Search results for: scanning electron microscope (SEM)

Authors: Maryam Kiani

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The aim of this study was to investigate the influence of carbon black additive on the properties of fly ash-based geopolymer. The geopolymer samples were prepared using fly ash as the primary source material, along with an alkali activator solution and different concentrations of carbon black additive. The effects of carbon black on the geopolymer binder were evaluated by analyzing the compressive strength, flexural strength, water absorption, and microstructural properties of the cured samples. The results revealed that the inclusion of carbon black additive significantly enhanced the mechanical properties of the geopolymer binder. The compressive and flexural strengths were found to increase with the addition of carbon black, showing improvements of up to 25% and 15%, respectively. Moreover, the water absorption of the geopolymer samples reduced due to the presence of carbon black, indicating improved resistance against water permeability. Microstructural analysis using scanning electron microscopy (SEM) revealed a more compact and homogenous structure in the geopolymer samples with carbon black. The dispersion of carbon black particles within the geopolymer matrix was observed, suggesting improved interparticle bonding and increased densification. Overall, this study demonstrates the positive impact of carbon black additive on the qualities of fly ash-based geopolymer, emphasizing its potential as an effective enhancer for geopolymer binder applications.

Keywords: fly-ash, carbon black, nanotechnology, geopolymer

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Authors: Ryan Brisbin, Hassan Harb, Justin Debow, Hrant Hratchian, Ryan Baxter

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Donor-Acceptor (DA) frameworks are crucial parts of any technology requiring charge transport. This type of behavior is ubiquitous across technologies from semi conductors to solar panels. Currently, most DA systems involve metallic components, but progressive research is being pursued to design fully organic DA systems to be used as both organic semi-conductors and light emitting diodes. These systems are currently comprised of conductive polymers and salts. However, little is known about the effect of various physical aspects (size, torsional angle, electron density) have on the act of reversible charge transfer. Herein, the effect of torsional angle on reductive stability in bis(imino)pyridines is analyzed using a combination of single crystal analysis and electro-chemical peak current ratios from cyclic voltammetry. The computed free energies of reduction and electron attachment points were also investigated through density functional theory and natural ionization orbital theory to gain greater understanding of the global effect torsional angles have on electron transfer in bis(imino)pyridines. Findings indicated that torsional angles are a multi-variable parameter affected by both local steric constraints and resonant electronic contributions. Local steric impacted torsional angles demonstrated a negligible effect on electrochemical reversibility, while resonant affected torsional angles were observed to significantly alter the electrochemical reversibility.

Keywords: cyclic voltammetry, bis(imino)pyridines, structure-activity relationship, torsional angles

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Authors: Gabriel K. Nzulu, Hans Högberg, Per Eklund, Lars Hultman, Martin Magnuson

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X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDX) are applied to investigate the properties of rock samples from a drill hole from the Kubi Gold Project of the Asante Gold Corporation near Dunwka-on-Offin in the Central Region of Ghana. The distribution of these minerals in the rocks were observed in the drill hole sections. X-ray diffraction indicates that the samples contain garnet, pyrite, periclase, and quartz as the main indicator minerals. SEM revealed morphologies of these minerals. From EDX and XPS, Fe, Mg, Al, S, O, Hg, Ti, Mn, Na, Ag, Au, Cu, Si, and K are identified as the pathfinder elements in the area that either form alloys with gold or inherent elements in the sediments. This finding can be ascribed to primary geochemical distribution, which developed from crystallization of magma and hydrothermal liquids as well as the movement of metasomatic elements and the precipitous rate of chemical weathering of lateralization in secondary processes. The results indicate that Au mineralization in the Kubi Mine area is controlled by garnet, pyrite, goethite, and kaolinite that grades up to the surface (oxides) with hematite and limonite alterations.

Keywords: gold, minerals, pathfinder element, spectroscopy, X-ray

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Authors: Rayan B. M. Ameen, Ian P. Jones, Yu Lung Chiu

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Single alpha-beta colony micro-pillars have been manufactured from a polycrystalline commercial Ti-6Al-4V sample using Focused Ion Beam (FIB). Each pillar contained two alpha lamellae separated by a thin fillet of beta phase. A nano-indenter was then used to conduct uniaxial micro-compression tests on Ti alloy single crystals, using a diamond flat tip as a compression platen. By controlling the crystal orientation along the micro-pillar using Electron back scattering diffraction (EBSD) different slip systems have been selectively activated. The advantage of the micro-compression method over conventional mechanical testing techniques is the ability to localize a single crystal volume which is characterizable after deformation. By matching the stress-strain relations resulting from micro-compression experiments to TEM (Transmission Electron Microscopy) studies of slip transmission mechanisms through the α-β interfaces, some proper constitutive material parameters such as the role of these interfaces in determining yield, strain-hardening behaviour, initial dislocation density and the critical resolved shear stress are suggested.

Keywords: α/β-Ti alloy, focused ion beam, micro-mechanical test, nano-indentation, transmission electron diffraction, plastic flow

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Authors: Raghvendra Singh Yadav, Ivo Kuřitka, Jarmila Vilcakova, Pavel Urbanek, Michal Machovsky, David Skoda

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In this report, the impact of Gd³⁺ substitution in ZnFe₂O₄ spinel ferrite nanoparticles on structural, optical and magnetic properties was investigated. ZnFe₂₋ₓGdₓO₄ (x=0.00, 0.05, 0.10, 0.15, 0.20) nanoparticles were synthesized by honey-mediated sol-gel combustion method. X-ray diffraction, Raman Spectroscopy and Fourier Transform Infrared Spectroscopy confirmed the formation of cubic spinel ferrite crystal structure. The morphology and elemental analysis were studied using field emission scanning electron microscopy (FE-SEM) and energy dispersive X-ray spectroscopy, respectively. UV-Visible reflectance spectroscopy revealed band gap variation with concentration of Gd³⁺ substitution in ZnFe₂O₄ nanoparticles. Magnetic property was studied using vibrating sample magnetometer at room temperature. The synthesized spinel ferrite nanoparticles showed ferromagnetic behaviour. The evaluated magnetic parameters such as saturation magnetization, coercivity and remanence showed variation with Gd³⁺ substitution in spinel ferrite nanoparticles. This work was supported by the Ministry of Education, Youth and Sports of the Czech Republic – Program NPU I (LO1504).

Keywords: sol-gel combustion method, nanoparticles, magnetic property, optical property

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Authors: Glauco M. M. M. Lustosa, João Paulo C. Costa, Leinig Antônio Perazolli, Maria Aparecida Zaghete

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SnO2 has electrical conductivity due to the excess of electrons and structural defects, being its electrical behavior highly dependent on sintering temperature and chemical composition. The addition of metals modifiers into the crystalline structure can improve and controlling the behavior of some semiconductor oxides that can therefore develop different applications such as varistors (ceramic with non-ohmic behavior between current and voltage, i.e. conductive during normal operation and resistive during overvoltage). The polymeric precursor method, based on the complexation reaction between metal ion and policarboxylic acid and then polymerized with ethylene glycol, was used to obtain nanopowders ceramic. The metal immobilization reduces its segregation during the decomposition of the polyester resulting in a crystalline oxide with high chemical homogeneity. The preparation of films from ceramics nanoparticles using electrophoretic deposition method (EPD) brings prospects for a new generation of smaller size devices with easy integration technology. EPD allows to control time and current and therefore it can have control of the thickness, surface roughness and the film density, quickly and with low production costs. The sintering process is key to control size and grain boundary density of the film. In this step, there is the diffusion of metals that promote densification and control of intrinsic defects or change these defects which will form and modify the potential barrier in the grain boundary. The use of microwave oven for sintering is an advantageous process due to the fast and homogeneous heating rate, promoting the diffusion and densification without irregular grain growth. This research was done a comparative study of sintering temperature by use of zinc as modifier agent to verify the influence on sintering step aiming to promote densification and grain growth, which influences the potential barrier formation and then changed the electrical behavior. SnO2-nanoparticles were obtained with 1 %mol of ZnO + 0.05 %mol of Nb2O5 (SZN), deposited as film through EPD (voltage 2 kV, time of 10 min) on Si/Pt substrate. Sintering was made in a microwave oven at 800, 900 and 1000 °C. For complete coverage of the substrate by nanoparticles with low surface roughness and uniform thickness was added 0.02 g of solid iodine in alcoholic suspension SnO2 to increase particle surface charge. They were also used magneto in EPD system that improved the deposition rate forming a compact film. Using a scanning electron microscope of high resolution (SEM_FEG) it was observed nanoparticles with average size between 10-20 nm, after sintering the average size was 150 to 200 nm and thickness of 5 µm. Also, it was verified that the temperature at 1000 °C was the most efficient in sintering. The best sintering time was also recorded and determined as 40 minutes. After sintering, the films were recovered with Cr3+ ions layer by EPD, then the films were again thermally treated. The electrical characterizations (nonlinear coefficient of 11.4, voltage rupture of ~60 V and leakage current = 4.8x10−6 A), allow considering the new methodology suitable for prepare SnO2-based varistor applied for development of electrical protection devices for low voltage.

Keywords: chemical synthesis, electrophoretic deposition, microwave sintering, tin dioxide

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Authors: Folorunso Omoniyi, Peter Olubambi, Rotimi Sadiku

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Thermal barrier coating (TBC) system is used in both aero engines and other gas turbines to offer oxidation protection to superalloy substrate component. In the present work, it shows the ability of a new fabrication technique to develop rapidly new coating composition and microstructure. The compact powders were prepared by Powder Metallurgy method involving powder mixing and the bond coat was synthesized through the application of Spark Plasma Sintering (SPS) at 10500C to produce a fully dense (97%) NiCrAl bulk samples. The influence of sintering temperature on the hardness of NiCrAl, done by Micro Vickers hardness tester, was investigated. And Oxidation test was carried out at 1100oC for 20h, 40h, and 100h. The resulting coat was characterized with optical microscopy, scanning electron microscopy (SEM), energy dispersive x-ray analysis (EDAX) and x-ray diffraction (XRD). Micro XRD analysis after the oxidation test revealed the formation of protective oxides and non-protective oxides.

Keywords: high-temperature oxidation, powder metallurgy, spark plasma sintering, thermal barrier coating

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Authors: Said Sair, Hanane Ait Ousaleh, Ilyas Belghazi, Othmane Amadine

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Plastic waste has become a major environmental issue, driving the need for innovative solutions to convert it into valuable resources. This study explores the catalytic pyrolysis of plastic waste to produce hydrogen, using zeolite catalysts as a key component in the process. Various zeolites, including types X, A, and P, are synthesized and characterized through X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), Brunauer–Emmett–Teller (BET) surface area analysis, thermogravimetric analysis (TGA), and scanning electron microscopy (SEM). These techniques are employed to assess the structural and chemical properties of the catalysts. Catalytic pyrolysis experiments are performed under different conditions, including variations in temperature, catalyst loading, and reaction time, to optimize hydrogen production. The results demonstrate that the choice of zeolite catalyst significantly impacts plastic waste conversion efficiency into hydrogen. This research contributes to advancing circular economy principles by providing an effective method for plastic waste management and clean energy production, promoting environmental sustainability.

Keywords: hydrogen production, plastic waste, zeolite catalysts, catalytic pyrolysis, circular economy, sustainable energy

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Authors: J. Ptačinová, J. Ďurica, P. Jurči, M Kusý

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Ledeburitic tool steel Vanadis 6 has been subjected to sub-zero treatment (SZT) at -140 °C and -196 °C, for different durations up to 48 h. The microstructure and hardness have been examined with reference to the same material after room temperature quenching, by using the light microscopy, scanning electron microscopy, X-ray diffraction, and Vickers hardness testing method. The microstructure of the material consists of the martensitic matrix with certain amount of retained austenite, and of several types of carbides – eutectic carbides, secondary carbides, and small globular carbides. SZT reduces the retained austenite amount – this is more effective at -196 °C than at -140 °C. Alternatively, the amount of small globular carbides increases more rapidly after SZT at -140 °C than after the treatment at -140 °C. The hardness of sub-zero treated material is higher than that of conventionally treated steel when tempered at low temperature. Compressive hydrostatic stresses are developed in the retained austenite due to the application of SZT, as a result of more complete martensitic transformation. This is also why the population density of small globular carbides is substantially increased due to the SZT. In contrast, the hardness of sub-zero treated samples decreases more rapidly compared to that of conventionally treated steel, and in addition, sub-zero treated material induces a loss the secondary hardening peak.

Keywords: microstructure, Vanadis 6 tool steel, sub-zero treatment, carbides

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Authors: Sumara Khursheed, Jitendra Sharma

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The present work reports synthesis of nanocomposites (NCs) of phosphor (KCaVO4:Sm3+) embedded poly(methylmethacrylate) (PMMA) using solution casting method and their optical properties measurements for their possible application in making flexible luminescent films. X-ray diffraction analyses were employed to obtain the structural parameters as crystallinity, shape and size of the obtained NCs. The emission and excitation spectra were obtained using Photoluminescence spectroscopy to quantify the spectral properties of these fluorescent polymer/phosphor films. Optical energy gap has been estimated using UV-VIS spectroscopy while differential scanning calorimetry (DSC) was exploited to measure the thermal properties of the NC films in terms of their thermal stability, glass transition temperature and degree of crystallinity etc.

Keywords: nanocomposites, luminescence, XRD, differential scanning calorimetry, PMMA

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Authors: Najme lari, Shahrokh Ahangarani, Ali Shanaghi

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Nanostructure silica antireflective surfaces were fabricated on glasses by Sol-Gel technique. Various silica sols (varying in composition: tetraethyl orthosilicate (TEOS) concentration and Triton additive) were synthesized by the polymeric process and then subsequently coated on substrates. Silica thin films were investigated by using UV-Visible Spectroscopy; Fourier-Transformed Infrared Spectrophotometer and Filed Emission Scanning Electron Microscopy were used. Results indicated that dense silica layers, obtained from the polymeric method, permit a considerable reduction of these light reflections compared with uncoated glasses in all the cases studied, but the degree of reduction is different depending on the composition of the precursor solution. It was found that the transmittance increased from 0.915 for the bare slide up to 0.96 for the best made sample corresponding to the Triton-doped silica. The addition of Triton x-100 to the silica sols improved the optical property of thin film because of it helps to create nanoporous in the coating. Also the results showed SiO2 content is an effective parameter to prepare the antireflective films. Loss of SiO2 cause to rapid the reactions and Si-O-Si bonding form better under this condition.

Keywords: sol–gel, silica thin films, antireflective coatings, optical properties, triton

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Authors: A. Abdikian

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Using the linearized quantum hydrodynamic model (QHD) and by considering the role of quantum parameter (Bohm’s potential) and electron exchange-correlation potential in conjunction with Maxwell’s equations, electromagnetic wave propagation in a single-walled carbon nanotubes was studied. The electronic excitations are described. By solving the mentioned equations with appropriate boundary conditions and by assuming the low-frequency electromagnetic waves, two general expressions of dispersion relations are derived for the transverse magnetic (TM) and transverse electric (TE) modes, respectively. The dispersion relations are analyzed numerically and it was found that the dependency of dispersion curves with the exchange-correlation effects (which have been ignored in previous works) in the low frequency would be limited. Moreover, it has been realized that asymptotic behaviors of the TE and TM modes are similar in single wall carbon nanotubes (SWCNTs). The results show that by adding the function of electron exchange-correlation potential lead to the phenomena and make to extend the validity range of QHD model. The results can be important in the study of collective phenomena in nanostructures.

Keywords: transverse magnetic, transverse electric, quantum hydrodynamic model, electron exchange-correlation potential, single-wall carbon nanotubes

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Authors: Norica Godja, Andreas Schindel, Luka Payrits, Zsolt Pasztor, Bálint Hegedüs, Petr Homola, Jan Horňas, Jiří Běhal, Roman Ruzek, Martin Holzleitner, Sascha Senck

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In order to reduce fuel consumption and CO₂ emissions in the aviation sector, innovative solutions are being sought to reduce the weight of aircraft, including additive manufacturing (AM). Of particular importance are the excellent mechanical properties that are required for aircraft structures. Ti6Al4V alloys, with their high mechanical properties in relation to weight, can reduce the weight of aircraft structures compared to structures made of steel and aluminium. Currently, conventional processes such as casting and CNC machining are used to obtain the desired structures, resulting in high raw material removal, which in turn leads to higher costs and impacts the environment. Additive manufacturing (AM) offers advantages in terms of weight, lead time, design, and functionality and enables the realisation of alternative geometric shapes with high mechanical properties. However, there are currently technological shortcomings that have led to AM not being approved for structural components with high safety requirements. An assessment of damage tolerance for AM parts is required, and quality control needs to be improved. Pores and other defects cannot be completely avoided at present, but they should be kept to a minimum during manufacture. The mechanical properties of the manufactured parts can be further improved by various treatments. The influence of different treatment methods (heat treatment, CNC milling, electropolishing, chemical polishing) and operating parameters were investigated by scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM/EDX), X-ray diffraction (XRD), electron backscatter diffraction (EBSD) and measurements with a focused ion beam (FIB), taking into account surface roughness, possible anomalies in the chemical composition of the surface and possible cracks. The results of the characterisation of the constructed and treated samples are discussed and presented in this paper. These results were generated within the framework of the 3TANIUM project, which is financed by EU with the contract number 101007830.

Keywords: Ti6Al4V alloys, laser powder bed fusion, damage tolerance, heat treatment, electropolishing, potential cracking

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Authors: A. Threepanich, S. Youngme, P. Praipipat

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Although ground egg shells had the ability to eliminate lead in water, their efficiency may decrease in a case of contaminating of other cations such as Na⁺, Ca²⁺ in the water. The development of ground egg shells may solve this problem in which metal oxides are a good choice for this case since they have the ability to remove any heavy metals including lead in the water. Therefore, this study attempts to use this advantage for improving ground egg shells for the specific lead removal efficiency in the water. X-ray fluorescence (XRF) technique was used for the chemical element contents analysis of ground egg shells (GES) and ground egg shells with metal oxide (GESM), and Transmission electron microscope (TEM) technique was used to examine the material sizes. The batch test studies were designed to investigate the factor effects on dose (5, 10, 15 grams), pH (5, 7, 9), and settling time (1, 3, 5 hours) for the lead removal efficiency in the water. The XRF analysis results showed GES contained calcium (Ca) 91.41% and Silicon (Si) 4.03% and GESM contained calcium (Ca) 91.41%, Silicon (Si) 4.03%, and Iron (Fe) 3.05%. TEM results confirmed the sizes of GES and GESM in the range of 1-20 nm. The batch test studies showed the best optimum conditions for the lead removal in the water of GES and GESM in dose, pH, and settling time were 10 grams, pH 9, 5 hours and 5 grams, pH 9, 3 hours, respectively. The competing ions (Na⁺ and Ca²⁺) study reported GESM had the higher % lead removal efficiency than GES at 90% and 60%, respectively. Therefore, this result can confirm that adding of metal oxide to ground egg shells helps to improve the lead removal efficiency in the water.

Keywords: nano material, ground egg shells, metal oxide, lead

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Authors: Kashif Jabbar

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Milk adulteration is a global concern, and the current study was plan to synthesize Selenium nanoparticles by green method using plant extract of garlic, Allium Sativum, and to characterize Selenium nanoparticles through different analytical techniques and to apply Selenium nanoparticles as fast and easy technique for the detection of salicylic acid in milk. The highly selective, sensitive, and quick interference green synthesis-based sensing of possible milk adulterants i.e., salicylic acid, has been reported here. Salicylic acid interacts with nanoparticles through strong bonding interactions, hence resulting in an interruption within the formation of selenium nanoparticles which is confirmed by UV-VIS spectroscopy, scanning electron microscopy, and x-ray diffraction. This interaction in the synthesis of nanoparticles resulted in transmittance wavelength that decrease with the increasing amount of salicylic acid, showing strong binding of selenium nanoparticles with adulterant, thereby permitting in-situ fast detection of salicylic acid from milk having a limit of detection at 10-3 mol and linear coefficient correlation of 0.9907. Conclusively, it can be draw that colloidal selenium could be synthesize successfully by garlic extract in order to serve as a probe for fast and cheap testing of milk adulteration.

Keywords: adulteration, green synthesis, selenium nanoparticles, salicylic acid, aggregation

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Authors: Abhisek Sinha, Debobrata Rajak, Shilpa Rani, Ram Gopal, Vandana Sharma

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The interaction of femtosecond laser pulses with metallic tips has been studied extensively, and they have proved to be a very good source of ultrashort electron pulses. A study of the interaction of femtosecond Laguerre-Gaussian (LG) laser modes with Tungsten tips is presented here. Laser pulses of 35 fs pulse durations were incident on Tungsten tips, and their electron emission rates were studied for LG (l=1, p=0) and Gaussian modes. A change in the order of the interaction for LG beams is reported, and the difference in the order of interaction is attributed to ponderomotive shifts in the energy levels corresponding to the enhanced near-field intensity supported by numerical simulations.

Keywords: femtosecond, Laguerre-Gaussian, OAM, tip

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Authors: A. Achour L. Chekour, A. Mekroud

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Tribology, the science of lubrication, friction and wear, plays an important role in science "crossroads" initiated by the recent developments in the industry. Its multidisciplinary nature reinforces its scientific interest. It covers all the sciences that deal with the contact between two solids loaded and relative motion. It is thus one of the many intersections more clearly established disciplines such as solid mechanics and the fluids, rheological, thermal, materials science and chemistry. As for his experimental approach, it is based on the physical and processing signals and images. The optimization of operating conditions by cutting tool must contribute significantly to the development and productivity of advanced automation of machining techniques because their implementation requires sufficient knowledge of how the process and in particular the evolution of tool wear. In addition, technological advances have developed the use of very hard materials, refractory difficult machinability, requiring highly resistant materials tools. In this study, we present the behavior wear a machining tool during the roughing operation according to the cutting parameters. The interpretation of the experimental results is based mainly on observations and analyzes of sharp edges e tool using the latest techniques: scanning electron microscopy (SEM) and optical rugosimetry laser beam.

Keywords: friction, wear, tool, cutting

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Authors: Mohamed Sifan, Brabha Nagaratnam, Julian Thamboo, Keerthan Poologanathan

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Ultra high performance concrete (UHPC) is a type of cementitious material known for its exceptional strength, ductility, and durability. However, its production is often associated with high costs due to the significant amount of cementitious materials required and the use of fine powders to achieve the desired strength. The aim of this research is to explore the feasibility of developing cost-effective UHPC mixes using locally available materials. Specifically, the study aims to investigate the use of coarse limestone sand along with other sand types, namely, basalt sand, dolomite sand, and river sand for developing UHPC mixes and evaluating its performances. The study utilises the particle packing model to develop various UHPC mixes. The particle packing model involves optimising the combination of coarse limestone sand, basalt sand, dolomite sand, and river sand to achieve the desired properties of UHPC. The developed UHPC mixes are then evaluated based on their workability (measured through slump flow and mini slump value), compressive strength (at 7, 28, and 90 days), splitting tensile strength, and microstructural characteristics analysed through scanning electron microscope (SEM) analysis. The results of this study demonstrate that cost-effective UHPC mixes can be developed using locally available materials without the need for silica fume or fly ash. The UHPC mixes achieved impressive compressive strengths of up to 149 MPa at 28 days with a cement content of approximately 750 kg/m³. The mixes also exhibited varying levels of workability, with slump flow values ranging from 550 to 850 mm. Additionally, the inclusion of coarse limestone sand in the mixes effectively reduced the demand for superplasticizer and served as a filler material. By exploring the use of coarse limestone sand and other sand types, this study provides valuable insights into optimising the particle packing model for UHPC production. The findings highlight the potential to reduce costs associated with UHPC production without compromising its strength and durability. The study collected data on the workability, compressive strength, splitting tensile strength, and microstructural characteristics of the developed UHPC mixes. Workability was measured using slump flow and mini slump tests, while compressive strength and splitting tensile strength were assessed at different curing periods. Microstructural characteristics were analysed through SEM and energy dispersive X-ray spectroscopy (EDS) analysis. The collected data were then analysed and interpreted to evaluate the performance and properties of the UHPC mixes. The research successfully demonstrates the feasibility of developing cost-effective UHPC mixes using locally available materials. The inclusion of coarse limestone sand, in combination with other sand types, shows promising results in achieving high compressive strengths and satisfactory workability. The findings suggest that the use of the particle packing model can optimise the combination of materials and reduce the reliance on expensive additives such as silica fume and fly ash. This research provides valuable insights for researchers and construction practitioners aiming to develop cost-effective UHPC mixes using readily available materials and an optimised particle packing approach.

Keywords: cost-effective, limestone powder, particle packing model, ultra high performance concrete

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Authors: Ane Escobar, Paula Angelomé, Mihaela Delcea, Marek Grzelczak, Sergio Enrique Moya

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The antibacterial capacity of bone-anchoring implants can be improved by the use of antibiotics that can be delivered to the media after the surgery. Mesoporous films have shown great potential in drug delivery for orthopedic applications, since pore size and thickness can be tuned to produce different surface area and free volume inside the material. This work shows the synthesis of mesoporous titania films (MTF) by sol-gel chemistry and evaporation-induced self-assembly (EISA) on top of glass substrates. Pores with a diameter of 12nm were observed by Transmission Electron Microscopy (TEM). A film thickness of 100 nm was measured by Scanning Electron Microscopy (SEM). Gentamicin was used to study the antibiotic delivery from the film by means of High-performance liquid chromatography (HPLC). The Staphilococcus aureus strand was used to evaluate the effectiveness of the penicillin loaded films toward inhibiting bacterial colonization. MC3T3-E1 pre-osteoblast cell proliferation experiments proved that MTFs have a good biocompatibility and are a suitable surface for MC3T3-E1 cell proliferation. Moreover, images taken by Confocal Fluorescence Microscopy using labeled vinculin, showed good adhesion of the MC3T3-E1 cells to the MTFs, as well as complex actin filaments arrangement. In order to improve cell proliferation Bone Morphogenetic Protein-2 (BMP-2) was adsorbed on top of the mesoporous film. The deposition of the protein was proved by measurements in the contact angle, showing an increment in the hydrophobicity while the protein concentration is higher. By measuring the dehydrogenase activity in MC3T3-E1 cells cultured in dually functionalized mesoporous titatina films with gentamicin and BMP-2 is possible to find an improvement in cell proliferation. For this purpose, the absorption of a yellow-color formazan dye, product of a water-soluble salt (WST-8) reduction by the dehydrogenases, is measured. In summary, this study proves that by means of the surface modification of MTFs with proteins and loading of gentamicin is possible to achieve an antibacterial effect and a cell growth improvement.

Keywords: antibacterial, biocompatibility, bone morphogenetic protein-2, cell proliferation, gentamicin, implants, mesoporous titania films, osteoblasts

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Authors: Sharifah Nabihah Syed Jaafar, Umar Adli Amran, Rasidi Roslan, Chia Chin Hua, Sarani Zakaria

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Bio-composites derived from plant fiber and bio-derived polymer, are likely more ecofriendly and demonstrate competitive performance with petroleum based. In this research, the green phenolic resin was used as a matrix and oil palm empty fruit bunch fiber (EFB) was used as filler. The matrix was synthesized from soda lignin, phenol and hydrochloric acid as a catalyst. The phenolic resin was synthesized via liquefaction and condensation to enhance the combination of phenol during the process. Later, the phenolic resin was mixed with EFB by using mechanical stirrer and was molded with hot press at 180 oC. In this research, the composites were prepared with EFB content of 5%, 10%, 15% and 20%. The samples that viewed under scanning electron microscopy (SEM) showed that the EFB filler remained embedded in the resin. From impact and hardness testing, samples 10% of EFB showed the optimum properties meanwhile sample 15% showed the optimum properties for flexural testing. Thermal stability of the composites was investigated using thermogravimetric (TGA) analysis and found that the weight loss and the activation energy (Ea) of the composites samples were decreased as the filler content increased.

Keywords: EFB, liquefaction, phenol formaldehyde, lignin

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Authors: Sharan K. Indrakar, Aakash B. Prasad, Arash Takshi, Sesha Srinivasan, Elias K. Stefanakos

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In this work, we present an exclusive study on the effect of the feeding ratio of polyaniline-based redox-active gel layer on electrical and optical properties of innovative electrochromic devices (ECs). An electrochromic device consisting of polyaniline (PANI) has a redox-active gel electrolyte placed between two conducting transparent fluorine-doped tin oxide glass substrates. The redox-active composite gel is a mixture of different concentrations of aniline (monomer), a water-soluble polymer poly (vinyl alcohol), hydrochloric acid, and an oxidant. The EC device shows the color change from dark green to transparent for the applied potential between -0.5 V to +2.0 V. The coloration and decoloration of the ECs were tested for electrochemical behavior using techniques such as cyclic voltammetry (CV), chronoamperometry (CA), and electrochemical impedance spectroscopy (EIS). The optical transparency of the EC devices was examined at two different biasing voltage conditions under UV-visible spectroscopic technique; the result showed 65% transmittance at 564 nm and zero transmittance when the cell was biased at 0.0 V and 2.0 V, the synthesized mol fraction gel was analyzed for surface morphology and structural properties by scanning electron microscopy and Fourier transformer spectroscopy.

Keywords: electrochromic, gel electrolyte, polyaniline, conducting polymer

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Authors: Shahin A. Abdel-Naby, James P. Colgan, Michael S. Pindzola

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A time-dependent close-coupling method is developed to calculate a total, double and triple autoionization rates for hollow atomic ions of four-electron systems. This work was motivated by recent observations of the four-electron Auger process in near K-edge photoionization of C+ ions. The time-dependent close-coupled equations are solved using lattice techniques to obtain a discrete representation of radial wave functions and all operators on a four-dimensional grid with uniform spacing. Initial excited states are obtained by relaxation of the Schrodinger equation in imaginary time using a Schmidt orthogonalization method involving interior subshells. The radial wave function grids are partitioned over the cores on a massively parallel computer, which is essential due to the large memory requirements needed to store the coupled-wave functions and the long run times needed to reach the convergence of the ionization process. Total, double, and triple autoionization rates are obtained by the propagation of the time-dependent close-coupled equations in real-time using integration over bound and continuum single-particle states. These states are generated by matrix diagonalization of one-electron Hamiltonians. The total autoionization rates for each L excited state is found to be slightly above the single autoionization rate for the excited configuration using configuration-average distorted-wave theory. As expected, we find the double and triple autoionization rates to be much smaller than the total autoionization rates. Future work can be extended to study electron-impact triple ionization of atoms or ions. The work was supported in part by grants from the American University of Sharjah and the US Department of Energy. Computational work was carried out at the National Energy Research Scientific Computing Center (NERSC) in Berkeley, California, USA.

Keywords: hollow atoms, autoionization, auger rates, time-dependent close-coupling method

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Authors: Edgar Ochoa, G. Torres-Villasenor

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Superplastic deformation is shown by materials with a fine grain size, usually less than 10 μm, when they are deformed within the strain rate range 10-5 10-1 s-1 at temperatures greater than 0.5Tm, where Tm is the melting point in Kelvin. According to the constitutive equation for superplastic flow, refinement of the grain size would be expected to increase the optimum strain rate and decrease the temperature required for superplastic flow. Ribbons of eutectic Ag-Cu and Bi-Cd alloys were manufactured by using a single roller melt-spinning technique to obtain a fine grain structure for later test in superplastic regime. The eutectics ribbons were examined by scanning electron microscopy and X-Ray diffraction, and the grain size was determined using the image analysis software ImageJ. The average grain size was less than 1 μm. Tensile tests were carried out from 10-4 to 10-1 s-1, at room temperature, to evaluate the superplastic behavior. The largest deformation was shown by the Bi-Cd eutectic ribbons, Ɛ=140 %, despite that these ribbons have a hexagonal unit cell. On the other hand, Ag-Cu eutectic ribbons have a minor grain size and cube unit cell, however they showed a lower deformation in tensile test under the same conditions than Bi-Cd ribbons. This is because the Ag-Cu grew in a strong cube-cube orientation relationship.

Keywords: eutectic ribbon, fine grain, superplastic deformation, cube-cube orientation

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Authors: Benalia Kouini, Aicha Serier

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This work aims to investigate the structure–property relationship in ternary nanocomposites consisting of polypropylene as the matrix, polyamide 66 as the minor phase and treated nanoclay DELLITE 67G as the reinforcement. All PP/PA66/Nanoclay systems with polypropylene grafted maleic anhydride PP-g-MAH as a compatibilizer were prepared via melt compounding and characterized in terms of nanoclay content. Morphological structure was investigated by scanning electron microscopy. The rheological behavior of the nanocomposites was determined by various methods, viz melt flow index (MFI) and parallel plate rheological measurements. The PP/PP-g-MAH/PA66 nanocomposites showed a homogeneous morphology supporting the compatibility improvement between PP, PA66 and nanoclay. SEM results revealed the formation of nanocomposites as the nanoclay was intercalated and exfoliated. In the ternary nanocomposites, the rheological behavior showed that, the complex viscosity is increased with increasing the nanoclay content; however, at low frequencies this increase is governed by the content of nanofiller while at high frequencies it is mainly determined by talc content. A similar trend was also observed for the variations of storage modulus (G′) and loss modulus (G″) with frequency. The results showed that the use of nanoclay considerably affects the melt elasticity.

Keywords: nanocomposites, polypropylene, polyamide66, modified nanoclay, rheology

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Authors: Warda Nasir, M. N. S. Qureshi

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Whistler waves are right handed circularly polarized waves and are frequently observed in space plasmas. The Low frequency branch of the Whistler waves having frequencies nearly around 100 Hz, known as Lion roars, are frequently observed in magnetosheath. Another feature of the magnetosheath is the observations of flat top electron distributions with single as well as two electron populations. In the past, lion roars were studied by employing kinetic model using classical bi-Maxwellian distribution function, however, could not be justified both on quantitatively as well as qualitatively grounds. We studied Whistler waves by employing kinetic model using non-Maxwellian distribution function such as the generalized (r,q) distribution function which is the generalized form of kappa and Maxwellian distribution functions by employing kinetic theory with single or two electron populations. We compare our results with the Cluster observations and found good quantitative and qualitative agreement between them. At times when lion roars are observed (not observed) in the data and bi-Maxwellian could not provide the sufficient growth (damping) rates, we showed that when generalized (r,q) distribution function is employed, the resulted growth (damping) rates exactly match the observations.

Keywords: kinetic model, whistler waves, non-maxwellian distribution function, space plasmas

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Authors: M. J. Shivaram, Shashi Bhushan Arya, Jagannath Nayak, Bharat Bhooshan Panigrahi

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Titanium and its alloys have become more significant implant materials due to their mechanical properties, excellent biocompatibility and high corrosion resistance. Biomaterials can be produce by using the powder metallurgy (PM) methods and required properties can tailored by varying the processing parameters, such as ball milling time, space holder particles, and sintering temperature. The desired properties such as, structural and mechanical properties can be obtained by powder metallurgy method.  In the present study, deals with fabrication of solid and porous Ti-20Nb-5Ag alloy using high energy ball milling for different times (5 and 20 h). The resultant powder particles were used to fabricate solid and porous Ti-20Nb-5Ag alloy by adding space holder particles (NH₄HCO₃). The resultant powder particles, fabricated solid and porous samples were characterized by scanning electron microscopy (SEM). The compressive strength, elastic modulus and microhardness properties were investigated. Solid and porous Ti-20Nb-5Ag alloy samples showed good mechanical properties for 20 h ball milling time as compare to 5 h ball milling.

Keywords: ball milling, compressive strengths, microstructure, porous titanium alloy

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Authors: Sara Scolari, Davide Mombelli, Gianluca Dall'Osto, Jasna Kastivnik, Gašper Tavčar, Carlo Mapelli

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The EIT Raw Materials RIS-DustRec-II project aims to transform Electric Arc Furnace Dust (EAFD) into a valuable resource by overcoming the challenges associated with traditional recycling approaches. EAFD, a zinc-rich industrial by-product typically recycled by the Waelz process, contains complex oxides such as franklinite (ZnFe₂O₄), which hinder the efficient extraction of zinc, by also introducing other valuable elements (Fe, Ni, Cr, Cu, …) in the slag. The project aims to develop a multistage multidisciplinary approach to separate EAFD into two streams: a magnetic and non-magnetic one. In this paper the production of self-reducing briquettes from the magnetic stream of EAFD with a reducing agent, aiming to drive carbothermic reduction and recover iron as a usable alloy, was investigated. Research was focused on optimizing the magnetic and subsequent gravimetric separation (MGS) processes, followed by high-temperature smelting to evaluate reduction efficiency and phase separation. The characterization of selected two different raw EAFD samples and their magnetic-gravitational separation to isolate zinc- and iron-rich fractions was performed by X-ray diffraction and scanning electron microscope. The iron-enriched concentrates were then agglomerated into self-reducing briquettes by mixing them with either biochar (olive pomace pyrolyzed at 350 and 750°C and wood chips pyrolyzed at 750 °C) and a Cupola Furnace dust as reducing agents, combined with gelatinized corn starch as a binder. Cylindrical briquettes were produced and cured for 14 days to ensure structural integrity during subsequent thermal treatments. Smelting tests were carried out at 1400 °C in an inert argon atmosphere to assess the metallization efficiency and the separation between metal and slag phases. A carbon/oxides mass ratio of 0.262 (C/(ZnO+Fe₂O₃)) was used in these tests to maintain continuity with previous studies and to standardize reduction conditions. The magnetic and gravimetric separations effectively isolated zinc- and iron-enriched fractions, particularly for one of the two EAFD, where the concentration of Zn in the concentration fraction was reduced by 8 wt.% while Fe reached 45 wt.%. The reduction tests conducted at 1400 °C showed that the chosen carbon/oxides ratio was sufficient for the smelting of the reducible oxides within the briquettes. However, an important limitation became apparent: the amount of carbon, exceeding the stochiometric value, proved to be excessive for the effective coalescence of metal droplets, preventing clear metal-slag separation. To address this, further smelting tests were carried out in an air atmosphere rather than inert conditions to burn off excess carbon. This paper demonstrates the potential of controlled carbothermic reduction for EAFD recycling. By carefully optimizing the C/(ZnO+Fe₂O₃) ratio, the process can maximize metal recovery while achieving better separation of the metal and slag phases. This approach offers a promising alternative to traditional EAFD recycling methods, with further studies recommended to refine the parameters for industrial application.

Keywords: biochars, electrical arc furnace dust, metallization, smelting

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Authors: Tomáš Dyk, Stanislav Procházka, Martin Drahanský

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The article proposes a new algorithm for detecting damaged areas of the tank barrel based on the image of the inner surface of the tank barrel. Damage position is calculated using image processing techniques such as edge detection, discrete wavelet transformation and image segmentation for accurate contour detection. The algorithm can detect surface damage in smoothbore and even in rifled tank barrels. The algorithm also calculates the volume of the detected damage from the depth map generated, for example, from the distance measurement unit. The proposed method was tested on data obtained by a tank barrel scanning device, which generates both surface image data and depth map. The article also discusses tank barrel scanning devices and how damaged surface impacts material resistance.

Keywords: barrel, barrel diagnostic, image processing, surface damage detection, tank

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Authors: Afifa Hafidh, Fathi Touati, Ahmed Hichem Hamzaoui, Sayda Somrani

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The objective of the present study has been to synthesize and to characterize silica hybrid materials using sol-gel technic and to investigate their properties. Silica materials were successfully fabricated using various bi-functional 1,3,4-thiadiazoles and tetraethoxysilane (TEOS) as co-precursors via a facile one-pot sol-gel pathway. TEOS was introduced at room temperature with 1,3,4-thiadiazole 2,5-difunctiunal adducts, in ethanol as solvent and using HCl acid as catalyst. The sol-gel process lead to the formation of monolithic, coloured and transparent gels. TEOS was used as a principal network forming agent. The incorporation of 1,3,4-thiadiazole molecules was realized by attachment of these later onto a silica matrix. This allowed covalent linkage between organic and inorganic phases and lead to the formation of Si-N and Si-S bonds. The prepared hybrid materials were characterized by Fourier transform infrared, NMR ²⁹Si and ¹³C, scanning electron microscopy and nitrogen absorption-desorption measurements. The optic and magnetic properties of hybrids are studied respectively by ultra violet-visible spectroscopy and electron paramagnetic resonance. It was shown in this work, that heterocyclic moieties were successfully attached in the hybrid skeleton. The formation of the Si-network composed of cyclic units (Q3 structures) connected by oxygen bridges (Q4 structures) was proved by ²⁹Si NMR spectroscopy. The Brunauer-Elmet-Teller nitrogen adsorption-desorption method shows that all the prepared xerogels have isotherms type IV and are mesoporous solids. The specific surface area and pore volume of these materials are important. The obtained results show that all materials are paramagnetic semiconductors. The data obtained by Nuclear magnetic resonance ²⁹Si and Fourier transform infrared spectroscopy, show that Si-OH and Si-NH groups existing in silica hybrids can participate in adsorption interactions. The obtained materials containing reactive centers could exhibit adsorption properties of metal ions due to the presence of OH and NH functionality in the mesoporous frame work. Our design of a simple method to prepare hybrid materials may give interest of the development of mesoporous hybrid systems and their use within the domain of environment in the future.

Keywords: hybrid materials, sol-gel process, 1, 3, 4-thiadaizole, TEOS

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Authors: Tatsuhiko Aizawa, Yohei Suzuki, Tomomi Shiratori

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The austenitic stainless steel type AISI316 has been widely utilized as structural members and mold die substrates. The low temperature plasma nitriding has been utilized to harden these AISI316 members, parts, and dies without loss of intrinsic corrosion resistance to AISI316 stainless steels. Formation of CrN precipitates by normal plasma nitriding processes resulted in severe deterioration of corrosion toughness. Most previous studies on this low temperature nitriding of AISI316 only described the lattice expansion of original AISI316 lattices by the occupation of nitrogen interstitial solutes into octahedral vacancy sites, the significant hardening by nitrogen solid solution, and the enhancement of corrosion toughness. In addition to those engineering items, this low temperature nitriding process was characterized by the nitrogen supersaturation and nitrogen diffusion processes. The nitrogen supersaturated zones expanded by the nitrogen solute occupation to octahedral vacancy sites, and the un-nitrided surroundings to these zones were plastically strained to compensate for the mismatch strains across these nitrided and nitrided zones. The microstructure of nitrided AISI316 was refined by this plastic straining. The nitrogen diffusion process was enhanced to transport nitrogen solute atoms through the refined zone boundaries. This synergetic collaboration among the nitrogen supersaturation, the lattice expansion, the plastic straining, and the grain refinement yielded a thick nitrogen supersaturated layer. This synergetic relation was also characterized by the multilevel two-phase structuring. In XRD (X-Ray Diffraction) analysis, the nitrided AISI316 layer had - and -phases with the peak shifts from original lattices. After EBSD (Electron Back Scattering Diffraction) analysis, -grains and -grains homogeneously distributed in the nitrided layer. The scanning transmission electron microscopy (STEM) revealed that g-phase zone is N-poor cluster and a-phase zone is N-rich cluster. This proves that nitrogen supersaturated AISI316 stainless steels have multi-level two-phase structure in a very fine granular system.

Keywords: AISI316 stainless steels, chemical affinity to nitrogen solutes, multi-level two-phase structuring, nitrogen supersaturation

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