Search results for: scanning electron microscopic analysis

Authors: Hamid Khachab, Yamani Abdelkafi, Mouna Barhmi

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The epitaxial growth has great important in the fabricate of the new semi-conductors devices and upgrading many factors, such as the quality of crystallization and efficiency with their deferent types and the most effective epitaxial technique is the molecular beam epitaxial. The MBE growth modeling allows to confirm the experiments results out by atomic beam and to analyze the microscopic phenomena. In of our work, we determined the growth processes specially the ZnSe epitaxial technique by Kinetic Monte Carlo method and we also give observations that are made in real time at the growth temperature using reflection high energy electron diffraction (RHEED) and photoemission current.

Keywords: molecular beam epitaxy, II-VI, morpholy, photoemission, RHEED, simulation, kinetic Monte Carlo, ZnSe

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Authors: Md. Hafezur Rahaman, Md. Sagor Hosen, Md. Abdul Gafur, Rasel Habib

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This research is a systematic study of effects of poly(D-lactic acid) (PDLA) on the properties of poly(L-lactic acid)(PLLA)/microcrystalline cellulose (MCC)/PDLA blends by stereo complex crystallization. Blends were prepared with constant percentage of (3 percent) MCC and different percentage of PDLA by solution casting methods. These blends were characterized by Fourier Transform Infrared Spectroscopy (FTIR) for the confirmation of blends compatibility, Wide-Angle X-ray Scattering (WAXS) and scanning electron microscope (SEM) for the analysis of morphology, thermo-gravimetric analysis (TGA) and differential thermal analysis (DTA) for thermal properties measurement. FTIR Analysis results confirm no new characteristic absorption peaks appeared in the spectrum instead shifting of peaks due to hydrogen bonding help to have compatibility of blends component. Development of three new peaks from XRD analysis indicates strongly the formation of stereo complex crystallinity in the PLLA structure with the addition of PDLA. TGA and DTG results indicate that PDLA can improve the heat resistivity of the PLLA/MCC blends by increasing its degradation temperature. Comparison of DTA peaks also ensure developed thermal properties. Image of SEM shows the improvement of surface morphology.

Keywords: microcrystalline cellulose, poly(l-lactic acid), stereocomplex crystallization, thermal stability

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Authors: Aboozar Aghaei

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In the present work, the dissimilar Monel400 and SS316 were joined by friction stir welding (FSW). The applied rotating speed was 400 rpm, whereas the traverse speed varied between 50 and 150 mm/min. At a constant rotating speed, the sound welds were obtained at the welding speeds of 50 and 100 mm/min. However, a groove-like defect was formed when the welding speed exceeded 100 mm/min. The mechanical properties of the joints were evaluated using tensile and fatigue tests. The fatigue strength of dissimilar FSWed specimen was higher than that of both Monel400 and SS316. To study the failure behavior of FSWed specimens, the fracture surfaces were analyzed using scanning electron microscope (SEM). The failure analysis indicates that different mechanisms may contribute to the fracture of welds. This was attributed to the dissimilar characteristics of dissimilar materials exhibiting different failure behaviors.

Keywords: mechanical properties, stainless steel, frictions, monel

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Authors: Soma Ghosh, Balaram Mohapatra, Pinaki Sar, Abhijeet Mukherjee

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Microbial role in arsenic (As) mobilization in the groundwater aquifers of Brahmaputra river basin (BRB) in India, severely threatened by high concentrations of As, remains largely unknown. The present study, therefore, is a molecular and ecophysiological characterization of an indigenous bacterium strain IIIJ3-1 isolated from As contaminated groundwater of BRB and application of this strain in several microcosm set ups differing in their organic carbon (OC) source and terminal electron acceptors (TEA), to understand its role in As dissolution under aerobic and anaerobic conditions. Strain IIIJ3-1 was found to be a new facultative anaerobic, gram-positive, endospore-forming strain capable of arsenite (As3+) oxidation and dissimilatory arsenate (As5+) reduction. The bacterium exhibited low genomic (G+C)% content (45 mol%). Although, its 16S rRNA gene sequence revealed a maximum similarity of 99% with Bacillus cereus ATCC 14579(T) but the DNA-DNA relatedness of their genomic DNAs was only 49.9%, which remains well below the value recommended to delimit different species. Abundance of fatty acids iC17:0, iC15:0 and menaquinone (MK) 7 though corroborates its taxonomic affiliation with B. cereus sensu-lato group, presence of hydroxy fatty acids (HFAs), C18:2, MK5 and MK6 marked its uniqueness. Besides being highly As resistant (MTC=10mM As3+, 350mM As5+), metabolically diverse, efficient aerobic As3+ oxidizer; it exhibited near complete dissimilatory reduction of As5+ (1 mM). Utilization of various carbon sources with As5+ as TEA revealed lactate to serve as the best electron donor. Aerobic biotransformation assay yielded a lower Km for As3+ oxidation than As5+ reduction. Arsenic homeostasis was found to be conferred by the presence of arr, arsB, aioB, and acr3(1) genes. Scanning electron microscopy (SEM) coupled with energy dispersive X-ray (EDX) analysis of this bacterium revealed reduction in cell size upon exposure to As and formation of As-rich electron opaque dots following growth with As3+. Incubation of this strain with sediment (sterilised) collected from BRB aquifers under varying OC, TEA and redox conditions revealed that the strain caused highest As mobilization from solid to aqueous phase under anaerobic condition with lactate and nitrate as electron donor and acceptor, respectively. Co-release of highest concentrations of oxalic acid, a well known bioweathering agent, considerable fold increase in viable cell counts and SEM-EDX and X-ray diffraction analysis of the sediment after incubation under this condition indicated that As release is consequent to microbial bioweathering of the minerals. Co-release of other elements statistically proves decoupled release of As with Fe and Zn. Principle component analysis also revealed prominent role of nitrate under aerobic and/or anaerobic condition in As release by strain IIIJ3-1. This study, therefore, is the first to isolate, characterize and reveal As mobilization property of a strain belonging to the Bacillus cereus sensu lato group isolated from highly As contaminated aquifers of Brahmaputra River Basin.

Keywords: anaerobic microcosm, arsenic rich electron opaque dots, Arsenic release, Bacillus strain IIIJ3-1

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Authors: H. Özkan Gülsoy, Antonyraj Arockiasamy

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The application of powder injection molding technology for the fabrication of metallic and non-metallic components is of growing interest as the process considerably saves time and cost. Utilizing this fabrication method, full dense components are being prepared in various sizes. In this work, our effort is focused to study the densification behavior of the parts made using different size 316L stainless steel powders. The metal powders were admixed with an adequate amount of polymeric compounds and molded as standard tensile bars. Solvent and thermal debinding was carried out followed by sintering in ultra pure hydrogen atmosphere based on the differential scanning calorimetry (DSC) cycle. Mechanical property evaluation and microstructural characterization of the sintered specimens was performed using universal Instron tensile testing machine, Vicker’s microhardness tester, optical (OM) and scanning electron microscope (SEM), energy dispersive spectroscopy (EDS), and X-ray diffraction were used. The results are compared and analyzed to predict the strength and weakness of the test conditions.

Keywords: powder injection molding, sintering, particle size, stainless steels

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Authors: D. Korsacilar, C. Atas

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In this study, first thermoplastic composite materials/plates that have high ballistic impact resistance were produced. For this purpose, the thermoplastic prepreg and the vacuum bagging technique were used to produce a composite material. Thermoplastic prepregs (resin-impregnated fiber) that are supplied ready to be used, namely high-density polyethylene (HDPE) was chosen as matrix and unidirectional glass fiber was used as reinforcement. In order to compare the fiber configuration effect on mechanical properties, unidirectional and biaxial prepregs were used. Then the microstructural properties of the composites were investigated with scanning electron microscopy (SEM) analysis. Impact properties of the composites were examined by Charpy impact test and tensile mechanical tests and then the effects of ultraviolet irradiation were investigated on mechanical performance.

Keywords: ballistic, composite, thermoplastic, prepreg

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Authors: Po-Hao Huang, Pei-Ju Chiang

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The structured light 3D scanner is commonly used for measuring the 3D shape of an object. Through projecting designed light patterns on the object, deformed patterns can be obtained and used for the geometric shape reconstruction. At present, Gray code is the most reliable and commonly used light pattern in the structured light 3D scanner. However, the trade-off between scanning efficiency and accuracy is a long-standing and challenging problem. The design of light patterns plays a significant role in the scanning efficiency and accuracy. Thereby, we proposed a novel encoding method integrating color information and Gray-code to improve the scanning efficiency. We will demonstrate that with the proposed method, the scanning time can be reduced to approximate half of the one needed by Gray-code without reduction of precision.

Keywords: gray-code, structured light scanner, 3D shape acquisition, 3D reconstruction

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Authors: Atef Y. Shenouda, Fei Xu

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Cu₃SbS₃ (CAS) was synthesized by direct solid-state reaction from elementary Cu, Sb, & S and hydrothermal reaction using thioacetamide (TAM). Crystal structure and morphology for the prepared phases of Cu₃SbS₃ were studied via X-ray diffraction (XRD) and field emission scanning electron microscope (FESEM). The band gap energies are 2 and 2.2 eV for the prepared samples. The two samples are as anode for Na ion storage. They show high initial capacity to 490 mAh/g. Na cell prepared from TAM sample shows 280 mAh/g after 25 cycles vs. 60 mAh/g for elemental sample.

Keywords: Cu3SbS3, sodium batteries, thioacetamide, sulphur sources

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Authors: Amit Mallik, Anil K. Barik, Biswajit Pal

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The galloping advancement of research work on glass-ceramics stems from their wide applications in electronic industry and also to some extent in application oriented medical dentistry. TiO2, even in low concentration has been found to strongly influence the physical and mechanical properties of the glasses. Glass-ceramics is a polycrystalline ceramic material produced through controlled crystallization of glasses. Crystallization is accomplished by subjecting the suitable parent glasses to a regulated heat treatment involving the nucleation and growth of crystal phases in the glass. Mica glass-ceramics is a new kind of glass-ceramics based on the system SiO2•MgO•K2O•F. The predominant crystalline phase is synthetic fluormica, named fluorophlogopite. Mica containing glass-ceramics flaunt an exceptional feature of machinability apart from their unique thermal and chemical properties. Machinability arises from the randomly oriented mica crystals with a 'house of cards' microstructures allowing cracks to propagate readily along the mica plane but hindering crack propagation across the layers. In the present study, we have systematically investigated the crystallization, microstructure and mechanical behavior of barium fluorophlogopite mica-containing glass-ceramics of composition BaO•4MgO•Al2O3•6SiO2•2MgF2 nucleated by addition of 2, 4, 6 and 8 wt% TiO2. The glass samples were prepared by the melting technique. After annealing, different batches of glass samples for nucleation were fired at 730°C (2wt% TiO2), 720°C (4 wt% TiO2), 710°C (6 wt% TiO2) and 700°C (8 wt% TiO2) batches respectively for 2 h and ultimately heated to corresponding crystallization temperatures. The glass batches were analyzed by differential thermal analysis (DTA) and x-ray diffraction (XRD), scanning electron microscopy (SEM) and micro hardness indenter. From the DTA study, it is found that the fluorophlogopite mica crystallization exotherm appeared in the temperature range 886–903°C. Glass transition temperature (Tg) and crystallization peak temperature (Tp) increased with increasing TiO2 content up to 4 wt% beyond this weight% the glass transition temperature (Tg) and crystallization peak temperature (Tp) start to decrease with increasing TiO2 content up to 8 wt%. Scanning electron microscopy confirms the development of an interconnected ‘house of cards’ microstructure promoted by TiO2 as a nucleating agent. The increase in TiO2 content decreases the vicker’s hardness values in glass-ceramics.

Keywords: crystallization, fluormica glass, ‘house of cards’ microstructure, hardness

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Authors: Akhila Konala, Jagadeeswara Reddy Vennapusa, Sujay Chattopadhyay

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The energy consumption of humankind is growing day by day due to an increase in the population, industrialization and their needs for living. Fossil fuels are the major source of energy to satisfy energy needs, which are non-renewable energy resources. So, there is a need to develop green resources for energy production and storage. Phase change materials (PCMs) derived from plants (green resources) are well known for their capacity to store the thermal energy as latent heat during their phase change from solid to liquid. This property of PCM could be used for storage of thermal energy. In this study, a composite with fatty acid (caprylic acid; M.P 15°C, Enthalpy 179kJ/kg) as a phase change material and expanded perlite as support porous matrix was prepared through direct impregnation method for thermal energy storage applications. The prepared composite was characterized using Differential scanning calorimetry (DSC), Field Emission Scanning Electron Microscope (FESEM), Thermal Gravimetric Analysis (TGA), and Fourier Transform Infrared (FTIR) spectrometer. The melting point of the prepared composite was 15.65°C, and the melting enthalpy was 82kJ/kg. The surface nature of the perlite was observed through FESEM. It was observed that there are micro size pores in the perlite surface, which were responsible for the absorption of PCM into perlite. In TGA thermogram, the PCM loss from composite was started at ~90°C. FTIR curves proved there was no chemical interaction between the perlite and caprylic acid. So, the PCM composite prepared in this work could be effective to use in temperature maintenance of buildings.

Keywords: caprylic acid, composite, phase change materials, PCM, perlite, thermal energy

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Authors: Oswaldo Otero, Eduardo A. Orozco, Ana M. Herrera

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In this work, we present results from analytical and numerical studies of the electron acceleration by a TE₀₁₁ cylindrical microwave mode in a static homogeneous magnetic field under electron cyclotron resonance (ECR) condition. The stability of the orbits is analyzed using the particle orbit theory. In order to get a better understanding of the interaction wave-particle, we decompose the azimuthally electric field component as the superposition of right and left-hand circular polarization standing waves. The trajectory, energy and phase-shift of the electron are found through a numerical solution of the relativistic Newton-Lorentz equation in a finite difference method by the Boris method. It is shown that an electron longitudinally injected with an energy of 7 keV in a radial position r=Rc/2, being Rc the cavity radius, is accelerated up to energy of 90 keV by an electric field strength of 14 kV/cm and frequency of 2.45 GHz. This energy can be used to produce X-ray for medical imaging. These results can be used as a starting point for study the acceleration of electrons in a magnetic field changing slowly in time (GYRAC), which has some important applications as the electron cyclotron resonance ion proton accelerator (ECR-IPAC) for cancer therapy and to control plasma bunches with relativistic electrons.

Keywords: Boris method, electron cyclotron resonance, finite difference method, particle orbit theory, X-ray

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Authors: S. Mohajeri

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Electrocodeposition of Ni-TiO2 nanocomposite single layers and Ni-TiO2/TiO2 multilayers from Watts bath containing TiO2 sol was carried out on copper substrate. Pulse plating and pulse reverse plating techniques were applied to facilitate higher incorporations of TiO2 nanoparticles in Ni-TiO2 nanocomposite single layers, and the results revealed that by prolongation of the current-off durations and the anodic cycles, deposits containing 11.58 wt.% and 13.16 wt.% TiO2 were produced, respectively. Multilayer coatings which consisted of Ni-TiO2 and TiO2-rich layers were deposited by pulse potential deposition through limiting the nickel deposition by diffusion control mechanism. The TiO2-rich layers thickness and accordingly, the content of TiO2 reinforcement reached 104 nm and 18.47 wt.%, respectively in the optimum condition. The phase structure and surface morphology of the nanocomposite coatings were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The cross sectional morphology and line scans of the layers were studied by field emission scanning electron microscopy (FESEM). It was confirmed that the preferred orientations and the crystallite sizes of nickel matrix were influenced by the deposition technique parameters, and higher contents of codeposited TiO2 nanoparticles refined the microstructure. The corrosion behavior of the coatings in 1M NaCl and 0.5M H2SO4 electrolytes were compared by means of potentiodynamic polarization and electrochemical impedance spectroscopy (EIS) techniques. Increase of corrosion resistance and the passivation tendency were favored by TiO2 incorporation, while the degree of passivation declined as embedded particles disturbed the continuity of passive layer. The role of TiO2 incorporation on the improvement of mechanical properties including hardness, elasticity, scratch resistance and friction coefficient was investigated by the means of atomic force microscopy (AFM). Hydrophilicity and wettability of the composite coatings were investigated under UV illumination, and the water contact angle of the multilayer was reduced to 7.23° after 1 hour of UV irradiation.

Keywords: electrodeposition, hydrophilicity, multilayer, pulse-plating

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Authors: Wan-Tzu Yen, Yu-Chen Luo, I-Ping Liu, Po-Hsuan Yeh, Sheng-Hsun Fu, Yuh-Lang Lee

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Self-assembled characteristics and adsorption performance of 1-dodecylamine molecules on gold (Au) (111) surfaces were characterized via cyclic voltammetry (CV), surface-enhanced infrared absorption spectroscopy (SEIRAS) and scanning tunneling microscopy (STM). The present study focused on the formation of 1-dodecylamine (DDA) on a gold surface with respect to the ex-situ arrangement of an adlayer on the Au(111) surface, and phase transition at potential dynamics carried out by EC-STM. This study reveals that alkyl amine molecules were formed an adsorption pattern with highly regular “lie down shape” on Au(111) surface, even in an extreme acid system (pH = 1). Acidic electrolyte (HClO₄) could protonate the surface of alkyl amine of a monolayer of the gold surface when potential shifts to negative. The quite stability of 1-dodecylamine on the gold surface maintained the monolayer across the potential window (0.1-0.8V). This transform model was confirmed by EC-STM. In addition, amine-modified Au(111) electrode adlayer used to examine how to affect an electron transfer across an interface using [Fe(CN)₆]³⁻/[Fe(CN)₆]⁴⁻ redox pair containing 0.1 M HClO₄ solution.

Keywords: cyclic voltammetry, dodecylamine, gold (Au)(111), scanning tunneling microscopy, self-assembled monolayer, surface-enhanced infrared absorption spectroscopy

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Authors: Jhen-Ting Huang, Chia-Chia Chang, Hu-Cheng Weng, An-Ya Lo

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In this study, Co3O4-CNT-Graphene composite electrode was deposited by electrophoretic deposition (EPD) method, where micro polystyrene spheres (PSs) were added for co-deposition. Applied with heat treatment, a hierarchical porosity is left in the electrode which is beneficial for supercapacitor application. In terms of charge and discharge performance, we discussed the optimal CNT/Graphene ratio, macroporous ratio, and the effect of Co3O4 addition on electrode capacitance. For materials characterization, scanning electron microscope (SEM), X-ray diffraction, and BET were applied, while cyclic voltammetry (CV) and chronopotentiometry (CP) measurements, and Ragone plot were applied as in-situ analyses. Based on this, the effects of PS amount on the structure, porosity and their effect on capacitance of the electrodes were investigated. Finally, the full device performance was examined with charge-discharge and electron impedance spectrum (EIS) methods. The results show that the EPD coating with hierarchical porosity was successfully demonstrated in this study. As a result, the capacitance was greatly enhanced by 2.6 times with the hierarchical structure.

Keywords: supercapacitor, nanocarbon tub, graphene, metal oxide

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Authors: Temitope Olumide Olugbade

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Low resistance and delayed fracture to corrosion, especially in harsh environmental conditions, often limit the wide application of high-manganese (high-Mn) steels. To address this issue, the present work investigates the influence of microalloying on the corrosion properties of high-Mn steels. Microalloyed and base high-Mn steels were synthesized through an arc melting process under an argon atmosphere. To generate different microstructures, the temperature and duration were varied via thermal homogenization treatments. The electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization techniques were used to determine the corrosion properties in 0.6 M NaCl aqueous solution at room temperature. The relationship between the microstructures and corrosion properties was investigated via Scanning Kelvin Probe Microscopy (SKPFM), energy dispersive X-ray spectroscopy (EDX), and Scanning electron microscopy (SEM) techniques. The local corrosion properties were investigated via in situ atomic force spectroscopy (AFM), considering the homogenization treatments. The results indicate that microalloying is a successful technique for enhancing the corrosion behavior of high-Mn steels. Compared to other alloying elements, Vanadium has shown improvement in corrosion properties for both general and local corrosion in chloride environments.

Keywords: corrosion, high-manganese steel, homogenization, microalloying, vanadium

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Authors: Reim A. Almotiri, Manal M. Alkhamisi

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Ternary nanocomposites based on hydroxyapatite (HAP) and alumina (Al2O3) were embedded through graphene oxide (GO) nanosheets to be investigated for medical applications. The composition of the preparations has been confirmed by X-ray photoelectron spectroscopy, energy-dispersive X-ray analysis, and Fourier-Transform infrared spectroscopy. Scanning and transmission electron microscopy have shown the typical morphologies of the components of the nanocomposites with hydroxyapatite nanorods reaching an average diameter of 22.26±2 nm and an average length of 69.56±19.25 nm in the ternary nanocomposites. The ternary nanocomposite has a microhardness of 5.8±0.1 GPa and a higher average roughness of 6.5 nm compared to pure HAP preparation with an average roughness of 2.7 nm. All preparations have shown an acceptable cytotoxicity profile with a percent osteoblasts cell viability of 98.6±1.3% after culturing with the ternary nanocomposite. The TNC has also shown the highest antibacterial activity compared to preparations of each of its constituents and their nanocomposites, with a zone of inhibition’s diameter of 14.1±0.8 mm and 13.6±0.6 mm against Staphylococcus aureus and Escherichia coli, respectively, compared to no zone of inhibition for the pure hydroxyapatite preparation.

Keywords: hydroxypatite, cytotoxicity, nanocomposites, X-ray analysis

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Authors: Chao Hu, Xinwen Liao, Qing-Hua Qin, Gang Wang

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The hierarchical carbon nanotube (CNT)/carbon fiber (CF)/high density polyethylene (HDPE) was fabricated via compound extrusion and injection molding, in which to author’s best knowledge CNT was employed as a nano-coatings on the surface of CF for the first time by spray coating technique. The CNT coatings relative to CF was set at 1 wt% and the CF content relative to the composites varied from 0 to 25 wt% to study the influence of CNT coatings and CF contents on the mechanical, thermal and morphological performance of this hierarchical composites. The results showed that with the rise of CF contents, the mechanical properties, including the tensile properties, flexural properties, and hardness of CNT/CF/HDPE composites, were effectively improved. Furthermore, the CNT-coated composites showed overall higher mechanical performance than the uncoated counterparts. It can be ascribed to the enhancement of interfacial bonding between the CF and HDPE via the incorporation of CNT, which was demonstrated by the scanning electron microscopy observation. Meanwhile, the differential scanning calorimetry data indicated that by the introduction of CNT and CF, the crystallization temperature and crystallinity of HDPE were affected while the melting temperature did not have an obvious alteration.

Keywords: carbon fibers, carbon nanotubes, extrusion, high density polyethylene

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Authors: Nasser A. M. Habib

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The impressive physical properties of graphene derivatives, including thermal properties, have made them an attractive addition to advanced construction nanomaterial. In this study, we investigated the impact of incorporating low amounts of graphene oxide (GO) into cement mixture nanocomposites on their heat storage and thermal stability. The composites were analyzed using Fourier transmission infrared, thermo-gravimetric analysis, and field emission scanning electron microscopy. Results showed that GO significantly improved specific heat by 32%, reduced thermal conductivity by 16%, and reduced thermal decomposition to only 3% at a concentration of 1.2 wt%. These findings suggest that the cement mixture can withstand high temperatures and may suit specific applications requiring thermal stability and insulation properties.

Keywords: cement mixture composite, graphene oxide, thermal decomposition, thermal conductivity

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Authors: Ali Obeydavi, Majid Rahimi

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This study explores the synthesis and characterization of Fe-Cr-Mo-Co-C-B-Si thin film metallic glasses fabricated using the pulsed laser deposition (PLD) technique on silicon wafer and 304 stainless steel substrates. it systematically varied the laser pulse numbers (20,000; 30,000; 40,000) and energies (130, 165, 190 mJ) to investigate their effects on the microstructural, mechanical, and corrosion properties of the deposited films. Comprehensive characterization techniques, including grazing incidence X-ray diffraction, field emission scanning electron microscopy, atomic force microscopy, and transmission electron microscopy with selected area electron diffraction, were utilized to assess the amorphous structure and surface morphology. Results indicated that increased pulse numbers and laser energies led to enhanced deposition rates and film thicknesses. Nanoindentation tests demonstrated that the hardness and elastic modulus of the amorphous thin films significantly surpassed those of the 304 stainless steel substrate. Additionally, electrochemical polarization and impedance spectroscopy revealed that the Fe-based metallic glass coatings exhibited superior corrosion resistance compared to the stainless steel substrate. The observed improvements in mechanical and corrosion properties are attributed to the unique amorphous structure achieved through the PLD process, highlighting the potential of these materials for protective coatings in aggressive environments.

Keywords: thin film metallic glasses, pulsed laser deposition, mechanical properties, corrosion resistance

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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: Ahmet Afyon, Dursun Yagiz, Kutret Gezer, Aziz Turkoglu

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This study was conducted in order to contribute to Turkey’s macrofungus flora. The fungi samples forming the study material were collected from Afyonkarahisar province in 2009. The photos of mushrooms were taken in their own habitats. Their tastes, odors and clours were determined. These samples were brought to the laboratory. The microscopic properties of fungi were determined in the laboratory. The fungi were identified according to their macroscopic and microscopic features with the help of written literature. The identified macrofungi are; Limacella furnace (Letell.) E.-J. Gilbert from the Amanitaceae familia, Marasmiellus vaiillantii (Pers.) Singer from Omphalotaceae familia, Mycena flos-nivium Kuhner from Mycenaceae familia. With this study, it has been contributed to Turkey’s macrofungi flora and biodiversity.

Keywords: Afyonkarahisar, macrofungi, records, Turkey

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

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

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

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Authors: Hilal T. Sasmazel, Seda Surucu

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Skin tissue engineering is a promising field for the treatment of skin defects using scaffolds. This approach involves the use of living cells and biomaterials to restore, maintain, or regenerate tissues and organs in the body by providing; (i) larger surface area for cell attachment, (ii) proper porosity for cell colonization and cell to cell interaction, and (iii) 3-dimensionality at macroscopic scale. Recent studies on this area mainly focus on fabrication of scaffolds that can closely mimic the natural extracellular matrix (ECM) for creation of tissue specific niche-like environment at the subcellular scale. Scaffolds designed as ECM-like architectures incorporating into the host with minimal scarring/pain and facilitate angiogenesis. This study is related to combining of synthetic PCL and natural chitosan polymers to form 3D PCL/Chitosan core-shell structures for skin tissue engineering applications. Amongst the polymers used in tissue engineering, natural polymer chitosan and synthetic polymer poly(ε-caprolactone) (PCL) are widely preferred in the literature. Chitosan has been among researchers for a very long time because of its superior biocompatibility and structural resemblance to the glycosaminoglycan of bone tissue. However, the low mechanical flexibility and limited biodegradability properties reveals the necessity of using this polymer in a composite structure. On the other hand, PCL is a versatile polymer due to its low melting point (60°C), ease of processability, degradability with non-enzymatic processes (hydrolysis) and good mechanical properties. Nevertheless, there are also several disadvantages of PCL such as its hydrophobic structure, limited bio-interaction and susceptibility to bacterial biodegradation. Therefore, it became crucial to use both of these polymers together as a hybrid material in order to overcome the disadvantages of both polymers and combine advantages of those. The scaffolds here were fabricated by using electrospinning technique and the characterizations of the samples were done by contact angle (CA) measurements, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-Ray Photoelectron spectroscopy (XPS). Additionally, gas permeability test, mechanical test, thickness measurement and PBS absorption and shrinkage tests were performed for all type of scaffolds (PCL, chitosan and PCL/chitosan core-shell). By using ImageJ launcher software program (USA) from SEM photographs the average inter-fiber diameter values were calculated as 0.717±0.198 µm for PCL, 0.660±0.070 µm for chitosan and 0.412±0.339 µm for PCL/chitosan core-shell structures. Additionally, the average inter-fiber pore size values exhibited decrease of 66.91% and 61.90% for the PCL and chitosan structures respectively, compare to PCL/chitosan core-shell structures. TEM images proved that homogenous and continuous bead free core-shell fibers were obtained. XPS analysis of the PCL/chitosan core-shell structures exhibited the characteristic peaks of PCL and chitosan polymers. Measured average gas permeability value of produced PCL/chitosan core-shell structure was determined 2315±3.4 g.m-2.day-1. In the future, cell-material interactions of those developed PCL/chitosan core-shell structures will be carried out with L929 ATCC CCL-1 mouse fibroblast cell line. Standard MTT assay and microscopic imaging methods will be used for the investigation of the cell attachment, proliferation and growth capacities of the developed materials.

Keywords: chitosan, coaxial electrospinning, core-shell, PCL, tissue scaffold

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Authors: Abubakar Umar Birnin-yauri

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Plastic wastes arising from Polyethylene (PE)-based materials are increasingly becoming environmental problem, this is owed to the fact that these PE waste materials will only decompose over hundreds, or even thousands of years, during which they cause serious environmental problems. In this research, Polymer blends prepared from PE, Cashewnut flour (CNF) and Gum Arabic (GA) were studied in order to assay their biodegradation potentials via composting method. Different sample formulations were made i.e., X1= (70% PE, 25% CNF and 5% GA, X2= (70% PE, 20% CNF and 10% GA), X3= (70% PE, 15% CNF and 15% GA), X4 = (70% PE, 10% CNF and 20% GA) and X5 = (70% PE, 5% CNF and 25% GA) respectively. The results obtained showed that X1 recorded weight loss of 9.89% of its original weight after the first 20 days and 37.45% after 100 day, and X2 lost 12.67 % after the first 20 days and 42.56% after 100day, sample X5 experienced the greatest weight lost in the two methods adopted which are 52.9% and 57.89%. Instrumental analysis such as Fourier Transform Infrared Spectroscopy, Thermogravimetric analysis and Scanning electron microscopy were performed on the polymer blends before and after biodegradation. The study revealed that the biodegradation of the polymer blends is influenced by the contents of both the CNF and GA added into the blends.

Keywords: polyethylene, cashewnut, gum Arabic, biodegradation, blend, environment

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Authors: Mohsen Adabi, Mahdi Adabi, Reza Saber

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The recent advancements in nanomaterials have provided a platform to develop efficient transduction matrices for sensors. Modified electrodes allow to electrochemists to enhance the property of electrode surface and provide desired properties such as improved sensing capabilities, higher electron transfer rate and prevention of undesirable reactions competing kinetically with desired electrode process. Nanostructured electrodes including arrays of carbon nanotubes have demonstrated great potential for the development of electrochemical sensors and biosensors. The aim of this work is to evaluate the concentration of multi-walled carbon nanotubes (MWCNTs) on the conductivity of gold electrode. For this work, raw MWCNTs was functionalized and shortened. Raw and shorten MWCNTs were characterized using transfer electron microscopy (TEM). Next, 0.5, 2 and 3.5 mg of Shortened and functionalized MWCNTs were dispersed in 2 mL Dimethyl formamide (DMF) and cysteamine modified gold electrodes were incubated in the different concentrations of MWCNTs for 8 hours. Then, the immobilization of MWCNTs on cysteamine modified gold electrode was characterized by scanning electron microscopy (SEM) and the effect of MWCNT concentrations on electron transfer of modified electrodes was investigated by cyclic voltammetry (CV). The results demonstrated that CV response of ferricyanide redox at modified gold electrodes increased as concentration of MWCNTs enhanced from 0.5 to 2 mg in 2 mL DMF. This increase can be attributed to the number of MWCNTs which enhance on the surface of cysteamine modified gold electrode as the MWCNTs concentration increased whereas CV response of ferricyanide redox at modified gold electrodes did not changed significantly as the MWCNTs concentration increased from 2 to 3.5 mg in 2 mL DMF. The reason may be that amine groups of cysteamine modified gold electrodes are limited to a given number which can interact with the given number of carboxylic groups of MWCNTs and CV response of ferricyanide redox at modified gold do not enhance after amine groups of cysteamine are saturated with carboxylic groups of MWCNTs.

Keywords: carbon nanotube, cysteamine, electrochemical sensor, gold electrode

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Authors: Aliyu Usman, Muhaammed Bello Ibrahim, Yusuf D. Amartey, Jibrin M. Kaura

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This research is aimed at investigating the effect of using amorphous silica ash (ASA) obtained from rice husk as a partial replacement of ordinary Portland cement (OPC) on the mechanical and microstructure properties of cement paste and mortar. ASA was used in partial replacement of ordinary Portland cement in the following percentages 3 percent, 5 percent, 8 percent and 10 percent. These partial replacements were used to produce Cement-ASA paste and Cement-ASA mortar. ASA was found to contain all the major chemical compounds found in cement with the exception of alumina, which are SiO2 (91.5%), CaO (2.84%), Fe2O3 (1.96%), and loss on ignition (LOI) was found to be 9.18%. It also contains other minor oxides found in cement. Consistency of Cement-ASA paste was found to increase with increase in ASA replacement. Likewise, the setting time and soundness of the Cement-ASA paste also increases with increase in ASA replacements. The test on hardened mortar were destructive in nature which include flexural strength test on prismatic beam (40mm x 40mm x 160mm) at 2, 7, 14 and 28 days curing and compressive strength test on the cube size (40mm x 40mm, by using the auxiliary steel platens) at 2,7,14 and 28 days curing. The Cement-ASA mortar flexural and compressive strengths were found to be increasing with curing time and decreases with cement replacement by ASA. It was observed that 5 percent replacement of cement with ASA attained the highest strength for all the curing ages and all the percentage replacements attained the targeted compressive strength of 6N/mm2 for 28 days. There is an increase in the drying shrinkage of Cement-ASA mortar with curing time, it was also observed that the drying shrinkages for all the curing ages were greater than the control specimen all of which were greater than the code recommendation of less than 0.03%. The scanning electron microscope (SEM) was used to study the Cement-ASA mortar microstructure and to also look for hydration product and morphology.

Keywords: amorphous silica ash, cement mortar, cement paste, scanning electron microscope

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Authors: Md. Maksudur Rahman Khan, Chee Wai Woon, Huei Ruey Ong, Vignes Rasiah, Chin Kui Cheng, Kar Min Chan, E. Baranitharan

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The present work represents a preparation of non-precious iron-based electrocatalyst (FeN) for ORR in air-cathode microbial fuel cell by pyrolysis treatment. Iron oxalate which recovered from the industrial wastewater and Phenanthroline (Phen) were used as the iron and nitrogen precursors, respectively in preparing FeN catalyst. The performance of as prepared catalyst (FeN) was investigated in a single chambered air cathode MFC in which anaerobic sludge was used as inoculum and palm oil mill effluent as substrate. The maximum open circuit potential (OCV) and the highest power density recorded were 0.543 V and 4.9 mW/m2, respectively. Physical characterization of FeN was elucidated by using Brunauner Emmett Teller (BET), X-Ray Diffraction (XRD) analysis and Field Emission Scanning Electron Microscopy (FESEM) while the electrochemical properties were characterized by cyclic voltammetry (CV) analysis. The presence of biofilm on anode surface was examined using FESEM and confirmed using Infrared Spectroscopy and Thermogravimetric Analysis. The findings of this study demonstrated that FeN is electrochemically active and further modification is needed to increase the ORR catalytic activity.

Keywords: iron based catalyst, microbial fuel cells, oxygen reduction reaction, palm oil mill effluent

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Authors: Suraj D. Khadka, Priyantha W. Jayawickrama

Abstract:

In search of a sustainable construction material, geopolymer has been investigated for past decades to evaluate its advantage over conventional products. Synthesis of geopolymer requires a source of aluminosilicate mixed with sodium hydroxide and sodium silicate at different proportions to maintain a Si/Al molar ratio of 1-3 and Na/Al molar ratio of unity. A comprehensive geopolymer study was performed with Metakaolin and Class C Fly ash as primary aluminosilicate sources. Synthesized geopolymer was analyzed for time-dependent viscosity, setting period and strength at varying initial moisture content, curing temperature and humidity. Different concentration of Ca(OH)₂ and CaSO₄.2H₂O were added to vary the amount of calcium contained in synthesized geopolymer. Influence of calcium content in unconfined compressive strength behavior of geopolymer were analyzed. Finally, Scanning Electron Microscopy-Energy Dispersive Spectroscopy (SEM-EDS) was performed to investigate the hardened product. It was observed that fly ash based geopolymer had shortened setting time and faster increase in viscosity as compared to geopolymer synthesized from metakaolin. This was primarily attributed to higher calcium content resulting in formation of calcium silicate hydrates (CSH). SEM-EDS was performed to verify the presence of CSH phases. Spectral analysis of geopolymer prepared by addition of Ca(OH)₂ and CaSO₄.2H₂O indicated higher CSH phases at higher concentration. It was observed that lower concentration of added calcium favored strength gain in geopolymer. However, at higher calcium concentration, decrease in strength was observed. Strength variation was also observed with humidity at initial curing condition. At 100% humidity, geopolymer with added calcium presented higher strength compared to samples cured at ambient humidity condition (40%). Reduction in strength in these samples at lower humidity was primarily attributed to reduction in moisture content in specimen due to the formation of CSH phases and loss of moisture through evaporation. For low calcium content geopolymers, with increase in temperature, gain in strength was observed with maximum strength observed at 200 ˚C. However, samples with higher calcium content demonstrated severe cracking resulting in low strength at elevated temperatures.

Keywords: calcium silicate hydrates, geopolymer, humidity, Scanning Electron Microscopy-Energy Dispersive Spectroscopy, unconfined compressive strength

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Authors: N. Boussouf, M. F. Mosbah, M.Hamel, S. Menassel

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SiO2 particles were inserted (added) into Bi2Sr2CaCu2O8+d precursor powders in various weight fractions. The influence of Si addition to the Bi2212 system on its phase formation, microstructure and transport properties is investigated. Samples are characterized by means of X ray diffraction analysis (XRD), scanning electron microscopy (SEM/EDX), magnetic AC susceptibility and resistivity measurements. For 1% of added Si, the results showed an increase of the apparent superconducting volume fraction. All the samples doped with Si contained a majority fraction of the high TC superconducting Bi2212 phase. SEM observation showed that the average grain size of the Si added samples increased more than that of the sample without Si. From resistivity measurement the Tconset was found to be increased by 7 K for 1% and 5% of added Si compared to the pure sample.

Keywords: superconductors, Bi2212, doping, SiO2 particles

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Authors: S. Al-Enezi, J. Samuel, A. Al-Banna

Abstract:

Polymer based membranes are one of the low-cost technologies available for the gas separation. Three major elements required for a commercial gas separating membrane are high permeability, high selectivity, and good mechanical strength. Poly(vinylidene fluoride) (PVDF) is a commercially available fluoropolymer and a widely used membrane material in gas separation devices since it possesses remarkable thermal, chemical stability, and excellent mechanical strength. The PVDF membrane was chemically modified by soaking in different ionic liquids and dried. The thermal behavior of modified membranes was investigated by differential scanning calorimetry (DSC), and thermogravimetry (TGA), and the results clearly show the best affinity between the ionic liquid and the polymer support. The porous structure of the PVDF membranes was clearly seen in the scanning electron microscopy (SEM) images. The CO₂ permeability of blended membranes was explored in comparison with the unmodified matrix. The ionic liquid immobilized in the hydrophobic PVDF support exhibited good performance for separations of CO₂/N₂. The improved permeability of modified membrane (PVDF-IL) is attributed to the high concentration of nitrogen rich imidazolium moieties.

Keywords: PVDF, polymer membrane, gas permeability, CO₂ separation, nanotubes

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