, glass fertilizers were synthesized via Polymer-Derived Ceramics (PDC) method. Despite the melt-casting procedure, PDC needs lower temperatures in heat treatment. The precursors consist of poly-siloxane and active fillers. Thus, thanks to gaseous release during heat treatment of the present active fillers, i.e. Ca(OH)₂, MgCO₃, and Al(OH)₃, a porous microstructure can be generated. In order to manipulate the pore size and specific surface area, fractions of active fillers were used as calcined. The experiments showed that upon increase of non-calcined active fillers, the specific surface area and the amount of porosity was increased due to more gaseous release during heat treatment. Thus, affected by microstructure, the release rate of macro and micro-elements was higher in the sample containing non-calcined active fillers, in comparison to other samples. Additionally, the porous samples were able to be loaded by extra nutrients containing Nitrogen, like KNO₃.