Search results for: x-ray diffraction analysis

Authors: Osama Saber

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Cyanate is one such anion which is produced during protein poisoning in the body and has been studied extensively in the field of biochemistry because of its toxicity. The present work aims at confinement and storage of cyanate in the nano scale. It was achieved through the intercalation of cyanate anions into nanolayerd structures of Ni-Al LDH. In addition, the effect of aging time on the intercalation of cyanate was clarified using X-ray diffraction and scanning electron microscopy. Furthermore, the effect of cations on the affinity towards the intercalation of cyanate anions inside LDH structure was studied by replacement of tetra-valent cations Ti4+ instead of the tri-vallent cations Al3+ during the preparation of LDH structure. X-ray diffraction patterns of the Ni-Ti LDH showed that the interlayer spacing was 0.73 nm. This spacing was smaller than that of Ni-Al LDH suggesting that the interlayered anions into Ni-Ti LDH are different from those into Ni-Al LDH. Thermal analyses (TG, DTG, and DTA) and Infra-red spectra revealed the presence of only cyanate anions into Ni-Ti LDH while, in the case of Ni-Al LDH, both cyanate and carbonate anions were observed. SEM images showed plate-like morphology for both Ni-Ti and Ni-Al LDHs although the shapes of their plates are not similar. Our results suggested that the LDH structures containing titanium cations have higher affinity for cyanate anions than those containing aluminum cations. Therefore, this choice for cyanate in the interlayered spacing widens the applicability to study the effect of the confinement on the toxicity of cyanate by bio researchers.

Keywords: nanolayered structures, Ni-Al LDH, Ni-Ti LDH, intercalation of cyanate anions, urea hydrolysis

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

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

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

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Authors: M. Sneha, N. Meenakshi Sundaram

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In recent times, magnetic hyperthermia is used for cancer treatment as a tool for active targeting of delivering drugs to the targeted site. It has a potential advantage over other heat treatment because there is no systemic buildup in organs and large doses are possible. The aim of this study is to develop a suitable magnetic biomaterial that can destroy the cancer cells as well as induce bone regeneration. In this work, the composite material was synthesized in two-steps. First, porous iron oxide nano needles were synthesized by hydrothermal process. Second, the hydroxyapatite, were synthesized from natural calcium (i.e., egg shell) and inorganic phosphorous source using wet chemical method. The crystalline nature is confirmed by powder X-ray diffraction analysis (XRD). Thermal analysis and the surface area of the material is studied by Thermo Gravimetric Analysis (TGA), Brunauer-Emmett and Teller (BET) technique. Scanning electron microscope (SEM) images show that the particles have nanoneedle-like morphology. The magnetic property is studied by vibrating sample magnetometer (VSM) technique which confirms the superparamagnetic behavior. This paper presents a simple and easy method for synthesis of magnetite/hydroxyapatite composites materials.

Keywords: iron oxide nano needles, hydroxyapatite, superparamagnetic, hyperthermia

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Authors: E. Changizi, E. Ghasemi, B. Ramezanzadeh, M. Mahdavian

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In this study, the graphene oxide was functionalized with polyisocyanate (piGO). The functionalization was carried out at 45⁰C for 24 hrs under nitrogen atmosphere. The X-ray diffraction (XRD), scanning electron microscope (SEM), Fourier transform infrared spectroscopy (FT-IR) and thermal gravimetric analysis (TGA) were utilized in order to evaluate the GO functionalization. The GO and piGO stability were then investigated in polar and nonpolar solvents. Results obtained showed that polyisocyanate was successfully grafted on the surface of graphen oxide sheets through covalent bonds formation. The surface nature of the graphen oxide was changed into the hydrophobic after functionalization. Moreover, the graphen oxide sheets interlayer distance increased after modification.

Keywords: graphen oxide, functionalization, polyisocyanate, XRD, TGA, FTIR

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Authors: Osamu Takakuwa, Yuta Mano, Hitoshi Soyama

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This paper reveals the interaction between hydrogen and surface stress in austenitic stainless steel by X-ray diffraction stress measurement and thermal desorption analysis before and after being charged with hydrogen. The surface residual stress was varied by surface finishing using several disc polishing agents. The obtained results show that the residual stress near surface had a significant effect on hydrogen absorption behavior, that is, tensile residual stress promoted the hydrogen absorption and compressive one did opposite. Also, hydrogen induced equi-biaxial stress and this stress has a linear correlation with hydrogen content.

Keywords: hydrogen embrittlement, residual stress, surface finishing, stainless steel

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Authors: Hiroyuki Aoki

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The physical properties of polymer materials are dependent on the conformation and molecular motion of a polymer chain. Therefore, the structure and dynamic behavior of the single polymer chain have been the most important concerns in the field of polymer physics. However, it has been impossible to directly observe the conformation of the single polymer chain in a bulk medium. In the current work, the novel techniques to study the conformation and dynamics of a single polymer chain are proposed. Since a fluorescence method is extremely sensitive, the fluorescence microscopy enables the direct detection of a single molecule. However, the structure of the polymer chain as large as 100 nm cannot be resolved by conventional fluorescence methods because of the diffraction limit of light. In order to observe the single chains, we developed the labeling method of polymer materials with a photo-switchable dye and the super-resolution microscopy. The real-space conformational analysis of single polymer chains with the spatial resolution of 15-20 nm was achieved. The super-resolution microscopy enables us to obtain the three-dimensional coordinates; therefore, we succeeded the conformational analysis in three dimensions. The direct observation by the nanometric optical microscopy would reveal the detailed information on the molecular processes in the various polymer systems.

Keywords: polymer materials, single molecule, super-resolution techniques, conformation

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Authors: P. M. Fonseca Alfonso, E. A. Murillo Ruiz, M. Diaz Lagos

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Understanding the physicochemical properties and mineralogy of fly ash from a particular source is essential for to protect the environment and considering its possible applications, specifically, in the production of geopolymeric materials that solidify/stabilize heavy metals ions. The results of the characterization of three fly ash samples are shown in this paper. The samples were produced in the TERMOPAIPA IV thermal power plant in the State of Boyaca, Colombia. The particle size distribution, chemical composition, mineralogy, and molecular structure of three samples were analyzed using laser diffraction, X-ray fluorescence, inductively coupled plasma mass spectrometry, X-ray diffraction, and infrared spectroscopy respectively. The particle size distribution of the three samples probably ranges from 0.128 to 211 μm. Approximately 59 elements have been identified in the three samples. It is noticeable that the ashes are made up of aluminum and silicon compounds. Besides, the iron phase in low content was also found. According to the results found in this study, the fly ash samples type F has a great potential to be used as raw material for the manufacture of geopolymers with potential use in the stabilization/solidification of heavy metals; mainly due to the presence of amorphous aluminosilicates typical of this type of ash, which react effectively with alkali-activator.

Keywords: fly ash, geopolymers, molecular structure, physicochemical properties.

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Authors: Tatsuhiko Aizawa, Yohei Suzuki, Tomomi Shiratori

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

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

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Authors: M. K. Deore

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The thick films of undoped and Al2O3 doped- ZnO were prepared by screen printing technique. AR grade (99.9 % pure) Zinc Oxide powder were mixed mechanochemically in acetone medium with Aluminium Chloride (AlCl2) material in various weight percentages such as 0.5, 1, 3 and 5 wt % to obtain Al2O3 - ZnO composite. The prepared materials were sintered at 1000oC for 12h in air ambience and ball milled to ensure sufficiently fine particle size. The electrical, structural and morphological properties of the films were investigated. The X-ray diffraction analysis of pure and doped ZnO shows the polycrystalline nature. The surface morphology of the films was studied by SEM. The final composition of each film was determined by EDAX analysis. The gas response of undoped and Al2O3- doped ZnO films were studied for different gases such as CO, H2, NH3, and H2S at operating temperature ranging from 50 oC to 450 o C. The pure film shows the response to H2S gas (500ppm) at 300oC while the film doped with 3 wt.% Al2O3 gives the good response to H2S gas(ppb) at 350oC. The selectivity, response and recovery time of the sensor were measured and presented.

Keywords: thick films, ZnO-Al2O3, H2S gas, sensitivity, selectivity, response and recovery time

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Authors: N. Boukabcha, Y. Megrouss, N. Benhalima, S. Yahiaoui, A. Chouaih, F. Hamzaoui

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We present the electron density analysis of organic compound 4-methyl-N-[(5- nitrothiophen-2-ylmethylidene)] aniline with chemical formula C12H10N2O2S. Indeed, determining the electrostatic properties of nonlinear optical organic compounds requires knowledge of the distribution of the electron density with high precision. On the other hand, a structural analysis is performed. Two methods are used to obtain the structure, X-ray diffraction and theoretical calculation with density functional theory (DFT). The electron density study is performed using the Mopro program1503 based on the multipolar model of Hansen and Coppens. Electron density analysis allows determination of the value and orientation of the dipole moment. The net atomic charges, electrostatic potential and the molecular dipole moment have been determined in order to understand the nature of inter- and intramolecular charge transfer. The study reveals the nature of intermolecular interactions including charge transfer and hydrogen bonds in the title compound. Crystallographic data: monoclinic system - space group P21 / n. Celle parameters: a = 4.7606 (4) Å, b = 22.415 (2) Å, c = 10.7008 (15) Å, β = 92.566 (13) 0, V = 1140.7 (2) Å3, Z = 4, R = 0.0034 for 2693 observed reflections.

Keywords: electron density, dipole moment, electrostatic potential, DFT, Mopro

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Authors: Z. Ž. Lazarević, Č. Jovalekić, V. N. Ivanovski, N. Ž. Romčević

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Nickel-zinc ferrite, Ni0.5Zn0.5Fe2O4 was prepared by mechanochemical route in a planetary ball mill starting from mixture of the appropriate quantities of the Ni(OH)2, Zn(OH)2 and Fe(OH)3 hydroxide powders. In order to monitor the progress of chemical reaction and confirm phase formation, powder samples obtained after 5 h and 10 h of milling were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), IR, Raman and Mössbauer spectroscopy. It is shown that the soft mechanochemical method, i.e. mechanochemical activation of hydroxides, produces high quality single phase Ni0.5Zn0.5Fe2O4 samples in much more efficient way. From the IR spectroscopy of single phase samples it is obvious that energy of modes depends on the ratio of cations. It is obvious that all samples have more than 5 Raman active modes predicted by group theory in the normal spinel structure. Deconvolution of measured spectra allows one to conclude that all complex bands in the spectra are made of individual peaks with the intensities that vary from spectrum to spectrum. The deconvolution of Raman spectra alows to separate contributions of different cations to a particular type of vibration and to estimate the degree of inversion.

Keywords: ferrite, X-ray diffraction, infrared spectroscopy, Raman spectroscopy, Mössbauer spectroscopy

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Authors: H. S. Assaedi, F. U. A. Shaikh, I. M. Low

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Geopolymer composites reinforced with flax fabrics and nano-clay are fabricated and studied for physical and mechanical properties using X-Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR) and Scanning Electron Microscope (SEM). Nanoclay platelets at a weight of 1.0%, 2.0%, and 3.0% were added to geopolymer pastes. Nanoclay at 2.0 wt.% was found to improve density and decrease porosity while improving flexural strength and post-peak toughness. A microstructural analysis indicated that nanoclay behaves as filler and as an activator supporting geopolymeric reaction while producing a higher content geopolymer gel improving the microstructure of binders. The process enhances adhesion between the geopolymer matrix and flax fibres.

Keywords: flax fibres, geopolymer, mechanical properties, nanoclay

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Authors: S. Zhuiykov, E. Kats

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Electrical properties and morphology of orthorhombic β–WO3 nano-flakes with thickness of ~7-9 nm were investigated at the nano scale using energy dispersive X-ray diffraction (XRD), X-ray photo electron spectroscopy (XPS) and current sensing force spectroscopy atomic force microscopy (CSFS-AFM, or PeakForce TUNATM). CSFS-AFM analysis established good correlation between the topography of the developed nano-structures and various features of WO3 nano-flakes synthesized via a two-step sol-gel-exfoliation method. It was determined that β–WO3 nano-flakes annealed at 550ºC possess distinguished and exceptional thickness-dependent properties in comparison with the bulk, micro- and nano-structured WO3 synthesized at alternative temperatures.

Keywords: electrical properties, layered semiconductors, nano-flake, sol-gel, exfoliation WO3

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Authors: Seyfullah Madakbas, Emrah Cakmakci

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Polyaniline (PANI), the most studied member of the conductive polymers, has a wide range of uses from several electronic devices to various conductive high-technology applications. Boron nitride (BN) is a boron and nitrogen containing compound with superior chemical and thermal resistance and thermal conductivity. Even though several composites of PANI was prepared in literature, the preparation of h-BN/PANI composites is rare. In this work PANI was polymerized in the presence of different amounts of h-BN (1, 3 and 5% with respect to PANI) by using 0.1 M solution of NH4S2O8 in HCl as the oxidizing agent and conductive composites were prepared. Composites were structurally characterized with FTIR spectroscopy and X-Ray Diffraction (XRD). Thermal properties of conductive composites were determined by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). Dielectric measurements were performed in the frequency range of 106–108 Hz at room temperature. The corresponding bands for the benzenoid and quinoid rings at around 1593 and 1496 cm-1 in the FTIR spectra of the composites proved the formation of polyaniline. Together with the FTIR spectra, XRD analysis also revealed the existence of the interactions between PANI and h-BN. Glass transition temperatures (Tg) of the composites increased with the increasing amount of PANI (from 87 to 101). TGA revealed that the char yield of the composites increased as the amount of h-BN was increased in the composites. Finally the dielectric permittivity of 3 wt.%h-BN-containing composite was measured and found as approximately 17. This work was supported by Marmara University, Commission of Scientific Research Project.

Keywords: dielectric permittivity, h-BN, PANI, thermal analysis

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Authors: M. Ertas, A. C. Onel, G. Ekinci, B. Toydemir, S. Durdu, M. Usta, L. Colakerol Arslan

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To develop AZ91D magnesium alloys with improved properties, we have applied TiN and VN/TiN multilayer coatings using DC magnetron sputter technique. Coating structure, surface morphology, chemical bonding and corrosion resistance of coatings were analyzed by x-ray diffraction (XRD), scanning electron microscope (SEM), x-ray photoelectron spectroscopy (XPS), and tafel extrapolation method, respectively. XPS analysis reveal that VN overlayer reacts with oxygen at the VN/TiN interface and forms more stable TiN layer. Morphological investigations and the corrosion results show that VN/TiN multilayer thin film coatings are quite effective to optimize the corrosion resistance of Mg alloys.

Keywords: AZ91D Mg alloys, high corrosion resistance, transition metal nitride coatings, magnetron sputter

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Authors: Demet Tatar, Bahattin Düzgün

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In this study, we have newly developed titanium-tin oxide (TiSnO) thin films as the transparent conducting oxides materials by the spray pyrolysis technique. Tin oxide thin films doped with different Ti content were successfully grown by spray pyrolysis and they were characterized as a function of Ti content. The effect of Ti contents on the crystalline structure and optical properties of the as-deposited SnO2:Ti films was systematically investigated by X-ray diffraction (XRD), scanning electronic microscopy (SEM), atomic force microscopy (AFM), UV-vis spectrometer and photoluminecenc spectrophotometer. The X-ray diffraction patterns taken at room temperature showed that the films are polycrystalline. The preferred directions of crystal growth appeared in the difractogram of SnO2: Ti (TiTO) films were correspond to the reflections from the (110), (200), (211) and (301) planes. The grain size varies from 21.8 to 27.8 nm for (110) preferred plane. SEM and AFM study reveals the surface of TiTO to be made of nanocrystalline particles. The highest visible transmittance (570 nm) of the deposited films is 80 % for 20 wt % titanium doped tin oxide films. The obtained results revealed that the structures and optical properties of the films were greatly affected by doping levels. These films are useful as conducting layers in electro chromic and photovoltaic devices.

Keywords: transparent conducting oxide, gas sensors, SnO2, Ti, optoelectronic, spray pyrolysis

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

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

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

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Authors: 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: Abbas R. Ali, Diana A. Bayiz

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14 mudstone samples were collected within the sedimentary succession of Mukdadiya Formation (Late Miocene – Early Pliocene) from Shewasoor area at Northeastern Iraq. The samples were subjected to laboratory studies including mineralogical analysis (using X-ray Diffraction technique) in order to identify the clay mineralogy of Mukdadiya Formation of both clay and non-clay minerals. The results of non-clay minerals are: quartz, feldspar and carbonate (calcite and dolomite) minerals. The clay minerals are: montmorillonite, kaolinite, palygorskite, chlorite, and illite by the major basal reflections of each mineral. The origins of these minerals are deduced also.

Keywords: Mukdadiya Formation, mudstone, clay minerals, XRD, Shewasoor

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Authors: Ngwenya M., Gumede T. P., Perez Camargo R. A., Motloung B.

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This study presents the development of eco-friendly bio-nanocomposites using poly(lactic acid) (PLA), poly(caprolactone) (PCL), and their blends with nanocellulose extracted from Saccharum Officinarum. The extracted nanocellulose was optimized through chemical treatment and hydrolysis processes, yielding a sustainable and renewable resource for enhancing polymer properties. Bio-nanocomposites of PLA/nanocellulose, PCL/nanocellulose, and PLA/PCL/nanocellulose with varying nanocellulose contents (1, 3, and 5 wt%) were prepared via melt-blending and characterized using Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), X-ray diffraction (XRD), dynamic mechanical analysis (DMA) and tensile testing. The results show significant improvements in the thermal and mechanical properties of the polymeric matrices upon the addition of nanocellulose, demonstrating the potential of these bio-nanocomposites for advanced applications. These developments are promising for obtaining bio-nanocomposites from local bio-sources, leading to more sustainable and eco-friendly alternatives to traditional materials.

Keywords: bionanocomposites, polycaprolactone, poly(lactic acid), nanocellulose, saccharum officinarum

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Authors: Tae Kyu An

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We demonstrate repurposing linear micropatterns on the CD as a master mold to fabricate TIPS-PEN microwires. From the micropatterns on CDs, we replicated polyurethane acrylate (PUA) templates which are robust and flexible until submicrometer scale patterns. Subsequently, 1.5 μm TIPS-PEN microwires separated by 1.5 μm were grown. Using crystal analysis tools with polarized optical microscopy and X-ray diffraction measurement, it was revealed that each TIPS-PEN microwires are highly crystalline and uniform compared to spin-coated films. It is attributed to the template-guided growth of TIPS-PEN crystals along the linear template, thus the OFETs comprised of TIPS-PEN microwires displayed the high field-effect mobility.

Keywords: compact disk, macro patterning, OFET, soft lithography

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Authors: J. Lyagaeva, D. Medvedev, A. Brouzgou, A. Demin, P. Tsiakaras

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The investigation of highly conductive and chemically stable electrolytes for solid oxide fuel cells (SOFC) is a necessity. The aim of the present work is to study the influence of acceptor dopant on the functional properties of textured BaCe0.5Zr0.3Ln0.2O3−δ (Ln = Yb, Y, Gd, Sm, Nd) ceramics. The X-Ray diffraction analysis, scanning electron microscopy, dilatometry and 4-probe dc method of conductivity measurements were used. It was found that the mean grain size of ceramics increases (from 1.4 to 3.2 μm), thermal expansion coefficient grows (from 7.6•10–6 to 10.7•10–6 К–1), but ionic conductivity decreases (from 14 to 3 mS cm–1 at 900°С), when ionic radii of impurity acceptor increases from 0.868 Å (Yb3+) to 0.983 Å (Nd3+).

Keywords: acceptor dopant, crystal structure, proton-conducting, SOFC

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Authors: A. Hamam, D. Oukil, A. Dib, L. Makhloufi

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The aim of this work is to synthesize modified Polypyrrole films (PPy) containing nanoparticles of copper oxides onto a non conducting cellulosic substrate. Firstly, the chemical polymerization of polypyrrole onto cellulosic substrate is carried out using FeCl3 as an oxidant and Pyrrole as monomer. Different parameters were optimized (monomer concentration, duration of the experiment, nature of supporting electrolyte, temperature, etc.) in order to obtain films with different thickness and different morphologies. Thickness and topography of different PPy deposits were estimated by a profilometer apparatus. The electrochemical reactivity of the obtained electrodes were tested by cyclic voltammetry technique (CV) and electrochemical impedance spectroscopy (EIS). Secondly, the modification of the PPy film surface by incorporation of copper oxide nanonoparticles is conducted by applying a galvanostatic procedure from CuCl2 solution. Surface characterization has been carried out using scanning microscope (SEM) coupled with energy dispersive X-ray analysis (EDX), Fourier-transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD). The analysis showed the presence of the copper oxide nanoparticles (CuO) in the polymer films with dimensions less than 50 nm.

Keywords: polypyrrole, modified electrode, cellulosic substrate, copper oxide

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Authors: Indu Elizabeth

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Antimony/Multi Walled Carbon nano tube nanocomposite (Sb/MWCNT) is synthesized using ethylene glycol mediated reduction process. Binder free, self-supporting and flexible Sb/MWCNT nanocomposite paper has been prepared by employing the vacuum filtration technique. The samples are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Raman spectroscopy (RS), and thermal gravimetric analysis (TGA) to evaluate the structure of anode and tested for its performance in a Lithium rechargeable cell. Electrochemical measurements demonstrate that the Sb/MWCNT composite paper anode delivers a specific discharge capacity of ~400 mAh g-1 up to a current density of 100 mA g-1.

Keywords: antimony, lithium ion battery, multiwalled carbon nanotube, specific capacity

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Authors: Eyyüp Murat Karakurt, Yan Huang, Mehmet Kaya, Hüseyin Demirtaş, Alper İncesu

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In this study, Ti-(x) Nb (at. %) master alloys (x:10, 20, and 30) were fabricated following a standard powder metallurgy route and were sintered at 1200 ˚C for 6h, under 300 MPa by powder metallurgy method. The effect of the Nb concentration in Ti matrix and porosity level was examined experimentally. For metallographic examination, the alloys were analysed by optical microscopy and energy dispersive spectrometry analysis. In addition, X-ray diffraction was performed on the alloys to determine which compound formed in the microstructure. The compression test was applied to the alloys to understand the mechanical behaviors of the alloys. According to Nb concentration in Ti matrix, the β phase increased. Also, porosity level played a crucial role on the mechanical performance of the alloys.

Keywords: Nb concentration, porosity level, powder metallurgy, The β phase

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Authors: Mahendrasingh J. Pawar, M. D. Gaoner

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Ta-doped Nb2O5 (Ta content 0.5-2% mole fraction) nanoparticles in the range of 20-40 nm were synthesized by combustion technique. The crystalline phase, morphology and size of the nanoparticles were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and UV-vis spectroscopy. The specific surface area of the nanoparticles was measured by nitrogen adsorption (BET analysis). The undoped Nb2O5 nanoparticles were found to have the particles size in the range of 50−80 nm. The photocatalytic performance of the samples was characterized by degrading 20 mg/L toluene under UV−Vis irradiation. The results show that the Ta-doped Nb2O5 nanoparticles exhibit a significant increase in photocatalytic performance over the undoped Nb2O5 nanoparticles, and the Nb2O5 nanoparticles doped with 1.5% Ta and calcined at 450°C show the best photocatalytic performance.

Keywords: Nb2O5, Ta-doped Nb2O5, photodegradation of Toluene, combustion method

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Authors: Ana Carolina Kogawa, Selma Gutierrez Antonio, Hérida Regina Nunes Salgado

Abstract:

Rifaximin is an oral antimicrobial, gut - selective and not systemic with adverse effects compared to placebo. It is used for the treatment of hepatic encephalopathy, travelers diarrhea, irritable bowel syndrome, Clostridium difficile, ulcerative colitis and acute diarrhea. The crystalline form present in the rifaximin with minimal systemic absorption is α, being the amorphous form significantly different. Regulators are increasingly attention to polymorphisms. Polymorphs can change the form by altering the drug characteristics compromising the effectiveness and safety of the finished product. International Conference on Harmonization issued the ICH Guidance Q6A, which aim to improve the control of polymorphism in new and existing pharmaceuticals. The objective of this study was to obtain polymorphic forms of rifaximin employing recrystallization processes and characterize them by thermal analysis (thermogravimetry - TG and differential scanning calorimetry - DSC), X-ray diffraction, scanning electron microscopy and solubility test. Six polymorphic forms of rifaximin, designated I to VI were obtained by the crystallization process by evaporation of the solvent. The profiles of the TG curves obtained from polymorphic forms of rifaximin are similar to rifaximin and each other, however, the DTG are different, indicating different thermal behaviors. Melting temperature values of all the polymorphic forms were greater to that shown by the rifaximin, indicating the higher thermal stability of the obtained forms. The comparison of the diffractograms of the polymorphic forms of rifaximin with rifaximin α, β and γ constant in patent indicate that forms III, V and VI are formed by mixing polymorph β and α and form III is formed by polymorph β. The polymorphic form I is formed by polymorph β, but with a significant amount of amorphous material. Already, the polymorphic form II consists of polymorph γ, amorphous. In scanning electron microscope is possible to observe the heterogeneity of morphological characteristics of crystals of polymorphic forms among themselves and with rifaximin. The solubility of forms I and II was greater than the solubility of rifaximin, already, forms III, IV and V presented lower solubility than of rifaximin. Similarly, the bioavailability of the amorphous form of rifaximin is considered significantly higher than the form α, the polymorphic forms obtained in this work can not guarantee the excellent tolerability of the reference medicine. Therefore, studies like these are extremely important and they point to the need for greater requirements by the regulatory agencies competent about polymorphs analysis of the raw materials used in the manufacture of medicines marketed globally. These analyzes are not required in the majority of official compendia. Partnerships between industries, research centers and universities would be a viable way to consolidate researches in this area and contribute to improving the quality of solid drugs.

Keywords: electronic microscopy, polymorphism, rifaximin, solubility, X-ray diffraction

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Authors: Alberto A. Escobar Puentes, G. Adriana García, Luis F. Cuevas G., Alejandro P. Zepeda, Fernando B. Martínez, Susana A. Rincón

Abstract:

Snack foods are usually classified as ‘junk food’ because have little nutritional value. However, due to the increase on the demand and third generation (3G) snacks market, low price and easy to prepare, can be considered as carriers of compounds with certain nutritional value. Resistant starch (RS) is classified as a prebiotic fiber it helps to control metabolic problems and has anti-cancer colon properties. The active compound can be developed by chemical cross-linking of starch with phosphate salts to obtain a type 4 resistant starch (RS4). The chemical reaction can be achieved by extrusion, a process widely used to produce snack foods, since it's versatile and a low-cost procedure. Starch is the major ingredient for snacks 3G manufacture, and the seeds of sorghum contain high levels of starch (70%), the most drought-tolerant gluten-free cereal. Due to this, the aim of this research was to develop a snack (3G), with RS4 in optimal conditions extrusion (previously determined) from sorghum starch, and carry on a sensory, chemically and structural characterization. A sample (200 g) of sorghum starch was conditioned with 4% sodium trimetaphosphate/ sodium tripolyphosphate (99:1) and set to 28.5% of moisture content. Then, the sample was processed in a single screw extruder equipped with rectangular die. The inlet, transport and output temperatures were 60°C, 134°C and 70°C, respectively. The resulting pellets were expanded in a microwave oven. The expansion index (EI), penetration force (PF) and sensory analysis were evaluated in the expanded pellets. The pellets were milled to obtain flour and RS content, degree of substitution (DS), and percentage of phosphorus (% P) were measured. Spectroscopy [Fourier Transform Infrared (FTIR)], X-ray diffraction, differential scanning calorimetry (DSC) and scanning electron microscopy (SEM) analysis were performed in order to determine structural changes after the process. The results in 3G were as follows: RS, 17.14 ± 0.29%; EI, 5.66 ± 0.35 and PF, 5.73 ± 0.15 (N). Groups of phosphate were identified in the starch molecule by FTIR: DS, 0.024 ± 0.003 and %P, 0.35±0.15 [values permitted as food additives (<4 %P)]. In this work an increase of the gelatinization temperature after the crosslinking of starch was detected; the loss of granular and vapor bubbles after expansion were observed by SEM; By using X-ray diffraction, loss of crystallinity was observed after extrusion process. Finally, a snack (3G) was obtained with RS4 developed by extrusion technology. The sorghum starch was efficient for snack 3G production.

Keywords: extrusion, resistant starch, snack (3G), Sorghum

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Authors: SeyedMohammad Hosseini, Amirhossein Moghanian

Abstract:

The main purpose of this research was to design a biomimetic system by freeze-drying method for evaluating the effect of adding 5 and 10 mol. % of zinc (Zn)in 58S bioactive glass and gelatin (5ZnBG/G and 10ZnBG/G) in terms of structural and biological changes. The structural analyses of samples were performed by X-Ray Diffraction (XRD), scanning electron microscopy (SEM), and Fourier-transform infrared spectroscopy (FTIR). Also, 3-(4,5dimethylthiazol-2-yl)-2,5-diphenyltetrazoliumbromide(MTT) and alkaline phosphate (ALP) activity test were carried out for investigation of MC3T3-E1cell behaviors. The SEM results demonstrated the spherical shape of the formed hydroxyapatite (HA) phases, and also HA characteristic peaks were detected by X-ray diffraction spectroscopy (XRD)after 3 days of immersion in the simulated body fluid (SBF) solution. Meanwhile, FTIR spectra proved that the intensity of P–O peaks for 5ZnBG/G was more than 10ZnBG/G and control samples. Moreover, the results of alkaline phosphatase activity (ALP) test illustrated that the optimal amount of Zn (5ZnBG/G) caused a considerable enhancement in bone cell growth. Taken together, the scaffold with 5 mol.% Zn was introduced as an optimal sample because of its higher biocompatibility, in vitro bioactivity, and growth of MC3T3-E1cellsin in comparison with other samples in bone tissue engineering.

Keywords: scaffold, gelatin, modified bioactive glass, alp, bone tissue engineering

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