Search results for: Sintering Aid

Authors: Yanbing Feng, Deqing Mei, Yancheng Wang, Zichen Chen

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With the advantage of low volume density, high specific surface area, light weight and good permeability, porous aluminum material has the potential to be used in automotive, railway, chemistry and construction industries, etc. A layered powder sintering and dissolution method were developed to fabricate the porous surface Al structure with high efficiency. However, the densification mechanism during the cold compaction of laminar composite powders is still unclear. In this study, multi particle finite element modelling (MPFEM) based on the cohesive zone method (CZM) is used to simulate the cold compaction behavior of laminar Al and NaCl composite powders. To obtain its densification mechanism, the macro and micro properties of final compacts are characterized and analyzed. The robustness and accuracy of the numerical model is firstly verified by experimental results and data fitting. The results indicate that the CZM-based multi particle FEM is an effective way to simulate the compaction of the laminar powders and the fracture process of the NaCl powders. In the compaction of the laminar powders, the void is mainly filled by the particle rearrangement, plastic deformation of Al powders and brittle fracture of NaCl powders. Large stress is mainly concentrated within the NaCl powers and the contact force network is formed. The Al powder near the NaCl powder or the mold has larger stress distribution on its contact surface. Therefore, the densification process of cold compaction of laminar Al and NaCl composite powders is successfully analyzed by the CZM-based multi particle FEM.

Keywords: cold compaction, cohesive zone, multi-particle FEM, numerical modeling, powder forming

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Authors: Wei-Jing Li, Ren-Xuan Yang, Kui-Hao Chuang, Ming-Yen Wey

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Nowadays, plastic product and utilization are extensive and have greatly improved our life. Yet, plastic wastes are stable and non-biodegradable challenging issues to the environment. Waste-to-energy strategies emerge a promising way for waste management. This work investigated the co-production of hydrogen and carbon nanotubes from the syngas which was from the gasification of polypropylene. A nickel-silica core-shell catalyst was applied for syngas reaction from plastic waste gasification in a fixed-bed reactor. SiO2 were prepared through various synthesis solvents by Stöber process. Ni plays a role as modified SiO2 support, which were synthesized by deposition-precipitation method. Core-shell catalysts have strong interaction between active phase and support, in order to avoid catalyst sintering. Moreover, Fe or Co metal acts as promoter to enhance catalytic activity. The effects of calcined atmosphere, second metal addition, and reaction temperature on hydrogen production and carbon yield were examined. In this study, the catalytic activity and carbon yield results revealed that the Ni/SiO2 catalyst calcined under H2 atmosphere exhibited the best performance. Furthermore, Co promoted Ni/SiO2 catalyst produced 3 times more than Ni/SiO2 on carbon yield at long-term operation. The structure and morphological nature of the calcined and spent catalysts were examined using different characterization techniques including scanning electron microscopy, transmission electron microscopy, X-ray diffraction. In addition, the quality and thermal stability of the nano-carbon materials were also evaluated by Raman spectroscopy and thermogravimetric analysis.

Keywords: plastic wastes, hydrogen, carbon nanotube, core-shell catalysts

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Authors: Fanyuan Shao, Wei Liu, Deli Gao

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Polycrystalline diamond composite (PDC) cutter is made of diamond powder as raw material, cobalt metal or non-metallic elements as a binder, mixed with WC cemented carbide matrix assembly, through high temperature and high-pressure sintering. PDC bits with PDC cutters are widely used in oil and gas drilling because of their high hardness, good wear resistance and excellent impact toughness. And PDC cutter is the main cutting tool of bit, which seriously affects the service of the PDC bit. The wear resistance of the PDC cutter is measured by cutting granite with a vertical turret lathe (VTL). This experiment can achieve long-distance cutting to obtain the relationship between the wear resistance of the PDC cutter and cutting distance, which is more closely to the real drilling situation. Load cell and 3D optical profiler were used to obtain the value of cutting forces and wear area, respectively, which can also characterize the damage and wear of the PDC cutter. PDC cutters were cut via electrical discharge machining (EDM) and then flattened and polished. A scanning electron microscope (SEM) was used to observe the distribution of binder cobalt and the size of diamond particles in a diamond PDC cutter. The cutting experimental results show that the wear area of the PDC cutter has a good linear relationship with the cutting distance. Simultaneously, the larger the wear area is and the greater the cutting forces are required to maintain the same cutting state. The size and distribution of diamond particles in the polycrystalline diamond layer have a great influence on the wear resistance of the diamond layer. And PDC cutter with fine diamond grains shows more wear resistance than that with coarse grains. The deep leaching process is helpful to reduce the effect of binder cobalt on the wear resistance of the polycrystalline diamond layer. The experimental study can provide an important basis for the application of PDC cutters in oil and gas drilling.

Keywords: polycrystalline diamond compact, scanning electron microscope, wear resistance, cutting distance

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Authors: Vidula Shevade, B. J. Nagare, Sajeev Chacko

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First principles simulation, meaning density functional theory (DFT) calculations with plane waves and pseudopotential, has become a prized technique in condensed matter theory. Nanoparticles (NP) have been known to possess good catalytic activities, especially for molecules such as CO, O₂, etc. Among the metal NPs, Aluminium based NPs are also widely known for their catalytic properties. Aluminium metal is a lightweight, excellent electrical, and thermal abundant chemical element in the earth’s crust. Aluminium NPs, when added to solid rocket fuel, help improve the combustion speed and considerably increase combustion heat and combustion stability. Adding aluminium NPs into normal Al/Al₂O₃ powder improves the sintering processes of the ceramics, with high heat transfer performance, increased density, and enhanced thermal conductivity of the sinter. We used VASP and Gaussian 0₃ package to compute the geometries, electronic structure, and bonding properties of Al₁₂Ni as well as its interaction with O₂ and CO molecules. Several MD simulations were carried out using VASP at various temperatures from which hundreds of structures were optimized, leading to 24 unique structures. These structures were then further optimized through a Gaussian package. The lowest energy structure of Al₁₂Ni has been reported to be a singlet. However, through our extensive search, we found a triplet state to be lower in energy. In our structure, the Ni atom is found to be on the surface, which gives the non-zero magnetic moment. Incidentally, O2 and CO molecules are also triplet in nature, due to which the Al₁₂-Ni cluster is likely to facilitate the oxidation process of the CO molecule. Our results show that the most favourable site for the CO molecule is the Ni atom and that for the O₂ molecule is the Al atom that is nearest to the Ni atom. Al₁₂Ni-O₂ and Al₁₂-Ni-CO structures we extracted using VMD. Al₁₂Ni nanocluster, due to in triplet electronic structure configuration, indicates it to be a potential candidate as a catalyst for oxidation of CO molecules.

Keywords: catalyst, gaussian, nanoparticles, oxidation

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Authors: N.Quaranta, M. Caligaris, R. Varoli, A. Cristobal, M. Unsen, H. López

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Corncobs are agricultural wastes and they can be used as fuel or as raw material in different industrial processes like cement manufacture, contaminant adsorption, chemical compound synthesis, etc. The aim of this work is to characterize this waste and analyze the feasibility of its use as a pore-forming material in the manufacture of lightweight ceramics for the civil construction industry. The characterization of raw materials is carried out by using various techniques: electron diffraction analysis X-ray, differential and gravimetric thermal analyses, FTIR spectroscopy, ecotoxicity evaluation, among others. The ground corncobs, particle size less than 2 mm, are mixed with clay up to 30% in volume and shaped by uniaxial pressure of 25 MPa, with 6% humidity, in moulds of 70mm x 40mm x 18mm. Then the green bodies are heat treated at 950°C for two hours following the treatment curves used in ceramic industry. The ceramic probes are characterized by several techniques: density, porosity and water absorption, permanent volumetric variation, loss on ignition, microscopies analysis, and mechanical properties. DTA-TGA analysis of corncobs shows in the range 20°-250°C a small loss in TGA curve and exothermic peaks at 250°-500°C. FTIR spectrum of the corncobs sample shows the characteristic pattern of this kind of organic matter with stretching vibration bands of adsorbed water, methyl groups, C–O and C–C bonds, and the complex form of the cellulose and hemicellulose glycosidic bonds. The obtained ceramic bodies present external good characteristics without loose edges and adequate properties for the market requirements. The porosity values of the sintered pieces are higher than those of the reference sample without waste addition. The results generally indicate that it is possible to use corncobs as porosity former in ceramic bodies without modifying the usual sintering temperatures employed in the industry.

Keywords: ceramic industry, biomass, recycling, hemicellulose glycosidic bonds

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Authors: Asif Mahmood, Yousef Alzeghayer

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The size effects of a precursor Y2BaCuO5 (Y211) powder on the microstructure and critical current density (Jc) of liquid infiltration growth (LIG)-processed YBa2Cu3O7-y (Y123) bulk superconductors were investigated in terms of milling time (t). YBCO bulk samples having high Jc values have been selected for the flywheel energy storage system. Y211 powders were attrition-milled for 0-10 h in 2 h increments at a fixed rotation speed of 400 RPM. Y211 pre-forms were made by pelletizing the milled Y211 powders followed by subsequent sintering, after which an LIG process with top seeding was applied to the Y211/Ba3Cu5O8 (Y035) pre-forms. Spherical pores were observed in all LIG-processed Y123 samples, and the pore density gradually decreased as t increased from 0 h to 8 h. In addition to the reduced pore density, the Y211 particle size in the final Y123 products also decreased with increasing t. As t increased further to 10 h, unexpected Y211 coarsening and large pore evolutions were observed. The magnetic susceptibility-temperature curves showed that the onset superconducting transition temperature (Tc, onset) of all samples was the same (91.5 K), but the transition width became greater as t increased. The Jc of the Y123 bulk superconductors fabricated in this study was observed to correlate well with t of the Y211 precursor powder. The maximum Jc of 1.0×105 A cm-2 (at 77 K, 0 T) was achieved at t = 8 h, which is attributed to the reduction in pore density and Y211 particle size. The prolonged milling time of t = 10 h decreased the Jc of the LIG-processed Y123 superconductor owing to the evolution of large pores and exaggerated Y211 growth. YBCO bulk samples having high Jc (samples prepared using 8 h milled powders) have been used for the energy storage system in flywheel energy storage system.

Keywords: critical current, bulk superconductor, liquid infiltration, bioinformatics

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Authors: P. Caimmi, E. Bele, A. Abolfathi

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Lattice materials are cellular structures composed of a periodic network of beams. They offer high weight-specific mechanical properties and lend themselves to numerous weight-sensitive applications. The periodic internal structure responds to external vibrations through characteristic frequency bandgaps, making these materials suitable for the reduction of noise and vibration. However, the deviation from architectural homogeneity, due to, e.g., manufacturing imperfections, has a strong influence on the mechanical properties and vibration response of these materials. In this work, we present results on the influence of geometric imperfections on the vibration response of hexagonal lattices. Three classes of geometrical variables are used: the characteristics of the architecture (relative density, ligament length/cell size ratio), imperfection type (degree of non-periodicity, cracks, hard inclusions) and defect morphology (size, distribution). Test specimens with controlled size and distribution of imperfections are manufactured through selective laser sintering. The Frequency Response Functions (FRFs) in the form of accelerance are measured, and the modal shapes are captured through a high-speed camera. The finite element method is used to provide insights on the extension of these results to semi-infinite lattices. An updating procedure is conducted to increase the reliability of numerical simulation results compared to experimental measurements. This is achieved by updating the boundary conditions and material stiffness. Variations in FRFs of periodic structures due to changes in the relative density of the constituent unit cell are analysed. The effects of geometric imperfections on the dynamic response of periodic structures are investigated. The findings can be used to open up the opportunity for tailoring these lattice materials to achieve optimal amplitude attenuations at specific frequency ranges.

Keywords: lattice architectures, geometric imperfections, vibration attenuation, experimental modal analysis

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Authors: Min Chang Shin, Byung Hun Jeong, Jeong Sik Han, Jung Hoon Park

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In modern times, as flight speeds have increased due to improvements in aircraft and missile engine performance, thermal loads have also increased. Because of the friction heat of air flow with high speed on the surface of the vehicle, it is not easy to cool the superheat of the vehicle by the simple air cooling method. For this reason, a cooling method through endothermic heat is attracting attention by using a fuel that causes an endothermic reaction in a high-speed vehicle. There are two main ways of cooling the fuel through the endothermic reaction. The first is physical heat absorption. When the temperature rises, there is a sensible heat that accompanies it. The second is the heat of reaction corresponding to the chemical heat absorption, which absorbs heat during the fuel decomposes. Generally, since the decomposition reaction of the fuel proceeds at a high temperature, it does not achieve a great efficiency in cooling the high-speed flight body. However, when the catalyst is used, decomposition proceeds at a low temperature thereby increasing the cooling efficiency. However, when the catalyst is used as a powder, the catalyst enters the engine and damages the engine or the catalyst can deteriorate the performance due to the sintering. On the other hand, when used in the form of pellets, catalyst loss can be prevented. However, since the specific surface of pellet is small, the efficiency of the catalyst is low. And it can interfere with the flow of fuel, resulting in pressure loss and problems with fuel injection. In this study, we tried to maximize the performance of the catalyst by preparing a hollow fiber type pellet for zeolite ZSM-5, which has a higher amount of heat absorption, than other conventional pellets. The hollow fiber type pellet was prepared by phase inversion method. The hollow fiber type pellet has a finger-like pore and sponge-like pore. So it has a higher specific surface area than conventional pellets. The crystal structure of the prepared ZSM-5 catalyst was confirmed by XRD, and the characteristics of the catalyst were analyzed by TPD/TPR device. This study was conducted as part of the Basic Research Project (Pure-17-20) of Defense Acquisition Program Administration.

Keywords: catalyst, endothermic reaction, high-speed vehicle cooling, zeolite, ZSM-5

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Authors: Edgar Gasafi, Robert Pardemann, Linus Perander

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For the production of lithium carbonate or hydroxide out of lithium bearing ores, a thermal activation (calcination/decrepitation) is required for the phase transition in the mineral to enable an acid respectively soda leaching in the downstream hydrometallurgical section. In this paper, traditional processing in Lithium industry is reviewed, and opportunities to reduce energy consumption and improve product quality and recovery rate will be discussed. The conventional process approach is still based on rotary kiln calcination, a technology in use since the early days of lithium ore processing, albeit not significantly further developed since. A new technology, at least for the Lithium industry, is fluidized bed calcination. Decrepitation of lithium ore was investigated at Outotec’s Frankfurt Research Centre. Focusing on fluidized bed technology, a study of major process parameters (temperature and residence time) was performed at laboratory and larger bench scale aiming for optimal product quality for subsequent processing. The technical feasibility was confirmed for optimal process conditions on pilot scale (400 kg/h feed input) providing the basis for industrial process design. Based on experimental results, a comprehensive Aspen Plus flow sheet simulation was developed to quantify mass and energy flow for the rotary kiln and fluidized bed system. Results show a significant reduction in energy consumption and improved process performance in terms of temperature profile, product quality and plant footprint. The major conclusion is that a substantial reduction of energy consumption can be achieved in processing Lithium bearing ores by using fluidized bed based systems. At the same time and different from rotary kiln process, an accurate temperature and residence time control is ensured in fluidized-bed systems leading to a homogenous temperature profile in the reactor which prevents overheating and sintering of the solids and results in uniform product quality.

Keywords: calcination, decrepitation, fluidized bed, lithium, spodumene

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Authors: María Magdalena Méndez-González, Miguel García Rocha, Carlos Manuel Yermo De la Cruz

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Calcium phosphate (Ca5(PO4)3(X)) is widely used in orthopedic applications and is widely used as powder and granules. However, their presence in bone is in the form of nanometric needles 60 nm in length with a non-stoichiometric phase of apatite contains CO3-2, Na+, OH-, F-, and other ions in a matrix of collagen fibers. The crystal size, morphology control and interaction with cells are essential for the development of nanotechnology. The structural results of calcium phosphate, synthesized by chemical precipitation with crystal size of 22.85 nm are presented in this paper. The calcium phosphate powders were analyzed by X-ray diffraction, energy dispersive spectroscopy (EDS), infrared spectroscopy and FT-IR transmission electron microscopy. Network parameters, atomic positions, the indexing of the planes and the calculation of FWHM (full width at half maximum) were obtained. The crystal size was also calculated using the Scherer equation d (hkl) = cλ/βcosѲ. Where c is a constant related to the shape of the crystal, the wavelength of the radiation used for a copper anode is 1.54060Å, Ѳ is the Bragg diffraction angle, and β is the width average peak height of greater intensity. Diffraction pattern corresponding to the calcium phosphate called hydroxyapatite phase of a hexagonal crystal system was obtained. It belongs to the space group P63m with lattice parameters a = 9.4394 Å and c = 6.8861 Å. The most intense peak is obtained 2Ѳ = 31.55 (FWHM = 0.4798), with a preferred orientation in 121. The intensity difference between the experimental data and the calculated values is attributable to the temperature at which the sintering was performed. The intensity of the highest peak is at angle 2Ѳ = 32.11. The structure of calcium phosphate obtained was a hexagonal configuration. The intensity changes in the peaks of the diffraction pattern, in the lattice parameters at the corners, indicating the possible presence of a dopant. That each calcium atom is surrounded by a tetrahedron of oxygen and hydrogen was observed by infrared spectra. The unit cell pattern corresponds to hydroxyapatite and transmission electron microscopic crystal morphology corresponding to the hexagonal phase with a preferential growth along the c-plane was obtained.

Keywords: structure, nanoparticles, calcium phosphate, metallurgical and materials engineering

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Authors: Hsueh-Hsing Lu, Thi-Cuc Le, Tung-Sheng Tsai, Chuen-Jinn Tsai

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This study designed and tested a novel wet electrostatic precipitators (WEP) system featuring a Pulse-Air-Jet-Assisted Water Flow (PJWF) to shorten water cleaning time, reduce water usage, and maintain high particle removal efficiency. The PJWF injected cleaning water tangentially at the cylinder wall, rapidly enhancing the momentum of the water flow for efficient dust cake removal. Each PJWF cycle uses approximately 4.8 liters of cleaning water in 18 seconds. Comprehensive laboratory tests were conducted using a single-tube WEP prototype within a flow rate range of 3.0 to 6.0 cubic meters per minute(CMM), operating voltages between -35 to -55 kV, and high-frequency power supply. The prototype, consisting of 72 sets of double-spike rigid discharge electrodes, demonstrated that with the PJWF, -35 kV, and 3.0 CMM, the PM2.5 collection efficiency remained as high as the initial value of 88.02±0.92% after loading with Al2O3 particles at 35.75± 2.54 mg/Nm3 for 20-hr continuous operation. In contrast, without the PJWF, the PM2.5 collection efficiency drastically dropped from 87.4% to 53.5%. Theoretical modeling closely matched experimental results, confirming the robustness of the system's design and its scalability for larger industrial applications. Future research will focus on optimizing the PJWF system, exploring its performance with various particulate matter, and ensuring long-term operational stability and reliability under diverse environmental conditions. Recently, this WEP was combined with a preceding CT (cooling tower) and a HWS (honeycomb wet scrubber) and pilot-tested (40 CMM) to remove SO2 and PM2.5 emissions in a sintering plant of an integrated steel making plant. Pilot-test results showed that the removal efficiencies for SO2 and PM2.5 emissions are as high as 99.7 and 99.3 %, respectively, with ultralow emitted concentrations of 0.3 ppm and 0.07 mg/m3, respectively, while the white smoke is also eliminated at the same time. These new technologies are being used in the industry and the application in different fields is expected to be expanded to reduce air pollutant emissions substantially for a better ambient air quality.

Keywords: wet electrostatic precipitator, pulse-air-jet-assisted water flow, particle removal efficiency, air pollution control

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Authors: Mitsunobu Iwasaki, Akifumi Iseda

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Yttrium aluminum garnet doped with cerium (Ⅲ) ions (Y3Al5O12:Ce3+, YAG:Ce3+) has attracted a great attention because it can efficiently convert the blue light into a very broad yellow emission band, which produces white light emitting diodes and is applied for panel displays. To improve the brightness and resolution of the display, a considerable attention has been directed to develop fine phosphor particles. We have prepared YAG:Ce3+ nanophosphors by environmental-friendly wet process. The peak maximum of absorption spectra of surface plasmon of Ag nanopaticles are close to that of the excitation spectra (460 nm) of YAG:Ce3+. It can be expected that Ag nanoparticles supported onto the surface of YAG:Ce3+ (Ag-YAG:Ce3+) enhance the absorption of Ce3+ ions. In this study, we have prepared Ag-YAG:Ce3+ nanophosphors and investigated their photoluminescent properties. YCl3･6H2O and AlCl3･6H2O with a molar ratio of Y:Al=3:5 were dissolved in ethanol (100 ml), and CeCl3•7H2O (0.3 mol%) was further added to the above solution. Then, NaOH (4.6×10-2 mol) dissolved in ethanol (50 ml) was added dropwise to the mixture under reflux over 2 hours, and the solution was further refluxed for 1 hour. After cooling to room temperature, precipitates in the reaction mixture were heated at 673 K for 1 hour. After the calcination, the particles were immersed in AgNO3 solution for 1 hour, followed by sintering at 1123 K for 1 hour. YAG:Ce3+ were confirmed to be nanocrystals with a crystallite size of 50-80 nm in diameter. Ag nanoparticles supported onto YAG:Ce3+ were single nanometers in diameter. The excitation and emission spectra were 454 nm and 539 nm at a maximum wavelength, respectively. The emission intensity was maximum for Ag-YAG:Ce3+ immersed into 0.5 mM AgCl (Ag-YAG:Ce (0.5 mM)). The absorption maximum (461 nm) was increased for Ag-YAG:Ce3+ in comparison with that for YAG:Ce3+, indicating that the absorption was enhanced by the addition of Ag. The external and internal quantum efficiencies became 11.2 % and 36.9 % for Ag-YAG:Ce (0.5 mM), respectively. The emission intensity and absorption maximum of Ag-YAG:Ce (0.5 mM)×n (n=1, 2, 3) were increased with an increase of the number of supporting times (n), respectively. The external and internal quantum efficiencies were increased for the increase of n, respectively. The external quantum efficiency of Ag-YAG:Ce (0.5 mM) (n=3) became twice as large as that of YAG:Ce. In conclusion, Ag nanoparticles supported onto YAG:Ce3+ increased absorption and quantum efficiency. Therefore, the support of Ag nanoparticles enhanced the photoluminescent properties of YAG:Ce3+.

Keywords: plasmon, quantum efficiency, silver nanoparticles, yttrium aluminum garnet

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Authors: Zbigniew Szklarz, Aldona Garbacz-Klempka, Magdalena Bisztyga-Szklarz

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Typical metallic alloys bases on one major alloying component, where the addition of other elements is intended to improve or modify certain properties, most of all the mechanical properties. However, in 1995 a new concept of metallic alloys was described and defined. High Entropy Alloys (HEA) contains at least five alloying elements in an amount from 5 to 20 at.%. A common feature this type of alloys is an absence of intermetallic phases, high homogeneity of the microstructure and unique chemical composition, what leads to obtaining materials with very high strength indicators, stable structures (also at high temperatures) and excellent corrosion resistance. Hence, HEA can be successfully used as a substitutes for typical metallic alloys in various applications where a sufficiently high properties are desirable. For fabricating HEA, a few ways are applied: 1/ from liquid phase i.e. casting (usually arc melting); 2/ from solid phase i.e. powder metallurgy (sintering methods preceded by mechanical synthesis) and 3/ from gas phase e.g. sputtering or 4/ other deposition methods like electrodeposition from liquids. Application of different production methods creates different microstructures of HEA, which can entail differences in their properties. The last two methods also allows to obtain coatings with HEA structures, hereinafter referred to as High Entropy Films (HEF). With reference to above, the crucial aim of this work was the optimization of the manufacturing process of the multi-component metallic layers (HEF) by the low- and high temperature electrochemical deposition ( ED). The low-temperature deposition process was crried out at ambient or elevated temperature (up to 100 ᵒC) in organic electrolyte. The high-temperature electrodeposition (several hundred Celcius degrees), in turn, allowed to form the HEF layer by electrochemical reduction of metals from molten salts. The basic chemical composition of the coatings was CoCrFeMnNi (known as Cantor’s alloy). However, it was modified by other, selected elements like Al or Cu. The optimization of the parameters that allow to obtain as far as it possible homogeneous and equimolar composition of HEF is the main result of presented studies. In order to analyse and compare the microstructure, SEM/EBSD, TEM and XRD techniques were employed. Morover, the determination of corrosion resistance of the CoCrFeMnNi(Cu or Al) layers in selected electrolytes (i.e. organic and non-organic liquids) was no less important than the above mentioned objectives.

Keywords: high entropy alloys, electrodeposition, corrosion behavior, microstructure

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Authors: Irene Buj-Corral, Ali Bagheri, Alejandro Dominguez-Fernandez

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In recent years, use of ceramic prostheses as an implant in some parts of body has become common. In the present study, research has focused on replacement of the acetabulum bone, which is a part of the pelvis bone. Metallic prostheses have shown some problems such as release of metal ions into patient's blood. In addition, fracture of liners and squeezing between surface of femoral head and inner surface of acetabulum have been reported. Ceramic prostheses have the advantage of low debris and high strength, although they are more difficult to be manufactured than metallic ones. Specifically, new designs try to attempt an acetabulum in which the outer surface will be porous for proliferation of cells and fixation of the prostheses by means of osteointegration, while inner surface must be smooth enough to assure that the movement between femoral head and inner surface will be carried out with on feasibility. In the present study, 3D printing technologies are used for manufacturing ceramic prostheses. In Fused Deposition Modelling (FDM) process, 3D printed plastic prostheses are obtained by means of melting of a plastic filament and subsequent deposition on a glass surface. A similar process is applied to ceramics in which ceramic powders need to be mixed with a liquid polymer before depositing them. After 3D printing, parts are subjected to a sintering process in an oven so that they can achieve final strength. In the present paper, influence of printing parameters on surface roughness 3D printed ceramic parts are presented. Three parameter full factorial design of experiments was used. Selected variables were layer height, infill and nozzle diameter. Responses were average roughness Ra and mean roughness depth Rz. Regression analysis was applied to responses in order to obtain mathematical models for responses. Results showed that surface roughness depends mainly on layer height and nozzle diameter employed, while infill was found not to be significant. In order to get low surface roughness, low layer height and low infill should be selected. As a conclusion, layer height and infill are important parameters for obtaining good surface finish in ceramic 3D printed prostheses. However, use of too low infill could lead to prostheses with low mechanical strength. Such prostheses could not be able to bear the static and dynamic charges to which they are subjected once they are implanted in the body. This issue will be addressed in further research.

Keywords: ceramic, hip prostheses, surface roughness, 3D printing

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Authors: Ana-Carolina Feltrin, Daniel Hedman, Farid Akhtar

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High entropy ceramic (HEC) materials are characterized by their compositional disorder due to different metallic element atoms occupying the cation position and non-metal elements occupying the anion position. Several studies have focused on the processing and characterization of high entropy carbides and high entropy borides, as these HECs present interesting mechanical and chemical properties. A few studies have been published on HECs containing two non-metallic elements in the composition. Dual-phase high entropy (Ti₀.₂₅V₀.₂₅Zr₀.₂₅Hf₀.₂₅)BxCy ceramics with different amounts of x and y, (0.25 HfC + 0.25 ZrC + 0.25 VC + 0.25 TiB₂), (0.25 HfC + 0.25 ZrC + 0.25 VB2 + 0.25 TiB₂) and (0.25 HfC + 0.25 ZrB2 + 0.25 VB2 + 0.25 TiB₂) were sintered from boride and carbide precursor powders using SPS at 2000°C with holding time of 10 min, uniaxial pressure of 50 MPa and under Ar atmosphere. The sintered specimens formed two HEC phases: a Zr-Hf rich FCC phase and a Ti-V HCP phase, and both phases contained all the metallic elements from 5-50 at%. Phase quantification analysis of XRD data revealed that the molar amount of hexagonal phase increased with increased mole fraction of borides in the starting powders, whereas cubic FCC phase increased with increased carbide in the starting powders. SPS consolidated (Ti₀.₂₅V₀.₂₅Zr₀.₂₅Hf₀.₂₅)BC0.5 and (Ti₀.₂₅V₀.₂₅Zr₀.₂₅Hf₀.₂₅)B1.5C0.25 had respectively 94.74% and 88.56% relative density. (Ti₀.₂₅V₀.₂₅Zr₀.₂₅Hf₀.₂₅)B0.5C0.75 presented the highest relative density of 95.99%, with Vickers hardness of 26.58±1.2 GPa for the borides phase and 18.29±0.8 GPa for the carbides phase, which exceeded the reported hardness values reported in the literature for high entropy ceramics. The SPS sintered specimens containing lower boron and higher carbon presented superior properties even though the metallic composition in each phase was similar to other compositions investigated. Dual-phase high entropy (Ti₀.₂₅V₀.₂₅Zr₀.₂₅H₀.₂₅)BxCy ceramics were successfully fabricated in a boride-carbide solid solution and the amount of boron and carbon was shown to influence the phase fraction, hardness of phases, and density of the consolidated HECs. The microstructure and phase formation was highly dependent on the amount of non-metallic elements in the composition and not only the molar ratio between metals when producing high entropy ceramics with more than one anion in the sublattice. These findings show the importance of further studies about the optimization of the ratio between C and B for further improvements in the properties of dual-phase high entropy ceramics.

Keywords: high-entropy ceramics, borides, carbides, dual-phase

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Authors: A. S. V. Carvalho, J. Luis, L. S. O. Pires, J. M. Oliveira

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Additive manufacturing technologies (AM) experienced a remarkable growth in the latest years due to the development and diffusion of a wide range of three-dimensional (3D) printing techniques. Nowadays we can find techniques available for non-industrial users, like fused filament fabrication, but techniques like 3D printing, polyjet, selective laser sintering and stereolithography are mainly spread in the industry. Robocasting (R3D) shows a great potential due to its ability to shape materials with a wide range of viscosity. Industrial porcelain compositions showing different rheological behaviour can be prepared and used as candidate materials to be processed by R3D. The use of this AM technique in industry is very residual. In this work, a specific porcelain composition with suitable rheological properties will be processed by R3D, and a systematic study of the printing parameters tuning will be shown. The porcelain composition was formulated based on an industrial spray dried porcelain powder. The powder particle size and morphology was analysed. The powders were mixed with water and an organic binder on a ball mill at 200 rpm/min for 24 hours. The batch viscosity was adjusted by the addition of an acid solution and mixed again. The paste density, viscosity, zeta potential, particle size distribution and pH were determined. In a R3D system, different speed and pressure settings were studied to access their impact on the fabrication of porcelain models. These models were dried at 80 °C, during 24 hours and sintered in air at 1350 °C for 2 hours. The stability of the models, its walls and surface quality were studied and their physical properties were accessed. The microstructure and layer adhesion were observed by SEM. The studied processing parameters have a high impact on the models quality. Moreover, they have a high impact on the stacking of the filaments. The adequate tuning of the parameters has a huge influence on the final properties of the porcelain models. This work contributes to a better assimilation of AM technologies in ceramic industry. Acknowledgments: The RoboCer3D project – project of additive rapid manufacturing through 3D printing ceramic material (POCI-01-0247-FEDER-003350) financed by Compete 2020, PT 2020, European Regional Development Fund – FEDER through the International and Competitive Operational Program (POCI) under the PT2020 partnership agreement.

Keywords: additive manufacturing, porcelain, robocasting, R3D

Procedia PDF Downloads 162

Authors: Jayashree Das, V. V. Srinivasu , D. K. Mishra, A. Maity

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Owing to the important potential applications over decades, transition metal (TM: Mn, Fe, Ni, Cu, Cr, V etc.) doped ZnO-based diluted magnetic semiconductors (DMS) always attract research attention for more and newer investigations. One of the interesting aspects of these materials is to study and understand the magnetic property at room temperature properly, which is very crucial to select a material for any related application. In this regard, Electron spin resonance (ESR) study has been proven to be a powerful technique to investigate the spin dynamics of electrons inside the system, which are responsible for the magnetic behaviour of any system. ESR as well as the Raman and Photoluminescence spectroscopy studies are also helpful to study the defects present or created inside the system in the form of oxygen vacancy or cluster instrumental in determining the room temperature ferromagnetic property of transition metal doped ZnO system, which can be controlled through varying dopant concentration, appropriate synthesis technique and sintering of the samples. For our investigation, we synthesised Cu-doped ZnO nanocrystalline samples with composition Zn1-xCux ( 0.005< x < 0.05) by pyrophoric method and sintered at a low temperature of 650 0C. The microwave absorption is studied by the Electron Spin Resonance (ESR) of X-band (9.46 GHz) at room temperature. Systematic analysis of the obtained ESR spectra reveals that all the compositions of Cu-doped ZnO samples exhibit resonance signals of appreciable line widths and g value ~ 2.2, typical characteristic of ferromagnetism in the sample. Raman scattering and the photoluminescence study performed on the samples clearly indicated the presence of pronounced defect related peaks in the respective spectra. Cu doping in ZnO with varying concentration also observed to affect the optical band gap and the respective absorption edges in the UV-Vis spectra. FTIR spectroscopy reveals the Cu doping effect on the stretching bonds of ZnO. To probe into the structural and morphological changes incurred by Cu doping, we have performed XRD, SEM and EDX study, which confirms adequate Cu substitution without any significant impurity phase formation or lattice disorder. With proper explanation, we attempt to correlate the results observed for the structural optical and magnetic behaviour of the Cu-doped ZnO samples. We also claim that our result can be instrumental for appropriate applications of transition metal doped ZnO based DMS in the field of optoelectronics and Spintronics.

Keywords: diluted magnetic semiconductors, electron spin resonance, raman scattering, spintronics.

Procedia PDF Downloads 312

Authors: Y. Mateyshina, A.Ulihin, N.Uvarov

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Electrolytes with different type of charge carrier can find widely application in different using, e.g. sensors, electrochemical equipments, batteries and others. One of important components ensuring stable functioning of the equipment is electrolyte. Electrolyte has to be characterized by high conductivity, thermal stability, and wide electrochemical window. In addition to many advantageous characteristic for liquid electrolytes, the solid state electrolytes have good mechanical stability, wide working range of temperature range. Thus search of new system of solid electrolytes with high conductivity is an actual task of solid state chemistry. Families of alkali perchlorates and nitrates have been investigated by us earlier. In literature data about transport properties of alkali nitrites are absent. Nevertheless, alkali nitrites MeNO2 (Me= Li+, Na+, K+, Rb+ and Cs+), except for the lithium salt, have high-temperature phases with crystal structure of the NaCl-type. High-temperature phases of nitrites are orientationally disordered, i.e. non-spherical anions are reoriented over several equivalents directions in the crystal lattice. Pure lithium nitrite LiNO2 is characterized by ionic conductivity near 10-4 S/cm at 180°C and more stable as compared with lithium nitrate and can be used as a component for synthesis of composite electrolytes. In this work composite solid electrolytes in the binary system LiNO2 - A (A= MgO, -Al2O3, Fe2O3, CeO2, SnO2, SiO2) were synthesized and their structural, thermodynamic and electrical properties investigated. Alkali nitrite was obtained by exchange reaction from water solutions of barium nitrite and alkali sulfate. The synthesized salt was characterized by X-ray powder diffraction technique using D8 Advance X-Ray Diffractometer with Cu K radiation. Using thermal analysis, the temperatures of dehydration and thermal decomposition of salt were determined.. The conductivity was measured using a two electrode scheme in a forevacuum (6.7 Pa) with an HP 4284A (Precision LCR meter) in a frequency range 20 Hz < ν < 1 MHz. Solid composite electrolytes LiNO2 - A A (A= MgO, -Al2O3, Fe2O3, CeO2, SnO2, SiO2) have been synthesized by mixing of preliminary dehydrated components followed by sintering at 250°C. In the series of nitrite of alkaline metals Li+-Cs+, the conductivity varies not monotonically with increasing radius of cation. The minimum conductivity is observed for KNO2; however, with further increase in the radius of cation in the series, the conductivity tends to increase. The work was supported by the Russian Foundation for Basic research, grant #14-03-31442.

Keywords: conductivity, alkali nitrites, composite electrolytes, transport properties

Procedia PDF Downloads 319

Authors: A. Talaei, M. Ahiduzzaman, A. Kumar

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In Canada, an increase in the production of iron and steel is anticipated for satisfying the increasing demand of iron and steel in the oil sands and automobile industries. It is predicted that GHG emissions from iron and steel sector will show a continuous increase till 2030 and, with emissions of 20 million tonnes of carbon dioxide equivalent, the sector will account for more than 2% of total national GHG emissions, or 12% of industrial emissions (i.e. 25% increase from 2010 levels). Therefore, there is an urgent need to improve the energy intensity and to implement energy efficiency measures in the industry to reduce the GHG footprint. This paper analyzes the current energy consumption in the Canadian iron and steel industries and identifies energy efficiency opportunities to improve the energy intensity and mitigate greenhouse gas emissions from this industry. In order to do this, a demand tree is developed representing different iron and steel production routs and the technologies within each rout. The main energy consumer within the industry is found to be flared heaters accounting for 81% of overall energy consumption followed by motor system and steam generation each accounting for 7% of total energy consumption. Eighteen different energy efficiency measures are identified which will help the efficiency improvement in various subsector of the industry. In the sintering process, heat recovery from coolers provides a high potential for energy saving and can be integrated in both new and existing plants. Coke dry quenching (CDQ) has the same advantages. Within the blast furnace iron-making process, injection of large amounts of coal in the furnace appears to be more effective than any other option in this category. In addition, because coal-powered electricity is being phased out in Ontario (where the majority of iron and steel plants are located) there will be surplus coal that could be used in iron and steel plants. In the steel-making processes, the recovery of Basic Oxygen Furnace (BOF) gas and scrap preheating provides considerable potential for energy savings in BOF and Electric Arc Furnace (EAF) steel-making processes, respectively. However, despite the energy savings potential, the BOF gas recovery is not applicable in existing plants using steam recovery processes. Given that the share of EAF in steel production is expected to increase the application potential of the technology will be limited. On the other hand, the long lifetime of the technology and the expected capacity increase of EAF makes scrap preheating a justified energy saving option. This paper would present the results of the assessment of the above mentioned options in terms of the costs and GHG mitigation potential.

Keywords: Iron and Steel Sectors, Energy Efficiency Improvement, Blast Furnace Iron-making Process, GHG Mitigation

Procedia PDF Downloads 396

Authors: M. Martín-Morales, D. Eliche-Quesada, L. Pérez-Villarejo, M. Zamorano

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Olive oil is a product of particular importance within the Mediterranean and Spanish agricultural food system, and more specifically in Andalusia, owing to be the world's main production area. Olive oil processing generates olive stones which are dried and cleaned to remove pulp and olive stones fines to produce biofuel characterized to have high energy efficiency in combustion processes. Olive stones fine fraction is not too much appreciated as biofuel, so it is important the study of alternative solutions to be valorized. Some researchers have studied recycling different waste to produce ceramic bricks. The main objective of this study is to investigate the effects of olive stones addition on the properties of fired clay bricks for building construction. Olive stones were substituted by volume (7.5%, 15%, and 25%) to brick raw material in three different sizes (lower than 1 mm, lower than 2 mm and between 1 and 2 mm). In order to obtain comparable results, a series without olive stones was also prepared. The prepared mixtures were compacted in laboratory type extrusion under a pressure of 2.5MPa for rectangular shaped (30 mm x 60 mm x 10 mm). Dried and fired industrial conditions were applied to obtain laboratory brick samples. Mass loss after sintering, bulk density, porosity, water absorption and compressive strength of fired samples were investigated and compared with a sample manufactured without biomass. Results obtained have shown that olive stone addition decreased mechanical properties due to the increase in water absorption, although values tested satisfied the requirements in EN 772-1 about methods of test for masonry units (Part 1: Determination of compressive strength). Finally, important advantages related to the properties of bricks as well as their environmental effects could be obtained with the use of biomass studied to produce ceramic bricks. The increasing of the percentage of olive stones incorporated decreased bulk density and then increased the porosity of bricks. On the one hand, this lower density supposes a weight reduction of bricks to be transported, handled as well as the lightening of building; on the other hand, biomass in clay contributes to auto thermal combustion which involves lower fuel consumption during firing step. Consequently, the production of porous clay bricks using olive stones could reduce atmospheric emissions and improve their life cycle assessment, producing eco-friendly clay bricks.

Keywords: clay bricks, olive stones, sustainability, valorization

Procedia PDF Downloads 152

Authors: Kwedi L. M. Nsah, Hisao Uchiki

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Quantum computation is a new and exciting field making use of quantum mechanical phenomena. In classical computers, information is represented as bits, with values either 0 or 1, but a quantum computer uses quantum bits in an arbitrary superposition of 0 and 1, enabling it to reach beyond the limits predicted by classical information theory. lanthanide ion quantum computer is an organic crystal, having a lanthanide ion. Europium is a favored lanthanide, since it exhibits nuclear spin coherence times, and Eu(III) is photo-stable and has two stable isotopes. In a europium organic crystal, the key factor is the mutual dipole-dipole interaction between two europium atoms. Crystals of the complex were formed by making a 2 :1 reaction of Eu(fod)3 and bpm. The transparent white crystals formed showed brilliant red luminescence with a 405 nm laser. The photoluminescence spectroscopy was observed both at room and cryogenic temperatures (300-14 K). The luminescence spectrum of [Eu(fod)3(μ-bpm) Eu(fod)3] showed characteristic of Eu(III) emission transitions in the range 570–630 nm, due to the deactivation of 5D0 emissive state to 7Fj. For the application of dinuclear Eu3+ complex to q-bit device, attention was focused on 5D0 -7F0 transition, around 580 nm. The presence of 5D0 -7F0 transition at room temperature revealed that at least one europium symmetry had no inversion center. Since the line was unsplit by the crystal field effect, any multiplicity observed was due to a multiplicity of Eu3+ sites. For q-bit element, more narrow line width of 5D0 → 7F0 PL band in Eu3+ ion was preferable. Cryogenic temperatures (300 K – 14 K) was applicable to reduce inhomogeneous broadening and distinguish between ions. A CCD image sensor was used for low temperature Photoluminescence measurement, and a far better resolved luminescent spectrum was gotten by cooling the complex at 14 K. A red shift by 15 cm-1 in the 5D0 - 7F0 peak position was observed upon cooling, the line shifted towards lower wavenumber. An emission spectrum at the 5D0 - 7F0 transition region was obtained to verify the line width. At this temperature, a peak with magnitude three times that at room temperature was observed. The temperature change of the 5D0 state of Eu(fod)3(μ-bpm)Eu(fod)3 showed a strong dependence in the vicinity of 60 K to 100 K. Thermal quenching was observed at higher temperatures than 100 K, at which point it began to decrease slowly with increasing temperature. The temperature quenching effect of Eu3+ with increase temperature was caused by energy migration. 100 K was the appropriate temperature for the observation of the 5D0 - 7F0 emission peak. Europium dinuclear complex bridged by bpm was successfully prepared and monitored at cryogenic temperatures. At 100 K the Eu3+-dope complex has a good thermal stability and this temperature is appropriate for the observation of the 5D0 - 7F0 emission peak. Sintering the sample above 600o C could also be a method to consider but the Eu3+ ion can be reduced to Eu2+, reasons why cryogenic temperature measurement is preferably over other methods.

Keywords: Eu(fod)₃, europium dinuclear complex, europium ion, quantum bit, quantum computer, 2, 2-bipyrimidine

Procedia PDF Downloads 180

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

Procedia PDF Downloads 182

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 177

Authors: T. Kuchukhidze, N. Jalagonia, T. Archuadze, G. Bokuchava

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The growing scientific-technological progress in modern civilization causes actuality of producing construction materials which can successfully work in conditions of high temperature, radiation, pressure, speed, and chemically aggressive environment. Such extreme conditions can withstand very few types of materials and among them, ceramic materials are in the first place. Corundum ceramics is the most useful material for creation of constructive nodes and products of various purposes for its low cost, easy accessibility to raw materials and good combination of physical-chemical properties. However, ceramic composite materials have one disadvantage; they are less plastics and have lower toughness. In order to increase the plasticity, the ceramics are reinforced by various dopants, that reduces the growth of the cracks. It is shown, that adding of even small amount of carbon fibers and carbon nanotubes (CNT) as reinforcing material significantly improves mechanical properties of the products, keeping at the same time advantages of alundum ceramics. Graphene in composite material acts in the same way as inorganic dopants (MgO, ZrO2, SiC and others) and performs the role of aluminum oxide inhibitor, as it creates shell, that gives possibility to reduce sintering temperature and at the same time it acts as damper, because scattering of a shock wave takes place on carbon structures. Application of different structural modification of carbon (graphene, nanotube and others) as reinforced material, gives possibility to create multi-purpose highly requested composite materials based on alundum ceramics. In the present work offers simplified technology for obtaining of aluminum oxide ceramics, reinforced with carbon nanostructures, during which chemical modification with doping carbon nanostructures will be implemented in the process of synthesis of final powdery composite – Alumina. In charge doping carbon nanostructures connected to matrix substance with C-O-Al bonds, that provide their homogeneous spatial distribution. In ceramic obtained as a result of consolidation of such powders carbon fragments equally distributed in the entire matrix of aluminum oxide, that cause increase of bending strength and crack-resistance. The proposed way to prepare the charge simplifies the technological process, decreases energy consumption, synthesis duration and therefore requires less financial expenses. In the implementation of this work, modern instrumental methods were used: electronic and optical microscopy, X-ray structural and granulometric analysis, UV, IR, and Raman spectroscopy.

Keywords: ceramic materials, α-Al₂O₃, carbon nanostructures, composites, characterization, hot-pressing

Procedia PDF Downloads 119

Authors: Chen Yuan, Nick Green, Stuart Blackburn

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The investment casting process offers a great freedom of design combined with the economic advantage of near net shape manufacturing. It is widely used for the production of high value precision cast parts in particularly in the aerospace sector. Various combinations of materials have been used to produce the ceramic moulds, but most investment foundries use a silica based binder system in conjunction with fused silica, zircon, and alumino-silicate refractories as both filler and coarse stucco materials. However, in the context of advancing alloy technologies, silica based systems are struggling to keep pace, especially when net-shape casting titanium alloys. Study has shown that the casting of titanium based alloys presents considerable problems, including the extensive interactions between the metal and refractory, and the majority of metal-mould interaction is due to reduction of silica, present as binder and filler phases, by titanium in the molten state. Cleaner, more refractory systems are being devised to accommodate these changes. Although yttria has excellent chemical inertness to titanium alloy, it is not very practical in a production environment combining high material cost, short slurry life, and poor sintering properties. There needs to be a cost effective solution to these issues. With limited options for using pure oxides, in this work, a silica-free magnesia spinel MgAl₂O₄ was used as a primary coat filler and alumina as a binder material to produce facecoat in the investment casting mould. A comparison system was also studied with a fraction of the rare earth oxide Y₂O₃ adding into the filler to increase the inertness. The stability of the MgAl₂O₄/Al₂O₃ and MgAl₂O₄/Y₂O₃/Al₂O₃ slurries was assessed by tests, including pH, viscosity, zeta-potential and plate weight measurement, and mould properties such as friability were also measured. The interaction between the face coat and titanium alloy was studied by both a flash re-melting technique and a centrifugal investment casting method. The interaction products between metal and mould were characterized using x-ray diffraction (XRD), scanning electron microscopy (SEM) and Energy Dispersive X-Ray Spectroscopy (EDS). The depth of the oxygen hardened layer was evaluated by micro hardness measurement. Results reveal that introducing a fraction of Y₂O₃ into magnesia spinel can significantly increase the slurry life and reduce the thickness of hardened layer during centrifugal casting.

Keywords: titanium alloy, mould, MgAl₂O₄, Y₂O₃, interaction, investment casting

Procedia PDF Downloads 113

Authors: Burçak Boztemur, Yue Xu, Laima Luo, M. Lütfi Öveçoğlu, Duygu Ağaoğulları

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Tungsten (W) is used chiefly as plasma-facing material. However, it has some problems, such as brittleness after plasma exposure. High-entropy alloys (RHEAs) are a new opportunity for this deficiency. So, the neutron shielding behavior of WNbMoVTa and WNbMoVTaCr₀.₅Al compositions were examined against He⁺ irradiation in this study. The mechanical and irradiation properties of the WNbMoVTa base composition were investigated by adding the Al and Cr elements. The mechanical alloying (MA) for 6 hours was applied to obtain RHEA powders. According to the X-ray diffraction (XRD) method, the body-centered cubic (BCC) phase and NbTa phase with a small amount of WC impurity that comes from vials and balls were determined after 6 h MA. Also, RHEA powders were consolidated with the spark plasma sintering (SPS) method (1500 ºC, 30 MPa, and 10 min). After the SPS method, (Nb,Ta)C and W₂C₀.₈₅ phases were obtained with the decomposition of WC and stearic acid that is added during MA based on XRD results. Also, the BCC phase was obtained for both samples. While the Al₂O₃ phase with a small intensity was seen for the WNbMoVTaCr₀.₅Al sample, the Ta₂VO₆ phase was determined for the base sample. These phases were observed as three different regions according to scanning electron microscopy (SEM). All elements were distributed homogeneously on the white region by measuring an electron probe micro-analyzer (EPMA) coupled with a wavelength dispersive spectroscope (WDS). Also, the grey region of the WNbMoVTa sample was rich in Ta, V, and O elements. However, the amount of Al and O elements was higher for the grey region of the WNbMoVTaCr₀.₅Al sample. The high amount of Nb, Ta, and C elements were determined for both samples. Archimedes’ densities that were measured with alcohol media were closer to the theoretical densities of RHEAs. These values were important for the microhardness and irradiation resistance of compositions. While the Vickers microhardness value of the WNbMoVTa sample was measured as ~11 GPa, this value increased to nearly 13 GPa with the WNbMoVTaCr₀.₅Al sample. These values were compatible with the wear behavior. The wear volume loss was decreased to 0.16×10⁻⁴ from 1.25×10⁻⁴ mm³ by the addition of Al and Cr elements to the WNbMoVTa. The He⁺ irradiation was conducted on the samples to observe surface damage. After irradiation, the XRD patterns were shifted to the left because of defects and dislocations. He⁺ ions were infused under the surface, so they created the lattice expansion. The peak shifting of the WNbMoVTaCr₀.₅Al sample was less than the WNbMoVTa base sample, thanks to less impact. A small amount of fuzz was observed for the base sample. This structure was removed and transformed into a wavy structure with the addition of Cr and Al elements. Also, the deformation hardening was actualized after irradiation. A lower amount of hardening was obtained with the WNbMoVTaCr₀.₅Al sample based on the changing microhardness values. The surface deformation was decreased in the WNbMoVTaCr₀.₅Al sample.

Keywords: refractory high entropy alloy, microhardness, wear resistance, He⁺ irradiation

Procedia PDF Downloads 65

Authors: Milos Beran, Josef Drahorad, Ondrej Vltavsky, Martin Fronek, Jiri Sova

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While most nanofibers are produced using electrospinning, this technique suffers from several drawbacks, such as the requirement for specialized equipment, high electrical potential, and electrically conductive targets. Consequently, recent years have seen the increasing emergence of novel strategies in generating nanofibers in a larger scale and higher throughput manner. The centrifugal spinning is simple, cheap and highly productive technology for nanofiber production. In principle, the drawing of solution filament into nanofibers using centrifugal spinning is achieved through the controlled manipulation of centrifugal force, viscoelasticity, and mass transfer characteristics of the spinning solutions. Engineering efforts of researches of the Food research institute Prague and the Czech Technical University in the field the centrifugal nozzleless spinning led to introduction of a pilot plant demonstrator NANOCENT. The main advantages of the demonstrator are lower investment cost - thanks to simpler construction compared to widely used electrospinning equipments, higher production speed, new application possibilities and easy maintenance. The centrifugal nozzleless spinning is especially suitable to produce submicron fibers from polymeric solutions in highly volatile solvents, such as chloroform, DCM, THF, or acetone. To date, submicron fibers have been prepared from PS, PUR and biodegradable polyesters, such as PHB, PLA, PCL, or PBS. The products are in form of 3D structures or nanofiber membranes. Unique self-supporting nanofiber membranes were prepared from the biodegradable polyesters in different mixtures. The nanofiber membranes have been tested for different applications. Filtration efficiencies for water solutions and aerosols in air were evaluated. Different active inserts were added to the solutions before the spinning process, such as inorganic nanoparticles, organic precursors of metal oxides, antimicrobial and wound healing compounds or photocatalytic phthalocyanines. Sintering can be subsequently carried out to remove the polymeric material and transfer the organic precursors to metal oxides, such as Si02, or photocatalytic Zn02 and Ti02, to obtain inorganic nanofibers. Electrospinning is more suitable technology to produce membranes for the filtration applications than the centrifugal nozzleless spinning, because of the formation of more homogenous nanofiber layers and fibers with smaller diameters. The self-supporting nanofiber membranes prepared from the biodegradable polyesters are especially suitable for medical applications, such as wound or burn healing dressings or tissue engineering scaffolds. This work was supported by the research grants TH03020466 of the Technology Agency of the Czech Republic.

Keywords: polymeric nanofibers, self-supporting nanofiber membranes, biodegradable polyesters, active inserts

Procedia PDF Downloads 165

Authors: Alessio Varotto, Lorenzo Freschi, Umberto Pasqual Laverdura, Anastasia Moschovi, Davide Pumiglia, Iakovos Yakoumis, Marta Feroci, Maria Luisa Grilli

Abstract:

Dry reforming of Methane (DRM) is considered one of the most valuable technologies for green-house gas valorization thanks to the fact that through this reaction, it is possible to obtain syngas, a mixture of H₂ and CO in an H₂/CO ratio suitable for utilization in the Fischer-Tropsch process of high value-added chemicals and fuels. Challenges of the DRM process are the reduction of costs due to the high temperature of the process and the high cost of precious metals of the catalyst, the metal particles sintering, and carbon deposition on the catalysts’ surface. The aim of this study is to demonstrate the feasibility of the synthesis of catalysts using a leachate solution containing Pt coming directly from the recovery of spent diesel oxidation catalysts (DOCs) without further purification. An unusual perovskite support for DRM, the BaCe₁₋ₓ₋ᵧZrₓGdᵧO₃ (BCZG) perovskite, has been chosen as the catalyst support because of its high thermal stability and capability to produce oxygen vacancies, which suppress the carbon deposition and enhance the catalytic activity of the catalyst. BCZG perovskite has been synthesized by a sol-gel modified Pechini process and calcinated in air at 1100 °C. BCZG supports have been impregnated with a Pt-containing leachate solution of DOC, obtained by a mild hydrometallurgical recovery process, as reported elsewhere by some of the authors of this manuscript. For comparison reasons, a synthetic solution obtained by digesting commercial Pt-black powder in aqua regia was used for BCZG support impregnation. Pt nominal content was 2% in both BCZG-based catalysts formed by real and synthetic solutions. The structure and morphology of catalysts were characterized by X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). Thermogravimetric Analysis (TGA) was used to study the thermal stability of the catalyst’s samples. Brunauer-Emmett-Teller (BET) analysis provided a high surface area of the catalysts. H₂-TPR (Temperature Programmed Reduction) analysis was used to study the consumption of hydrogen for reducibility, and it was associated with H₂-TPD characterization to study the dispersion of Pt on the surface of the support and calculate the number of active sites used by the precious metal. Dry reforming of methane (DRM) reaction, carried out in a fixed bed reactor, showed a high conversion efficiency of CO₂ and CH4. At 850°C, CO₂ and CH₄ conversion were close to 100% for the catalyst obtained with the aqua regia-based solution of commercial Pt-black, and ~70% (for CH₄) and ~80 % (for CO₂) in the case of real HCl-based leachate solution. H₂/CO ratios were ~0.9 and ~0.70 in the first and latter cases, respectively. As far as we know, this is the first pioneering work in which a BCGZ catalyst and a real Pt-containing leachate solution were successfully employed for DRM reaction.

Keywords: dry reforming of methane, perovskite, PGM, recycled Pt, syngas

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Authors: Anastasia Beketova, Emmanouil-George C. Tzanakakis, Ioannis G. Tzoutzas, Eleana Kontonasaki

Abstract:

In restorative dentistry, yttria-stabilized zirconia (YSZ) nanoparticles can be applied as fillers to improve the mechanical properties of various resin-based materials. Using sol-gel based synthesis as simple and cost-effective method, nano-sized YSZ particles with high purity can be produced. The aim of this study was to synthesize YSZ nanoparticles by the Pechini sol-gel method at different temperatures and to investigate their composition, structure, and morphology. YSZ nanopowders were synthesized by the sol-gel method using zirconium oxychloride octahydrate (ZrOCl₂.8H₂O) and yttrium nitrate hexahydrate (Y(NO₃)₃.6H₂O) as precursors with the addition of acid chelating agents to control hydrolysis and gelation reactions. The obtained powders underwent TG_DTA analysis and were sintered at three different temperatures: 800, 1000, and 1200°C for 2 hours. Their composition and morphology were investigated by Fourier Transform Infrared Spectroscopy (FTIR), X-Ray Diffraction Analysis (XRD), Scanning Electron Microscopy with associated with Energy Dispersive X-ray analyzer (SEM-EDX), Transmission Electron Microscopy (TEM) methods, and Dynamic Light Scattering (DLS). FTIR and XRD analysis showed the presence of pure tetragonal phase in the composition of nanopowders. By increasing the calcination temperature, the crystallinity of materials increased, reaching 47.2 nm for the YSZ1200 specimens. SEM analysis at high magnifications and DLS analysis showed submicron-sized particles with good dispersion and low agglomeration, which increased in size as the sintering temperature was elevated. From the TEM images of the YSZ1000 specimen, it can be seen that zirconia nanoparticles are uniform in size and shape and attain an average particle size of about 50 nm. The electron diffraction patterns clearly revealed ring patterns of polycrystalline tetragonal zirconia phase. Pure YSZ nanopowders have been successfully synthesized by the sol-gel method at different temperatures. Their size is small, and uniform, allowing their incorporation of dental luting resin cements to improve their mechanical properties and possibly enhance the bond strength of demanding dental ceramics such as zirconia to the tooth structure. This research is co-financed by Greece and the European Union (European Social Fund- ESF) through the Operational Programme 'Human Resources Development, Education and Lifelong Learning 2014- 2020' in the context of the project 'Development of zirconia adhesion cements with stabilized zirconia nanoparticles: physicochemical properties and bond strength under aging conditions' (MIS 5047876).

Keywords: dental cements, nanoparticles, sol-gel, yttria-stabilized zirconia, YSZ

Procedia PDF Downloads 147

Authors: D. Varadaradjou, H. Kebir, J. Mespoulet, D. Tingaud, S. Bouvier, P. Deconick, K. Ameyama, G. Dirras

Abstract:

The development of new architecture metallic alloys with controlled microstructures is one of the strategic ways for designing materials with high innovation potential and, particularly, with improved mechanical properties as required for structural materials. Indeed, unlike conventional counterparts, metallic materials having so-called harmonic structure displays strength and ductility synergy. The latter occurs due to a unique microstructure design: a coarse grain structure surrounded by a 3D continuous network of ultra-fine grain known as “core” and “shell,” respectively. In the present study, pure harmonic-structured (HS) Nickel samples were processed via controlled mechanical milling and followed by spark plasma sintering (SPS). The present work aims at characterizing the mechanical properties of HS pure Nickel under room temperature dynamic loading through a Split Hopkinson Pressure Bar (SHPB) test and the underlying microstructure evolution. A stopper ring was used to maintain the strain at a fixed value of about 20%. Five samples (named B1 to B5) were impacted using different striker bar velocities from 14 m/s to 28 m/s, yielding strain rate in the range 4000-7000 s-1. Results were considered until a 10% deformation value, which is the deformation threshold for the constant strain rate assumption. The non-deformed (INIT – post-SPS process) and post-SHPB microstructure (B1 to B5) were investigated by EBSD. It was observed that while the strain rate is increased, the average grain size within the core decreases. An in-depth analysis of grains and grain boundaries was made to highlight the thermal (such as dynamic recrystallization) or mechanical (such as grains fragmentation by dislocation) contribution within the “core” and “shell.” One of the most widely used methods for determining the dynamic behavior of materials is the SHPB technique developed by Kolsky. A 3D simulation of the SHPB test was created through ABAQUS in dynamic explicit. This 3D simulation allows taking into account all modes of vibration. An inverse approach was used to identify the material parameters from the equation of Johnson-Cook (JC) by minimizing the difference between the numerical and experimental data. The JC’s parameters were identified using B1 and B5 samples configurations. Predictively, identified parameters of JC’s equation shows good result for the other sample configuration. Furthermore, mean rise of temperature within the harmonic Nickel sample can be obtained through ABAQUS and show an elevation of about 35°C for all fives samples. At this temperature, a thermal mechanism cannot be activated. Therefore, grains fragmentation within the core is mainly due to mechanical phenomena for a fixed final strain of 20%.

Keywords: 3D simulation, fragmentation, harmonic structure, high strain rate, Johnson-cook model, microstructure

Procedia PDF Downloads 231