Search results for: calcination of metakaolinite

Authors: Mohammed Mesrar, Hamza El Malki, Hamza Mesrar

Abstract:

In this study, ceramics of (1-x)(Na0.5Bi0.5)TiO3 x(K0.5 Bi0.5)TiO3 were synthesized through a conventional calcination process (solid-state method) at 1000°C for 4 hours, with x(%) values ranging from 0.0 to 100. Room temperature XRD patterns confirmed the phase formation of the samples. The Rietveld refinement method was employed to verify the morphotropic phase boundary (MPB) at x(%)=16-20. We investigated the average crystallite size and lattice strain using Scherrer's formula and Williamson-Hall (W-H) analysis. SEM image analyses provided additional evidence of the impact of doping on structural growth under low temperatures. Relaxation time extracted from Z″(f) and M″(f) spectra for x(%) = 0.0, 12, 16, 20, and 30 followed the Arrhenius law, revealing the presence of three distinct relaxation mechanisms with varying activation energies. The shoulder response in M″(f) indirectly indicated the existence of highly polarizable entities in the samples, serving as a signature of polar nanoregions (PNRs) within the grains.In this study, ceramics of (1-x)(Na0.5Bi0.5)TiO3 x(K0.5 Bi0.5)TiO3 were synthesized through a conventional calcination process (solid-state method) at 1000°C for 4 hours, with x(%) values ranging from 0.0 to 100. Room temperature XRD patterns confirmed the phase formation of the samples. The Rietveld refinement method was employed to verify the morphotropic phase boundary (MPB) at x(%)=16-20. We investigated the average crystallite size and lattice strain using Scherrer's formula and Williamson-Hall (W-H) analysis. SEM image analyses provided additional evidence of the impact of doping on structural growth under low temperatures. Relaxation time extracted from Z″(f) and M″(f) spectra for x(%) = 0.0, 12, 16, 20, and 30 followed the Arrhenius law, revealing the presence of three distinct relaxation mechanisms with varying activation energies. The shoulder response in M″(f) indirectly indicated the existence of highly polarizable entities in the samples, serving as a signature of polar nanoregions (PNRs) within the grains.

Keywords: (1-x)(Na0.5Bi0.5)TiO3 x(K0.5 Bi0.5)TiO3, Rietveld refinement, Scanning electron microscopy (SEM), Williamson-Hall plots, charge density distribution, dielectric properties

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Authors: M. Bahgat, F. M. Awan, H. A. Hanafy

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The conventional ceramic route was utilized to prepare a hard magnetic powder (M-type strontium ferrite, SrFe12O19). The stoichiometric mixture of iron oxide and strontium carbonate were calcined at 1000°C and then fired at various temperatures. The influence of various reaction parameters such as mixing ratio, calcination temperature, firing temperature and firing time on the magnetic behaviors of the synthesized magnetic powder were investigated.The magnetic properties including Coercivity (Hc), Magnetic saturation (Ms), and Magnetic remnance (Mr) were measured by vibrating sample magnetometer. Morphologically the produced magnetic powder has a dense hexagonal grain shape structure.

Keywords: hard magnetic materials, ceramic route, strontium ferrite, magnetic properties

Procedia PDF Downloads 652

Authors: W. Kritsarikan, T. Patcharawit, T. Yingnakorn, S. Khumkoa

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Neodymium-iron-boron (NdFeB) magnets classified as high-power magnets are widely used in various applications such as electrical and medical devices and account for 13.5 % of the permanent magnet’s market. Since its typical composition of 29 - 32 % Nd, 64.2 – 68.5 % Fe and 1 – 1.2 % B contains a significant amount of rare earth metals and will be subjected to shortages in the future. Domestic NdFeB magnet waste recycling should therefore be developed in order to reduce social, environmental impacts toward a circular economy. Most research works focus on recycling the magnet wastes, both from the manufacturing process and end of life. Each type of wastes has different characteristics and compositions. As a result, these directly affect recycling efficiency as well as the types and purity of the recyclable products. This research, therefore, focused on the recycling of manufacturing NdFeB magnet waste obtained from the sintering stage of magnet production and the waste contained 23.6% Nd, 60.3% Fe and 0.261% B in order to recover high purity neodymium oxide (Nd₂O₃) using hybrid metallurgical process via oxidative roasting and selective leaching techniques. The sintered NdFeB waste was first ground to under 70 mesh prior to oxidative roasting at 550 - 800 °C to enable selective leaching of neodymium in the subsequent leaching step using H₂SO₄ at 2.5 M over 24 h. The leachate was then subjected to drying and roasting at 700 – 800 °C prior to precipitation by oxalic acid and calcination to obtain neodymium oxide as the recycling product. According to XRD analyses, it was found that increasing oxidative roasting temperature led to an increasing amount of hematite (Fe₂O₃) as the main composition with a smaller amount of magnetite (Fe₃O₄) found. Peaks of neodymium oxide (Nd₂O₃) were also observed in a lesser amount. Furthermore, neodymium iron oxide (NdFeO₃) was present and its XRD peaks were pronounced at higher oxidative roasting temperatures. When proceeded to acid leaching and drying, iron sulfate and neodymium sulfate were mainly obtained. After the roasting step prior to water leaching, iron sulfate was converted to form hematite as the main compound, while neodymium sulfate remained in the ingredient. However, a small amount of magnetite was still detected by XRD. The higher roasting temperature at 800 °C resulted in a greater Fe₂O₃ to Nd₂(SO₄)₃ ratio, indicating a more effective roasting temperature. Iron oxides were subsequently water leached and filtered out while the solution contained mainly neodymium sulfate. Therefore, low oxidative roasting temperature not exceeding 600 °C followed by acid leaching and roasting at 800 °C gave the optimum condition for further steps of precipitation and calcination to finally achieve neodymium oxide.

Keywords: NdFeB magnet waste, oxidative roasting, recycling, selective leaching

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Authors: Woranittha Kritsarikan

Abstract:

Neodymium-iron-boron (NdFeB) magnets classified as high-power magnets are widely used in various applications such as electrical and medical devices and account for 13.5 % of the permanent magnet’s market. Since its typical composition of 29 - 32 % Nd, 64.2 – 68.5 % Fe and 1 – 1.2 % B contains a significant amount of rare earth metals and will be subjected to shortages in the future. Domestic NdFeB magnet waste recycling should therefore be developed in order to reduce social, environmental impacts toward the circular economy. Most research works focus on recycling the magnet wastes, both from the manufacturing process and end of life. Each type of wastes has different characteristics and compositions. As a result, these directly affect recycling efficiency as well as the types and purity of the recyclable products. This research, therefore, focused on the recycling of manufacturing NdFeB magnet waste obtained from the sintering stage of magnet production and the waste contained 23.6% Nd, 60.3% Fe and 0.261% B in order to recover high purity neodymium oxide (Nd₂O₃) using hybrid metallurgical process via oxidative roasting and selective leaching techniques. The sintered NdFeB waste was first ground to under 70 mesh prior to oxidative roasting at 550 - 800 ᵒC to enable selective leaching of neodymium in the subsequent leaching step using H₂SO₄ at 2.5 M over 24 hours. The leachate was then subjected to drying and roasting at 700 – 800 ᵒC prior to precipitation by oxalic acid and calcination to obtain neodymium oxide as the recycling product. According to XRD analyses, it was found that increasing oxidative roasting temperature led to the increasing amount of hematite (Fe₂O₃) as the main composition with a smaller amount of magnetite (Fe3O4) found. Peaks of neodymium oxide (Nd₂O₃) were also observed in a lesser amount. Furthermore, neodymium iron oxide (NdFeO₃) was present and its XRD peaks were pronounced at higher oxidative roasting temperature. When proceeded to acid leaching and drying, iron sulfate and neodymium sulfate were mainly obtained. After the roasting step prior to water leaching, iron sulfate was converted to form hematite as the main compound, while neodymium sulfate remained in the ingredient. However, a small amount of magnetite was still detected by XRD. The higher roasting temperature at 800 ᵒC resulted in a greater Fe2O3 to Nd2(SO4)3 ratio, indicating a more effective roasting temperature. Iron oxides were subsequently water leached and filtered out while the solution contained mainly neodymium sulfate. Therefore, low oxidative roasting temperature not exceeding 600 ᵒC followed by acid leaching and roasting at 800 ᵒC gave the optimum condition for further steps of precipitation and calcination to finally achieve neodymium oxide.

Keywords: NdFeB magnet waste, oxidative roasting, recycling, selective leaching

Procedia PDF Downloads 155

Authors: M. Ghobeiti-Hasab, Z. Shariati

Abstract:

In this paper, strontium ferrite (SrO.6Fe2O3) was synthesized by the sol-gel auto-combustion process. The thermal behavior of powder obtained from self-propagating combustion of initial gel was evaluated by simultaneous differential thermal analysis (DTA) and thermo gravimetric (TG), from room temperature to 1200°C. The as-burnt powder was calcined at various temperatures from 700-900°C to achieve the single-phase Sr-ferrite. Phase composition, morphology and magnetic properties were investigated using X-ray diffraction (XRD), transmission electron microscopy (TEM) and vibrating sample magnetometry (VSM) techniques. Results showed that the single-phase and nano-sized hexagonal strontium ferrite particles were formed at calcination temperature of 800°C with crystallite size of 27 nm and coercivity of 6238 Oe.

Keywords: hard magnet, Sr-ferrite, sol-gel auto-combustion, nano-powder

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Authors: I. Grigoraviciute-Puroniene, K. Tsuru, E. Garskaite, Z. Stankeviciute, A. Beganskiene, K. Ishikawa, A. Kareiva

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Tricalcium phosphate (β-Ca₃(PO₄)₂, β-TCP) powders were synthesized using wet polymeric precipitation method for the first time to our best knowledge. The results of X-ray diffraction analysis showed the formation of almost single a Ca-deficient hydroxyapatite (CDHA) phase of a poor crystallinity already at room temperature. With continuously increasing the calcination temperature up to 800 °C, the crystalline β-TCP was obtained as the main phase. It was demonstrated that infrared spectroscopy is very effective method to characterize the formation of β-TCP. The SEM results showed that β-TCP solids were homogeneous having a small particle size distribution. The β-TCP powders consisted of spherical particles varying in size from 100 to 300 nm. Fabricated β-TCP specimens were placed to the bones of the rats and maintained for 1-2 months.

Keywords: Tricalcium phosphate (β-Ca3(PO4)2, bone regeneration, wet chemical processing, polymeric precipitation

Procedia PDF Downloads 267

Authors: S. V. Kuznetsov, M. N. Mayakova, V. Yu. Proydakova, V. V. Pavlov, A. S. Nizamutdinov, O. A. Morozov, V. V. Voronov, P. P. Fedorov

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Increase in the share of electricity received by conversion of solar energy results in the reduction of the industrial impact on the environment from the use of the hydrocarbon energy sources. One way to increase said share is to improve the efficiency of solar energy conversion in silicon-based solar panels. Such efficiency increase can be achieved by transferring energy from sunlight-insensitive areas of work of silicon solar panels to the area of their photoresistivity. To achieve this goal, a transition to new luminescent materials with the high quantum yield of luminescence is necessary. Improvement in the quantum yield can be achieved by quantum cutting, which allows obtaining a quantum yield of down conversion of more than 150% due to the splitting of high-energy photons of the UV spectral range into lower-energy photons of the visible and near infrared spectral ranges. The goal of present work is to test approach of excitation through sensibilization of 4f-4f fluorescence of Yb3+ by various RE ions absorbing in UV and Vis spectral ranges. One of promising materials for quantum cutting luminophores are fluorides. In our investigation we have developed synthesis of nano- and submicron powders of calcium fluoride and strontium doped with rare-earth elements (Yb: Ce, Yb: Pr, Yb: Eu) of controlled dimensions and shape by co-precipitation from water solution technique. We have used Ca(NO3)2*4H2O, Sr(NO3)2, HF, NH4F as precursors. After initial solutions of nitrates were prepared they have been mixed with fluorine containing solution by dropwise manner. According to XRD data, the synthesis resulted in single phase samples with fluorite structure. By means of SEM measurements, we have confirmed spherical morphology and have determined sizes of particles (50-100 nm after synthesis and 150-300 nm after calcination). Temperature of calcination appeared to be 600°C. We have investigated the spectral-kinetic characteristics of above mentioned compounds. Here the diffuse reflection and laser induced fluorescence spectra of Yb3+ ions excited at around 4f-4f and 4f-5d transitions of Pr3+, Eu3+ and Ce3+ ions in the synthesized powders are reported. The investigation of down conversion luminescence capability of synthesized compounds included measurements of fluorescence decays and quantum yield of 2F5/2-2F7/2 fluorescence of Yb3+ ions as function of Yb3+ and sensitizer contents. An optimal chemical composition of CaF2-YbF3- LnF3 (Ln=Ce, Eu, Pr), SrF2-YbF3-LnF3 (Ln=Ce, Eu, Pr) micro- and nano- powders according to criteria of maximal IR fluorescence yield is proposed. We suppose that investigated materials are prospective in solar panels improvement applications. Work was supported by Russian Science Foundation grant #17-73- 20352.

Keywords: solar cell, fluorides, down-conversion luminescence, maximum quantum yield

Procedia PDF Downloads 240

Authors: M. Bahgat, F. M. Awan, H. A. Hanafy, O. N. Alzeghaibi

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Strontium hexaferrite (SrFe12O19; Sr-ferrite) is one of the well-known materials for permanent magnets. In this study, M-type strontium ferrite was prepared by following the conventional ceramic method from steelmaking by-product. Initial materials; SrCO3 and by-product, were mixed together in the composition of SrFe12O19 in different Sr/Fe ratios. The mixtures of these raw materials were dry-milled for 6h. The blended powder was pre-sintered (i.e. calcination) at 1000°C for different times periods, then cooled down to room temperature. These pre-sintered samples were re-milled in a dry atmosphere for 1h and then fired at different temperatures in atmospheric conditions, and cooled down to room temperature. The produced magnetic powder has a dense hexagonal grain shape structure. The calculated energy product values for the produced samples ranged from 0.3 to 2.4 MGOe.

Keywords: hard magnetic materials, ceramic route, strontium ferrite, synthesis

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Authors: Lovepreet Kaur Dhugga, Dwijendra P. Singh

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Calcium copper titanate (CCTO) was synthesized via the sol-gel auto-combustion method. The precursor was calcined at 800°C and 1000°C for 6 hours providing brown-coloured powders, which were pelletized and sintered at 1000°C for 12 hrs to determine their dielectric behaviour in the frequency range (100Hz-10MHz) at room temperature. The dielectric constant(εr) and loss tangent (tanδ) has been found to be ~ 6153 and 0.5 for 800°C and ~ 5504 and 0.2 for 1000°C respectively, at frequency 1kHz. Microstructure study revealed maximum grain growth occurs in sample calcined at 800°C, responsible for its high dielectric constant. Phase identification of CaCu₃Ti₄O₁₂ has been carried out through X-ray diffraction. It can be used in various electronic applications as it shows large εᵣ and low tanδ values over a wide frequency spectrum, including energy storage devices, microwave shielding, and sensors.

Keywords: calcium copper titanate, dielectric behaviour, microstructure, X-ray diffraction

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Authors: Ali Akbar Kazemi Asl, Mansour Rahsepar

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Mesoporous carbon nanospheres (MCNs) with uniform particle size distribution having an average of 290 nm and large specific surface area (274.4 m²/g) were synthesized by a one-step hydrothermal method followed by the calcination process and then utilized as an enzyme-free glucose biosensor. Morphology, crystal structure, and porous nature of the synthesized nanospheres were characterized by scanning electron microscopy (SEM), X-Ray diffraction (XRD), and Brunauer–Emmett–Teller (BET) analysis, respectively. Also, the electrochemical performance of the MCNs@GCE electrode for the measurement of glucose concentration in alkaline media was investigated by electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), and chronoamperometry (CA). MCNs@GCE electrode shows good sensing performance, including a rapid glucose oxidation response within 3.1 s, a wide linear range of 0.026-12 mM, a sensitivity of 212.34 μA.mM⁻¹.cm⁻², and a detection limit of 25.7 μM with excellent selectivity.

Keywords: biosensor, electrochemical, glucose, mesoporous carbon, non-enzymatic

Procedia PDF Downloads 155

Authors: Aleksander Ejsmont, Stefan Wuttke, Joanna Goscianska

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Gaining control over particle shape, size and crystallinity is an ongoing challenge for many materials. Especially metalorganic frameworks (MOFs) are recently widely studied. Besides their remarkable porosity and interesting topologies, morphology has proven to be a significant feature. It can affect the further material application. Thus seeking new approaches that enable MOF morphology modulation is important. MOFs are reticular structures, where building blocks are made up of organic linkers and metallic nodes. The most common strategy of ensuring metal source is using salts, which usually exhibit high solubility and hinder morphology control. However, there has been a growing interest in using metal oxides as structure-directing agents towards MOFs due to their very low solubility and shape preservation. Metal oxides can be treated as a metal reservoir during MOF synthesis. Up to now, reports in which receiving MOFs from metal oxides mostly present ZnO conversion to ZIF-8. However, there are other oxides, for instance, Co₃O₄, which often is overlooked due to their structural stability and insolubility in aqueous solutions. Cobalt-based materials are famed for catalytic activity. Therefore the development of their efficient synthesis is worth attention. In the presented work, an optimized Co₃O₄transition to Co-MOFviaa solvothermal approach was proposed. The starting point of the research was the synthesis of Co₃O₄ flower petals and needles under hydrothermal conditions using different cobalt salts (e.g., cobalt(II) chloride and cobalt(II) nitrate), in the presence of urea, and hexadecyltrimethylammonium bromide (CTAB) surfactant as a capping agent. After receiving cobalt hydroxide, the calcination process was performed at various temperatures (300–500 °C). Then cobalt oxides as a source of cobalt cations were subjected to reaction with trimesic acid in solvothermal environment and temperature of 120 °C leading to Co-MOF fabrication. The solution maintained in the system was a mixture of water, dimethylformamide, and ethanol, with the addition of strong acids (HF and HNO₃). To establish how solvents affect metal oxide conversion, several different solvent ratios were also applied. The materials received were characterized with analytical techniques, including X-ray powder diffraction, energy dispersive spectroscopy,low-temperature nitrogen adsorption/desorption, scanning, and transmission electron microscopy. It was confirmed that the synthetic routes have led to the formation of Co₃O₄ and Co-based MOF varied in shape and size of particles. The diffractograms showed receiving crystalline phase for Co₃O₄, and also for Co-MOF. The Co₃O₄ obtained from nitrates and with using low-temperature calcination resulted in smaller particles. The study indicated that cobalt oxide particles of different size influence the efficiency of conversion and morphology of Co-MOF. The highest conversion was achieved using metal oxides with small crystallites.

Keywords: Co-MOF, solvothermal synthesis, morphology control, core-shell

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Authors: Lucie Speyer, Vincent Lecocq, Séverine Humbert, Antoine Hugon

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Mesoporous alumina is commonly used as a catalyst support for the hydrotreating of heavy petroleum cuts. The process of fabrication usually involves: the synthesis of the boehmite AlOOH precursor, a kneading-extrusion step, and a calcination in order to obtain the final alumina extrudates. Alumina is described as a complex porous medium, generally agglomerates constituted of aggregated nanocrystallites. Its porous texture directly influences the active phase deposition and mass transfer, and the catalytic properties. Then, it is easy to figure out that each step of the fabrication of the supports has a role on the building of their porous network, and has to be well understood to optimize the process. The synthesis of boehmite by precipitation of aluminum salts was extensively studied in the literature and the effect of various parameters, such as temperature or pH, are known to influence the size and shape of the crystallites and the specific surface area of the support. The calcination step, through the topotactic transition from boehmite to alumina, determines the final properties of the support and can tune the surface area, pore volume and pore diameters from those of boehmite. However, the kneading extrusion step has been subject to a very few studies. It generally consists in two steps: an acid, then a basic kneading, where the boehmite powder is introduced in a mixer and successively added with an acid and a base solution to form an extrudable paste. During the acid kneading, the induced positive charges on the hydroxyl surface groups of boehmite create an electrostatic repulsion which tends to separate the aggregates and even, following the conditions, the crystallites. The basic kneading, by reducing the surface charges, leads to a flocculation phenomenon and can control the reforming of the overall structure. The separation and reassembling of the particles constituting the boehmite paste have a quite obvious influence on the textural properties of the material. In this work, we are focused on the influence of the kneading step on the alumina catalysts supports. Starting from an industrial boehmite, extrudates are prepared using various kneading conditions. The samples are studied by nitrogen physisorption in order to analyze the evolution of the textural properties, and by synchrotron small-angle X-ray scattering (SAXS), a more original method which brings information about agglomeration and aggregation of the samples. The coupling of physisorption and SAXS enables a precise description of the samples, as same as an accurate monitoring of their evolution as a function of the kneading conditions. These ones are found to have a strong influence of the pore volume and pore size distribution of the supports. A mechanism of evolution of the texture during the kneading step is proposed and could be attractive in order to optimize the texture of the supports and then, their catalytic performances.

Keywords: alumina catalyst support, kneading, nitrogen physisorption, small-angle X-ray scattering

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Authors: Faezeh Aghazadeh

Abstract:

The catalytic activity of Pt/γ-Al₂O₃ and Pt-Fe/γ-Al₂O₃ catalysts was investigated to bring about the complete oxidation of 2-Propanol. Among them, Pt-Fe/γ-Al₂O₃ was found to be the most promising catalyst based on activity. The catalysts were characterized by (XRD), (SEM), (TEM) and ICP-AES techniques. Iron loadings on Pt/γ-Al₂O₃ had a great effect on catalytic activity, and Pt-Fe/γ-Al₂O₃ (1.75 wt% Fe) catalyst at calcination temperature 300°C was observed to be the most active, which might be contributed to the favorable synergetic effects between Pt and Fe, high activity and the well-dispersed bimetallic phase. The combustion of 2-Propanol in the vapor phase was carried out in a conventional flow U-shape glass reactor used in the differential mode at atmospheric pressure. 2-Propanol was analyzed by a gas chromatograph VARIAN 3800 CX equipped with an FID. As observed, better performance and activity were observed for Pt-Fe/Al₂O₃ bimetallic catalyst. These results indicate that the high dispersion on support gives a positive effect on catalytic activity.

Keywords: volatile organic compounds, bimetallic catalyst, catalytic activity, low temperature

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Authors: Wei-Bo Hua, Zhuo Zheng, Xiao-Dong Guo, Ben-He Zhong

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The layered structure LiNi1/3Co1/3Mn1/3-xAlxO2 (x = 0 ~ 0.04) series cathode materials were synthesized by a carbonate co-precipitation method, followed by a high temperature calcination process. The influence of Al substitution on the microstructure and electrochemical performances of the prepared materials was investigated by X-Ray diffraction (XRD), scanning electron microscopy (SEM), and galvanostatic charge/discharge test. The results show that the LiNi1/3Co1/3Mn1/3-xAlxO2 has a well-ordered hexagonal "α" -NaFeO2 structure. Although the discharge capacity of Al-doped samples decreases as x increases, LiNi1/3Co1/3Mn1/3-0.02Al0.02O2 exhibits superior capacity retention at high voltage (4.6 V). Therefore, LiNi1/3Co1/3Mn1/3-0.02Al0.02O2 is a promising material for “green” vehicles.

Keywords: lithium ion battery, carbonate co-precipitation, doping, microstructure, electrochemical properties

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Authors: N. Bouhamou, F. Mostefa, A. Mebrouki, N. Belas

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Every year, millions of cube meters are dredged from dams and restraints as an entertaining and prevention procedure all over the world. These dredged sediments are considered as natural waste leading to an environmental, ecological and even an economical problem in their processing and deposing. Nevertheless, in the context of the sustainable development policy, a way of management is opened aiming to the valorization of sediments as a building material and particularly as a new binder that can be industrially exploited and that improve the physical, chemical and mechanical characteristics of the concrete. This study is a part of the research works realized in the civil engineering department at the university of Mostaganem (Algeria), on the impact of the dredged mud of Fergoug dam on the behaviour of self-consolidating concrete in fresh and hardened state, such as the mechanical performance of SCC and its impact on the differed deformations (shrinkage). The work aims to valorize this mud in SCC and to show eventual interactions between constituents. The results obtained presents a good perspectives in order to perform SCC based in calcined mud.

Keywords: sediment, calcination, reuse, self-consolidating concrete, fresh state, hard state, shrinkage

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Authors: M. Ghobeiti-Hasab

Abstract:

Magnetic powder of Sr-ferrite was prepared by conventional and sol-gel auto-combustion methods. In conventional method, strontium carbonate and ferric oxide powders were mixed together and then mixture was calcined. In sol-gel auto-combustion method, a solution containing strontium nitrate, ferric nitrate and citric acid was heated until the combustion took place automatically; then, as-burnt powder was calcined. Thermal behavior, phase identification, morphology and magnetic properties of powders obtained by these two methods were compared by DTA, XRD, SEM, and VSM techniques. According to the results of DTA analysis, formation temperature of Sr-ferrite obtained by conventional and sol-gel auto-combustion methods were 1300 °C and 1000 °C, respectively. XRD results confirmed the formation of pure Sr-ferrite at the mentioned temperatures. Plate and hexagonal-shape particles of Sr-ferrite were observed using SEM. The Sr-ferrite powder obtained by sol-gel auto-combustion method had saturation magnetization of 66.03 emu/g and coercivity of 5731 Oe in comparison with values of 58.20 emu/g and 4378 Oe obtained by conventional method.

Keywords: Sr-ferrite, sol-gel, magnetic properties, calcination

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Authors: Charmaine Lamiel, Van Hoa Nguyen, Jae-Jin Shim

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Supercapacitors are energy storage devices capable of storing more energy than conventional capacitors and have higher power density than batteries. The advantages of this method include the non-use of reducing agents and acidic medium, and no further use of a post-heat treatment unlike the conventional processes, in which calcination is generally employed after obtaining the initial product. Furthermore, it also offers a shorter reaction time at low temperatures and low power requirements, which allows low fabrication and energy cost. In this study, microwave irradiation was used for the facile and rapid synthesis of mesoporous RGO@(Co,Mn)3O4 nanosheets as an electrode material. The as-prepared electrode exhibited a high capacitance of 953 F•g^−1 at 1 A•g^−1 in a 6 M KOH electrolyte solution. Moreover, the electrode exhibited a high energy density of 76.2 Wh•kg^−1 at a power density of 720 W•kg^−1, and a high power density of 7200 W•kg^−1 at an energy density of 38 Wh•kg^−1. The successful methodology was considered to be efficient and cost-effective, thereby providing an active electrode material with very promising electrochemical performance.

Keywords: cobalt-manganese oxide, electrochemical, graphene, microwave synthesis, supercapacitor

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Authors: M. Masar, P. Janota, J. Sedlak, M. Machovsky, I. Kuritka

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Zinc oxide (ZnO) nano crystals assembled porous architecture was prepared by thermal decomposition of zinc oxalate precursor at various temperatures ranging from 400-900°C. The effect of calcining temperature on structure and morphology was examined by scanning electron microscopy (SEM), X-ray diffractometry, thermogravimetry, and BET adsorption analysis. The porous nano crystalline ZnO morphology was developed due to the release of volatile precursor products, while the overall shape of ZnO micro crystals was retained as a legacy of the precursor. The average crystallite size increased with increasing temperature of calcination from approximately 21 nm to 79 nm, while the specific surface area decreased from 30 to 1.7 m2g-1. The photo catalytic performance of prepared ZnO powders was evaluated by degradation of methyl violet 2B, a model compound. The significantly highest photo catalytic activity was achieved with powder calcined at 500°C. This may be attributed to the sufficiently well-developed crystalline arrangement, while the specific surface area is still high enough.

Keywords: ZnO, porous structure, photodegradation, methyl violet

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Authors: Ximena Castillo, Jaime Pizarro

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This research describes the development of a very cheap mesoporous silica material similar to hexagonal mesoporous silica (HMS) and using a silicate extract as precursor. This precursor is obtained from cheap fly ash by an easy calcination process at 850 °C and a green extraction with water. The obtained mesoporous fly ash material had a surface area of 282 m2 g-1 and a pore size of 5.7 nm. It was functionalized with ethylene diamino moieties via the well-known SAMMS method, followed by a DRIFT analysis that clearly showed the successful functionalization. An excellent adsorbent was obtained for the adsorption of sulfate anions by the solid’s modification with copper forming a copper-ethylenediamine complex. The adsorption of sulfates was studied in a batch system ( experimental conditions: pH=8.0; 5 min). The kinetics data were adjusted according to a pseudo-second order model with a high coefficient of linear regression at different initial concentrations. The adsorption isotherm that best fitted the experimental data was the Freundlich model. The maximum sulfate adsorption capacity of this very cheap fly ash based adsorbent was 146.1 mg g-1, 3 times greater than the values reported in literature and commercial adsorbent materials.

Keywords: fly ash, mesoporous materials, SAMMS, sulfate

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Authors: S. Toufigh Bararpour, Davood Karami, Nader Mahinpey

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Dependence of global economics on fossil fuels has led to a large growth in the emission of greenhouse gases (GHGs). Among the various GHGs, carbon dioxide is the main contributor to the greenhouse effect due to its huge emission amount. To mitigate the threatening effect of CO₂, carbon capture and sequestration (CCS) technologies have been studied widely in recent years. For the combustion processes, three main CO₂ capture techniques have been proposed such as post-combustion, pre-combustion and oxyfuel combustion. Post-combustion is the most commonly used CO₂ capture process as it can be readily retrofit into the existing power plants. Multiple advantages have been reported for the post-combustion by solid sorbents such as high CO₂ selectivity, high adsorption capacity, and low required regeneration energy. Chemical adsorption of CO₂ over alkali-metal-based solid sorbents such as K₂CO₃ is a promising method for the selective capture of diluted CO₂ from the huge amount of nitrogen existing in the flue gas. To improve the CO₂ capture performance, K₂CO₃ is supported by a stable and porous material. Al₂O₃ has been employed commonly as the support and enhanced the cyclic CO₂ capture efficiency of K₂CO₃. Different phases of alumina can be obtained by setting the calcination temperature of boehmite at 300, 600 (γ-alumina), 950 (δ-alumina) and 1200 °C (α-alumina). By increasing the calcination temperature, the regeneration capacity of alumina increases, while the surface area reduces. However, sorbents with lower surface areas have lower CO₂ capture capacity as well (except for the sorbents prepared by hydrophilic support materials). To resolve this issue, a highly efficient alumina-aerogel support was synthesized with a BET surface area of over 2000 m²/g and then calcined at a high temperature. The synthesized alumina-aerogel was impregnated on K₂CO₃ based on 50 wt% support/K₂CO₃, which resulted in the preparation of a sorbent with remarkable CO₂ capture performance. The effect of synthesis conditions such as types of alcohols, solvent-to-co-solvent ratios, and aging times was investigated on the performance of the support. The best support was synthesized using methanol as the solvent, after five days of aging time, and at a solvent-to-co-solvent (methanol-to-toluene) ratio (v/v) of 1/5. Response surface methodology was used to investigate the effect of operating parameters such as carbonation temperature and H₂O-to-CO₂ flowrate ratio on the CO₂ capture capacity. The maximum CO₂ capture capacity, at the optimum amounts of operating parameters, was 7.2 mmol CO₂ per gram K₂CO₃. Cyclic behavior of the sorbent was examined over 20 carbonation and regenerations cycles. The alumina-aerogel-supported K₂CO₃ showed a great performance compared to unsupported K₂CO₃ and γ-alumina-supported K₂CO₃. Fundamental performance analyses and long-term thermal and chemical stability test will be performed on the sorbent in the future. The applicability of the sorbent for a bench-scale process will be evaluated, and a corresponding process model will be established. The fundamental material knowledge and respective process development will be delivered to industrial partners for the design of a pilot-scale testing unit, thereby facilitating the industrial application of alumina-aerogel.

Keywords: alumina-aerogel, CO₂ capture, K₂CO₃, optimization

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Authors: Andualem Workie

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In this study, we examined the sinterability and bioactivity of MgO-SiO₂-P₂O₅-CaO-CaF₂ glass compositions created through spray pyrolysis. We evaluated the bioactivity of the materials by immersing them for varying periods of time in simulated bodily fluid (SBF) and found that bioactivity was related to the sintering temperature and soaking time. The material's pH value during immersion in SBF was within the range of 7.4-8.2, which is below 8.5 and improves compatibility and reduces toxicity in biological applications. We used X-ray diffraction and scanning electron microscopy to determine the phase compositions and morphologies of the samples and found that the 1100°C sintered A-W GC sample exhibited the highest bioactivity after soaking in SBF. This sample was dominated by fluorapatite, wollastonite, and whitlockite crystals scattered throughout the glass matrix. The crystallinity (%) of the A-W GC increased as its bioactivity improved, making it more suitable for use in pharmaceutical applications. We also conducted a cytotoxicity test on A-W GC samples sintered at different temperatures and found that the glass-ceramics were non-toxic to MC3T3-E1 cells at all extraction concentrations, except for those sintered at 700°C at concentrations of 250, 200, and 150 mg/ml where cell viability (%) was below the threshold of 70%.

Keywords: apatite wollastonite glass ceramics, bioactivity, calcination, cell viability

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Authors: Tarun Jain, Lovnish Gupta, Soumen Basu

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Organic pollutants like phenols and organic dyes present in industrial waste water are posing a hazardous threat to aquatic ecosystem. Several measures have been adopted for the neutralization and photodecomposition of these harmful organic moieties, among these semiconductor photocatalysis has been provided a major thrust after the discovery of Honda-Fujishema effect. Present study demonstrates the adsorption of TiO2- P25 in nano size (~36 nm) on cement balls for effective photodegradation of Alizarin and penta chlorophenol (PCP) under UV light illumination. Triton-X was used as a stabilizer for effective adsorption of TiO2 on cement balls (TCB) followed by calcination at ~300oC for 4 h. The TCB’s were dispersed randomly in a self designed reactor for phototcatalytic performance as shown in scheme 1. The change in concentration of alizarin and PCP was observed under UV-Vis spectroscopy, PCP was detoxified within 40 min while alizarin photodecomposed within 15 min of UV light irradiation. Taking into consideration the go green slogan and future prospective this technique can be also utilized under visible light and on mass scale because this is an effective tool for environmental remediation and waste water treatment.

Keywords: organic pollutants, TiO2 cement balls, photodegradation, UV light irradiation

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Authors: Eden G. Mariquit, Winarto Kurniawan, Masahiro Miyauchi, Hirofumi Hinode

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This research studied the effect of adding surfactant to the titanium dioxide (TiO2) sol-gel solution that was used to immobilize TiO2 on glass substrates by dip coating technique using TiO2 sol-gel solution mixed with different types of surfactants. After dipping into the TiO2 sol, the films were calcined and produced pure anatase crystal phase. The thickness of the thin film was varied by repeating the dip and calcine cycle. The prepared films were characterized using FE-SEM, TG-DTA, and XRD, and its photocatalytic performances were tested on degradation of an organic dye, methylene blue. Aside from its phocatalytic performance, the photo-induced hydrophilicity of thin TiO2 films surface was also studied. Characterization results showed that the addition of surfactant gave rise to characteristic patterns on the surface of the TiO2 thin film which also affects the photocatalytic activity. The addition of CTAB to the TiO2 dipping solution had a negative effect because the calcination temperature was not high enough to burn all the surfactants off. As for the surface wettability, the addition of surfactant also affected the induced surface hydrophilicity of the TiO2 films when irradiated under UV light.

Keywords: photocatalysis, surface hydrophilicity, TiO2 thin films, surfactant

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Authors: Jong Kook Lee, Sangcheol Eum, Jaehong Kim

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Wollastonite/hydroxyapatite composite coatings on zirconia were obtained by room temperature spray process. Wollastonite powder was synthesized by solid-state reaction between calcite and silica powder. Hydroxyapatite powder was prepared from bovine bone by the calcination at 1200oC 1h. From two starting raw powders, three kinds of powder mixture were obtained by the ball milling for 24h. By using these powders, wollastonite/hydroxyapatite coatings were fabricated on zirconia substrates by a room temperature spray process, and their microstructure and biological behavior were investigated and compared with pure wollastonite and hydroxyapatite coatings. Wollastonite/hydroxyapatite coatings on zirconia substrates were homogeneously formed in microstructure and had a nanoscaled grain size. The phase composition of the resultant wollastonite/hydroxyapatite coatings was similar to that of the starting powders, however, the grain size of the wollastonite or hydroxyapatite particles was reduced to about 100 nm due to their formation by particle impaction and fracture. The wollastonite/hydroxyapatite coating layer exhibited bioactivity in a stimulated body fluid and forming ability of new hydroxyapatite precipitates of 25 nm during in vitro test in SBF solution, which was enhanced by the increasing wollastonite content.

Keywords: wollastonite, hydroxyapatite composite coatings, room temperature spay process, zirconia

Procedia PDF Downloads 446

Authors: P. Comendador, M. Suarez, L. Olazar, M. Cortazar, M. Artetxe, G. Lopez, M. Olazar

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H₂ production from fast biomass pyrolysis and line Steam Reforming (SR) has been extensively studied in the last years. However, Sorption Enhanced Steam Reforming (SESR) is gaining attention as an alternative to the conventional SR since it allows obtaining higher H₂ yields and a purity near 100 % in the product stream. In this work, both alternatives were compared through an energy analysis. The processes were modeled with PRO II v.2021 software. First, general energy balances were carried out in order to identify the total energy requirements in a wide range of operating conditions. At H₂ yield optimum conditions for both processes (steam to biomass ratio of 2 and temperature of 600 ºC), the total energy requirement for the SR alternative is 936 kJ/kgH₂, whereas for the SESR alternative is 1134 kJ/kgH₂. Then, the energy needs were grouped into operation stages, aiming at identifying the energy sinks and sources of the processes. It was determined that the SESR alternative is more energy intensive due to the need for a calcination stage for regenerating the sorbent. Finally, a configuration of the SESR alternative with energy integration was developed in order to compensate for the energy demand.

Keywords: Biomass valorization, CO₂ capture, Energy analysis, H₂ production

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Authors: Rupan Das Chakraborty, Surendra K. Martha

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Hard carbons (HCs) are extensively used as anode materials for sodium-ion batteries due to their availability, low cost, and ease of synthesis. It possesses the ability to store Na ion between stacked sp2 carbon layers and micropores. In this work, hard carbons are synthesized from different concentrations (0.5M to 5M) of dextrose solutions by hydrothermal synthesis followed by high-temperature calcination at 1100 ⁰C in an inert atmosphere. Dextrose has been chosen as a precursor material as it is a eco-friendly and renewable source. Among all hard carbon derived from different concentrations of dextrose solutions, hard carbon derived from 3M dextrose solution delivers superior electrochemical performance compared to other hard carbons. Hard carbon derived from 3M dextrose solution (Dextrose derived Hard Carbon-3M) provides an initial reversible capacity of 257 mAh g-1 with a capacity retention of 83 % at the end of 100 cycles at 30 mA g-1). The carbons obtained from different dextrose concentration show very similar Cyclic Voltammetry and chargedischarging behavior at a scan rate of 0.05 mV s-1 the Cyclic Voltammetry curve indicate that solvent reduction and the solid electrolyte interface (SEI) formation start at E < 1.2 V (vs Na/Na+). Among all 3M dextrose derived electrode indicate as a promising anode material for Sodium-ion batteries (SIBs).

Keywords: dextrose derived hard carbon, anode, sodium-ion battery, electrochemical performance

Procedia PDF Downloads 69

Authors: Bezzi Nacer

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The study focused on the qualitative and quantitative study of Trace elements contained in the natural phosphate ore of Djebel Onk layer and their behaviour to the various mineralurgic modes of treatment. The main objective is to locate the importance of these contents according to granulometry and their association with the existing mineralogical species and to define how the most appropriate treatment. The raw ore is in first submitted to a prior mechanical treatment consisting of homogenization operations, of grinding and of sifting, in order to separate it into three particle-size classes: fine <100 µm (F); medium 100-500 µm (I) and coarse > 500 µm (G), and then treated by calcination, washing and floatation. The identification of the different mineralogical phases, the chemical composition and the thermal behaviour of these samples were realized by various techniques: MEB, DRX, ATG-ATD, etc. The study of Trace elements, carried out by ICP-MS, identified thirty items, consisting mainly of rare earths and of transition metals. A close relation between trace elements and various minerals phases (apatite, dolomite and silicates), through operations of substitution. These elements are distributed between several mineralogical phases, in particular apatite (strontium, uranium, chrome, barium, cadmium) and silicates (strontium, sodium, nickel, zinc and copper).

Keywords: valorization of natural phosphate ore, heavy metals, qualitative and quantitative analysis, various mineralurgic

Procedia PDF Downloads 311

Authors: Navid Zanganeh, Hafez Balavi, Farbod Sharif, Mahla Zabet, Marzieh Bakhtiary Noodeh

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Cerium oxide (CeO2) also known as cerium dioxide or ceria is a pale yellow-white powder with various applications in the industry from wood coating to cosmetics, filtration, fuel cell electrolytes, gas sensors, hybrid solar cells and catalysts. In this research, attempts were made to synthesize and characterization of CeO2 nano-particles via sol-gel method. In addition, the effect of aging time on the size of particles was investigated. For this purpose, the aging times adjusted 48, 56, 64, and 72 min. The obtained particles were characterized by x-ray diffraction spectroscopy (XRD), scanning electron microscopy (SEM), transmitted electron microscopy (TEM), and Brunauer–Emmett–Teller (BET). As a result, XRD patterns confirmed the formation of CeO2 nanoparticles. SEM and TEM images illustrated the nano-particles with cluster shape, spherical and a nano-size range which was in agreement with XRD results. The finest particles (7.3 nm) was obtained at the optimum condition which was aging time of 48 min, calcination temperature at 400 ⁰C, and cerium concentration of 0.004 mol. Average specific surface area of the particles at optimum condition was measured by BET analysis and recorded as 47.57 m2/g.

Keywords: aging time, CeO2 nanoparticles, size distribution, sol-gel

Procedia PDF Downloads 423

Authors: John O. Akindoyo, M. D. H. Beg, Suriati Binti Ghazali, Nitthiyah Jeyaratnam

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Regeneration of bone due to the many health challenges arising from traumatic effects of bone loss, bone tumours and other bone infections is fast becoming indispensable. Over the period of time, some approaches have been undertaken to mitigate this challenge. This includes but not limited to xenografts, allografts, autografts as well as artificial substitutions like bioceramics, synthetic cements and metals. However, most of these techniques often come along with peculiar limitation and problems such as morbidity, availability, disease transmission, collateral site damage or absolute rejection by the body as the case may be. Hydroxyapatite (HA) is very compatible and suitable for this application. However, most of the common methods for HA synthesis are expensive and environmentally unfriendly. Extraction of HA from bio-wastes have been perceived not only to be cost effective, but also environment-friendly. In this research, HA was produced from bio-waste: namely bovine bones through a combination of hydrothermal chemical processes and ordinary calcination techniques. Structure and property of the HA was carried out through different characterization techniques (such as TGA, FTIR, DSC, XRD and BET). The synthesized HA was found to possess similar properties to stoichiometric HA with highly desirable thermal, degradation, structural and porous properties. This material is unique for its potential minimal cost, environmental friendliness and property controllability. It is also perceived to be suitable for tissue and bone engineering applications.

Keywords: biomaterial, biopolymer, bone, hydroxyapatite

Procedia PDF Downloads 290

Authors: Sudhir Kumar Sharma, Ramesh Jagannathan

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The interaction of organic and inorganic matrices of biological origin resulting in self-assembled structures with unique properties is well established. The development of such self-assembled nanostructures by synthetic and bio-inspired techniques is an established field of active research. Among bio-materials, nacre, a laminar stack of calcium carbonate nanosheets, which are interleaved with organic material, has long been focused research due to its unique mechanical properties. In this paper, we present the development of nacre-like lamellar structures made up of calcium carbonate via a wet chemical route. We used the binding affinity of carboxylate anions and calcium cations using poly (acrylic) acid (PAA) to lead CaCO₃ crystallization. In these experiments, we selected calcium acetate as the precursor molecule along with PAA (Mw ~ 8000 Da). We found that Ca⁺²/COO⁻ ratio provided a tunable control for the morphology and growth of CaCO₃ nanostructures. Drop casting one such formulation on a silicon substrate followed by calcination resulted in co-planner, molecular sheets of CaCO₃, separated by a spacer layer of carbon. The scope of our process could be expanded to produce unit cell thick molecular sheets of other important inorganic materials.

Keywords: self-assembled structures, bio-inspired materials, calcium carbonate, wet chemical route

Procedia PDF Downloads 103