Iranian Journal of Materials Science and Engineering

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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.

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The control of silicone rubber’s viscoelastic properties namely loss factor, storage and loss moduli during crosslinking are crucial as its malleable behaviour changes differently under different conditions and affecting the final product. Hence, it becomes the objective of this study to investigate the rheological behaviour of silicone rubber cured under different formulation ratios with platinum catalysts and triethylamine, methanol & ethanolamine solvent. Measurement was conducted for the silicone rubber to crosslinker ratios of 2.5:7.5, 5:5, 7.5:2.5 and 10:1 at different elevated temperatures, and for the silicone rubber with triethylamine, methanol and ethanolamine at different angular frequencies. While the crossover of storage and modulus curve which signifies a gel point was not observed at higher ratios of platinum used across the temperature range of 25 – 100°C, it was found at 89°C and 95°C with the formulation ratios of 10:1 and 7.5:2.5, respectively. On the other hand, the crossover point was observed for silicone rubber at 100 s^-1 for triethylamine, 3 s^-1 and 100 s^-1 for methanol, and 70 s^-1 alongside 290 s^-1 for ethanolamine. The presence of gel point indicates that crosslinking of silicone rubber successfully took place and this study proves that controlling the crosslinking behaviour was possible.

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Biocompatible ceramics, commonly known as “bioceramics”, are an extremely versatile class of materials with a wide range of applications in modern medicine. Given the inorganic nature and physico-mechanical properties of most bioceramics, which are relatively close to the mineral phase of bone, orthopedics and dentistry are the preferred areas of usage for such biomaterials. Another clinical field where bioceramics play an important role is oculo-orbital surgery, a highly cross- and interdisciplinary medical specialty addressing to the management of injured eye orbit, with particular focus on the repair of orbital bone fractures and/or the placement of orbital implants following removal of a diseased eye. In the latter case, orbital implants are not intended for bone repair but, being placed inside the ocular cavity, have to be biointegrated in soft ocular tissues. This article reviews the state of the art of currently-used bioceramics in orbital surgery, highlighting the current limitations and the promises for the future in this field.

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The optimization of biomaterials biodegradation rate similar to tissue regeneration, is one of the main
goals in the field of tissue engineering. However, the necessity to assess their possible toxicity is always considered.
The aim of this study was cytotoxicity and genotoxicity evaluation of fluorapatite/bioactive glass (FA/BG)
nanocomposite foams with two various weight ratios to determine the optimal composition. Nanocomposite foams
were made by gel-casting method with FA and BG as precursors in two weight ratios (A and B). Nanocomposite
foam extracts (CFEX) were prepared by shaking 100 mg/mL of each foam in a complete culture medium for 72 h in
a shaker incubator at 120 rpm/37ºC. Saos-II cells were exposed to different concentrations of CFEXs for 24 and
48 h and then cytotoxicity and genotoxicity were evaluated by MTT and comet assay, respectively. Based on the MTT
assay results after 24 h exposure, CFEX A at concentrations ≥75% and CFEX B at concentrations ≥50% had a
cytotoxic effect, while after 48 h, both CFEXs showed similar cytotoxicity at concentrations ≥25%. According to the
result of the comet assay, DNA damage increased with the increase of CFEXs concentration and exposure time.
Both CFEXs showed significantly higher comet tails elongation scores at concentrations ≥50% and ≥25% after 24
and 48 h exposure, respectively. Both composite foams could be considered as a non-toxic candidate for tissue
engineering at concentrations <25% which was less than FA50%/BG50% composite. Therefore, the composite with
equal FA/BG proportion has priority if similar results are obtained in in vivo complementary experiments.

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Temperature is one of the key factor that affecting the electrical, physical, structural, and morphological properties as well as the crystallinity of the nanomaterials. The current study investigates the effect of annealing temperature on the structural and electrical properties of lanthanum oxide (La2O3) thick films. La2O3 thick films were prepared on a glass substrate using a conventional screen printing technique. In this work, T1 is an unannealed prepared film, whereas T2 and T3 are annealed in a muffle furnace for 3 hours at 350°C and 450°C, respectively. XRD technique was exploited to investigate the crystallization behavior of the films. It was found that the crystal structure of La2O3 thick films are pure hexagonal phase. The annealing temperatures were revealed to have influence on the crystallite sizes of the films. SEM and EDS was used to study the morphology and elemental analysis of the films respectively. The electrical properties of the films were explored by measuring resistivity, temperature coefficient of resistivity (TCR), and activation energy at lower and higher temperatures regions. The film annealed at 450°C has high resistivity, a high TCR, and small crystallite size. The thickness of the La2O3 thick films was also found to decrease as the annealing temperature increased.

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Abstract
The effect of different heat-treatment temperatures on the magnetic, crystallization, and structural properties of 20SiO2.50FeO.30CaO (mol%) glass ceramics was studied. The initial glass was synthesized by the sol-gel method at 25℃  with a precursors to solvent ratio of 1/5. After aging the resulted gel for 24 h at room temperature, it was dried in an electric dryer at 110 ℃ . By heat treatment at different temperatures, different phases such as magnetite, maghemite, and hematite were crystallized in the glass. The maximum stability temperature of magnetite and maghemite were 360℃  and 440℃  respectively. By increasing the heat treatment temperature to higher than 440℃ , the oxidation of maghemite to hematite was occureds. The highest magnetization amount (1.9 emu/g) belonged to sample heat treated at 680℃ . By increasing the heat treatment temperature to 840℃ , the magnetization decreased to 0.8 emu/g, due to the oxidation of maghemite. By increasing the heat treatment temperature from 440℃  to 680℃ , crystalline size of maghemite was increased from 40 to 200 nm. By forther increment of temperature to 840℃ , the size of maghemite crystals decreased to 17nm, due to the oxidation of maghemite to hematite.
Abstract
The effect of different heat-treatment temperatures on the magnetic, crystallization, and structural properties of 20SiO2.50FeO.30CaO (mol%) glass ceramics was studied. The initial glass was synthesized by the sol-gel method at 25℃  with a precursors to solvent ratio of 1/5. After aging the resulted gel for 24 h at room temperature, it was dried in an electric dryer at 110 ℃ . By heat treatment at different temperatures, different phases such as magnetite, maghemite, and hematite were crystallized in the glass. The maximum stability temperature of magnetite and maghemite were 360℃  and 440℃  respectively. By increasing the heat treatment temperature to higher than 440℃ , the oxidation of maghemite to hematite was occureds. The highest magnetization amount (1.9 emu/g) belonged to sample heat treated at 680℃ . By increasing the heat treatment temperature to 840℃ , the magnetization decreased to 0.8 emu/g, due to the oxidation of maghemite. By increasing the heat treatment temperature from 440℃  to 680℃ , crystalline size of maghemite was increased from 40 to 200 nm. By forther increment of temperature to 840℃ , the size of maghemite crystals decreased to 17nm, due to the oxidation of maghemite to hematite.
 

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Glasses in the B₂O₃-Li₂ (O, Cl₂, I₂) system were prepared through the conventional melt-quenching method. Then, the conductivity of the molten and glassy states of these compositions was evaluated. Furthermore, the thermal and crystallization behavior of the glasses was determined using simultaneous thermal analysis (STA) and X-ray diffractometry (XRD). The electrical conductivity of the melts was measured at temperatures ranging from 863 to 973 K, and the activation energy of the samples was calculated using the data obtained from ion conduction in the molten state and found to be in the vicinity of 32 kcal/mol. In glassy states, electrical conductivity was also measured. To determine this property, the electrochemical impedance spectroscopy method (EIS) was used. In the molten state, temperature played an important role in the ion conductivity; however, at lower temperatures, other factors became important. Based on the results, the addition of LiI and LiCl to the B₂O₃-Li₂O base glass system (75 B₂O₃, 10 Li₂O, 7.5 LiI, 7.5 LiCl) (mol%) increases the ionic conductivity of the glass from 3.2 10^-8 S.cm^-1 to 1.4 10^-7 S.cm^-1 at 300 K.
 

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This study explores the fabrication, structural analysis, and cytocompatibility of cobalt-doped bioactive glass scaffolds for potential applications in bone tissue engineering. A specific glass composition modified from Hench's original formulation was melted, quenched, and ground to an average particle size of 10 μm. The resulting amorphous powder underwent controlled sintering to form green bodies and was extensively characterized using simultaneous differential thermal analysis (DTA), Raman spectroscopy, and Fourier Transform Infrared analysis (FTIR). After mixing with a resin and a dispersant, the composite was used in digital light processing (DLP) 3D printing to construct scaffolds with interconnected macropores. Thermal post-treatment of 3D printed scaffolds, including debinding (Removing the binder that used for shaping) and sintering, was optimized based on thermogravimetric analysis (TG) and the microstructure was examined using FE-SEM and XRD. In vitro bioactivity was assessed by immersion in simulated body fluid (SBF), while cytocompatibility with MC3T3 cells was evaluated through SEM following a series of ethanol dehydrations. The study validates the fabrication of bioactive glass scaffolds with recognized structural and morphological properties, establishing the effects of cobalt doping on glass behavior and its implications for tissue engineering scaffolds. Results show, Low cobalt levels modify the glass network and reduce its Tg to 529 ^oC, while higher concentrations enhance the structure in point of its connectivity. XRD results shows all prepared glasses are amorphous nature, and DTA suggests a concentration-dependent Tg relationship. Spectroscopy indicates potential Si-O-Co bonding and effects on SiO2 polymerization. Cobalt's nucleating role promotes crystalline phases, enhancing bioactivity seen in rapid CHA layer formation in SBF, advancing the prospects for bone tissue engineering materials.