Preparation and Crystallization of Magnetic Glass-Ceramics from the Residues after Sulfur Release and Iron Recovery from Copper Ore Tailings with Varied CaO Content

To comprehensively reuse copper ore tailings (COT), the fabrication of glass-ceramics by the direct sintering method was investigated, where the residues after sulfur release and iron recovery from copper ore tailings were used as raw materials. The effect of the CaO added on the fabrication of glass-ceramics was emphasized. After analysis of chemical composition and thermodynamics, crystallization kinetics were analyzed by Differential Scanning Calorimetry (DSC) and fitted to the Kissinger equation. The crystal phase and microstructure of sintered glass-ceramics heated between 1080 °C and 1100 °C were estimated by X-Ray diffraction analysis (XRD) and Scanning Electron Microscopy (SEM), respectively. Furthermore, the effects of the addition of CaO on the properties of the sintered glass-ceramics have been discussed. The results showed that the magnetic glass-ceramics were sintered by the residues successfully, the color of which was lighter than that of glass-ceramics sintered by raw materials before iron recovery. According to the XRD analysis, hedenbergite, wollastonite and sekaninaite were formed with traces of maghemite and quartz. In terms of crystallization kinetics and sintering results, a decrease in the activation energies of crystallization and in sintering temperature were observed for an increase in the addition of CaO of up to 10 wt.%. Moreover, the properties of the sintered glass-ceramics, including bulk density, linear shrinkage and flexural strength, were enhanced, while water absorption and true density were reduced with the increase of the amount of CaO added.     

Calculation of viscosity–temperature curves for glass obtained from four wastewater treatment plants in Egypt

This article establishes the relationship between the chemical composition, temperature and viscosity of glasses obtained from the four sludge treatment plants of urban and industrial wastewater from the Nile Delta in Egypt. In order to determine the working conditions of these glasses and their growth temperature, different techniques have been used: differential thermal analysis, hot stage microscopy and dilatometry. We used a prototype of hot stage microscopy, with the help of an image analysis programme developed in the present study. The chemical composition of major oxides sludge ranging from: SiO₂ (36–48 wt%), Al₂O₃ (9–16 wt%), CaO (5–25 wt%), P₂O₅ (1.5–11 wt%), and Fe₂O₃ (~9 wt%), this composition is close to a basalt rock, being necessary to incorporate some raw materials to adjust it to the basalt rock that has a good viscosity-temperature curve. The glass transition temperatures of the four glasses obtained vary between 650 and 725 °C and the growth occurs between 938 and 1,033 °C. We also obtained the viscosity–temperature curves with the aid of the hot stage microscopy that has allowed us to determine the working temperatures of the four glasses, ranging from 926 to 1,419 °C, depending on the type of forming process used.     

Hydrothermal solidification of municipal solid waste incineration fly ash

Hydrothermal solidification of municipal solid waste incineration (MSWI) fly ash has been conducted under saturated steam pressure at 200 °C for up to 48 h with quartz addition. To enhance the strength of solidified specimens further, the raw fly ash was pre-treated by water-washing and mixed with NaOH solution (2 M) as reaction solvent. Experimental results showed that curing time and temperature had significant effects on strength development. Strength development was found to be mainly due to tobermorite formation, and addition of quartz and NaOH solution promoted tobermorite formation. The raw fly ash could also be used as an additive to solidify MSWI bottom ash, and with raw fly ash addition (10%) the flexural strength of solidified specimens reached more than 21 MPa, suggesting high potential to recycle 100% MSWI ash (e.g. as 10% fly ash + 90% bottom ash). Leaching tests were conducted to determine amounts of heavy metals dissolved from solidified specimens. The results showed that under the hydrothermal conditions of this study, leaching of heavy metals was very low. As such, the hydrothermal processing method might have high potential for recycling/reusing MSWI fly ash on a large scale.     

Room-temperature curing epoxies and their elevated-temperature properties

Low-temperature curing epoxy formulations for elevated-temperature service were developed and characterized for adhesive repair and composite matrix. Balanced lap-shear and peel strengths for adhesive applications and flexural and interlaminar shear strengths for composites were obtained when a blend of tetra-functional and tri-functional epoxies was used. For low-temperature curing triethylenetetraamine (TETA) was proven to be effective combined with an amine terminated elastomer. The latter component served also as a toughener. Lower-functional epoxies and curing agents resulted in a peel strength increase and a simultaneous decrease in shear strength. Furthermore, the incorporation of the lower-functional constituents or silanes, resulted in development of a three-phase morphology compared to a conventional two-phase elastomer-epoxy morphology. Thermal analysis carried out by Differential Scanning Calorimetry (DSC) and Dielectric Loss Factor (DLF) indicated that the reduced temperature-curing formulations have relatively low activation energy and that the main cross-linking reaction takes place close to 50°C and is completed at 120°C with a maximum glass transition temperature at 180°C. Mechanical properties of the adhesive formulation were comparable or better than existing commercial products. Flexural and interlaminar shear strengths, for glass-epoxy composites incorporating a selected low-curing-temperature formulation, exhibited enhanced properties compared to commercially 120°C epoxy-glass prepreg composites.     

High temperature properties of MDF composite based on calcium aluminate cement and polyvinyl alcohol

The macro-defect-free composites belong to the well-known group of promising materials consisting of inorganic binder and organic polymer. MDF composites exhibit unusual mechanical properties, especially the flexural strength that can reach over 200 MPa. Moreover, the MDF composites based on calcium aluminate cement have a good temperature resistance because of the Al₂O₃ content in the cement. This paper deals with the preparation and high temperature characterization of MDF composite based on calcium aluminate cement combined with polyvinyl alcohol that could enable its utilization as a refractory material in industrial kilns. The composition of the MDF mixture has been optimized for an easy high-shear processing and flexural strength of the resulting 7-days cured material has been studied under laboratory condition and after heating at 240, 300, 600, 1,000, and 1,500 °C. The structure changes during the heating have been observed by SEM and the course of processes during the heating has been investigated by TG–DTA–EGA, TMA and heating microscopy.     

Oligomeric bisphenol A‐based PEEK‐like phthalonitrile‐cure and polymer properties

The cure behavior and properties of oligomeric bisphenol A‐based PEEK‐like phthalonitrile (PN) are thoroughly examined in this article. The resin is easily processed from the melt at a relatively low temperature (150–200 °C) and the monomer cure occurs in a controlled manner as a function of the amine content and processing thermal conditions. Dynamic mechanical measurements and thermogravimetric analysis show that the polymer properties improve as the maximum PN postcure temperature is increased to 415 °C. The effects of the amine and polymer postcure conditions on the flexural and tensile properties of the PN polymer are investigated. The mechanical properties of the polymer are maximized after postcuring to moderate temperatures (330–350 °C). The polymer exhibits an average flexural strength and tensile strength at break of 117 and 71 MPa, respectively. After oxidative aging at 302 °C for 100 h, the polymer retains excellent mechanical properties. The average flexural and tensile strength retention of the polymers are 81 and 75%, respectively. Microscale calorimetric measurements reveal that the flammability parameters of the oligomeric PN are low compared to other thermosets. © 2016 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2016 , 54, 3769–3777     

Thermogravimetry of ternary cement blends

This study reports the microstructure characteristic and compressive strength of multi-blended cement under different curing methods. Fly ash, ground bottom ash, and undensified silica fume were used to replace part of cement at 50 % by mass. Mortar and paste specimens were cured in air at ambient temperature, water at 25, 40, and 60 °C and sealed with plastic sheeting for 28 days. In addition, these specimens were cured in an autoclave for 6, 9, and 12 h. Results indicated that the compressive strength of multi-blended mixes containing silica fume 10 % by mass cured with plastic sealed and cured in water at 25 and 40 °C was similar to or higher than the corresponding Portland cement control at 28 day. Moreover, the mixes containing silica fume 10 % by mass cured in water at 60 °C had higher compressive strength than Portland cement control. X-ray diffraction and thermogravimetry results confirmed that there was increased pozzolanic reaction with increasing silica fume content which relates to the increasing in strength. For autoclaved curing, the compressive strength of multi-blended cement specimens with silica fume (total of 50 % replacement) was noticeably higher than control Portland cement mix and was highest when autoclaving time was 9 h. X-ray diffraction results showed the pattern of 0.9, 1.1, and 1.4 nm tobermorite crystalline phases as the main product of this curing. Thermogravimetry results showed dehydration of 1.4 nm tobermorite and 1.1 nm tobermorite at about 80–90 and 135–150 °C, respectively. Tobermorite (also shown by scanning electron microscope) thereby as a result lead to significant compressive strength improvement in the short time of autoclaved curing.     

Synthesis and hydrogen absorption kinetics of V4Cr4Ti alloy

V₄Cr₄Ti alloy is synthesized by aluminothermy process followed by electron beam refining. Hydrogen absorption characteristics of the alloy have been evaluated by measuring the pressure composition isotherm (PCIT) at 57 °C temperature. Two plateau pressures are observed in the PCIT curve. Substantial decrease in the hydrogen absorption capacity of the alloy as compared to vanadium has been recorded. Hydrogen absorption kinetics of the alloy was investigated in the temperature range of 200–500 °C. Three-dimensional diffusion appears to be the rate controlling step of the hydrogen absorption. The apparent activation energy was calculated as 0.16 eV/atom-hydrogen.     

Effect of additives on the performance of Dyckerhoff cement,Class G,submitted to simulated hydrothermal curing

Stability of Dyckerhoff cement Class G partially substituted (15 mass%) by metakaolin (MK), silica fume (SF) and ground granulated blast-furnace slag (BFS) was investigated after 7 days of curing under standard and two different autoclaving conditions. Mercury intrusion porosimetry, X-ray diffraction analysis and combined thermogravimetric–differential scanning calorimetry were used to evaluate pore structure development, compressive strength and their dependence on the type of additives in relation to the particular phase composition. Hydrothermal curing led to the formation of α-C₂SH and jaffeite, mostly in the case of referential samples and compositions with addition of slowly reacting BFS. Whilst modest hydrothermal curing (0.6 MPa, 165 °C) favoured formation of α-C₂SH, larger amounts of jaffeite were determined after curing at the highest used pressure and temperature (2.0 MPa, 220 °C). Undesired transformation of primary hydration products was prevented especially by addition of highly reactive and very fine SF. Particular composition attained the best pore structure characteristics and compressive strength after curing at 0.6 MPa and 165 °C. Formation of more stable phases with C/S ratio close to 1 was proved by wollastonite formation during DSC analyses. More severe conditions of curing, however, led to the significant deterioration of microstructure and strength of corresponding sample, probably due to the formation of trabzonite, killalaite and zoisite. Considering the values of hydraulic permeability coefficient and compressive strength, replacement of cement by MK improved significantly the properties of cement when compared with the referential as well as with other blended compositions under the mentioned curing conditions.     

Effects of nucleating agent 1,3,5-benzenetricarboxylic acid tris(cyclohexylamide) on properties and crystallization behaviors of isotactic polypropylene

Amide derivatives of 1,3,5-benzenetricarboxylic acid are a type of novel nucleating agents for isotactic polypropylene (iPP). Effects of nucleating agent 1,3,5-benzenetricarboxylic acid tris(cyclohexylamide) (BTCA-TCHA) on properties and crystallization behaviors of iPP were investigated and the results were compared with those of iPP nucleated with a highly effective commercial nucleating agent Millad 3988. The results showed that BTCA-TCHA was highly effective and it improved greatly the mechanical and optical properties of iPP and increased crystallization peak temperature of iPP obviously. When the addition concentration of BTCA-TCHA was 0.2 wt.%, tensile strength and flexural modulus of iPP were increased by 9.7 and 12.4 %, respectively, and the haze value of iPP was decreased by 53.5 %. When the cooling rate was 20 °C/min, the crystallization peak temperature of iPP was increased from 114.6 °C of virgin iPP to 126.8 °C. In addition, it was found that the nucleation efficiency of BTCA-TCHA was comparable for that of Millad 3988.     

Synthesis and thermal properties of parent and modified DMN–<Emphasis Type="Italic">co</Emphasis>-GMA copolymers

The crystal structure, the unit cell parameters and the extent of mullitization were determined, using the Rietveld method, for range of mullite matrix formulations in which kyanite is used as particles reinforcement. The results combined with the mechanical properties and microstructure indicated the effectiveness of the kyanite particles to enhance the strength (>200 MPa), the Vickers hardness (>11 GPa) and the elastic modulus (150 GPa). The strengthening mechanism was particularly linked action of particles reinforcement. At low temperature, kyanite acts as fillers reducing the porosity and playing the role of nucleation sites for the crystallization of metakaolin to mullite. At high temperature (>1350 °C), kyanite decomposes to mullite avoiding the grain growth of the existing crystals and delaying the densification. The extent of the reduction in porosity and the extreme limitation of the liquid phase ensure the homogeneity and the refractoriness that justify the strength enhancement. The unit cell parameters and the crystal structure confirmed predominance of the mullite 3:2 with their small grain size being one of the most stable mullite phases. The small size of their particles and the continuity into the mullite matrix composites allow good packing process for the optimum characteristics achieved: strength, microstructure and thermal expansion coefficient.     

Thermal compatibility between hydroquinone and retinoic acid in pharmaceutical formulations

Thermogravimetry (TG) and differential scanning calorimetry (DSC) are used in pharmaceutical studies for characterization of drugs, purity, compatibility of formulations, identification of polymorphism, evaluation of stability, and thermal decomposition of drugs and pharmaceutical formulations. Hydroquinone (HQ) and products containing HQ have been widely used as depigmentation agents for lightening the skin. Retinoids are compounds that have the basic core structure of vitamin A and its oxidized metabolites, or synthetic compounds that share similar mechanisms of action as naturally occurring retinoids. Depigmentants and excipients were analyzed by TG and DSC. The dynamic thermogravimetric curves were obtained on a SHIMADZU thermobalance, model DTG-60, using an alumina crucible, at the heating rate of 10 °C min^?1, in the temperature range of 25–900 °C, under an atmosphere of nitrogen at 50 mL min^?1. The sample's mass was 10 ± 0.05 mg. The DSC curves were obtained using Shimadzu calorimeter, model DSC-60, using aluminum crucible, at the heating rate of 10 °C min^?1, in the temperature range of 25–400 °C. The thermogravimetric and calorimetric curves were analyzed using TASYS software SHIMADZU. In this study were found the interaction between retinoic acid (RA) and the following excipients: cetyl alcohol(CA), cetostearyl alcohol (CTA), glycerin(GLY), and dipropylene glycol (DPG), and that between HQ and the excipient, DPG. Therefore, additional studies are necessary to evaluate final formulations. Thermal analysis is an effective and reliable technique that can be used in the control of raw materials and pharmaceutical products, and for evaluating their employment potential in the development and characterization of products.     

Phase diagram study of CaBr2–LiBr system using DTA

The phase diagram of binary LiBr–CaBr₂ system was investigated using differential thermal analysis (DTA) between room temperature and 800 °C. From the DTA results obtained over the entire range of composition from pure LiBr to pure CaBr₂ in steps of ~5 mol%, the phase diagram was constructed and is reported here. The results indicated the possible existence of a compound at 50 mol% LiBr, namely, LiCaBr₃. The compound undergoes peritectic decomposition at 552 °C. The system shows a eutectic reaction at 532 °C between this compound and LiBr phase, and the eutectic composition is close to 80 mol% LiBr. The compound LiCaBr₃ decomposes into CaBr₂ and LiBr phases below 272 °C. Co-existing phases in different phase fields are characterized by X-ray diffraction analysis.     

Thermal transformations of gamma alumina with phosphorus oxide surface nanostructures

Differential scanning calorimetry, thermogravimetry, and X-ray diffraction analysis were used to study the fundamental aspects of structural-chemical transformations occurring under the action of temperature in the range 50–1530°C in the system constituted by alumina core and phosphorus oxide shell synthesized by the molecular-layering method. It was shown that, as the P/Al molar ratio in the system increases from 0.05 to 0.14, the stability range of low-temperature forms of alumina extends to higher temperatures because crystalline aluminum phosphate is formed on the surface. It was demonstrated that using an inorganic binder based on a silicate binding agent and alumina modified with an aluminum phosphate layer provides a ~3.5-fold increase in the mechanical strength of the material at a ~5-fold decrease in the internal stress as compared with the composition with the unmodified oxide.     

Mechanical, thermal, and moisture absorption properties of nano-clay reinforced nano-cellulose biocomposites

In this research, fully environment-friendly, sustainable and biodegradable ‘green’ composites were fabricated. A novel material comprised of microfibrillated cellulose and laponite clay with different inorganic/organic ratios (m/m) was prepared. The composites were characterized by tensile, bending and water absorption tests as well as dynamic mechanical analysis. The morphologies of these nanocomposites were evaluated through scanning electron microscopy. Results showed considerable improvement of mechanical properties; specifically in elastic modulus, tensile strength and flexural modulus with the addition of nanoclay up to 7.5 wt% nano-clay. The modulus of elasticity increased significantly by about 26 % at 5 wt% nanocaly. The flexural modulus increased by about 90 % at 7.5 wt% nanoclay. However, with an increased load of clay in the nanocomposite, the mechanical properties decreased due to the agglomeration of excessive nanoclay. The storage modulus was significantly increased at high temperature with increasing the load of nanoclay.     

Fire resistance properties of heavyweight magnetite concrete in comparison with normal basalt- and quartz-based concrete

Nowadays application of radiation shielding structures grows over the world. Nuclear buildings represent one of the most complicated radiation shielding structures; that is why a particular type of concrete is required to withstand different conditions during their lifespan. Unique properties such as the behaviour under elevated temperatures, radiation shielding, and thermal stability properties are essential to guarantee the fire resistance safety of nuclear buildings. However, some gaps are still there, warranting further investigation, particularly the thermal stability and fire-resistance properties of the heavyweight concrete. The properties are mechanical, physical, and deformation properties of concrete after being subjected to elevated temperature. This paper investigated the fire resistance properties of three concrete mixes. There were magnetite-based concrete, basalt-based concrete, and quartz-based concrete. Compressive and flexural strength, spalling, mass loss, porosity, and scanning electron microscopy were measured for the three concrete types after being subjected to different temperature steps at 20, 150, 300, 500, and 800 °C. The three types of concrete showed different fire resistance properties. Magnetite-based concrete has better heat/fire resistance than basalt- and quartz-based concrete; there was no significant change up to 500 °C, and explosive spalling occurred at 800 °C. Correspondingly, the maximum change in porosity and reduction in the compressive and flexural strength occurred at 300 °C, which indicates the good thermal stability of magnetite-based concrete. Concerning basalt-based and quartz-based concretes, cracks were observed at 500 °C, and cracks with colour change and small spalling were initiated at 800 °C. Therefore, the maximum growth in the porosity and the high reduction in the compressive and flexural strength in basalt-based concrete occurred at 800 °C. Likewise, the extreme change in the porosity occurred at 500 °C, and the drastic reduction in the compressive and the flexural strength in the quartz-based concrete was relatively high at 500 °C and 800 °C. The SEM observations and analysis obtained the appearance of microcracks, voids and degradation of C-S-H in different concrete mixes at 500 and 800℃.

     

Synthesis and characterization of Na2O–CaO–SiO2 glass–ceramic

The Na₂O–CaO–SiO₂ ternary glass–ceramic with the composition of 49 mass% Na₂O, 20 mass% CaO, and 31 mass% SiO₂ was prepared by the conventional method. The ternary glass–ceramic was characterized using X-ray diffraction (XRD), differential thermal analysis (DTA), thermogravimetric analysis, Fourier transform infrared spectroscopy, and scanning electron microscopy techniques. The Na₂CaSiO₄ phase, having the cubic crystal system, with the crystallite size of 25.14 nm and lattice parameter of 0.7506 nm was determined from the XRD pattern. The activation energy of the glass–ceramic calculated from the DTA curves was found to be 162.02 kJ mol^?1. The Avrami exponent was found to be ~2 indicating a one-dimensional growth process. The mass loss percent from ambient temperature to 1,173 K is less than 1 %. The density was calculated to be 2,723 kg m^?3. The fine-grained microstructure with the particle sizes less than 1 μm was confirmed by the scanning electron microscope micrograph.     

Influence of temperature and light intensity on the photocuring process and kinetics parameters of a pigmented UV curable system

The photopolymerization of pigmented coatings is a great challenge and hardly investigated in the literature. Therefore, in this work, the effect of photopolymerization temperature and light intensity on the curing behavior of a TiO₂-pigmented UV curable epoxy acrylate system was investigated by using photo-differential scanning calorimetry (photo-DSC) analysis. The rate of conversion and ultimate conversion at four different temperatures (i.e., 25, 45, 65, and 85 °C) and four light intensities (i.e. 2, 20, 40 and 80 mW cm^?2) for unpigmented and pigmented formulations were measured. The effect of photo-polymerization temperature and light intensity on the kinetics constants was also evaluated. It was observed that the rate of conversion and final conversion values were affected by the temperature and UV-light intensity. It was seen that the rate of conversion and ultimate conversion had their maximum values at 65 °C for unpigmented formulations. However, in pigmented formulations, these two parameters improved by increasing the temperature even up to 85 °C. Increasing the temperature caused an increase in the amount of propagation and termination rate constants in both pigmented and unpigmented formulations although the changes in the pigmented formulation were more pronounced. It was observed that the rate of polymerization and ultimate conversion for unpigmented formulations increased by increasing the light intensity up to 20 mW cm^?2 and then decreased. On the other hand, it was found that these two parameters increased by increasing light intensity up to 40 mW cm^?2 when pigmented formulations used. Finally, the dependence of termination and propagation kinetics constants on light intensity was established for both unpigmented and pigmented coatings.     

Heat resistance of portland cements

Recent fire cases indicated again the importance of fire research. Fast development of construction technology requires new materials. Initiation and development of fire are strongly influenced by the choice of construction materials. In addition to their mechanical properties, their behaviour in elevated temperature is also of high importance. Residual compressive strength of concrete exposed to high temperatures is influenced by the following factors: water-to-cement ratio, cement-to-aggregate ratio, type of aggregate and water content of concrete before exposing it to high temperatures and the fire process. Therefore, mix design and composition of concrete are of high importance for high temperatures. Based on the literature, the fire resistance of concrete is influenced by the used cement type. As regards the cement type, considerable importance has been attached to the various auxiliary materials, such as slag, fly ash, trass, metakaolines and silica fume. There has been no special research devoted to the fire behaviour of pure portland cements. Pure portland cements can be made with various oxide compositions or with different grinding fineness, which increases the resistance of cements to fire. The question arises what effects grinding fineness and oxide composition have on fire resistance of cements. In my experiments, the resistance of portland cements of different composition and grinding fineness to fire (high temperature) were examined. For the test of the solidified cement paste, cement paste cubes of 30-mm edge length were prepared. The specimens were stored in water for 7 days and then in laboratory conditions for 21 days. The cubes of more than 28 days were heated to the given temperature in the furnace and then kept at the given temperature for 2 h (50, 150, 300, 500, 800 °C). Following the 2 h of thermal load, the specimens were examined once their temperature cooled down to room temperature. I have experimentally demonstrated that in case of portland cements, the grinding fineness and aluminate modulus of the cement (i.e. the oxide composition of the cement) have a significant effect on its fire resistance.