Search results for: powder x-ray diffraction

Authors: Ayla Roberta Galaco, Juliana Fonseca De Lima, Osvaldo Antonio Serra

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Coordination polymers, also known as metal-organic frameworks (MOFs) or lanthanoide organic frameworks (LOFs) have been reported due of their promising applications in gas storage, separation, catalysis, luminescence, magnetism, drug delivery, and so on. As a type of organic–inorganic hybrid materials, the properties of coordination polymers could be chosen by deliberately selecting the organic and inorganic components. LOFs have received considerable attention because of their properties such as porosity, luminescence, and magnetism. Methods such as solvothermal synthesis are important as a strategy to control the structural and morphological properties as well as the composition of the target compounds. In this work the first solvothermal synthesis was employed to obtain the compound [Y0.4,Yb0.4,Er0.2(dmf)(for)(H2O)(tft)], by using terephthalic acid (tft) and oxalic acid, decomposed in formate (for), as ligands; Yttrium, Ytterbium and, Erbium as metal centers, in DMF and water for 4 days under 160 °C. The semi-rigid terephthalic acid (dicarboxylic) coordinates with Ln3+ ions and also is possible to form a polyfunctional bridge. On the other hand, oxalate anion has no high-energy vibrational groups, which benefits the excitation of Yb3+ in upconversion process. It was observed that the compounds with water molecules in the coordination sphere of the lanthanoide ions cause lower crystalline properties and change the structure of the LOF (1D, 2D, 3D). In the FTIR, the bands at 1589 and 1500 cm-1 correspond to the asymmetric stretching vibration of –COO. The band at 1383 cm-1 is assigned to the symmetric stretching vibration of –COO. Single crystal X-ray diffraction study reveals an infinite 3D coordination framework that crystalizes in space group P21/c. The other three products, [TR(chel)(ofd)0,5(H2O)2], where TR= Eu3+, Y3, and Yb3+/Er3+ were obtained by using 1, 2-phenylenedioxydiacetic acid (ofd) and chelidonic acid (chel) as organic ligands. Thermal analysis shows that the lanthanoide organic frameworks do not collapse at temperatures below 250 °C. By the polycrystalline X-ray diffraction patterns (PXRD) it was observed that the compounds with Eu3+, Y3+, and Yb3+/Er3+ ions are isostructural. From PXRD patterns, high crystallinity can be noticed for the complexes. The final products were characterized by single X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), energy dispersive spectroscopy (EDS) and thermogravimetric analysis (TGA). The X-ray diffraction (XRD) is an effective method to investigate crystalline properties of synthesized materials. The solid crystal obtained in the synthesis show peaks at 2θ < 10°, indicating the MOF formation. The chemical composition of LOFs was also confirmed by EDS.

Keywords: isostructural, lanthanoids, lanthanoids organic frameworks (LOFs), metal organic frameworks (MOFs), thermogravimetry, X-Ray diffraction

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Authors: Khalid H. Abass

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Al-Ni-Cr alloy contains different ratios of Ni and Cr was prepared by mixing Al, Ni and Cr at 800oC under an argon atmosphere. The prepared alloys were heated for 1300 hr to 560oC, and then cooled rapidly by water at the ambient temperature. Surface morphology for alloys is studied by scanning electron microscope (SEM). The resultant homogeneous surface is a result of heat treatment. The X-ray diffraction patterns showed (111), (200), and (220) diffraction lines from cubic Al crystal structure, and suggested that the intensity of peak (111) orientation is predominant. Three binary phases were observed and grown in alloys: Al3Ni (Orthorhombic, a = 6.598Ǻ, b = 7.352 Ǻ, c = 4.802 Ǻ), Cr9Al17 (Rhombohedra, a = 12.910 Ǻ, c = 15.677), and Ni2Cr3 (Tetragonal, a = 8.82 Ǻ, c = 4.58 Ǻ). The average crystallite sizes of the prepared samples were found to be from 3000 to 3094 nm by SEM, which is much smaller than that estimated from XRD data. Corrosion resistance increases with increasing Ni-Cr content in Al alloys. The electrical volume resistivity decreased with increasing Ni-Cr content at low frequency. This behavior can be seen generally at 50Hz, where the electrical volume resistivity reached the value of 3.98×10-8Ω.cm for the ratio Al-1.8 at.%Ni-0.18at.%Cr.

Keywords: Al-Ni-Cr alloy, corrosion current, electrical volume resistivity, binary phase, homogeneous surface

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Authors: Laura Frydel, Piotr M. Slomkiewicz, Beata Szczepanik

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Triclosan has been used as a disinfectant in many medical products, such as: hand disinfectant soaps, creams, mouthwashes, pastes and household cleaners. Due to its strong antimicrobial activity, triclosan is becoming more and more popular and the consumption of disinfectants with triclosan in it is increasing. As a result, this compound increasingly finds its way into waters and soils in an unchanged form, pollutes the environment and may have a negative effect on organisms. The aim of this study was to investigate the synthesis of cellulose-based halloysite-carbon adsorbent and perform its characterization. The template in the halloysite-carbon adsorbent was halloysite nanotubes and the carbon precursor was microcrystalline cellulose. Scanning electron microscope (SEM) images were obtained and the elementary composition (qualitative and quantitative) of the sample was determined by energy dispersion spectroscopy (EDS). The identification of the crystallographic composition of the halloysite nanotubes and the sample of the halloysite-carbon composite was carried out using the X-ray powder diffraction (XRPD) method. The FTIR spectra were acquired before and after the adsorption process in order to determine the functional groups on the adsorbent surface and confirm the interactions between adsorbent and adsorbate molecules. The parameters of the porous structure of the adsorbent, such as the specific surface area (Brunauer-Emmett-Teller method), the total pore volume and the volume of mesopores and micropores were determined. Total carbon and total organic carbon were also determined in the samples. A cellulose-based halloysite-carbon adsorbent was used to remove triclosan from water. The degree of removal of triclosan from water was approximately 90%. The results indicate that the halloysite-carbon composite can be successfully used as an effective adsorbent for removing triclosan from water.

Keywords: Adsorption, cellulose, halloysite, triclosan

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Authors: Juan Patricio Ibáñez, Exequiel López

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A method for synthesizing copper nanoparticles through an electrochemical approach is proposed, employing surfactants to stabilize the size of the newly formed nanoparticles. The electrolyte was made up of a matrix of H₂SO₄ (190 g/L) having Cu²⁺ (from 3.2 to 9.5 g/L), sodium dodecyl sulfate -SDS- (from 0.5 to 1.0 g/L) and Tween 80 (from 0 to 7.5 mL/L). Tween 80 was used in a molar relation of 1 to 1 with SDS. A glass cell was used, which was in a thermostatic water bath to keep the system temperature, and the electrodes were cathodic copper as an anode and stainless steel 316-L as a cathode. This process was influenced by the control exerted through the initial copper concentration in the electrolyte and the applied current density. Copper nanoparticles of electrolytic purity, exhibiting a spherical morphology of varying sizes with low dispersion, were successfully produced, contingent upon the chemical composition of the electrolyte and current density. The minimum size achieved was 3.0 nm ± 0.9 nm, with an average standard deviation of 2.2 nm throughout the entire process. The deposited copper mass ranged from 0.394 g to 1.848 g per hour (over an area of 25 cm²), accompanied by an average Faradaic efficiency of 30.8% and an average specific energy consumption of 4.4 kWh/kg. The chemical analysis of the product employed X-ray powder diffraction (XRD), while physical characteristics such as size and morphology were assessed using atomic force microscopy (AFM). It was identified that the initial concentration of copper and the current density are the variables defining the size and dispersion of the nanoparticles, as they serve as reactants in the cathodic half-reaction. The presence of surfactants stabilizes the nanoparticle size as their molecules adsorb onto the nanoparticle surface, forming a thick barrier that prevents mass transfer with the exterior and halts further growth.

Keywords: copper nanopowder, electrochemical synthesis, current density, surfactant stabilizer

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Authors: S. Boudali, A. M. Soliman, B. Abdulsalam, K. Ayed, D. E. Kerdal, S. Poncet

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This study investigates the potential of using crushed concrete as aggregates to produce green and sustainable concrete. Crushed concrete was sieved to powder fine recycled aggregate (PFRA) less than 80 µm and coarse recycled aggregates (CRA). Physical, mechanical, and microstructural properties for PFRA and CRA were evaluated. The effect of the additional rates of PFRA and CRA on strength development of recycled aggregate concrete (RAC) was investigated. Additionally, the characteristics of interfacial transition zone (ITZ) between cement paste and recycled aggregate were also examined. Results show that concrete mixtures made with 100% of CRA and 40% PFRA exhibited similar performance to that of the control mixture prepared with 100% natural aggregate (NA) and 40% natural pozzolan (NP). Moreover, concrete mixture incorporating recycled aggregate exhibited a slightly higher later compressive strength than that of the concrete with NA. This was confirmed by the very dense microstructure for concrete mixture incorporating recycled concrete aggregates compared to that of conventional concrete mixture.

Keywords: compressive strength, recycled concrete aggregates, microstructure, interfacial transition zone, powder fine recycled aggregate

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Authors: Zahra Bahadoran, Parvin Mirmiran, Hanieh-Sadat Ejtahed, Maryam Tohidi, Fereidoun Azizi

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Background and Aim: Broccoli sprouts, rich source of bioactive compounds specially sulforaphane (SFN), have unique functional properties. This study was conducted to investigate the possible treatment effects of high-SFN broccoli sprouts powder on metabolic and liver disorders in rats fed with high-fructose corn syrup. Methods: Thirty-two male wistar rats, pretreated with an eight-week high-fructose diet (water containing 30% fructose), were randomly allocated into three groups: Baseline control (BC), control (C) (normal diet), and BSP-diet (normal diet+5% BSP). The duration of the study was 6 weeks. Biochemical measurements, liver weight and triglyceride content were evaluated and histopathological examination of liver was performed. Results: After 6-weeks, the liver weight was significantly lower in BSP group compared to controls (13.4 g vs. 11.4 g, P<0.05). After 6 weeks, a significant decrease was observed in fasting serum glucose, total cholesterol and triglyceride levels in both experimental groups (P<0.05). Compared to controls, serum levels of HDL-C were significantly higher in BSP group. The liver TG content in BSP compared to control group was lower (14.6 vs. 16.4 mg/mg tissue). The hepatic levels of alanine aminotransferase, aspartate aminotransferase and γ-glutamyl transferase had not considerable changes in the groups after the intervention period but the level of alkaline phosphatase significantly decreased in BSP group (P<0.05). The histopathological examination of liver confirmed a decrease lobular and portal inflammation and ballooning in BSP group compared to control. Conclusion: High-SFN broccoli sprouts powder has beneficials effect on metabolic and liver changes-induced by high fructose corn syrup.

Keywords: broccoli sprouts, metabolic disorders, fatty liver, food science

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Authors: Carlos Alberto Ríos Reyes

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Traditionally, clays have been considered as one of the main problems in the flow of fluids in hydrocarbon reservoirs. However, there is not known the significance of zeolites formed from the reactivity of clays and their effect not only on the costs of operations carried out by the oil industry in the world but also on production. The present work focused on understanding the interaction between clay minerals with brines and alkaline solutions used in the oil industry. For this, a comparative study was conducted where the reaction of sedimentary rocks under laboratory conditions was examined. Original and treated rocks were examined by X-ray powder diffraction (XRPD) and Scanning Electron Microscopy (SEM) to determine the changes that these rocks underwent upon contact with fluids of variable chemical composition. As a result, zeolite Linde Type A (LTA), sodalite (SOD), and cancrinite (CAN) can be formed after experimental work, which coincided with the dissolution of kaolinite and smectite. Results reveal that the Oil Industry should invest efforts and focus its gaze to understand at the pore scale the problem that could arise as a consequence of the clay-fluid interaction in hydrocarbon reservoir rocks due to the presence of clays in their porous system, as well as the formation of zeolites, which are better hydrocarbon absorbents. These issues could be generating losses in world production. We conclude that there is a critical situation that may be occurring in the stimulation of hydrocarbon reservoirs, where real solutions are necessary not only for the formulation of more efficient and effective injection fluids but also to contribute to the improvement of production and avoid considerable losses in operating costs.

Keywords: clay minerals, zeolites, rock-fluid interaction, experimental work, reactivity

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Authors: Wegene Demisie Jima

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Leather is a durable and flexible material used for various purposes including clothing, footwear, upholstery and gloves. However, the use of leather for smart product applications is a challenge since it is electrically insulating material. Here, we report a simple method to produce conducting glove leathers using an in-situ polymerization of pyrrole. The concentrations of pyrrole, ferric chloride and anthraquinone-2-sulfonic acid sodium salt monohydrate were optimized to produce maximum conductivity in the treated leathers. The coating of polypyrrole in the treated leathers was probed using FT-IR, X-ray diffraction and electron microscopic analysis. FTIR confirms that the formation of polypyrrole on the leather surface as well as presence of prominent N-C stretching band. X-ray diffraction analysis suggests para-crystallinity in the PPy-treated leathers.We further demonstrate that the treated leathers, with maximum conductivity of 7.4 S/cm, can be used for making conductive gloves for operating touch-screen devices apart from other smart product applications.

Keywords: electrical conductivity, in-situ polymerization, pyrrole, smart product

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Authors: Ayu Dwi Hardiyanti, Bernardus Anggit Winahyu, I. Gusti Agung Ayu Sugita Sari, Lestari Sutra Simamora, I. Wayan Warmada

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The Penosogan Formation sandstone, that has Middle Miosen age, has been deemed as a reservoir potential based on sample data from sandstone outcrop in Kebakalan and Kedawung villages, Karangsambung sub-district, Kebumen Regency, Central Java. This research employs the following analytical methods; petrography, X-ray diffraction (XRD), and porosity test. Based on the presence of micritic sandstone, muddy micrite, and muddy sandstone, the Penosogan Formation sandstone has a fine-coarse granular size and middle-to-fine sorting. The composition of the sandstone is mostly made up of plagioclase, skeletal grain, and traces of micrite. The percentage of clay minerals based on petrographic analysis is 10% and appears to envelop grain, resulting enveloping grain which reduces the porosity of rocks. The porosity types as follows: interparticle, vuggy, channel, and shelter, with an equant form of cement. Moreover, the diagenesis process involves compaction, cementation, authigenic mineral growth, and dissolving due to feldspar alteration. The maturity of the reservoir can be seen through the X-ray diffraction analysis results, using ethylene glycol solution for clay minerals fraction transformed from smectite–illite. Porosity test analysis showed that the Penosogan Formation sandstones has a porosity value of 22% based on the Koeseomadinata classification, 1980. That shows high maturity is very influential for the quality of reservoirs sandstone of the Penosogan Formation.

Keywords: sandstone reservoir, Penosogan Formation, smectite, XRD

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Authors: Laura C. Loaiza, Elodie Salager, Nicolas Louvain, Athmane Boulaoued, Antonella Iadecola, Patrik Johansson, Lorenzo Stievano, Vincent Seznec, Laure Monconduit

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Lithium-ion batteries (LIBs) have an important place among energy storage devices due to their high capacity and good cyclability. However, the advancements in portable and transportation applications have extended the research towards new horizons, and today the development is hampered, e.g., by the capacity of the electrodes employed. Silicon and germanium are among the considered modern anode materials as they can undergo alloying reactions with lithium while delivering high capacities. It has been demonstrated that silicon in its highest lithiated state can deliver up to ten times more capacity than graphite (372 mAh/g): 4200 mAh/g for Li₂₂Si₅ and 3579 mAh/g for Li₁₅Si₄, respectively. On the other hand, germanium presents a capacity of 1384 mAh/g for Li₁₅Ge₄, and a better electronic conductivity and Li ion diffusivity as compared to Si. Nonetheless, the commercialization potential of Ge is limited by its cost. The synergetic effect of Si₁₋ₓGeₓ alloys has been proven, the capacity is increased compared to Ge-rich electrodes and the capacity retention is increased compared to Si-rich electrodes, but the exact performance of this type of electrodes will depend on factors like specific capacity, C-rates, cost, etc. There are several reports on various formulations of Si₁₋ₓGeₓ alloys with promising LIB anode performance with most work performed on complex nanostructures resulting from synthesis efforts implying high cost. In the present work, we studied the electrochemical mechanism of the Si₀.₅Ge₀.₅ alloy as a realistic micron-sized electrode formulation using carboxymethyl cellulose (CMC) as the binder. A combination of a large set of in situ and operando techniques were employed to investigate the structural evolution of Si₀.₅Ge₀.₅ during lithiation and delithiation processes: powder X-ray diffraction (XRD), X-ray absorption spectroscopy (XAS), Raman spectroscopy, and 7Li solid state nuclear magnetic resonance spectroscopy (NMR). The results have presented a whole view of the structural modifications induced by the lithiation/delithiation processes. The Si₀.₅Ge₀.₅ amorphization was observed at the beginning of discharge. Further lithiation induces the formation of a-Liₓ(Si/Ge) intermediates and the crystallization of Li₁₅(Si₀.₅Ge₀.₅)₄ at the end of the discharge. At really low voltages a reversible process of overlithiation and formation of Li₁₅₊δ(Si₀.₅Ge₀.₅)₄ was identified and related with a structural evolution of Li₁₅(Si₀.₅Ge₀.₅)₄. Upon charge, the c-Li₁₅(Si₀.₅Ge₀.₅)₄ was transformed into a-Liₓ(Si/Ge) intermediates. At the end of the process an amorphous phase assigned to a-SiₓGey was recovered. Thereby, it was demonstrated that Si and Ge are collectively active along the cycling process, upon discharge with the formation of a ternary Li₁₅(Si₀.₅Ge₀.₅)₄ phase (with a step of overlithiation) and upon charge with the rebuilding of the a-Si-Ge phase. This process is undoubtedly behind the enhanced performance of Si₀.₅Ge₀.₅ compared to a physical mixture of Si and Ge.

Keywords: lithium ion battery, silicon germanium anode, in situ characterization, X-Ray diffraction

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Authors: B. S. So, Y. H. Yoon, J. O. Jung, K. S. Bae

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Metal Injection Molding (MIM) is a technology that combines powder metallurgy and injection molding. Particularly, it is widely applied to the manufacture of precision mobile parts and automobile turbocharger parts because compact precision parts with complicated three-dimensional shapes that are difficult to machining are formed into a large number of finished products. The swing valve is a valve that adjusts the boost pressure of the turbocharger. Since the head portion is exposed to the harsh temperature condition of about 900 degrees in the gasoline GDI engine, it is necessary to use Inconel material with excellent heat resistance and abrasion resistance, resulting in high manufacturing cost. In this study, we developed a swing valve using a metal powder injection molding based hybrid material (Inconel 713C material with heat resistance is applied to the head part, and HK30 material with low price is applied to the rest of the body part). For this purpose, the process conditions of the metal injection molding were optimized to minimize the internal defects, and the effectiveness was confirmed by the fracture strength and fatigue test.

Keywords: hybrid metal injection molding, swing valve, turbocharger, double injection

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Authors: Abdulmajeed Dabwan, Saqib Anwar, Ali Al-Samhan

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Electron Beam Melting (EBM) is a metal powder bed-based Additive Manufacturing (AM) technology, which uses computer-controlled electron beams to create fully dense three-dimensional near-net-shaped parts from metal powder. It gives the ability to produce any complex parts directly from a computer-aided design (CAD) model without tools and dies, and with a variety of materials. However, the quality of the surface finish in EBM process has limitations to meeting the performance requirements of additively manufactured components. The aim of this study is to investigate the cutting forces induced during milling Ti6Al4V produced by EBM as well as the surface quality of the milled surfaces. The effects of cutting speed and radial depth of cut on the cutting forces, surface roughness, and surface morphology were investigated. The results indicated that the cutting speed was found to be proportional to the resultant cutting force at any cutting conditions while the surface roughness improved significantly with the increase in cutting speed and radial depth of cut.

Keywords: electron beam melting, additive manufacturing, Ti6Al4V, surface morphology

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Authors: Tarikayehu Amanuel, Abraham Mohammed

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The production of biodiesel from waste materials is becoming an increasingly important research area in the field of renewable energy. One potential waste material source is avocado, a fruit with a large seed and peel that are typically discarded after consumption. This research aims to investigate the feasibility of using avocado waste as a feedstock for the production of biodiesel. The study focuses on extracting oil from the waste material using the transesterification technique and then characterizing the properties of oil to determine its suitability for conversion to biodiesel. The study was conducted experimentally, and a maximum oil yield of 11.583% (150g of oil produced from 1.295kg of avocado waste powder) was obtained from avocado waste powder at an extraction time of 4hr. An 87% fatty acid methyl ester (biodiesel) conversion was also obtained using a methanol/oil ratio of 6:1, 1.3g NaOH, reaction time 60min, and 65°C reaction temperature. Furthermore, from 145 ml of avocado waste oil, 126.15 ml of biodiesel was produced, indicating a high percentage of conversion (87%). Conclusively, the produced biodiesel showed comparable physical and chemical characteristics to that of standard biodiesel samples considered for the study. The results of this research could help to identify a new source of biofuel production while also addressing the issue of waste disposal in the food industry.

Keywords: biodiesel, avocado, transesterification, soxhlet extraction

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Authors: A. Taoufyq, B. Bakiz, A. Benlhachemi, L. Patout, D. V. Chokouadeua, F. Guinneton, G. Nolibe, A. Lyoussi, J-R. Gavarri

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Currently, the photo catalytic reactions occurring under solar illumination have attracted worldwide attentions due to a tremendous set of environmental problems. Taking the sunlight into account, it is indispensable to develop highly effective visible-light-driver photo catalysts. Nano structured materials such as MxM’1-xWO6 system are widely studied due to its interesting piezoelectric, dielectric and catalytic properties. These materials can be used in photo catalysis technique for environmental applications, such as waste water treatments. The aim of this study was to investigate the photo catalytic activity of polycrystalline phases of bismuth tungstate of formula Bi2WO6. Polycrystalline samples were elaborated using a coprecipitation technique followed by a calcination process at different temperatures (300, 400, 600 and 900°C). The obtained polycrystalline phases have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Crystal cell parameters and cell volume depend on elaboration temperature. High-resolution electron microscopy images and image simulations, associated with X-ray diffraction data, allowed confirming the lattices and space groups Pca21. The photo catalytic activity of the as-prepared samples was studied by irradiating aqueous solutions of Rhodamine B, associated with Bi2WO6 additives having variable crystallite sizes. The photo catalytic activity of such bismuth tungstates increased as the crystallite sizes decreased. The high specific area of the photo catalytic particles obtained at 300°C seems to condition the degradation kinetics of RhB.

Keywords: Bismuth tungstate, crystallite sizes, electron microscopy, photocatalytic activity, X-ray diffraction.

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Authors: Kamel Taıbı, Abdelmadjid Rais

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Nickel–Aluminium ferrites with the general formula Ni Alx Fe2-x O4 (0 ≤ x ≤ 1) were studied using X-ray diffraction, Infra Red and Raman spectroscopy. XRD diffraction patterns and their Reitveld refinements show that all samples have a pure single-phase cubic spinel structure. From these patterns, the lattice parameters of these samples have been calculated and compared with those predicted theoretically. Most of the values were found to decrease with increasing Al content. Infra Red spectra showed two significant absorption bands. The high band corresponds to tetrahedral (A) sites and the lower band to octahedral [B] sites, thus confirming the single phase spinel structure. For all compositions, Raman spectra show the five active modes A1g + E1g + 3 T2g of the motion of O2- ions and both the A-site and B-site ions. The Raman frequencies trend with aluminium concentration show a blue shift for all modes consistent with the replacement of Fe3+ by lower mass Al3+. Composition dependence of the Raman frequency modes is discussed in relationship with the cations distribution among the A-sites and B-sites.

Keywords: Ni-Al ferrites, spinel structure, XRD, Raman spectroscopy

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Authors: Devarakonda Ramadevi, Dasari Rambabu, K. Suresh Babu, Battu Ganga Rao, Lakshmi Sirisha Kotikalapudi

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The phytochemical and biological evaluation of the whole plant of Derris scandens is belonging to the family fabaceae. The dried plant of D.scandens was procured from the tirumala. The completely dried powder of the whole plant was taken and ground to a coarse powder which was then subjected to Soxhlet extraction with hexane and chloroform successively for 36 hrs. Chloroform extract was filtered and concentrated by using rotary evaporator an about 100g extract was obtained. The chloroform extract was subjected to column chromatographed over silicagel. From the column chromatography seven compounds were isolated named as osajin, scandinone, scandenone, 4,5,7-tri hydroxy biprenyl isoflavone, derris isoflavone-A, scandenin and isoscandinone. D.scandens resulting in the isolation of seven compounds in the plant was confirmed by spectral data (1H NMR, 13C NMR, ESI-MS and FTIR). The isolated compounds were screened for antioxidant activity, antidiabetic activity, α-glucosidase (inhibitory activity) and anti-bacterial activity. The isolated seven compounds were tested for α-glucosidase inhibitory activity and antioxidant activity. All the seven compounds showed good α-glucosidase inhibitory activity and moderate antioxidant activity.

Keywords: Derris scandens, phytochemical, antioxident, antidiabetic, antibacterial activity

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Authors: Mona Mihailescu, Rebeca Tudor, Irina A. Paun, Cristian Kusko, Eugen I. Scarlat, Mihai Kusko

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Specific intensity distributions in the laser beams are required in many fields: optical communications, material processing, microscopy, optical tweezers. In optical communications, the information embedded in specific beams and the superposition of multiple beams can be used to increase the capacity of the communication channels, employing spatial modulation as an additional degree of freedom, besides already available polarization and wavelength multiplexing. In this regard, optical vortices present interest due to their potential to carry independent data which can be multiplexed at the transmitter and demultiplexed at the receiver. Also, in the literature were studied their combinations: 1) axial or perpendicular superposition of multiple optical vortices or 2) with other laser beam types: Bessel, Airy. Optical vortices, characterized by stationary ring-shape intensity and rotating phase, are achieved using computer generated holograms (CGH) obtained by simulating the interference between a tilted plane wave and a wave passing through a helical phase object. Here, we propose a method to combine information through the reunion of two CGHs. One is obtained using the helical phase distribution, characterized by its topological charge, m. The other is obtained using conical phase distribution, characterized by its radial factor, r0. Each CGH is obtained using plane wave with different tilts: km and kr for CGH generated from helical phase object and from conical phase object, respectively. These reunions of two CGHs are calculated to be phase optical elements, addressed on the liquid crystal display of a spatial light modulator, to optically process the incident beam for investigations of the diffracted intensity pattern in far field. For parallel reunion of two CGHs and high values of the ratio between km and kr, the bright ring from the first diffraction order, specific for optical vortices, is changed in an asymmetric intensity pattern: a number of circle arcs. Both diffraction orders (+1 and -1) are asymmetrical relative to each other. In different planes along the optical axis, it is observed that this asymmetric intensity pattern rotates around its centre: in the +1 diffraction order the rotation is anticlockwise and in the -1 diffraction order, the rotation is clockwise. The relation between m and r0 controls the diameter of the circle arcs and the ratio between km and kr controls the number of arcs. For perpendicular reunion of the two CGHs and low values of the ratio between km and kr, the optical vortices are multiplied and focalized in different planes, depending on the radial parameter. The first diffraction order contains information about both phase objects. It is incident on the phase masks placed at the receiver, computed using the opposite values for topological charge or for the radial parameter and displayed successively. In all, the proposed method is exploited in terms of constructive parameters, for the possibility offered by the combination of different types of beams which can be used in robust optical communications.

Keywords: asymmetrical diffraction orders, computer generated holograms, conical phase distribution, optical vortices, spatial light modulator

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Authors: Yaniv Knop, Alva Peled

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Over the past few years there has been a growing interest in the development of Portland Composite Cement, by partial replacement of the clinker with mineral additives. The motivations to reduce the clinker content are threefold: (1) Ecological - due to lower emission of CO2 to the atmosphere; (2) Economical - due to cost reduction; and (3) Scientific\Technology – improvement of performances. Among the mineral additives being used and investigated, limestone is one of the most attractive, as it is considered natural, available, and with low cost. The goal of the research is to develop green cement, by partial replacement of the clinker with limestone powder while improving the performances of the cement paste. This work studied blended cements with three limestone powder particle diameters: smaller than, larger than, and similarly sized to the clinker particle. Blended cement with limestone consisting of one particle size distribution and limestone consisting of a combination of several particle sizes were studied and compared in terms of hydration rate, hydration degree, and water demand to achieve normal consistency. The performances of these systems were also compared with that of the original cement (without added limestone). It was found that the ability to replace an active material with an inert additive, while achieving improved performances, can be obtained by increasing the packing density of the cement-based particles. This may be achieved by replacing the clinker with limestone powders having a combination of several different particle size distributions. Mathematical and physical models were developed to simulate the setting history from initial to final setting time and to predict the packing density of blended cement with limestone having different sizes and various contents. Besides the effect of limestone, as inert additive, on the packing density of the blended cement, the influence of the limestone particle size on three different chemical reactions were studied; hydration of the cement, carbonation of the calcium hydroxide and the reactivity of the limestone with the hydration reaction products. The main results and developments will be presented.

Keywords: packing density, hydration degree, limestone, blended cement

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Authors: S. B. Bansode, V. G. Wagh, R. S. Kapadnis, S. S. Kale, M. Pathan Habib

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Indium sulfide films have been deposited using chemical bath deposition onto glass and indium tin oxide coated glass substrates. The influences of different deposition parameters viz. substrate and pH have been studied. The films were characterized by different techniques with respect to their crystal structure, surface morphology and compositional property by means of X-ray diffraction, scanning electron microscopy, Energy dispersive spectroscopy and optical absorption. X-ray diffraction studies revealed that amorphous nature of the films. The scanning electron microscopy of as deposited indium sulfide film on ITO coated glass substrate shows random orientation of grains where as those on glass substrates show dumbbell shape. Optical absorption study revealed that band gap varies from 2.29 to 2.79 eV for the deposited film.

Keywords: chemical bath deposition, optical properties, structural property, Indium sulfide

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Authors: Adriana Souza M. Batista, Cláubia Pereira, Luiz O. Faria

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The irradiation of polymeric materials has received much attention because it can produce diverse changes in chemical structure and physical properties. Thus, studying the chemical and structural changes of polymers is important in practice to achieve optimal conditions for the modification of polymers. The effect of gamma irradiation on the crystalline structure of poly(vinylidene fluoride) (PVDF) has been investigated using differential scanning calorimetry (DSC) and X-ray diffraction techniques (XRD). Gamma irradiation was carried out in atmosphere air with doses between 100 kGy at 3,000 kGy with a Co-60 source. In the melting thermogram of the samples irradiated can be seen a bimodal melting endotherm is detected with two melting temperature. The lower melting temperature is attributed to melting of crystals originally present and the higher melting peak due to melting of crystals reorganized upon heat treatment. These results are consistent with those obtained by XRD technique showing increasing crystallinity with increasing irradiation dose, although the melting latent heat is decreasing.

Keywords: differential scanning calorimetry, gamma irradiation, PVDF, X-ray diffraction technique

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Authors: Tatyana T. Tabakova, Elitsa N. Kolentsova, Dimitar Y. Dimitrov, Krasimir I. Ivanov, Yordanka G. Karakirova, Petya Cv. Petrova, Georgi V. Avdeev

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The catalytic oxidation of CO and volatile organic compounds (VOCs) is considered as one of the most efficient ways to reduce harmful emissions from various chemical industries. The effectiveness of gold-based catalysts for many reactions of environmental significance was proven during the past three decades. The aim of this work was to combine the favorable features of Au and Cu-Ce mixed oxides in the design of new catalytic materials of improved efficiency and economic viability for removal of air pollutants in waste gases from formaldehyde production. Supported oxides of copper and cerium with Cu: Ce molar ratio 2:1 and 1:5 were prepared by wet impregnation of g-alumina. Gold (2 wt.%) catalysts were synthesized by a deposition-precipitation method. Catalysts characterization was carried out by texture measurements, powder X-ray diffraction, temperature programmed reduction and electron paramagnetic resonance spectroscopy. The catalytic activity in the oxidation of CO, CH₃OH and (CH₃)₂O was measured using continuous flow equipment with fixed bed reactor. Both Cu-Ce/alumina samples demonstrated similar catalytic behavior. The addition of gold caused significant enhancement of CO and methanol oxidation activity (100 % degree of CO and CH₃OH conversion at about 60 and 140 ^oC, respectively). The composition of Cu-Ce mixed oxides affected the performance of gold-based samples considerably. Gold catalyst on Cu-Ce/γ-Al₂O₃ 1:5 exhibited higher activity for CO and CH₃OH oxidation in comparison with Au on Cu-Ce/γ-Al₂O₃ 2:1. The better performance of Au/Cu-Ce 1:5 was related to the availability of highly dispersed gold particles and copper oxide clusters in close contact with ceria.

Keywords: CO and VOCs oxidation, copper oxide, Ceria, gold catalysts

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Authors: A. Javadi, H. Asad Beygi

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In line with the increasing demand for high-quality and safe food products, the present study is intended to examine the crude extract and juice of the fruit of Cucumis melo var. dudaim on tenderization of meat. Cubic pieces were selected from the biceps fermoris muscle of a five year-old female water buffalo; then, they were cut two or three hours after the buffalo was slaughtered. The selected samples were superficially exposed to the resolution obtained from the powder of the extract of Cucumis melo var. dudaim. Distilled water as a control sample and the powder of fruit extract of the mentioned plant with 0.5, 1 and 1.5 percent concentrations were experimented in the study. These samples were kept for three time spans of 2 hours, 7 and 14 days. Then, some tests were conducted on the samples both before and after cooking them. In general, with regard to the results obtained from the experiments and the investigations of the impact of time and different concentrations on the tenderization of buffalo meat, it can be argued that the time span of 2 hours and the concentration of 1.5 % can be considered as the best time and concentration for obtaining the most desirable tenderness. Also, tenderness increased in the samples kept for 7 and 14 days; however, due to the extraordinary decomposition, the samples were rather doughy and pasty.

Keywords: meat, Cucumis melo var. dudaim, tenderization, water buffalo

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Authors: Nazanin Sheibanian, Raffaella Sesana, Sedat Ozbilen

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In recent years, high-entropy alloys (HEAs) have attracted considerable attention due to their unique properties and potential applications. In this study, novel HEA coatings were prepared on Mg substrates using mechanically alloyed HEA powder feedstocks based on Al_(0.1-0.5)CoCrCuFeNi and MnCoCrCuFeNi multi-material systems. The coatings were deposited by the Cold Spray (CS) process using three different temperatures of the process gas (N2) (650°C, 750°C, and 850°C) to examine the effect of gas temperature on coating properties. In this study, Infrared Thermography (non-destructive) was examined as a possible quality control technique for HEA coatings applied to magnesium substrates. Active Thermography was employed to characterize coating properties using the thermal response of the coating. Various HEA chemical compositions and deposition temperatures have been investigated. As a part of this study, a comprehensive macro and microstructural analysis of Cold Spray (CS) HEA coatings has been conducted using macrophotography, optical microscopy, scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM+EDS), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), microhardness tests, roughness measurements, and porosity assessments. These analyses provided insight into phase identification, microstructure characterization, deposition, particle deformation behavior, bonding mechanisms, and identifying a possible relationship between physical properties and thermal responses. Based on the figures and tables, it is evident that the Maximum Relative Radiance (∆RMax) of each sample differs depending on both the chemical composition of HEA and the temperature at which Cold Spray is applied.

Keywords: active thermography, coating, cold spray, high- entropy alloy, material characterization

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Authors: M. Yadegari, M. Nourbakhsh, N. Arbabzadeh

Abstract:

The skeletal system injuries are of major importance. In addition, it is recommended to use materials for hard tissue repair in open or closed fractures. It is important to use complex minerals with a beneficial effect on hard tissue repair, stimulating cell growth in the bone. Materials that could help avoid bone fracture inflammatory reaction and speed up bone fracture repair are of utmost importance in the treatment of bone fractures. Similar to minerals, the inner eggshell membrane consists of carbohydrates, lipids, proteins with the high pH, high calcium absorptive capacity and with faster bone fracture repair ability. In the present radiographic survey, eggshell-derived bone graft substitutes were used for bone defect repair in 8 dog tibia, measuring bone density on the day of implant placement and 30 and 60 days after placement. In fact, the result of this study shows the difference in bone growth and misshapen bones between treatment and control sites. Cell growth was adequate in treatment sites and misshapen bones were less frequent here than in control sites.

Keywords: bone repair, eggshell powder, implant, radiography

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Authors: Michael A. Sprayberry, Vincent C. Paquit

Abstract:

Process parameter optimization in metal powder bed electron beam melting (MPBEBM) is crucial to ensure the technology's repeatability, control, and industry-continued adoption. Despite continued efforts to address the challenges via the traditional design of experiments and process mapping techniques, there needs to be more successful in an on-the-fly optimization framework that can be adapted to MPBEBM systems. Additionally, data-intensive physics-based modeling and simulation methods are difficult to support by a metal AM alloy or system due to cost restrictions. To mitigate the challenge of resource-intensive experiments and models, this paper introduces a Multi-Objective Reinforcement Learning (MORL) methodology defined as an optimization problem for MPBEBM. An off-policy MORL framework based on policy gradient is proposed to discover optimal sets of beam power (P) – beam velocity (v) combinations to maintain a steady-state melt pool depth and phase transformation. For this, an experimentally validated Eagar-Tsai melt pool model is used to simulate the MPBEBM environment, where the beam acts as the agent across the P – v space to maximize returns for the uncertain powder bed environment producing a melt pool and phase transformation closer to the optimum. The culmination of the training process yields a set of process parameters {power, speed, hatch spacing, layer depth, and preheat} where the state (P,v) with the highest returns corresponds to a refined process parameter mapping. The resultant objects and mapping of returns to the P-v space show convergence with experimental observations. The framework, therefore, provides a model-free multi-objective approach to discovery without the need for trial-and-error experiments.

Keywords: additive manufacturing, metal powder bed fusion, reinforcement learning, process parameter optimization

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Authors: Anshu Tyagi

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Zeolitic imidazolate frameworks (ZIFs), a subclass of metal-organic frameworks (MOFs) with structures resembling aluminosilicate zeolites, are gaining significant attention due to their unique properties. ZIF-8, in particular, has shown high surface area and enhanced hydrophobicity, making it a promising candidate for catalytic applications. In this study, ZIF-8 was synthesized in an aqueous medium by mixing 2-methylimidazole (mIm) with zinc nitrate hexahydrate (Zn) in deionized water. To improve the basicity and catalytic performance of ZIF-8, a series of K-loaded ZIF-8 catalysts (K/ZIF-8) were prepared by varying the KOH content from 5 to 10 wt%. Characterization of the synthesized catalysts was conducted using powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), high-resolution transmission electron microscopy (HRTEM), and temperature-programmed desorption (TPD) techniques. The ZIF-8 and K/ZIF-8 catalysts were applied in the transesterification of glycerol (GL) and dimethyl carbonate (DMC) to form glycerol carbonate (GLC). Various reaction parameters, including DMC/GL molar ratio, KOH loading, catalyst amount, and reaction temperature, were systematically studied to optimize the GLC yield. Under optimized conditions, the 10 wt% KOH-loaded ZIF-8 catalyst (10-K/ZIF-8) demonstrated excellent catalytic activity, achieving up to 95% GLC yield at a DMC/GL molar ratio of 3:1 within 0.5 hours. Remarkably, despite the hygroscopic nature of potassium, the catalyst exhibited significant water resistance, maintaining performance with up to 5 wt% water in relation to GL. Furthermore, the catalyst retained its activity after three recycling cycles without any notable loss in catalytic efficiency. This study highlights the potential of K/ZIF-8 as an efficient, water-tolerant catalyst for the transesterification of GL with DMC, offering high GLC yields and recyclability.

Keywords: metal-organic frameworks (MOFs), zeolitic imidazolate frameworks (ZIFs), transesterification, sustainable catalytic

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Authors: T. O. Adejumo, O. S. Akinyemi

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Powders and oils of Aframomum melegueta, Garcinia kola and Piper guineense were tested as preservatives for the storage of maize grains for four weeks. The concentrations of the powders were 32.5gkg-1, 65.0gkg-1 and 97.5gkg-1 maize, while those of oils were 0.85mlkg-1, 0.50mlkg-1 and 0.75mlkg-1 maize respectively. Powders of the three botanicals at 97.5gkg-1 maize possessed insecticidal effect on Sitophilus zeamais and also inhibitory activities on Aspergillus flavus, A. fumigatus, A. niger and Fusarium verticillioides, while little effect was observed for other concentrations. Oils of the three botanicals at 0.50mlkg-1 and 0.75mlkg-1 maize showed an insecticidal effect on S. zeamais and also inhibitory activities on A. flavus, A. fumigatus, A. niger, F. verticillioides, Penicillium and Rhizopus species. Oils showed more potential as a protectant against fungal and insect pest in storage maize grains than powders. Powders and oils of A. melegueta, G. kola and P. guineense could be successfully used as biopesticides.

Keywords: aframomum melegueta, garcinia kola, maize, powder, oils, piper guineense

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Authors: Le Nguyen Binh, Luong Xuan Binh, Le Van Tuan, Tran Binh Duong, Truong Nguyen Khanh Hung, Do Le Hoang Son, Pham Quang Vinh, Hoang Quoc Huy, Nguyen Bach, Nguyen Quoc Khanh Le, Jiunn Horng Kang

Abstract:

Introduction: Traumatic hip dislocation is an emergency in young adult which can cause avascular necrosis of femoral head or osteoarthritis of hip joint. The reasons for these may be the loose body of bony or chondral fragments, which are difficult to be detected on CT scan or MRI. In those cases, Hip arthroscopy may be the method of choice for diagnosis and treatment of loose bodies in hip joint after traumatic dislocation. Methods: A case report is performed. A 55-year-old male patient was under hip arthroscopy to retrieve the loose body in the right hip joint. Results: The patient’s hip was reduced under anesthesia in the opeation room. Xray and CT scan post-reduction showed that his right hip was wide and a small fragment of femoral head (< 5mm) locking inside the joint. A hip arthroscopy was done to take the fragment out. Post-operation, the patient went under rehabilition. After 6 months, he can walk with full-weight bearing; no further dislocaion was noted, and the Harris score was 84 points. Conclusions: Although acute traumatic injury of hip joint is usually treated with open surgeries, these methods have many drawbacks, such as soft tissue destruction, blood-loss,….Despite its technical requirement, hip arthroscopy is less invasive and effective treatment. Therefore, it may be an alternative treatment for a traumatic hip injury and can be applied frequently in the near future.

Keywords: hip dislocation, hip arthroscopy, hip osteoarthritis, acute hip trauma

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Authors: Raymond Dominic Uzoh

Abstract:

Starch fillers were extracted from three plant sources namely amora tuber (a wild variety of Irish potato), sweet potato and yam starch and their particle size, pH, amylose, and amylopectin percentage decomposition determined accordingly by high performance liquid chromatography (HPLC). The starch was introduced into natural rubber in liquid phase (through gelatinization) by the latex compounding method and compounded according to standard method. The prepared starch/natural rubber composites was characterized by Instron Universal testing machine (UTM) for tensile mechanical properties. The composites was further characterized by x-ray diffraction and crosslink density analysis. The particle size determination showed that amora starch granules have the highest particle size (156 × 47 μm) followed by yam starch (155× 40 μm) and then the sweet potato starch (153 × 46 μm). The pH test also revealed that amora starch has a near neutral pH of 6.9, yam 6.8, and sweet potato 5.2 respectively. Amylose and amylopectin determination showed that yam starch has a higher percentage of amylose (29.68), followed by potato (22.34) and then amora starch with the lowest value (14.86) respectively. The tensile mechanical properties testing revealed that yam starch produced the best tensile mechanical properties followed by amora starch and then sweet potato starch. The structure, crystallinity/amorphous nature of the product composite was confirmed by x-ray diffraction, while the nature of crosslinking was confirmed by swelling test in toluene solvent using the Flory-Rehner approach. This research study has rendered a workable strategy for enhancing interfacial interaction between a hydrophilic filler (starch) and hydrophobic polymeric matrix (natural rubber) yielding moderately good tensile mechanical properties for further exploitation development and application in the rubber processing industry.

Keywords: natural rubber, fillers, starch, amylose, amylopectin, crosslink density

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Authors: Mohamed M. Emara, Heba Ashraf

Abstract:

This study is to investigation the effect of silicon carbide (SiC) particle size and thermo-mechanical processing on dimensional stability of aluminum alloy 2124. Three combinations of SiC weight fractions are investigated, 2.5, 5, and 10 wt. % with different SiC particle sizes (25 μm, 5 μm, and 100nm) were produced using mechanical ball mill. The standard testing samples were fabricated using powder metallurgy technique. Both samples, prior and after extrusion, were heated from room temperature up to 400ºC in a dilatometer at different heating rates, that is, 10, 20, and 40ºC/min. The analysis showed that for all materials, there was an increase in length change as temperature increased and the temperature sensitivity of aluminum alloy decreased in the presence of both micro and nano-sized silicon carbide. For all conditions, nanocomposites showed better dimensional stability compared to conventional Al 2124/SiC composites. The after extrusion samples showed better thermal stability and less temperature sensitivity for the aluminum alloy for both micro and nano-sized silicon carbide.

Keywords: aluminum 2124 metal matrix composite, SiC nano-sized reinforcements, powder metallurgy, extrusion mechanical ball mill, dimensional stability

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