Search results for: neutron diffraction

Authors: Opeyemi Atiba-Oyewo, Maurice S. Onyango, Christian Wolkersdorfer

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Characterization and nanostructure formation of banana peels as sorbent material are described in this paper. The transformation of this agricultural waste via mechanical milling to enhance its properties such as changed in microstructure and surface area for water pollution control and other applications were studied. Mechanical milling was employed using planetary continuous milling machine with ethanol as a milling solvent and the samples were taken at time intervals between 10 h to 30 h to examine the structural changes. The samples were characterised by X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infra-red (FTIR), Transmission electron microscopy (TEM) and Brunauer Emmett and teller (BET). Results revealed three typical structures with different deformation mechanisms and the grain-sizes within the range of (71-12 nm), nanostructure of the particles and fibres. The particle size decreased from 65µm to 15 nm as the milling progressed for a period of 30 h. The morphological properties of the materials indicated that the particle shapes becomes regular and uniform as the milling progresses. Furthermore, particles fracturing resulted in surface area increment from 1.0694-4.5547 m2/g. The functional groups responsible for the banana peels capacity to coordinate and remove metal ions, such as the carboxylic and amine groups were identified at absorption bands of 1730 and 889 cm-1, respectively. However, the choice of this sorbent material for the sorption or any application will depend on the composition of the pollutant to be eradicated.

Keywords: characterization, nanostructure, nanosorbent, eco-friendly, banana peels, mechanical milling, water quality

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Authors: Ts. Lazarova, V. Tumbalev, S. Atanacova-Vladimirova, G. Ivanov, A. Naydenov, D. Kovacheva

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Methane is a major Greenhouse Gas (GHG) that accounts for 14% of the world’s total amount of GHG emissions, originating mainly from agriculture, Coal mines, land fields, wastewater and oil and gas facilities. Nowadays the problem caused by the methane emissions has been a subject of an increased concern. One of the methods for neutralization of the methane emissions is it's complete catalytic oxidation. The efforts of the researchers are focused on the development of new types of catalysts and optimizing the existing catalytic systems in order to prevent the sintering of the palladium, providing at the same time a sufficient activity at temperatures below 500oC. The aim of the present work is to prepare mixed Cu-Ag-Pd oxide catalysts supported on alumina and to test them for methane complete catalytic oxidation. Cu-Ag-Pd/Al2O3 were prepared on a γ-Al2O3 (BET surface area = 220 m2/g) by the incipient wetness method using the corresponding metal nitrates (Cu:Ag = 90:10, Cu:Pd =97:3, Cu:Ag:Pd= 87:10:3) as precursors. A second set of samples were prepared with addition of urea to the metal nitrate solutions with the above mentioned ratios assuming increased dispersivity of the catalysts. The catalyst samples were dried at 100°C for 3 hours and calcined at 550°C for 30 minutes. Catalysts samples were characterized using X-ray diffraction (XRD), low temperature adsorption of nitrogen (BET) and scanning electron microscopy (SEM). The catalytic activity tests were carried out in a continuous flow type of reactor at atmospheric pressure. The effect of catalyst aging at 500 oC for 120 h on the methane combustion activity was also investigated. The results clearly indicate the synergetic effect of Ag and Pd on the catalytic activity.

Keywords: catalysts, XRD, BET, SEM, catalytic oxidation

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Authors: Rudra Vaghela, P. K. Kulkarni

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The aim of the present research was to develop oral Amphotericin B (AmB) nanocrystals (Nc) grafted with suitable ligand in order to enhance drug transport across the intestinal epithelial barrier and subsequently, active uptake by macrophages. AmB Nc were prepared by liquid anti-solvent precipitation technique (LAS). Poloxamer 188 was used to stabilize the prepared AmB Nc and grafted with mannose for actively targeting M cells in Peyer’s patches. To prevent shedding of the stabilizer and ligand, N,N’-Dicyclohexylcarbodiimide (DCC) was used as a cross-linker. The prepared AmB Nc were characterized for particle size, PDI, zeta potential, X-ray diffraction (XRD) and surface morphology using scanning electron microscope (SEM) and evaluated for drug content, in vitro drug release and cell uptake studies using caco-2 cells. The particle size of stabilized AmB Nc grafted with WGA was in the range of 287-417 nm with negative zeta potential between -18 to -25 mV. XRD studies revealed crystalline nature of AmB Nc. SEM studies revealed that ungrafted AmB Nc were irregular in shape with rough surface whereas, grafted AmB Nc were found to be rod-shaped with smooth surface. In vitro drug release of AmB Nc was found to be 86% at the end of one hour. Cellular studies revealed higher invasion and uptake of AmB Nc towards caco-2 cell membrane when compared to ungrafted AmB Nc. Our findings emphasize scope on developing oral delivery system for passively targeting M cells in Peyer’s patches.

Keywords: leishmaniasis, amphotericin b nanocrystals, macrophage targeting, LAS technique

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Authors: Savvas Varitis, Panagiotis Kavouras, George Kaimakamis, Eleni Pavlidou, George Vourlias, Konstantinos Chrysafis, Philomela Komninou, Theodoros Karakostas

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Tannery industry produces high quantities of chromium containing waste which also have high organic content. Processing of this waste is important since the organic content is above the disposal limits and the containing trivalent chromium could be potentially oxidized to hexavalent in the environment. This work aims to fabricate new vitreous and glass ceramic materials which could incorporate the tannery waste in stabilized form either for safe disposal or for the production of useful materials. Tannery waste was incinerated at 500oC in anoxic conditions so most of the organic content would be removed and the chromium remained trivalent. Glass forming agents SiO2, Na2O and CaO were mixed with the resulting ash in different proportions with decreasing ash content. Considering the low solubility of Cr in silicate melts, the mixtures were melted at 1400oC and/or 1500oC for 2h and then casted on a refractory steel plate. The resulting vitreous products were characterized by X-Ray Diffraction (XRD), Differential Thermal Analysis (DTA), Scanning and Transmission Electron Microscopy (SEM and TEM). XRD reveals the existence of Cr2O3 (eskolaite) crystallites embedded in a glassy amorphous matrix. Such crystallites are not formed under a certain proportion of the waste in the ash-vitrified material. Reduction of the ash proportion increases chromium content in the silicate matrix. From these glassy products, glass-ceramics were produced via different regimes of thermal treatment.

Keywords: chromium containing tannery ash, glass ceramic materials, thermal processing, vitrification

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Authors: Elmineh Tsegahun Gedif

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Zinc oxide nanoparticles (ZnO NPs) have attracted huge attention due to catalytic, optical, photonic, and antibacterial activity. Zinc oxide nanoparticles were successfully synthesized via a fast, non-toxic, cost-effective, and eco-friendly method by biologically reducing Zn(NO3)2.6H2O solution with Neem (Azadirachta indica) leaf extract under optimum conditions (pH = 9). The presence of active flavonoids, phenolic groups, alkaloids, terpenoids, and tannins, which were in the biomass of the Neem leaf extract before and after reduction, was identified using qualitative screening methods (observing the color changes) and FT-IR Spectroscopy. The formation of ZnO NPs was visually indicated by the color changes from colorless to light yellow color. Biosynthesized nanoparticles were also characterized by UV-visible, FT-IR, and XRD spectroscopies. The reduction process was simple and convenient to handle and was monitored by UV-visible spectroscopy that showed surface plasmon resonance (SPR) of the ZnO NPs at 321 nm. This result clearly revealed the formation of ZnO NPs. X-ray diffraction was used to investigate the crystal structure. The average particle size of ZnO powder and around 20 nm using the line width of the plane, and the refraction peak using Scherrer’s equation. The synthesized zinc oxide nanoparticles were evaluated for antimicrobial activities against Gram-positive and Gram-negative bacteria. Zinc nanoparticles exhibited the maximum zone of inhibition against Escherichia coli (15 mm), while the least activity was seen against Staphylococcus aureus.

Keywords: antimicrobial activity, azadirachta indica, green synthesis, ZnO NPs

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Authors: Rimzhim Gupta, Bhanupriya Boruah, Jayant M. Modak, Giridhar Madras

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Microbial contamination is one of the major concerns in the field of water treatment. AOP (advanced oxidation processes) is well-established method to resolve the issue of removal of contaminants in water. A Z-scheme composite g-C₃N₄/CuWO₄ was synthesized by sol-gel method for the photocatalytic inactivation of a mixed population of Gram-positive bacteria (S. aureus) and Gram-negative bacteria (E. coli). The photoinactivation was observed for different types of bacteria in the same medium together and individually in the absence of the nutrients. The lattice structures and phase purities were determined by X-ray diffraction. For morphological and topographical features, scanning electron microscopy and transmission electron microscopy analyses were carried out. The band edges of the semiconductor (valence band and conduction band) were determined by ultraviolet photoelectron microscopy. The lifetime of the charge carriers and band gap of the semiconductors were determined by time resolved florescence spectroscopy and diffused reflectance spectroscopy, respectively. The effect of weight ratio of C₃N₄ and CuWO₄ was observed by performing photocatalytic experiments. To investigate the exact mechanism and major responsible radicals for photocatalysis, scavenger studies were performed. The rate constants and order of the inactivation reactions were obtained by power law kinetics. For E. coli and S. aureus, the order of reaction and rate constants are 1.15, 0.9 and 1.39 ± 0.03 (CFU/mL)⁻⁰.¹⁵ h⁻¹, 47.95 ± 1.2 (CFU/mL)⁰.¹ h⁻¹, respectively.

Keywords: z-scheme, E. coli, S. aureus, sol-gel

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Authors: Muhammad Arshad, Ghulam Hussain Bhatti, Abdul Qayyum

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Zinc-doped silica oxide nanoparticles having size 7.93nm were synthesized by the deposition precipitation method by using different solvents (acetonitrile, n-hexane, isoamylalchol). Biological potential such as antibacterial activities against Bacillussubtilusand Escherichia coli, and antifungal activities against Candida parapsilosis and Aspergilusniger were also investigated by Disc diffusion method. Different characterizations techniques including Fournier Transmission Infrared Spectroscopy (FT-IR), X-ray diffraction (XRD), Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM), Thermo-gravimeteric Analysis (TGA), Atomic forced microscopy (AFM), and Dynamic Light Scattering (DLS) were used. FT-IR characterization confirmed the presence of metal oxide bond (SiO2) while XRD showed the hexagonal structure. SEM and TEM characterization showed the morphology of nanoparticles. AFM study showed good particle size distribution as depicted by a histogram. DLS study showed the gradual decease in the size of nanoparticles from 24.86nm to 13.24 nm. Highest antibacterial activities revealed by acetonitrile solvents (6%and 4.5%) followed by isoamylalchol (3% and 2.4%) while n-hexane solvent showed the lowest activity (2%and 1%) respectively. Higher antifungal activities exhibited by n-hexane (0.34 % and 0.43%) followed by isoamylalchol (0.27% and 0.19%) solvent while acetonitrile (0.21% and 0.17%) showed least activity respectively. Statistical analysis by using one-way ANOVA also indicated the significant results of both biological activities.

Keywords: nanoparticles, precipitation methods, antibacterial, antifungal, characterizations

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Authors: Djamil Guettiche, Ahmed Mekki, Tighilt Fatma-Zohra, Rachid Mahmoud

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The aim of this study was to synthesize and characterize conducting polymer composites of polypyrrole and graphene, including pristine and surface-treated graphene (PPy/GO, PPy/rGO, and PPy/rGO-ArCOOH), for use as sensitive elements in a homemade chemiresistive module for on-line detection of nitrogen oxides vapors. The chemiresistive module was prepared, characterized, and evaluated for performance. Structural and morphological characterizations of the composite were carried out using FTIR, Raman spectroscopy, and XRD analyses. After exposure to NO and NO₂ gases in both static and dynamic modes, the sensitivity, selectivity, limit of detection, and response time of the sensor were determined at ambient temperature. The resulting sensor showed high sensitivity, selectivity, and reversibility, with a low limit of detection of 1 ppm. A composite of polypyrrole and graphene functionalized with aryl 4-carboxy benzene diazonium salt was synthesized and characterized using FTIR, scanning electron microscopy, transmission electron microscopy, UV-visible, and X-ray diffraction. The PPy-rGOArCOOH composite exhibited a good electrical resistance response to NO₂ at room temperature and showed enhanced NO₂-sensing properties compared to PPy-rGO thin films. The selectivity and stability of the NO₂ sensor based on the PPy/rGO-ArCOOH nanocomposite were also investigated.

Keywords: conducting polymers, surface treated graphene, diazonium salt, polypyrrole, Nitrogen oxide sensing

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Authors: Marwa M. Abu-Serie, Marwa M. Eltarahony

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The search for reliable, effective, and safe nanoparticles (NPs) as a treatment for cancer is a pressing priority. In this study, Cu-NPs were fabricated by Streptomyces cyaneofuscatus through simultaneous bioreduction strategy of copper nitrate salt. The as-prepared Cu-NPs subjected to structural analysis; energy-dispersive X-ray spectroscopy, elemental mapping, X-ray diffraction, transmission electron microscopy, and ζ-potential. These biological synthesized Cu-NPs were mixed with disulfiram (DS), forming a nanocomplex of Cu-DS with a size of ~135 nm. The prepared nanocomplex (nanoCu-DS) exhibited higher anticancer activity than that of free complex of DS-Cu, Cu-NPs, and DS alone. This was illustrated by the lowest IC50 of nanoCu-DS (< 4 µM) against human breast and liver cancer cell lines comparing with DS-Cu, Cu-NPs, and DS (~8, 22.98-33.51 and 11.95-14.86, respectively). Moreover, flow cytometric analysis confirmed that higher apoptosis percentage range of nanoCu-DS-treated in MDA-MB 231, MCF-7, Huh-7, and HepG-2 cells (51.24-65.28%) than free complex of Cu-DS ( < 4.5%). Regarding inhibition potency of liver and breast cancer cell migration, no significant difference was recorded between free and nanocomplex. Furthermore, nanoCu-DS suppressed gene expression of β-catenine, Akt, and NF-κB and upregulated p53 expression (> 3, >15, > 5 and ≥ 3 folds, respectively) more efficiently than free complex (all ~ 1 fold) in MDA-MB 231 and Huh-7 cells. Our finding proved this prepared nano complex has a powerful anticancer activity relative to free complex, thereby offering a promising cancer treatment.

Keywords: biologically prepared Cu-NPs, breast cancer cell lines, liver cancer cell lines, nanoCu- disulfiram

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Authors: Zohreh Derikvand

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One new 2D metal-organic coordination polymer of Ni(II) namely [Ni2(ndc)2(DMSO)4(H2O)]n, where ndc = naphthalene-1,4-dicarboxylic acid and DMSO= dimethyl sulfoxide has been synthesized and characterized by elemental analysis, spectral (IR, UV-Vis), thermal (TG/DTG) analysis and single crystal X-ray diffraction. Compound 1 possesses a 2D layer structure constructed from dinuclear nickel(II) building blocks in which two crystallographically independent Ni2+ ions are bridged by ndc2– ligands and water molecule. The ndc2– ligands adopt μ3 bridging modes, linking the metal centers into a two-dimensional coordination framework. The two independent NiII cations are surrounded by dimethyl sulfoxide and naphthalene-1,4-dicarboxylate molecules in distorted octahedron geometry. In the crystal structures of 1 there are non-classical hydrogen bonding arrangements and C-H–π stacking interactions. Electrochemical behavior of [Ni2(ndc)2(DMSO)4(H2O)]n, (Ni-NDA) on the surface of carbon nanotube (CNTs) glassy carbon electrode (GCE) was described. The surface structure and composition of the sensor were characterized by scanning electron microscopy (SEM). Oxidation of fructose on the surface of modified electrode was investigated with cyclic voltammetry and electrochemical impedance spectroscopy (EIS) and the results showed that the Ni-NDA/CNTs film displays excellent electrochemical catalytic activities towards fructose oxidation.

Keywords: naphthalene-1, 4-dicarboxylic acid, crystal structure, coordination polymer, electrocatalysis, impedance spectroscopy

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Authors: S. Abd Rahim, F. A. Rahman, E. M. Nasir, N. A. Ramle

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Co-crystal is believed to improve the solubility and dissolution rates and thus, enhanced the bioavailability of poor water soluble drugs particularly during the oral route of administration. With the existing of poorly soluble drugs in pharmaceutical industry, the screening of co-crystal formation using carbamazepine (CBZ) as a model drug compound with dicarboxylic acids co-crystal formers (CCF) namely fumaric (FA) and succinic (SA) acids in ethanol has been studied. The co-crystal formations were studied by varying the mol ratio values of CCF to CBZ to access the effect of CCF concentration on the formation of the co-crystal. Solvent evaporation, slurry, and cooling crystallisations which representing the solution based method co-crystal screening were used. The product crystal from the screening was characterized using X-ray powder diffraction (XRPD). The XRPD pattern profile analysis has shown that the CBZ co-crystals with FA and SA were successfully formed for all ratios studied. The findings revealed that CBZ-FA co-crystal were formed in two different polymorphs. It was found that CBZ-FA form A and form B were formed from evaporation and slurry crystallisation methods respectively. On the other hand, in cooling crystallisation method, CBZ-FA form A was formed at lower mol ratio of CCF to CBZ and vice versa. This study disclosed that different methods and mol ratios during the co-crystal screening can affect the outcome of co-crystal produced such as polymorphic forms of co-crystal and thereof. Thus, it was suggested that careful attentions is needed during the screening since the co-crystal formation is currently one of the promising approach to be considered in research and development for pharmaceutical industry to improve the poorly soluble drugs.

Keywords: co-crystal, dicarboxylic acid, carbamazepine, industry

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Authors: Michael Munther, Keivan Davami

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One significant roadblock for additively manufactured (AM) parts is the buildup of residual tensile stresses during the fabrication process. These residual stresses are formed due to the intense localized thermal gradients and high cooling rates that cause non-uniform material expansion/contraction and mismatched strain profiles during powder-bed fusion techniques, such as direct metal laser sintering (DMLS). The residual stresses adversely affect the fatigue life of the AM parts. Moreover, if the residual stresses become higher than the material’s yield strength, they will lead to acute geometric distortion. These are limiting the applications and acceptance of AM components for safety-critical applications. Herein, we discuss laser shock peening method as an advanced technique for the manipulation of the residual stresses in AM parts. An X-ray diffraction technique is used for the measurements of the residual stresses before and after the laser shock peening process. Also, the hardness of the structures is measured using a nanoindentation technique. Maps of nanohardness and modulus are obtained from the nanoindentation, and a correlation is made between the residual stresses and the mechanical properties. The results indicate that laser shock peening is able to induce compressive residual stresses in the structure that mitigate the tensile residual stresses and increase the hardness of AM IN718, a superalloy, almost 20%. No significant changes were observed in the modulus after laser shock peening. The results strongly suggest that laser shock peening can be used as an advanced post-processing technique to optimize the service lives of critical components for various applications.

Keywords: additive manufacturing, Inconel 718, laser shock peening, residual stresses

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Authors: Magdalena Wilk-Kozubek, Jakub Pawłów, Maciej Czajkowski, Maria Zdończyk, Katarzyna Ślepokura, Joanna Cybińska

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Thermochromic materials belong to the family of intelligent materials that change their color in response to temperature changes; this ability is called thermochromism. Thermochromic behavior can be displayed by both isolated compounds and multicomponent mixtures. Fluoran leuco dye-based mixtures are well-known thermochromic systems used, for example, in heat-sensitive FAX paper. Weak acids often serve as color developers for such systems. As the temperature increases, the acids melt, and the mixtures become colored. The objective of this research is to determine the influence of acids showing a liquid crystalline nematic phase on the development of the fluoran dye. For this purpose, fluoran-based mixtures with 4-n-alkylbenzoic acids were prepared. The mixtures are colored at room temperature, but they become colorless upon the melting of the acids. The melting of acids is associated not only with a change in the color of the mixtures but also with a change in their emission color. Phase transitions were investigated by temperature-dependent powder X-ray diffraction and differential scanning calorimetry; nematic phases were visualized by polarized optical microscopy, and color and emission changes were studied by UV-Vis diffuse reflectance and photoluminescence spectroscopies, respectively. When 4-n-alkylbenzoic acids are used as color developers, the fluoran-based mixtures become colorless after the melting of the acids. This is because the melting of acids is accompanied by the transition from the crystalline phase to the nematic phase, in which the molecular arrangement of the acids does not allow the fluoran dye to be developed.

Keywords: color developer, leuco dye, liquid crystal, thermochromism

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Authors: S. V. N. Pammi, Soon-Gil Yoon

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In the present study, we report a facile chemical vapor deposition (CVD) method for Perovskite MAPbI3 thin films by doping with Br and Cl. We performed a systematic optimization of CVD parameters such as deposition temperature, working pressure and annealing time and temperature to obtain high-quality films of CH3NH3PbI3, CH3NH3PbI3-xBrx and CH3NH3PbI3-xClx perovskite. Scanning electron microscopy and X-ray Diffraction pattern showed that the perovskite films have a large grain size when compared to traditional spin coated thin films. To the best of our knowledge, there are very few reports on highly quality perovskite thin films by various doping such as Br and Cl using one step CVD and there is scope for significant improvement in device efficiency. In addition, their band-gap can be conveniently and widely tuned via doping process. This deposition process produces perovskite thin films with large grain size, long diffusion length and high surface coverage. The enhancement of the output power, CH3NH3PbI3 (MAPbI3) dye films when compared to spin coated films and enhancement in output power by doping in doped films was demonstrated in detail. The facile one-step method for deposition of perovskite thin films shows a potential candidate for photovoltaic and energy harvesting applications.

Keywords: perovskite thin films, chemical vapor deposition, energy harvesting, photovoltaics

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Authors: Chaima Zoulikha Tabet Zatla, Nihel Dib, Sumeya Bedrane, Juan Carlos Hernandez Garrido, Redouane Bachir, Miguel Angel Cauqui, Jose Juan Calvino Gamez

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These last year's our planet has witnessed global warming, which is a serious threat to our lives; it has many causes, such as the CO₂ excess in the atmosphere that results from our activity, for the purpose of living in a neater and better environment, working and improving an eco-responsible energy system is a must. Valorization of biomass to produce biofuels is among the most compelling routes to decrease air pollution without considerable modification in current vehicle technology. Effective transformation of lignocellulosic biomass-derived compounds into liquid fuels and value-added chemicals is an economically viable solution. Presently, very competitive technics for the conversion of lignocellulosic biomass into platform chemicals, such as furfural and Hydroxymethylfurfural (HMF), are used. Furfural (C₅H₄O₂) is a major hemi cellulosic biomass-derived platform molecule. In our work, we focus on the valorization of lignocellulosic biomass derivative furfural that is transformed into biofuel through a hydrodeoxygenation reaction in general and involving a catalytic process. In order to get to this point, we are synthesizing and characterizing a series of catalysts with different amounts of Ru (0.5%, 1% and 2%) supported on alumina-silica mixed oxides with various molar ratios (Si/Al = 2.5; 5; 7; 10; 15). These catalysts will be characterized by numerous technics such as N₂ adsorption/desorption, Pyridine adsorption (acidity measure), FTIR, X-rays diffraction, AAS, TEM and SEM.

Keywords: furfural, ruthenium, silica-alumina, biomass, biofuel

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Authors: M. Murmu, Govardhan, J. Satya Eswari

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Concrete is the most common and widely used building material. Concrete is basically made of aggregates, both fine and coarse, glued by a cement paste which is made of cement and water. Each one of these constituents of concrete has a negative environmental impact and gives rise to different sustainability issues. The current concrete construction practice is unsustainable because, not only it consumes enormous quantities of stones, sand, and drinking water, but also one billion tons a year of cement, which is not an environment friendly material. Preventing the reduction of natural resources and enhancing the usage of waste materials has become a challenge to the scientist and engineers. A number of studies have been conducted concerning the protection of natural resources, prevention of environmental pollution and contribution to the economy by using this waste material. This paper outlines the influence of Ground Granulated Blast furnace Slag (GGBS) as partial replacement of fine aggregate on mechanical properties of concrete. The strength of concrete is determined having OPC binder, replaced the fine aggregate with15%, 30%, 45% respectively. For this purpose, characteristics concrete mix of M25 with partial replacement of cement with GGBS is used and the strength of concrete cubes and cylinder have determined. The strength of concrete specimens has been compared with the reference specimen. Also X-ray diffraction (XRD) and scanning electron microscope (SEM) tests have been performed to examine the hydration products and the microstructure of the tested specimens. A correlation has been established between the developmental strength concrete with and without GGBS through analysis of hydration products and the microstructure.

Keywords: GGBS, sand, concrete, workability

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Authors: Mohamed Loutou, Mohamed Hajjaji, Mohamed Ait Babram, Mohammed Mansori, Rachid Hakkou, Claude Favotto

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More than 26,4 million tons of phosphates are produced by the phosphates industries in Morocco (2010), generating huge amounts of sludge by flocculation during the ore beneficiation. They way are stored at the end of the process in open air ponds. Its accumulation and storage may have an impact on several scales such as ground water and human being. For this purpose, an efficient way to use it the field of the ceramic is proposed. The as received sludge and a clay-rich sediment have been studied in terms of chemical, mineralogical and micro-structural side using various analytical methods. Several formulations have been performed by mixing the sludge with the binder shaped in the form of granules. After being dried at 105 °C, the samples were heated in the range of 900-1200 °C. As well as the ceramic properties (firing shrinkage, water absorption, total porosity and compressive strength) the micro structure has been investigated using X-ray diffraction, scanning electron microscopy and Fourier transform infrared spectroscopy. The relations between properties and the operating factors were formulated using the design of experiments (DOE). Gehlenite was the only phase neo-formed in the sintering samples. SEM micrographs revealed the presence of nano metric stains. Based on RSM results, all factors had positive effects on Firing shrinkage, compressive strength and total porosity. However, they manifested opposite effects on density and water absorption.

Keywords: phosphate sludge, clay, ceramic properties, granule

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Authors: Murtaza Adil, Sen Yang, Zhou Chao, Song Xiaoping

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The morphotropic phase boundary (MPB) recently has attracted constant interest in ferromagnetic systems for obtaining enhanced large magnetoelastic response. In the present study, structural and magnetoelastic properties of MPB involved ferromagnetic Tb_1-xGd_xFe₂ (0≤x≤1) system has been investigated. The change of easy magnetic direction from <111> to <100> with increasing x up MPB composition of x=0.9 is detected by step-scanned [440] synchrotron X-ray diffraction reflections. The Gd substitution for Tb changes the composition for the anisotropy compensation near MPB composition of x=0.9, which was confirmed by the analysis of detailed scanned XRD, magnetization curves and the calculation of the first anisotropy constant K₁. The spin configuration diagram accompanied with different crystal structures for Tb_1-xGd_xFe₂ was designed. The calculated first anisotropy constant K₁ shows a minimum value at MPB composition of x=0.9. In addition, the large ratio between magnetostriction, and the absolute values of the first anisotropy constant │λ_S∕K₁│ appears at MPB composition, which makes it a potential material for magnetostrictive application. Based on experimental results, a theoretically approach was also proposed to signify that the facilitated magnetization rotation and enhanced magnetoelastic effect near MPB composition are a consequence of the anisotropic flattening of free energy of ferromagnetic crystal. Our work specifies the universal existence of MPB in ferromagnetic materials which is important for substantial improvement of magnetic and magnetostrictive properties and may provide a new route to develop advanced functional materials.

Keywords: free energy, magnetic anisotropy, magnetostriction, morphotropic phase boundary (MPB)

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Authors: Chandra Sekhar Singh, P. Chakrapani, B. Arun Jyothi, A. Roja Rani

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The green synthesis of metallic nanoparticles (NPs) involves biocompatible ingredients under physiological conditions of temperature and pressure. Moreover, the biologically active molecules involved in the green synthesis of NPs act as functionalizing ligands, making these NPs more suitable for biomedical applications. Among the most important bioreductants are plant extracts, which are relatively easy to handle, readily available, low cost, and have been well explored for the green synthesis of other nanomaterials. Various types of metallic NPs have already been synthesized using plant extracts. They have wide applicability in various areas such as electronics, catalysis, chemistry, energy, and medicine. Metallic nanoparticles are traditionally synthesized by wet chemical techniques, where the chemicals used are quite often toxic and flammable. In our study, we were described a cost effective and environment friendly technique for green synthesis of silver nanoparticles from 1mM AgNO3 solution through the aqueous extract of Erythrina indica as reducing as well as capping agent. Nanoparticles were characterized using UV–Vis absorption spectroscopy, FTIR, XRD, X-ray diffraction, SEM and TEM analysis showed the average particle size of 30 nm as well as revealed their spherical structure. Further these biologically synthesized nanoparticles were found to be highly toxic against different human pathogens viz. two Gram positive namely Klebsiella pneumonia and Bacillus subtilis bacteria and two were Gram negative bacteria namely Staphylococcus aureus and Escherichia coli (E. coli). This is for the first time reporting that Erythrina indica plant extract was used for the synthesis of nanoparticles.

Keywords: silver nanoparticles, green synthesis, antibacterial activity, FTIR, TEM, SEM

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Authors: Sirirat Jangkorn, Pornsawai Praipipat

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Sugarcane bagasse ash of sugar factories is solid wastes that the richest source of silica. The alkali fusion method, quartz particles in material can be dissolved and they can be used as the silicon source for synthesizing silica-based materials such as zeolites. Zeolites have many advantages such as catalyst to improve the chemical reactions and they can also remove heavy metals in the water including lead. Therefore, this study attempts to synthesize zeolites from the sugarcane bagasse ash, investigate their structure characterizations and chemical components to confirm the happening of zeolites, and examine their lead removal efficiency through the batch test studies. In this study, the sugarcane bagasse ash was chosen as the silicon source to synthesize zeolites, X-ray diffraction (XRD) and X-ray fluorescence spectrometry (XRF) were used to verify the zeolite pattern structures and element compositions, respectively. The batch test studies in dose (0.05, 0.1, 0.15 g.), contact time (1, 2, 3), and pH (3, 5, 7) were used to investigate the lead removal efficiency by the synthesized zeolite. XRD analysis result showed the crystalline phase of zeolite pattern, and XRF result showed the main element compositions of the synthesized zeolite that were SiO₂ (50%) and Al₂O₃ (30%). The batch test results showed the best optimum conditions of the synthesized zeolite for lead removal were 0.1 g, 2 hrs., and 5 of dose, contact time, and pH, respectively. As a result, this study can conclude that the zeolites can synthesize from the sugarcane bagasse ash and they can remove lead in the water.

Keywords: sugarcane bagasse ash, solid wastes, zeolite, lead

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Authors: Ayda Khosravanihaghighi, Pramod Koshy, Bill Walsh, Vedran Lovric, Charles Christopher Sorrell

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There is an increasing demand for orthopedic implants owing to the increasing numbers of the aging population. Titanium alloy (Ti6Al4V) is a common material used for orthopedic implants owing to its advantageous properties in terms of good corrosion resistance, minimal elastic modulus mismatch with bone, bio-inertness, and high mechanical strength. However, it is important to improve the bioactivity and osseointegration of the titanium alloy and this can be achieved by coating the implant surface with suitable ceramic materials. In the present work, pure and doped-ceria (CeO₂) coatings were deposited by spin coating on the titanium alloy surface in order to enhance the biological interactions between the surface of the implant and the surrounding tissue. In order to examine the bone-binding ability of an implant, simulated body fluid (SBF) tests were conducted in order to assess the capability of apatite layer formation on the surface and thus predict in vivo bone bioactivity. Characterization was done using scanning electron microscopy (SEM) and X-ray diffraction (XRD) analyses to determine the extent of apatite formation. Preliminary tests showed that the CeO₂ coatings were biocompatible and that the extent of apatite formation and its characteristics can be enhanced by doping with suitable metal ions.

Keywords: apatite layer, biocompatibility, ceria, orthopaedic implant, SBF, spin coater, Ti-implant

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Authors: Junior Nomani

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This paper presents a novel approach to modelling the metal cutting of duplex stainless steels, a two-phase alloy regarded as a difficult-to-machine material. Calculation and control of shear strain and stresses during cutting are essential to achievement of ideal cutting conditions. Too low or too high leads to higher required cutting force or excessive heat generation causing premature tool wear failure. A 2D finite element cutting model was created based on electron backscatter diffraction (EBSD) data imagery of duplex microstructure. A mesh was generated using ‘object-oriented’ software OOF2 version V2.1.11, converting microstructural images to quadrilateral elements. A virtual workpiece was created on ABAQUS modelling software where a rigid body toolpiece advanced towards workpiece simulating chip formation, generating serrated edge chip formation cutting. Model results found calculated stress strain contour plots correlated well with similar finite element models tied with austenite stainless steel alloys. Virtual chip form profile is also similar compared experimental frozen machining chip samples. The output model data provides new insight description of strain behavior of two phase material on how it transitions from workpiece into the chip.

Keywords: Duplex stainless steel, ABAQUS, OOF2, Chip formation

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Authors: Raghvendra Singh Yadav, Ivo Kuřitka, Jaromir Havlica, Zuzana Kozakova, Jiri Masilko, Lukas Kalina, Miroslava Hajdúchová, Vojtěch Enev, Jaromir Wasserbauer

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In this work, we investigated the structural and magnetic properties of CoFe2O4:Nd3+/Dy3+/Pr3+/Gd3+ nanoparticles synthesized by starch-assisted sol-gel combustion method. X-ray diffraction pattern confirmed the formation of cubic spinel structure of rare-earth ions (Nd3+, Dy3+, Pr3+, Gd3+) doped CoFe2O4 spinel ferrite nanoparticles. Raman and Fourier Transform Infrared spectroscopy study also confirmed cubic spinel structure of rare-earth ions (Nd3+, Dy3+, Pr3+, Gd3+) substituted CoFe2O4 nanoparticles. The field emission scanning electron microscopy study revealed the effect of annealing temperature on size of rare-earth ions (Nd3+, Dy3+, Pr3+, Gd3+) substituted CoFe2O4 nanoparticles and particles were in the range of 10-100 nm. The magnetic properties of rare-earth ions (Nd3+, Dy3+, Pr3+, Gd3+) substituted CoFe2O4 nanoparticles were investigated by using vibrating sample magnetometer. The variation in saturation magnetization, coercivity and remanent magnetization with annealing temperature/ particle size of rare-earth ions (Nd3+, Dy3+, Pr3+, Gd3+) substituted CoFe2O4 nanoparticles was observed. Acknowledgment: This work was supported by the Ministry of Education, Youth and Sports of the Czech Republic – Program NPU I (LO1504).

Keywords: starch, sol-gel combustion method, rare-earth ions, spinel ferrite nanoparticles, magnetic properties

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Authors: Javiera Poblete, Fernando Gajardo, Katherina Fernandez

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Graphene, and its derivatives such as graphene oxide (GO), are emerging nanoscopic materials, with interesting physical and chemical properties. From them, it is possible to develop three-dimensional macrostructures, such as aerogels, which are characterized by a low density, high porosity, and large surface area, having a promising structure for the development of materials. The use of GO as a precursor of these structures provides a wide variety of materials, which can be developed as a result of the functionalization of their oxygenated groups, with specific compounds such as polyethylene glycol (PEG). The synthesis of aerogels of GO-PEG for non-covalent interactions has not yet been widely reported, being of interest due to its feasible escalation and economic viability. Thus, this work aims to develop a non-covalently functionalized GO-PEG aerogels and characterize them physicochemically. In order to get this, the GO was synthesized from the modified hummers method and it was functionalized with the PEG by polymer-assisted GO gelation (crosslinker). The gelation was obtained for GO solutions (10 mg/mL) with the incorporation of PEG in different proportions by weight. The hydrogel resulting from the reaction was subsequently lyophilized, to obtain the respective aerogel. The material obtained was chemically characterized by analysis of Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy and X-ray diffraction (XRD), and its morphology by scanning electron microscopy (SEM) images; as well as water absorption tests. The results obtained showed the formation of a non-covalent aerogel (FTIR), whose structure was highly porous (SEM) and with a water absorption values greater than 50% g/g. Thus, a methodology of synthesis for GO-PEG was developed and validated.

Keywords: aerogel, graphene oxide, polyethylene glycol, synthesis

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Authors: Ahmed Salim, A. El Bouari, M. Tahiri, O. Tanane

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This research aims to develop and comprehensively characterize a cost-effective activated carbon derived from date residues, with a focus on optimizing its physicochemical properties to achieve superior performance in a variety of applications. The samples were synthesized via a chemical activation process utilizing phosphoric acid (H₃PO₄) as the activating agent. Activated carbon, produced through this method, functions as a vital adsorbent for the removal of contaminants, with a specific focus on methylene blue, from industrial wastewater. This study meticulously examined the influence of various parameters, including carbonization temperature and duration, on both the combustion properties and adsorption efficiency of the resultant material. Through extensive analysis, the optimal conditions for synthesizing the activated carbon were identified as a carbonization temperature of 600°C and a duration of 2 hours. The activated carbon synthesized under optimized conditions demonstrated an exceptional carbonization yield and methylene blue adsorption efficiency of 99.71%. The produced carbon was subsequently characterized using X-ray diffraction (XRD) analysis. Its effectiveness in the adsorption of methylene blue from contaminated water was then evaluated. A comprehensive assessment of the adsorption capacity was conducted by varying parameters such as carbon dosage, contact time, initial methylene blue concentration, and pH levels.

Keywords: environmental pollution, adsorbent, activated carbon, phosphoric acid, date Kernels, pollutants, adsorption

Procedia PDF Downloads 41

Authors: Kishor C. Poria, Deepak Adroja, Arvind Bajaj

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During the last few decades, the growth of single crystals has attained enormous importance for both academic research and technology. Single crystals are pillars of modern technology. In recent emerging trends of photonics and optoelectronics technology, there has been increased need for organic and semi organic materials for Non-Linear Optical (NLO) applications. The paper dealt with the initiation of good single crystals of thiourea and metal doped thiourea. The authors have successfully grown thiourea (pure) and metal doped thiourea crystals using relatively simple and inexpensive slow evaporation of aqueous solution technique. Pure thiourea crystals were grown with different light intensities and frequencies as there growth conditions. Metals (Cu, Co, Ni, Fe) doped crystals were grown using a simple evaporation technique. The paper explains growth methods and associated grown parameters in detail. The average size of the crystal is varied in size from 40 mm x 1mm to 1.5 mm x 1.5 mm to 0.5 mm. Crystals obtained are hexagonal, tetragonal, and rectangular in shape with different optical qualities. All grown crystals are characterized using X-Ray Diffraction Analysis (XRD), Ultra Violet Visible analysis, and Fourier Transform Infrared Spectrometry. Their non-linear optical characteristics were determined by Second Harmonic Generation (SHG) and their Laser Dispersive analysis. The grown crystals are characterized using Nd:YAG laser and the highest conversion efficiency of the signal pass light are calculated. It shows 58 % of standard values for KDP crystals. All results are summarized in this work.

Keywords: crystal, metal-doped thiourea, non-linear optical, NLO, thiourea

Procedia PDF Downloads 136

Authors: Augustas Vaitkevicius, Mikhail Korjik, Eugene Tretyak, Ekaterina Trusova, Gintautas Tamulaitis

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Silicate materials are widely used as luminescent materials in amorphous and crystalline phase. Lithium silicate glass is popular for making neutron sensitive scintillation glasses. Cerium-doped single crystalline silicates of rare earth elements and yttrium have been demonstrated to be good scintillation materials. Due to their high thermal and photo-stability, silicate glass ceramics are supposed to be suitable materials for producing light converters for high power white light emitting diodes. In this report, the influence of glass composition and crystallization on photoluminescence (PL) of different silicate glasses was studied. Barium (BaO-2SiO₂) and lithium (Li₂O-2SiO₂) glasses were under study. Cerium, dysprosium, erbium and europium ions as well as their combinations were used for doping. The influence of crystallization was studied after transforming the doped glasses into glass ceramics by heat treatment in the temperature range of 550-850 degrees Celsius for 1 hour. The study was carried out by comparing the photoluminescence (PL) spectra, spatial distributions of PL parameters and quantum efficiency in the samples under study. The PL spectra and spatial distributions of their parameters were obtained by using confocal PL microscopy. A WITec Alpha300 S confocal microscope coupled with an air cooled CCD camera was used. A CW laser diode emitting at 405 nm was exploited for excitation. The spatial resolution was in sub-micrometer domain in plane and ~1 micrometer perpendicularly to the sample surface. An integrating sphere with a xenon lamp coupled with a monochromator was used to measure the external quantum efficiency. All measurements were performed at room temperature. Chromatic properties of the light emission from the glasses and glass ceramics have been evaluated. We observed that the quantum efficiency of the glass ceramics is higher than that of the corresponding glass. The investigation of spatial distributions of PL parameters revealed that heat treatment of the glasses leads to a decrease in sample homogeneity. In the case of BaO-2SiO₂: Eu, 10 micrometer long needle-like objects are formed, when transforming the glass into glass ceramics. The comparison of PL spectra from within and outside the needle-like structure reveals that the ratio between intensities of PL bands associated with Eu²⁺ and Eu³⁺ ions is larger in the bright needle-like structures. This indicates a higher degree of crystallinity in the needle-like objects. We observed that the spectral positions of the PL bands are the same in the background and the needle-like areas, indicating that heat treatment imposes no significant change to the valence state of the europium ions. The evaluation of chromatic properties confirms applicability of the glasses under study for fabrication of white light sources with high thermal stability. The ability to combine barium and lithium glass matrixes and doping by Eu, Ce, Dy, and Tb enables optimization of chromatic properties.

Keywords: glass ceramics, luminescence, phosphor, silicate

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Authors: Carolin Lutz, Jörg Matthes, Patrick Waibel, Ulrich Precht, Krassimir Garbev, Günter Beuchle, Uwe Schweike, Peter Stemmermann, Hubert B. Keller

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Online measurement of the product quality is a challenging task in cement production, especially in the production of Celitement, a novel environmentally friendly hydraulic binder. The mineralogy and chemical composition of clinker in ordinary Portland cement production is measured by X-ray diffraction (XRD) and X ray fluorescence (XRF), where only crystalline constituents can be detected. But only a small part of the Celitement components can be measured via XRD, because most constituents have an amorphous structure. This paper describes the development of algorithms suitable for an on-line monitoring of the final processing step of Celitement based on NIR-data. For calibration intermediate products were dried at different temperatures and ground for variable durations. The products were analyzed using XRD and thermogravimetric analyses together with NIR-spectroscopy to investigate the dependency between the drying and the milling processes on one and the NIR-signal on the other side. As a result, different characteristic parameters have been defined. A short overview of the Celitement process and the challenging tasks of the online measurement and evaluation of the product quality will be presented. Subsequently, methods for systematic development of near-infrared calibration models and the determination of the final calibration model will be introduced. The application of the model on experimental data illustrates that NIR-spectroscopy allows for a quick and sufficiently exact determination of crucial process parameters.

Keywords: calibration model, celitement, cementitious material, NIR spectroscopy

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Authors: Yih-Chien Chen, Yue-Xuan Du, Min-Zhe Weng

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Carbon monoxide is a substance produced by the incomplete combustion. It is toxic even at concentrations of less than 100ppm. Since it is colorless and odorless, it is difficult to detect. CO sensors have been developed using a variety of physical mechanisms, including semiconductor oxides, solid electrolytes, and organic semiconductors. Many works have focused on using semiconducting sensors composed of sensitive layers such as ZnO, TiO₂, and NiO with high sensitivity for gases. However, these sensors working at high temperatures increased their power consumption. On the other hand, the dielectric resonator (DR) is attractive for gas detection due to its large surface area and sensitivity for external environments. Materials that are to be employed in sensing devices must have a high-quality factor. Numerous researches into the fergusonite-type structure and related ceramic systems have explored. Extensive research into RENbO₄ ceramics has explored their potential application in resonators, filters, and antennas in modern communication systems, which are operated at microwave frequencies. Nd(Ti₀.₅W₀.₅)O₄ ceramics were synthesized herein using the conventional mixed-oxide method. The Nd(Ti₀.₅W₀.₅)O₄ ceramics were prepared using the conventional solid-state method. Dielectric constants (εᵣ) of 15.4-19.4 and quality factor (Q×f) of 3,600-11,100 GHz were obtained at sintering temperatures in the range 1425-1525°C for 4 h. The dielectric properties of the Nd(Ti₀.₅W₀.₅)O₄ ceramics at microwave frequencies were found to vary with the sintering temperature. For a further understanding of these microwave dielectric properties, they were analyzed by densification, X-ray diffraction (XRD), and by making microstructural observations.

Keywords: dielectric constant, dielectric resonators, sensors, quality factor

Procedia PDF Downloads 256

Authors: Masoumeh Tabatabaee, Zahra Shahryarzadeh, Masoud R. Shishebor

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Advanced oxidation process (AOPs) is alternative method for the complete degradation many organic pollutants. When a photocatalyst absorbs radiation whose energy hν > Eg an ē from its filled valance band (VB) is promoted to its conduction band (CB) and valance band holes h+ are formed. Electron would reduce any available species, including O2, water and hydroxide ion to form hydroxyl radicals. ZnO and TiO2 are important photocatalysts with high catalytic activity that have attracted much research attention. TiO2 can only absorb a small portion of solar spectrum in the UV region and many methods such as dye sensitization, doping of other metals and using TiO2 with another semiconductor have been used to improve the photocatalytic activity of TiO2 under solar irradiation. Studies have shown that the use of metal oxides or sulfide such as WO3, MoO3, SiO2, MgO, ZnO, and CdS with TiO2 can significantly enhance the photocatalytic activity of TiO2. Due to similarity of photodegradation mechanism of ZnO with TiO2, it is a suitable semiconductor using with TiO2 and recently nanosized bicomponent TiO2-ZnO photocatalysts were prepared and used for degradation of some pollutants. In this study, Nano-sized ZnO/TiO2 composite was synthesized. Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) and scanning electron microscope (SEM) were used to characterize the structure and morphology of it. The effect of photocatalytic activity of prepared ZnO/TiO2 on the degradation of cyanide ion under UV was investigated. The effect of various parameters such as ZnO/TiO2 concentration, amount of photocatalyst, amount of H2O2, initial dye or cyanide ion concentration, pH and irradiation time on were investigated. Results show that more than 95% of 4 mgL-1 cyanide ion degraded after 60-min reaction time and under UV irradiation.

Keywords: photodegradation, ZnO/TiO2, nanoparticle, cyanide ion

Procedia PDF Downloads 390