Search results for: in-situ synchrotron X-ray diffraction

Authors: Navneet Dabra, Baljinder Kaur, Lakhbir Singh, V. Annapu Reddy, R. Nath, Dae-Yong Jeong, Jasbir S. Hundal

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The ferroelectric properties of fused potassium nitrate (KNO3)- polyvinyl alcohol (PVA) composite films have been investigated. The composite films of KNO3-PVA have been prepared by solvant cast technique and then fused over the brass substrate. The ferroelectric hysteresis loops (P-E) have been obtained at room temperature using modified Sawyer-Tower circuit. Percentage of back switching and differential dielectric constant has been derived from P-V loops. The x-ray diffraction (XRD) studies confirm the formation of ferroelectric phase (phase III) in these composite films. The AFM and FE-SEM studies have been used to study the surface morphology of these composite films. The values of remanemt polarization, coercive field, back switching, crystallite size, lattice parameters, and surface roughness have been estimated and correlated.

Keywords: ferroelectric polymer composite, remanemt polarization, back switching, crystallite size, lattice parameters and surface roughness

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Authors: Suneeta Kumari, Abanti Sahoo

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Industrial effluents treatment is a major problem in the world. All wastewater treatment methods have some problems in the environment. Due to this reason, today many natural biopolymers are being used in the waste water treatment because those are safe for our environment. In this study, synthesis and characterization of polyethersulfone/chitosan membranes (Thin film composite membrane) are carried out. Fish scales are used as raw materials. Different characterization techniques such as Fourier transform infrared spectroscopy (FTIR), X-ray powder diffraction (XRD), scanning electron microscope (SEM) and Thermal gravimetric analysis (TGA) are analysed for the synthesized membrane. The performance of membranes such as flux, rejection, and pore size are also checked. The synthesized membrane is used for the treatment of steel industry waste water where Biochemical oxygen demand (BOD), Chemical Oxygen Demand (COD), pH, colour, Total dissolved solids (TDS), Total suspended solids (TSS), Electrical conductivity (EC) and Turbidity aspects are analysed.

Keywords: fish scale, membrane synthesis, treatment of industrial effluents, chitosan

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Authors: Leila Mosafa, Majid Moghadam, Mohammad Shahedi

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In this work, pectinase was immobilized on the surface of silica-coated magnetite nanoparticles via covalent attachment. The magnetite-immobilized enzyme was characterized by Fourier transform infrared spectroscopy, X-ray powder diffraction, scanning electron microscopy and vibrating sample magnetometry techniques. Response surface methodology using Minitab Software was applied for statistical designing of operating conditions in order to immobilize pectinase on magnetic nanoparticles. The optimal conditions were obtained at 30°C and pH 5.5 with 42.97 µl pectinase for 2 h. The immobilization yield was 50.6% at optimized conditions. Compared to the free pectinase, the immobilized pectinase was found to exhibit enhanced enzyme activity, better tolerance to the variation of pH and temperature, and improved storage stability. Both free and immobilized samples reduced the viscosity of apple juice from 1.12 to 0.88 and 0.92 mm2s-1, respectively, after 30 min at their optimum temperature. Furthermore, the immobilized enzyme could be reused six consecutive cycles and the efficiency loss in viscosity reduction was found to be only 8.16%.

Keywords: magnetite nanoparticles, pectinase enzyme, immobilization, juice clarification, enzyme activity

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Authors: Ammar Z. Alshemary, Zafer Evis

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In this study, nanorods of Cr³⁺/SiO₄⁴⁻ codoped hydroxyapatite (Cr³⁺/SiO₄⁴⁻-HA) were synthesized successfully and rapidly through microwave irradiation technique, using (Ca(NO₃)₂•4H₂O), ((NH₄)₂HPO₄), (SiC₈H₂₀O₄) and (Cr(NO₃)₃.9H₂O) as source materials for Ca²⁺, PO₄³⁻, SiO₄⁴⁻ and Cr³⁺ ions, respectively. The impact of dopants on the phase formation and microstructure of the powders were investigated by means of X-ray diffraction (XRD), Fourier transform infrared spectrum analysis (FT-IR) and Field emission electron microscopy (FESEM) techniques. XRD analysis showed that with an incorporation of Cr³⁺/SiO₄⁴⁻ ions into HA structure resulted in peak broadening and reduced peak height due to the amorphous nature and reduced crystallinity of the resulting HA powder. FTIR spectroscopy revealed the existence of the different vibrational modes matching to phosphates and hydroxyl groups. The FESEM analysis showed a change in the crystal shape from spherical to rod shaped particles upon Cr³⁺ doping into the crystal structure. Acknowledgments: This study was supported by Karabük University (Project no. KBÜBAP-17-YD-144). The authors would like to thank for support.

Keywords: nano-hydroxyapatite, microwave, dopants, characterization, microstructure

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Authors: Farid Amidi Fazli, Afshin Babazadeh, Farnaz Amidi Fazli

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In contrast with literal meaning of nano, researchers have been achieving mega adventures in this area and every day more nanomaterials are being introduced to the market. After long time application of fossil-based plastics, nowadays accumulation of their waste seems to be a big problem to the environment. On the other hand, mankind has more attention to safety and living environment. Replacing common plastic packaging materials with degradable ones that degrade faster and convert to non-dangerous components like water and carbon dioxide have more attractions; these new materials are based on renewable and inexpensive sources of starch and cellulose. However, the functional properties of them do not suitable for packaging. At this point, nanotechnology has an important role. Utilizing of nanomaterials in polymer structure will improve mechanical and physical properties of them; nanocrystalline cellulose (NCC) has this ability. This work has employed a chemical method to produce NCC and starch bio nanocomposite containing NCC. X-Ray Diffraction technique has characterized the obtained materials. Results showed that applied method is a suitable one as well as applicable one to NCC production.

Keywords: biofilm, cellulose, nanocomposite, starch

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Authors: Wenliang Song, Yu Zhang, Hua Jin, Il Kim

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The self-assembly of the polypeptide (PP) into well-defined structures at different length scales is both biomimetic relevant and fundamentally interesting. Although there are various reports of nanostructures fabricated by the self-assembly of various PPs, directed self-assembly of PP into three-dimensional (3D) hierarchical structure has proven to be difficult, despite their importance for biological applications. Herein, an efficient method has been developed through living polymerization of phenylalanine N-Carboxy anhydride (NCA) towards the linear and cyclic polyphenylalanine, and the new invented swelling methodology can form diverse hierarchical polypeptide crystals. The solvent-dependent self-assembly behaviors of these homopolymers were characterized by high-resolution imaging tools such as atomic force microscopy, transmission electron microscopy, scanning electron microscope. The linear and cyclic polypeptide formed 3D nano hierarchical shapes, such as a sphere, cubic, stratiform and hexagonal star in different solvents. Notably, a crystalline packing model was proposed to explain the formation of 3D nanostructures based on the various diffraction patterns, looking forward to give an insight for their dissimilar shape inflection during the self-assembly process.

Keywords: self-assembly, polypeptide, bio-polymer, crystalline polymer

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Authors: Sidi Mohamed Mesli, Mohamed Habchi, Arslane Boudghene Stambouli, Rafik Benallal

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The BaMnMF7 (M=Fe,V, transition metal fluoride glass, assuming isomorphous replacement) have been structurally studied through the simultaneous simulation of their neutron diffraction patterns by reverse Monte Carlo (RMC) and by the Hybrid Reverse Monte Carlo (HRMC) analysis. This last is applied to remedy the problem of the artificial satellite peaks that appear in the partial pair distribution functions (PDFs) by the RMC simulation. The HRMC simulation is an extension of the RMC algorithm, which introduces an energy penalty term (potential) in acceptance criteria. The idea of this work is to apply the Buckingham potential at the title glass by ignoring the van der Waals terms, in order to make a fit of the partial pair distribution functions and give the most possible realistic features. When displaying the partial PDFs, we suggest that the Buckingham potential is useful to describe average correlations especially in similar interactions.

Keywords: fluoride glasses, RMC simulation, hybrid RMC simulation, Buckingham potential, partial pair distribution functions

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Authors: Mingchuan Zhou, Haitao Zhang, Hongfang Ma, Weiyong Ying

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Alumina supported PtSn catalysts with cylindrical particles were prepared and characterized by using low temperature N2 adsorption/desorption and X-ray diffraction. Low temperature N2 adsorption/desorption demonstrate that the tableting changed the texture properties of catalysts. XRD pattern indicate that the crystal structure of supports had no change after reaction. The performances over particles of PtSn/Al2O3 catalysts were investigated with regards to reaction temperature, pressure, and H2/AcOH mole ratio. After tableting, the conversion of acetic acid and selectivity of ethanol and acetyl acetate decreased. High reaction temperature and pressure can improve conversion of acetic acid. H2/AcOH mole ratio of 9.36 showed the best performance on acetic acid hydrogenation. High pressure had benefits for the selectivity of ethanol and other two parameters had no obvious effect on selectivity.  

Keywords: acetic acid hydrogenation, cylindrical particles, ethanol, PtSn

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Authors: Indah Kurniawaty, Yoki Yulizar, Haryo Satriya Oktaviano, Adam Kusuma Rianto

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Magnesium oxide nanoparticles (MgO NP) were successfully synthesized in this study using a one-pot green synthesis mediated by Calliandra Calothyrsus leaf extract (CLE). CLE was prepared by maceration of the leaf using methanol with a ratio of 1:5 for 7 days. Secondary metabolites in CLE, such as alkaloids and flavonoids, served as a weak base provider and capping agent in the formation of MgO NP. CLE Fourier Transform Infra-Red (FTIR) spectra peak at 3255, 1600, 1384, 1205, 1041, and 667 cm-1 showing the presence of vibrations O-H stretching, N-H bending, C-C stretching, C-N stretching and N-H wagging. During the experiment, different CLE volumes and calcined temperatures were used, resulting in a variety of structures. Energy Dispersive X-ray Spectrometer (EDS) and FTIR were used to characterize metal oxide particles. MgO diffraction pattern at 2θ of 36.9°; 42.9°; 62.2°; 74.6°; and 78.5° which can be assigned to crystal planes (111), (200), (220), (311), and (222), respectively. Scanning Electron Microscopy (SEM) was used to characterize the surface morphology. The morphology ranged from sphere to flower-like resulting in crystallite sizes of 28, 23, 12, and 9 nm.

Keywords: MgO, nanoparticle, calliandra calothyrsus, green-synthesis

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Authors: Xiaohong Yang, Haitao Fu, Xizhong An, Aibing Yu

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Silver@titanium dioxide (Ag@TiO2) core-shell nanostructures and Ag surface doped TiO2 particles (TiO2@Ag) have been designed and synthesized by sol-gel and hydrothermal methods under mild conditions. These two types of Ag/TiO2 nanocomposites were characterized in terms of their properties by various techniques such as transmission electron microscope (TEM), X-ray diffraction (XRD), Brunauer Emmett Teller (BET) and ultra violet-visible absorption spectroscopy (UV-Vis). Specifically, the photocatalystic performance and antibacterial behavior of such nanocomposites have been investigated and compared. It was found that The Ag@TiO2 core-shell nanostructures exhibit superior photocatalytic property to the Ag surface doped TiO2 particles under the reported conditions. While with UV pre-irradiation, the Ag@TiO2 core-shell composites exhibit better bactericidal performance. This is probably because the Ag cores tend to facilitate charge separation for TiO2, producing greater hydroxyl radicals on the surface of the TiO2 particles. These findings would be useful for the design and synthesis of Ag/TiO2 nanocomposites with desirable photocatalystic and antimicrobial activity for environmental applications.

Keywords: Ag@TiO2 core-shell nanoparticles, Ag surface doped TiO2 nanoparticles, photocatalysis, antibacterial

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Authors: F. Amor, A. Bouregba, N. El Fami, A. Diouri

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This study provides insights into the role of alkalis in modifying the hydration kinetics and microstructural development of β-dicalcium silicate, highlighting potential pathways for enhancing the performance of belite-based cements in various construction applications. It investigates the behavior of β-dicalcium silicates (β-Ca₂SiO₄) when hydrated in various alkaline environments, including deionized water and solutions containing 2M concentrations of Na₂CO₃, NaOH, KOH, and water glass. The dicalcium silicate was synthesized with laboratory reagents, calcium carbonate, and gel silica. The hydration process was carried out over different periods, ranging from 7 to 90 days. The hydrated samples were characterized using X-ray diffraction, infrared spectroscopy, and scanning electron microscopy, while the mechanical strength tests were performed at 28 and 90 days. The results indicate that the presence of alkalis significantly influences the hydration of belite cement. Early hydration is accelerated, which is evident from the faster dissolution of C₂S, a decrease in C₂S peaks, and the formation of C-S-H products, including sodium-containing C-(N)-S-H and potassium-containing C-(K)-S-H.

Keywords: dicalcium silicate, alkali activator, hydration, water glass, Na₂CO₃, NaOH, KOH

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Authors: Aiswarea Mathew, Smita Mohanty, Jr., S. K. Nayak

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Polyurethane networks based on castor oil (CO) as a renewable resource polyol were synthesized. Polyurethane/epoxy resin interpenetrating network nanocomposites containing modified montmorillonite organoclay (C30B-PU/EP nanocomposites) were prepared by an in situ intercalation method. The conventional spectroscopic characterization of the synthesized samples using FT-IR confirms the existence of the proposed castor oil based PU structure and also showed that strong interactions existed between C30B and EP/PU matrix. The dispersion degree of C30B in EP/PU matrix was characterized by X-Ray diffraction (XRD) method. Scanning electronic microscopy analysis showed that the interpenetrating process of PU and EP increases the exfoliation degree of C30B, and it improves the compatibility and the phase structure of polyurethane/epoxy resin interpenetrating polymer networks (PU/EP IPNs). The thermal stability improves compared to the polyurethane when the PU/EP IPN is formed. Mechanical properties including the Young’s modulus and tensile strength reflected marked improvement with addition of C30B.

Keywords: castor oil, epoxy, montmorillonite, polyurethane

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Authors: H. Farokhi, A. Bahadoran

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This paper is focused on the absorbance and magnetic properties of a novel nanocomposite based on conducting polymer, carbon black and barium hexaferrite in epoxy resin on the E-glass fibre substrate. The highly conductive nanocomposite was provided by in-situ polymerization of aniline in the presence of carbon black (C) and barium hexaferrite (BaFe12O19) as electromagnetic absorbance material. The structure, morphology, and magnetic properties of samples were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). SEM images showed the uniformly coated PAni on the surface of carbon black and barium hexaferrite. XRD peaks also verified the presence of carbon black and barium hexaferrite in the nanocomposite. The microwave characteristics determined from the magnetic and dielectric properties of the elastomeric composites obtained from scattering data by fitting the samples in a waveguide, where measured in the frequency in X-band frequency range, the range of 8 to 12 GHz. The reflection losses were evaluated to be less than −5dB over the whole X-band frequency (8–12 GHz) for the thickness of 1.4mm.

Keywords: conductive polymer, magnetic materials, capacitance, electrochemical cell

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Authors: Raghvendra Singh Yadav, Ivo Kuřitka

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In this report, we studied the impact of Gd3+ substitution on structural, magnetic and electrical properties of CoFe2O4 nanoparticles synthesized by sonochemical method. X-ray diffraction pattern confirmed the formation of cubic spinel structure at low concentration of Gd3+ ions, however, GdFeO3 additional phase was observed at higher concentration of Gd3+ ions. Raman and Fourier Transform Infrared spectroscopy study also confirmed cubic spinel structure of Gd3+ substituted CoFe2O4 nanoparticles. The field emission scanning electron microscopy study revealed that Gd3+ substituted CoFe2O4 nanoparticles were in the range of 5-20 nm. The magnetic properties of Gd3+ substituted CoFe2O4 nanoparticles were investigated by using vibrating sample magnetometer. The variation in saturation magnetization, coercivity and remanent magnetization with Gd3+ concentration in CoFe2O4 nanoparticles was observed. The variation of real and imaginary part of dielectric constant, tan δ, and AC conductivity were studied at room temperature.

Keywords: spinel ferrites, nanoparticles, sonochemical method, magnetic properties

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Authors: C. D. Gomez-Esparza, Z. V. Hernandez-Castro, C. A. Rodriguez-Gonzalez, R. Martinez-Sanchez, A. Duarte-Moller

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Recently, the high entropy alloys (HEA) are the focus of attention in metallurgical and materials science due to their desirable and superior properties in comparison to conventional alloys. The HEA field has promoted the exploration of several compositions including the addition of non-metallic elements like carbon, which in traditional metallurgy is mainly used in the steel industry. The aim of this work was the synthesis of equiatomic FeCrNiMnTi high entropy alloys, with minor carbon content, by mechanical alloying and sintering. The effect of the addition of carbon nanotubes and graphite were evaluated by X-ray diffraction, scanning electron microscopy, and microhardness test. The structural and microstructural characteristics of the equiatomic alloys, as well as their hardness were compared with those of an austenitic AISI 321 stainless steel processed under the same conditions. The results showed that porosity in bulk samples decreases with carbon nanotubes addition, while the equiatomic composition favors the formation of titanium carbide and increased the AISI 321 hardness more than three times.

Keywords: carbon nanotubes, graphite, high entropy alloys, mechanical alloying

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Authors: Nuray Güy, Mahmut Özacar

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Semiconductor nanoparticles such as TiO₂ and ZnO as photocatalysts are very efficient catalysts for wastewater treatment by the chemical utilization of light energy, which is capable of converting the toxic and nonbiodegradable organic compounds into carbon dioxide and mineral acids. ZnO semiconductor has a wide bandgap energy of 3.37 eV and a relatively large exciton binding Energy (60 meV), thus can absorb only UV light with the wavelength equal to or less than 385 nm. It exhibits low efficiency under visible light illumination due to its wide band gap energy. In order to improve photocatalytic activity of ZnO under visible light, band gap of ZnO may be narrowed by doping such as N, C, S nonmetal ions and coupled two separate semiconductors possessing different energy levels for their corresponding conduction and valence bands. ZnS has a wider band gap (Eg=3.7 eV) than ZnO and generates electron–hole pairs by photoexcitation rapidly. In the present work, N doped ZnO/ZnS nano photocatalysts with visible-light response were synthesized by microwave-hydrothermal method using thiourea as N source. The prepared photocatalysts were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and UV–visible (UV–vis). The photocatalytic activities samples and undoped ZnO have been studied for the degradation of dye, and have also been compared with together.

Keywords: photocatalyst, synthesis, visible light, ZnO/ZnS

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Authors: Abbas Nasir, Xiong Zhang, Sohail Ahmad, Yiping Cui

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Non-polar a-plane AlGaN epilayers of high structural quality have been grown on r-sapphire substrate by using metalorganic chemical vapor deposition (MOCVD). A graded non-polar AlGaN buffer layer with variable aluminium concentration was used to improve the structural quality of the non-polar a-plane AlGaN epilayer. The characterisations were carried out by high-resolution X-ray diffraction (HR-XRD), atomic force microscopy (AFM) and Hall effect measurement. The XRD and AFM results demonstrate that the Al-composition-graded non-polar AlGaN buffer layer significantly improved the crystalline quality and the surface morphology of the top layer. A low root mean square roughness 1.52 nm is obtained from AFM, and relatively low background carrier concentration down to 3.9×  cm^-3 is obtained from Hall effect measurement.

Keywords: non-polar AlGaN epilayer, Al composition-graded AlGaN layer, root mean square, background carrier concentration

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Authors: Ahmet Yönetken

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Al metal matrix composites reinforced with AlN have been fabricated by Tube furnace sintering at various temperatures. A uniform nickel layer on Al(%1AlN)%19Ni, Al(%2AlN)%18Ni, Al(%3AlN)%17Ni, Al(%4AlN)%16Ni, Al(%5AlN)%15Ni powders were deposited prior to sintering using electroless plating technique, allowing closer surface contact than can be achieved using conventional methods such as mechanical alloying. A composite consisting of quaternary additions, a ceramic phase, AlN, within a matrix of Al, AlN, Ni has been prepared at the temperature range between 550°C and 650°C under Ar shroud. X-Ray diffraction, SEM (Scanning Electron Microscope) density, and hardness measurements were employed to characterize the properties of the specimens. Experimental results carried out for 650°C suggest that the best properties as comprehension strength σmax and hardness 681.51(HV) were obtained at 650°C, and the tube furnace sintering of electroless Al plated (%5AlN)%15Ni powders is a promising technique to produce ceramic reinforced Al (%5AlN)%15Ni composites.

Keywords: electroless nickel plating, ceramic-metal composites, powder metallurgy, sintering

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Authors: Kaiyuan Chena, Senentxu Lanceros-Méndeza, Laijun Liub, Qi Zhanga

Abstract:

0.6Bi(Mg1/2Ti1/2)O3-0.4Ba0.8Ca0.2(Nb0.125Ti0.875)O3 (0.6BMT-0.4BCNT) ceramics with a pseudo-cubic structure and re-entrant dipole glass behavior have been investigated via X-ray diffraction and dielectric permittivity-temperature spectra. It shows an excellent dielectric-temperature stability with small variations of dielectric permittivity (± 5%, 420 - 802 K) and dielectric loss tangent (tanδ < 2.5%, 441 - 647 K) in a wide temperature range. Three dielectric anomalies are observed from 290 K to 1050 K. The low-temperature weakly coupled re-entrant relaxor behavior was described using Vogel-Fulcher law and the new glass model. The mid- and high-temperature dielectric anomalies are characterized by isothermal impedance and electrical modulus. The activation energy of both dielectric relaxation and conductivity follows the Arrhenius law in the temperature ranges of 633 - 753 K and 833 - 973 K, respectively. The ultrahigh thermal stability of the dielectric permittivity is attributed to the weakly coupling of polar clusters, the formation of diffuse phase transition (DPT) and the local phase transition of calcium-containing perovskite.

Keywords: permittivity, relaxor, electronic ceramics, activation energy

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Authors: K. N. Kipreou, E. Efthmiadou, G. Kordas

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Biofouling represents one of the most crucial problems in the present maritime industries when its control still challenges the researchers all over the world. The present work is referred to the synthesis and characterization CeMo and Cu2O nanocontainers by using a wide range of techniques including scanning electron microscopy (SEM), X-ray diffraction (XRD) and thermogravimetric analysis (TGA) for marine applications. The above nanosystems will be loaded with active monomers and corrosion rendering healing ability to marine paints. The objective of this project is their ability for self-healing, self-polishing and finally for anti-corrosion activity. One of the driving forces for the exploration of CeMo, is the unique anticorrosive behavior, which will be confirmed by the electrochemistry methodology. It has be highlighted that the nanocontainers of Cu2O with the appropriate antibacterial inhibitor will improve the hydrophobicity and the morphology of the coating surfaces reducing the water friction. In summary, both novel nanoc will increase the lifetime of the paints releasing the antifouling agent in a control manner.

Keywords: marinepaints, nanocontainer, antifouling, anticorrosion, copper, electrochemistry, coating, biofouling, inhibitors, copper oxide, coating, SEM

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Authors: H. Maachou, A. Chagnes, G. Cote

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The present work reports the properties of chitosan/hydroxyapatite (Cs/HA: 100/00, 70/30 and 30/70) composite microspheres obtained by emulsification processing route. The morphology of chitosane microspheres was observed by a scanning electron microscope (SEM) which shows an aggregate of spherical microspheres with a particle size, determined by optical microscope, ranged from 4 to 10 µm. Thereafter, a biomimetic approach was used to study the in vitro biomineralization of these composites. It concerns the composites immersion in simulated body fluid (SBF) for different times. The deposited calcium phosphate was studied using X-ray diffraction analysis (XRD), FTIR spectroscopy and ICP analysis of phosphorus. In fact, the mineral formed on Cs/HA microspheres was a mixture of carbonated HA and β-TCP as showed by FTIR peaks at 1419,5 and 871,8 cm-1 and XRD peak at 29,5°. This formation was induced by the presence of HA in chitosan microspheres. These results are confirmed by SEM micrographs which chow the Ca-P crystals growth in form of cauliflowers. So, these materials are of great interest for bone regeneration applications due to their ability to nucleate calcium phosphates in presence of simulated body fluid (SBF).

Keywords: hydroxyapatite, chitosan, microsphere, composite, bone regeneration

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Authors: Yong Pan, Li Wang, Xue Qiong Su, Dong Wen Gao

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To date, nanomaterials have received extensive attention over the years because of their wide application. Various nanomaterials such as nanoparticles, nanowire, nanoring, nanostars and other nanostructures have begun to be systematically studied. The preparation of these materials by chemical methods is not only costly, but also has a long cycle and high toxicity. At the same time, preparation of nanoparticles of multi-doped composites has been limited due to the special structure of the materials. In order to prepare multi-doped composites with the same structure as macro-materials and simplify the preparation method, the Ga_xCo_1-xZnSe_0.4 (x = 0.1, 0.3, 0.5) nanoparticles are prepared by Pulse Laser Ablation (PLA) method. The particle component and structure are systematically investigated by X-ray diffraction (XRD) and Raman spectra, which show that the success of our preparation and the same concentration between nanoparticles (NPs) and target. Morphology of the NPs characterized by Transmission Electron Microscopy (TEM) indicates the circular-shaped particles in preparation. Fluorescence properties are reflected by PL spectra, which demonstrate the best performance in concentration of Ga_0.3Co_0.3ZnSe_0.4. Therefore, all the results suggest that PLA is promising to prepare the multi-NPs since it can modulate performance of NPs.

Keywords: PLA, physics, nanoparticles, multi-doped

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Authors: Essam Shalaby, Alexander Churyumov, Malak Abou El-Khair, Atef Daoud

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A comparative study of the thermal and mechanical behavior of squeezed A359 composites containing 5, 10 and 15 wt.% SiC, (SiC+ Si3N4) and AlN particulates was investigated. Stir followed by squeeze casting techniques are used to produce A359 composites. It was noticed that, A359/AlN composites have high thermal conductivity as compared to A359 alloy and even to A359/SiC or A359/(SiC+Si3N4) composites. Microstructures of the composites have shown homogeneous and even distribution of reinforcements within the matrix. Interfacial reactions between particles and matrix were investigated using X-ray diffraction and energy dispersive X-ray analysis. The presence of particles led not only to increase peak hardness of the composites but also to accelerate the aging kinetics. As compared with A359 matrix alloy, compression test of the composites has exhibited a significant increase in the yield and the ultimate compressive strengths with a relative reduction in the failure strain. Those light weight composites have a high potential to be used for automotive and aerospace applications.

Keywords: metal-matrix composite, squeeze, microstructure, thermal conductivity, compressive properties

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Authors: B. Benalioua, I. Benyamina, A. Bentouami, B. Boury

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The objective of this study is based on the synthesis of a new photocatalyst based on TiO2 and its application in the photo-degradation of an acid dye under the visible light. The material obtained was characterized by different techniques like diffuse reflectance UV–Vis spectroscopy (DRS), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The photocatalytic efficiency of the Bi, N co-doped TiO2 treated at 600°C for 1 h was tested on the Indigo Carmine under the irradiation of visible light and compared with that of the commercial titanium oxide TiO2-P25 (Degussa). The XRD characterization of the material Bi -N- TiO2 (600°C) revealed the presence of the anatase phase and the absence of the rutile phase in comparison of the TiO2 P25 diffractogram. Characterization by UV- visible diffuse reflection (DRS) material showed that the Bi-N-TiO2 exhibits redshift (move visible) relative to commercial titanium oxide TiO2-P25, this property promises a photocatalytic activity of Bi-N-TiO2 under visible light. Indeed, the efficiency of photocatalytic Bi-N-TiO2 as a visible light is shown by a complete discoloration of indigo carmine solution of 16 mg/L after 40 minutes, whereas with the P25-TiO2 discoloration is achieved after 90 minutes.

Keywords: POA, heterogeneous photocatalysis, TiO2, co-doping

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Authors: Benamar Makhoukhi

Abstract:

Clay ion-exchange using bismidazolium salts (MBIM) could provide organophilic clays materials that allow effective retention of polluting dyes. The present investigations deal with bentonite (Bt) modification using (ortho, meta and para) bisimidazolium cations and attempts to remove a synthetic textile dyes, such as (Telon-Orange, Telon-Red and Telon-Blue) by adsorption, from aqueous solutions. The surface modification of MBIM–Bt was examined using infrared spectroscopy (FTIR), X-ray diffraction (XRD) and thermogravimetric analysis (TGA). Adsorption tests applied to Telon dyes revealed a significant increase of the maximum adsorption capacity from ca. 21-28 to 88-108 mg.g-1 after intercalation. The highest adsorption level was noticed for Telon-Orange dye on the p-MBIM–Bt, presumably due higher interlayer space and better diffusion. The pseudo-first order rate equation was able to provide the best description of adsorption kinetics data for all three dyestuffs. The Langmuir and Freundlich adsorption models were applied to describe the equilibrium isotherms and the isotherm constants were also determined. The results show that MBIM–Bt could be employed as low-cost material for the removal of Telon dyes from effluents.

Keywords: Bentonite, Organoclay, Bisimidazolium, Dyes, Isotherms, Adsorption

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Authors: Kirsten Techmer, Jan-Erik Rybak, Simon Rudolph

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Natural formed pyrites (FeS2) are frequent sulfides in sedimentary and metamorphic rocks. Growth textures of idiomorphic pyrite assemblages reflect the conditions during their formation in the geologic sequence, furtheron the local texture analyses of the growth patterns of pyrite assemblages by EBSD reveal the possibility to resolve the growth conditions during the formation of pyrite at the micron scale. The spatial resolution of local texture measurements in the Scanning Electron Microscope used can be in the nanomete scale. Orientation contrasts resulting from domains of smaller misorientations within larger pyrite crystals can be resolved as well. The electron optical studies have been carried out in a Field-Emission Scanning Electron Microscope (FEI Quanta 200) equipped with a CCD camera to study the orientation contrasts along the surfaces of pyrite. Idiomorphic cubic single crystals of pyrite, polycrystalline assemblages of pyrite, spherically grown spheres of pyrite as well as pyrite-bearing ammonites have been studied by EBSD in the Scanning Electron Microscope. Samples were chosen to show no or minor secondary deformation and an idiomorphic 3D crystal habit, so the local textures of pyrite result mainly from growth and minor from deformation. The samples studied derived from Navajun (Spain), Chalchidiki (Greece), Thüringen (Germany) and Unterkliem (Austria). Chemical analyses by EDAX show pyrite with minor inhomogeneities e.g., single crystals of galena and chalcopyrite along the grain boundaries of larger pyrite crystals. Intergrowth between marcasite and pyrite can be detected in one sample. Pyrite may form intense growth twinning lamellae on {011}. Twinning, e.g., contact twinning is abundant within the crystals studied and the individual twinning lamellaes can be resolved by EBSD. The ammonites studied show a replacement of the shale by newly formed pyrite resulting in an intense intergrowth of calcite and pyrite. EBSD measurements indicate a polycrystalline microfabric of both minerals, still reflecting primary surface structures of the ammonites e.g, the Septen. Discs of pyrite (“pyrite dollar”) as well as pyrite framboids show growth patterns comprising a typical microfabric. EBSD studies reveal an equigranular matrix in the inner part of the discs of pyrite and a fiber growth with larger misorientations in the outer regions between the individual segments. This typical microfabric derived from a formation of pyrite crystals starting at a higher nucleation rate and followed by directional crystal growth. EBSD studies show, that the growth texture of pyrite in the samples studied reveals a correlation between nucleation rate and following growth rate of the pyrites, thus leading to the characteristic crystal habits. Preferential directional growth at lower nucleation rates may lead to the formation of 3D framboids of pyrite. Crystallographic misorientations between the individual fibers are similar. In ammonites studied, primary anisotropies of the substrates like e.g., ammonitic sutures, influence the nucleation, crystal growth and habit of the newly formed pyrites along the surfaces.

Keywords: Electron Back Scatter Diffraction (EBSD), growth pattern, Fe-sulfides (pyrite), texture analyses

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Authors: Aswin Kumar Krishnan, Yat Choy Wong, Reiza Mukhlis, Zipeng Zhang, Arul Arulrajah

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The continuous increase in vehicle uptake escalates the number of rubber tyre waste which need to be managed to avoid landfilling and stockpiling. The present research focused on the sustainable use of rubber crumbs in clay roof tiles. The properties of roof tiles composed of clay, rubber crumbs, NaOH, and Na₂SiO₃ with a 10% alkaline activator were studied. Tile samples were fabricated by heating the compacted mixtures at 50°C for 72 hours, followed by a higher heating temperature of 200°C for 24 hours. The effect of rubber crumbs aggregates as a substitution for the raw clay materials was investigated by varying their concentration from 0% to 2.5%. X-ray diffraction (XRD) and scanning electron microscopy (SEM) analyses have been conducted to study the phases and microstructures of the samples. It was found that the optimum rubber crumbs concentration was at 0.5% and 1%, while cracks and larger porosity were found at higher crumbs concentrations. Water absorption and compressive strength test results demonstrated that rubber crumbs and clay satisfied the standard requirement for the roof tiles.

Keywords: rubber crumbs, clay, roof tiles, alkaline activators

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Authors: Mahdi Almaky

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Conducting polymer of N-(3-pyrrol-1-yl-propyl)-2,2`-bipyridinium hexafluoro-phosphate (PPBH) was prepared via chemical and electrochemical polymerization methods. The bulk polymer showed conductivity in the order of 10-12 S cm-1. DNA-templated polymer nano wires of PPBH (PolyPPBH-DNA) have been chemically prepared then used as templates to direct the formation of metal nanowires (Cu) in order to enhance the electrical properties of the polymer/DNA wires. The chemical structures, morphology and the electrical characterisation of the as obtained structures have been characterized through spectroscopic (FTIR, UV-vis and XPS), single-crystal X-ray diffraction and microscopic (AFM, EFM and c-AFM) techniques. The morphology of the nanomaterials has been observed by AFM; showing the nanowires are uniform and continuous. The polymer conductivity was slightly improved after metallization. The conductivity of Cu-PolyPPBH-DNA nanowires was estimated to be 7.1x10-2 S cm-1. This conductivity is slightly higher than the conductivity of PolyPPBH-DNA nano wires (2.0 x 10-2 S cm-1), but it is lower than the measurements for PPy/DNA nano wires (2.1 x 10-1 S cm-1) prepared and measured by using c-AFM probe. These results reflect the large effect of the chemical structure (N-substitution) on the electrical properties of these polymers by reducing the extended conjugation.

Keywords: DNA, template, nano wires, N-Alkylatedpyrrole, copper

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Authors: Igor B. Sivaev

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Design of molecular machines is an extraordinary growing and very important area of research that it was recognized by awarding Sauvage, Stoddart and Feringa the Nobel Prize in Chemistry in 2016 'for the design and synthesis of molecular machines'. Based on the type of motion being performed, molecular machines can be divided into two main types: molecular motors and molecular switches. Molecular switches are molecules or supramolecular complexes having bistability, i.e., the ability to exist in two or more stable forms, among which may be reversible transitions under external influence (heating, lighting, changing the medium acidity, the action of chemicals, exposure to magnetic or electric field). Molecular switches are the main structural element of any molecular electronics devices. Therefore, the design and the study of molecules and supramolecular systems capable of performing mechanical movement is an important and urgent problem of modern chemistry. There is growing interest in molecular switches and other devices of molecular electronics based on transition metal complexes; therefore choice of suitable stable organometallic unit is of great importance. An example of such unit is bis(dicarbollide) complexes of transition metals [3,3’-M(1,2-C₂B₉H₁₁)₂]ⁿ⁻. The control on the ligand rotation in such complexes can be reached by introducing substituents which could provide stabilization of certain rotamers due to specific interactions between the ligands, on the one hand, and which can participate as Lewis bases in complex formation with external metals resulting in a change in the rotation angle of the ligands, on the other hand. A series of isomeric methyl sulfide derivatives of cobalt bis(dicarbollide) complexes containing methyl sulfide substituents at boron atoms in different positions of the pentagonal face of the dicarbollide ligands [8,8’-(MeS)₂-3,3’-Co(1,2-C₂B₉H₁₀)₂]⁻, rac-[4,4’-(MeS)₂-3,3’-Co(1,2-C₂B₉H₁₀)₂]⁻ and meso-[4,7’-(MeS)₂-3,3’-Co(1,2-C₂B₉H₁₀)₂]⁻ were synthesized by the reaction of CoCl₂ with the corresponding methyl sulfide carborane derivatives [10-MeS-7,8-C₂B₉H₁₁)₂]⁻ and [10-MeS-7,8-C₂B₉H₁₁)₂]⁻. In the case of asymmetrically substituted cobalt bis(dicarbollide) complexes the corresponding rac- and meso-isomers were successfully separated by column chromatography as the tetrabutylammonium salts. The compounds obtained were studied by the methods of ¹H, ¹³C, and ¹¹B NMR spectroscopy, single crystal X-ray diffraction, cyclic voltammetry, controlled potential coulometry and quantum chemical calculations. It was found that in the solid state, the transoid- and gauche-conformations of the 8,8’- and 4,4’-isomers are stabilized by four intramolecular CH···S(Me)B hydrogen bonds each one (2.683-2.712 Å and 2.709-2.752 Å, respectively), whereas gauche-conformation of the 4,7’-isomer is stabilized by two intramolecular CH···S hydrogen bonds (2.699-2.711 Å). The existence of the intramolecular CH·S(Me)B hydrogen bonding in solutions was supported by the 1H NMR spectroscopy. These data are in a good agreement with results of the quantum chemical calculations. The corresponding iron and nickel complexes were synthesized as well. The reaction of the methyl sulfide derivatives of cobalt bis(dicarbollide) with various labile transition metal complexes results in rupture of intramolecular hydrogen bonds and complexation of the methyl sulfide groups with external metal. This results in stabilization of other rotational conformation of cobalt bis(dicarbollide) and can be used in design of molecular switches. This work was supported by the Russian Science Foundation (16-13-10331).

Keywords: molecular switches, NMR spectroscopy, single crystal X-ray diffraction, transition metal bis(dicarbollide) complexes, quantum chemical calculations

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Authors: Naima Boudieb, Mohamed Loucif Seaid, Imad Rati, Imane Benammane

Abstract:

The aim of this study is to synthesis of a copolymer PANI/PEDOT:PSS by electrochemical means to apply in supercapacitors. Polyaniline (PANI) is a conductive polymer; it was synthesized by electrochemical polymerization. It exhibits very stable properties in different environments, whereas PEDOT:PSS is a conductive polymer based on poly(3,4-ethylenedioxythiophene) (PEDOT) and poly(styrene sulfonate)(PSS). It is commonly used with polyaniline to improve its electrical conductivity. Several physicochemical and electrochemical techniques were used for the characterization of PANI/PEDOT:PSS: cyclic voltammetry (VC), electrochemical impedance spectroscopy (EIS), open circuit potential, SEM, X-ray diffraction, etc. The results showed that the PANI/PEDOT:PSS composite is a promising material for supercapacitors due to its high electrical conductivity and high porosity. Electrochemical and physicochemical characterization tests have shown that the composite has high electrical and structural performances, making it a material of choice for high-performance energy storage applications.

Keywords: energy storage, supercapacitors, SIE, VC, PANI, poly(3, 4-ethylenedioxythiophene, PEDOT, polystyrene sulfonate

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