Search results for: study nucleus as crystal

Authors: Ram Mohan, Mahendran Samykano, Shyam Aravamudhan

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Metallic nanowires with sub-micron and hundreds of nanometer diameter have a diversity of applications in nano/micro-electromechanical systems (NEMS/MEMS). Characterizing the mechanical properties of such sub-micron and nano-scale metallic nanowires are tedious; require sophisticated and careful experimentation to be performed within high-powered microscopy systems (scanning electron microscope (SEM), atomic force microscope (AFM)). Also, needed are nanoscale devices for placing the nanowires; loading them with the intended conditions; obtaining the data for load–deflection during the deformation within the high-powered microscopy environment poses significant challenges. Even picking the grown nanowires and placing them correctly within a nanoscale loading device is not an easy task. Mechanical characterizations through experimental methods for such nanowires are still very limited. Various techniques at different levels of fidelity, resolution, and induced errors have been attempted by material science and nanomaterial researchers. The methods for determining the load, deflection within the nanoscale devices also pose a significant problem. The state of the art is thus still at its infancy. All these factors result and is seen in the wide differences in the characterization curves and the reported properties in the current literature. In this paper, we discuss and present our experimental method, results, and discussions of uniaxial tensile loading and the development of subsequent stress–strain characteristics curves for Nickel nanowires. Nickel nanowires in the diameter range of 220–270 nm were obtained in our laboratory via an electrodeposition method, which is a solution based, template method followed in our present work for growing 1-D Nickel nanowires. Process variables such as the presence of magnetic field, its intensity; and varying electrical current density during the electrodeposition process were found to influence the morphological and physical characteristics including crystal orientation, size of the grown nanowires1. To further understand the correlation and influence of electrodeposition process variables, associated formed structural features of our grown Nickel nanowires to their mechanical properties, careful experiments within scanning electron microscope (SEM) were conducted. Details of the uniaxial tensile characterization, testing methodology, nanoscale testing device, load–deflection characteristics, microscopy images of failure progression, and the subsequent stress–strain curves are discussed and presented.

Keywords: uniaxial tensile characterization, nanowires, electrodeposition, stress-strain, nickel

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Authors: Belen Montero, Carmen Ramirez, Maite Rico, Rebeca Bouza, Irene Derungs

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Starch is a promising polymer for producing biocomposite materials because it is renewable, completely biodegradable and easily available at a low cost. Thermoplastic starches (TPS) can be obtained after the disruption and plasticization of native starch with a plasticizer. In this work, the solvent casting method was used to obtain TPS films from wheat starch plasticized with glycerol and reinforced with nanocellulose (CNC). X-ray diffraction analysis was used to follow the evolution of the crystallinity. The native wheat starch granules have shown a profile corresponding to A-type crystal structures typical for cereal starches. When TPS films are analyzed a high amorphous halo centered on 19º is obtained, indicating the plasticization process is completed. SEM imaging was made in order to analyse the morphology. The image from the raw wheat starch granules shows a bimodal granule size distribution with some granules in large round disk-shape forms (A-type) and the others as smaller spherical particles (B-type). The image from the neat TPS surface shows a continuous surface. No starch aggregates or swollen granules can be seen so, the plasticization process is complete. In the surfaces of reinforced TPS films aggregates are seen as the CNC concentration in the matrix increases. The CNC influence on the mechanical properties of TPS films has been studied by dynamic mechanical analysis. A direct relation exists between the storage modulus values, E’, and the CNC content in reinforced TPS films: higher is the content of nanocellulose in the composite, higher is the value of E’. This reinforcement effect can be explained by the appearance of a strong and crystalline nanoparticle-TPS interphase. Thermal stability of films was analysed by TGA. It has not observed any influence on the behaviour related to the thermal degradation of films with the incorporation of the CNC. Finally, the resistance to the water absorption films was analysed following the standard UNE-EN ISO 1998:483. The percentage of water absorbed by the samples at each time was calculated. The addition of 5 wt % of CNC to the TPS matrix leads to a significant improvement in the moisture resistance of the starch based material decreasing their diffusivity. It has been associated to the formation of a nanocrystal network that prevents swelling of the starch and therefore water absorption and to the high crystallinity of cellulose compared to starch. As a conclusion, the wheat film reinforced with 5 wt % of cellulose nanocrystals seems to be a good alternative for short-life applications into the packaging industry, because of its greatest rigidity, thermal stability and moisture sorption resistance.

Keywords: biocomposites, nanocellulose, starch, wheat

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Authors: Dong Zhao

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Even though the recent claim of room temperature superconductivity by LK-99 was confirmed an unsuccessful attempt, this work reawakened people’s century striving to get applicable superconductors with Tc of room temperature or higher and under ambient pressure. One of the efforts was focusing on exploring the thorium salts. This is because certain thorium compounds revealed an unusual property of having both high electrical conductivity and diamagnetism or the so-called “coexistence of high electrical conductivity and diamagnetism.” It is well known that this property of the coexistence of high electrical conductivity and diamagnetism is held by superconductors because of the electron pairings. Consequently, the likelihood for these thorium compounds to have superconducting properties becomes great. However, as a surprise, these thorium salts possess this property at room temperature and atmosphere pressure. This gives rise to solid evidence for these thorium compounds to be room-temperature superconductors without a need for external pressure. Among these thorium compound superconductors claimed in that work, thorium di-iodide (ThI₂) is a unique one and has received comprehensive discussion. ThI₂ was synthesized and structurally analyzed by the single crystal diffraction method in the 1960s. Its special property of coexistence of high electrical conductivity and diamagnetism was revealed. Because of this unique property, a special molecular configuration was sketched. Except for an ordinary oxidation of +2 for the thorium cation, the thorium’s oxidation state in ThI₂ is +4. According to the experimental results, ThI₂‘s actual molecular configuration was determined as an unusual one of [Th4+(e-)2](I-)2. This means that the ThI₂ salt’s cation is composed of a [Th4+(e-)2]2+ cation core. In other words, the cation of ThI₂ is constructed by combining an oxidation state +4 of the thorium atom and a pair of electrons or an electron lone pair located on the thorium atom. This combination of the thorium atom and the electron lone pair leads to an oxidation state +2 for the [Th4+(e-)2]2+ cation core. This special construction of the thorium cation is very distinctive, which is believed to be the factor that grants ThI₂ the room temperature superconductivity. Actually, the key for ThI₂ to become a room-temperature superconductor is this characteristic electron lone pair residing on the thorium atom along with the formation of a network constructed by the thorium atoms. This network specializes in a way that allows the electron lone pairs to hop over it and, thus, to generate the supercurrent. This work will discuss, in detail, the special electrical and magnetic properties of ThI₂ as well as its structural features at ambient conditions. The exploration of how the electron pairing in combination with the structurally specialized network works together to bring ThI₂ into a superconducting state. From the experimental results, strong evidence has definitely pointed out that the ThI₂ should be a superconductor, at least at room temperature and under atmosphere pressure.

Keywords: co-existence of high electrical conductivity and diamagnetism, electron lone pair, room temperature superconductor, special molecular configuration of thorium di-iodide ThI₂

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Authors: S. Mamoucha, N.Tsafantakis, T. Ioannidis, S. Chatzipanagiotou, C. Nikolaou, L. Skaltsounis, N. Fokialakis, N. Christodoulakis

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Introduction: Pistacia lentiscus L. (well known as Mastic tree) is an evergreen sclerophyllous shrub that extensively thrives in the eastern Mediterranean area yet only the trees cultivated in the southern region of the Greek island Chios produces mastic resin. Different parts of P. lentiscus L. var. chia have been used in folk medicine for various purposes, such as tonic, aphrodisiac, antiseptic, antihypertensive and management of dental, gastrointestinal, liver, urinary, and respiratory tract disorders. Several studies have focused on the antibacterial activity of its resin (gum) and its essential oil. However, there is no study combining anatomy of the plant organs, phytochemical profile, and antibacterial screening of the plant. In our attempt to discover novel bioactive metabolites from the mastic tree, we screened its antibacterial activity not only against ATCC strains but also against clinical, resistant strains. Materials-methods: Leaves were investigated using Transmission (ΤΕΜ) and Scanning Εlectron Microscopy (SEM). Histochemical tests were performed on fresh and fixed tissue. Extracts prepared from dried, powdered leaves using 3 different solvents (DCM, MeOH and H2O) the waste water obtained after a hydrodistillation process for essential oil production were screened for their phytochemical content and antibacterial activity. Μetabolite profiling of polar and non-polar extracts was recorded by GC-MS and LC-HRMS techniques and analyzed using in-house and commercial libraries. The antibacterial screening was performed against Staphylococcus aureus ATCC25923, Escherichia coli ATCC25922, Pseudomonas aeruginosa ATCC27853 and against clinical, resistant strains Methicillin-resistant S. aureus (MRSA), Carbapenem-Resistant Metallo-β-Lactamase (carbapenemase) P. aeruginosa (VIM), Klebsiella pneumoniae carbapenemases (KPCs) and Acinetobacter baumanii resistant strains. The antibacterial activity was tested by the Kirby Bauer and the Agar Well Diffusion method. The zone of inhibition (ZI) of each extract was measured and compared with those of common antibiotics. Results: Leaf is compact with inosclereids and numerous idioblasts containing a globular, spiny crystal. The major nerves of the leaf contain a resin duct. Mesophyll cells showed accumulation of osmiophillic metabolites. Histochemical treatments defined secondary metabolites in subcellular localization. The phytochemical investigation revealed the presence of a large number of secondary metabolites, belonging to different chemical groups, such as terpenoids, phenolic compounds (mainly myricetin, kaempferol and quercetin glycosides), phenolic, and fatty acids. Among the extracts, the hydrostillation wastewater achieved the best results against most of the bacteria tested. MRSA, VIM and A. baumanii were inhibited. Conclusion: Extracts from plants have recently been of great interest with respect to their antimicrobial activity. Their use emerged from a growing tendency to replace synthetic antimicrobial agents with natural ones. Leaves of P. lentiscus L. var. chia showed a high antimicrobial activity even against drug - resistant bacteria. Future prospects concern the better understanding of mode of action of the antibacterial activity, the isolation of the most bioactive constituents and the clarification if the activity is related to a single compound or to the synergistic effect of several ones.

Keywords: antibacterial screening, leaf anatomy, phytochemical profile, Pistacia lentiscus var. chia

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Authors: Taro Komori, Toshiki Gushi, Akihito Anzai, Taku Hirose, Kaoru Toko, Shinji Isogami, Takashi Suemasu

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Ferrimagnetic antiperovskite Mn₄₋ₓNiₓN thin film exhibits both small saturation magnetization and rather large perpendicular magnetic anisotropy (PMA) when x is small. Both of them are suitable features for application to current induced domain wall motion devices using spin transfer torque (STT). In this work, we successfully grew antiperovskite 30-nm-thick Mn₄₋ₓNiₓN epitaxial thin films on MgO(001) and STO(001) substrates by MBE in order to investigate their crystalline qualities and magnetic and magneto-transport properties. Crystalline qualities were investigated by X-ray diffraction (XRD). The magnetic properties were measured by vibrating sample magnetometer (VSM) at room temperature. Anomalous Hall effect was measured by physical properties measurement system. Both measurements were performed at room temperature. Temperature dependence of magnetization was measured by VSM-Superconducting quantum interference device. XRD patterns indicate epitaxial growth of Mn₄₋ₓNiₓN thin films on both substrates, ones on STO(001) especially have higher c-axis orientation thanks to greater lattice matching. According to VSM measurement, PMA was observed in Mn₄₋ₓNiₓN on MgO(001) when x ≤ 0.25 and on STO(001) when x ≤ 0.5, and MS decreased drastically with x. For example, MS of Mn₃.₉Ni₀.₁N on STO(001) was 47.4 emu/cm³. From the anomalous Hall resistivity (ρAH) of Mn₄₋ₓNiₓN thin films on STO(001) with the magnetic field perpendicular to the plane, we found out Mr/MS was about 1 when x ≤ 0.25, which suggests large magnetic domains in samples and suitable features for DW motion device application. In contrast, such square curves were not observed for Mn₄₋ₓNiₓN on MgO(001), which we attribute to difference in lattice matching. Furthermore, it’s notable that although the sign of ρAH was negative when x = 0 and 0.1, it reversed positive when x = 0.25 and 0.5. The similar reversal occurred for temperature dependence of magnetization. The magnetization of Mn₄₋ₓNiₓN on STO(001) increases with decreasing temperature when x = 0 and 0.1, while it decreases when x = 0.25. We considered that these reversals were caused by magnetic compensation which occurred in Mn₄₋ₓNiₓN between x = 0.1 and 0.25. We expect Mn atoms of Mn₄₋ₓNiₓN crystal have larger magnetic moments than Ni atoms do. The temperature dependence stated above can be explained if we assume that Ni atoms preferentially occupy the corner sites, and their magnetic moments have different temperature dependence from Mn atoms at the face-centered sites. At the compensation point, Mn₄₋ₓNiₓN is expected to show very efficient STT and ultrafast DW motion with small current density. What’s more, if angular momentum compensation is found, the efficiency will be best optimized. In order to prove the magnetic compensation, X-ray magnetic circular dichroism will be performed. Energy dispersive X-ray spectrometry is a candidate method to analyze the accurate composition ratio of samples.

Keywords: compensation, ferrimagnetism, Mn₄N, PMA

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Authors: M. Kowalik, J. Masternak, K. Kazimierczuk, O. V. Khavryuchenko, B. Kupcewicz, B. Barszcz

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Recently, the growing interest of chemists in metal-organic coordination polymers (MOCPs) is primarily derived from their intriguing structures and potential applications in catalysis, gas storage, molecular sensing, ion exchanges, nonlinear optics, luminescence, etc. Currently, we are devoting considerable effort to finding the proper method of synthesizing new coordination polymers containing S- or N-heteroaromatic carboxylates as linkers and characterizing the obtained Pb(II) compounds according to their structural diversity, luminescence, and thermal properties. The choice of Pb(II) as the central ion of MOCPs was motivated by several reasons mentioned in the literature: i) a large ionic radius allowing for a wide range of coordination numbers, ii) the stereoactivity of the 6s2 lone electron pair leading to a hemidirected or holodirected geometry, iii) a flexible coordination environment, and iv) the possibility to form secondary bonds and unusual non-covalent interactions, such as classic hydrogen bonds and π···π stacking interactions, as well as nonconventional hydrogen bonds and rarely reported tetrel bonds, Pb(lone pair)···π interactions, C–H···Pb agostic-type interactions or hydrogen bonds, and chelate ring stacking interactions. Moreover, the construction of coordination polymers requires the selection of proper ligands acting as linkers, because we are looking for materials exhibiting different network topologies and fluorescence properties, which point to potential applications. The reaction of Pb(NO₃)₂ with 1H-pyrrole-2-carboxylic acid (2prCOOH) leads to the formation of a new four-nuclear Pb(II) polymer, [Pb4(2prCOO)₈(H₂O)]ₙ, which has been characterized by CHN, FT-IR, TG, PL and single-crystal X-ray diffraction methods. In view of the primary Pb–O bonds, Pb1 and Pb2 show hemidirected pentagonal pyramidal geometries, while Pb2 and Pb4 display hemidirected octahedral geometries. The topology of the strongest Pb–O bonds was determined as the (4·8²) fes topology. Taking the secondary Pb–O bonds into account, the coordination number of Pb centres increased, Pb1 exhibited a hemidirected monocapped pentagonal pyramidal geometry, Pb2 and Pb4 exhibited a holodirected tricapped trigonal prismatic geometry, and Pb3 exhibited a holodirected bicapped trigonal prismatic geometry. Moreover, the Pb(II) lone pair stereoactivity was confirmed by DFT calculations. The 2D structure was expanded into 3D by the existence of non-covalent O/C–H···π and Pb···π interactions, which was confirmed by the Hirshfeld surface analysis. The above mentioned interactions improve the rigidity of the structure and facilitate the charge and energy transfer between metal centres, making the polymer a promising luminescent compound.

Keywords: coordination polymers, fluorescence properties, lead(II), lone electron pair stereoactivity, non-covalent interactions

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Authors: Veronica Caprai, Katrin Schollbach, Miruna V. A. Florea, H. J. H. Brouwers

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Nowadays MSWI (Municipal Solid Waste Incineration) bottom ash (BA) produced by Waste-to-Energy (WtE) plants represents the majority of the solid residues derived from MSW incineration. Once processed, the BA is often landfilled resulting in possible environmental problems, additional costs for the plant and increasing occupation of public land. In order to limit this phenomenon, European countries such as the Netherlands aid the utilization of MSWI BA in the construction field, by providing standards about the leaching of contaminants into the environment (Dutch Soil Quality Decree). Commonly, BA has a particle size below 32 mm and a heterogeneous chemical composition, depending on its source. By washing coarser BA, an MSWI sludge is obtained. It is characterized by a high content of heavy metals, chlorides, and sulfates as well as a reduced particle size (below 0.25 mm). To lower its environmental impact, MSWI sludge is filtered or centrifuged for removing easily soluble contaminants, such as chlorides. However, the presence of heavy metals is not easily reduced, compromising its possible application. For lowering the leaching of those contaminants, the use of MSWI residues in combination with cement represents a precious option, due to the known retention of those ions into the hydrated cement matrix. Among the applications, the European standard for common cement EN 197-1:1992 allows the incorporation of up to 5% by mass of a minor additional constituent (MAC), such as fly ash or blast furnace slag but also an unspecified filler into cement. To the best of the author's knowledge, although it is widely available, it has the appropriate particle size and a chemical composition similar to cement, FC has not been investigated as possible MAC in cement production. Therefore, this paper will address the suitability of MSWI FC as MAC for CEM I 52.5 R, within a 5% maximum replacement by mass. After physical and chemical characterization of the raw materials, the crystal phases of the pastes are determined by XRD for 3 replacement levels (1%, 3%, and 5%) at different ages. Thereafter, the impact of FC on mechanical and environmental performances of cement is assessed according to EN 196-1 and the Dutch Soil Quality Decree, respectively. The investigation of the reaction products evidences the formation of layered double hydroxides (LDH), in the early stage of the reaction. Mechanically the presence of FC results in a reduction of 28 days compressive strength by 8% for a replacement of 5% wt., compared with the pure CEM I 52.5 R without any MAC. In contrast, the flexural strength is not affected by the presence of FC. Environmentally, the Dutch legislation for the leaching of contaminants for unshaped (granular) material is satisfied. Based on the collected results, FC represents a suitable candidate as MAC in cement production.

Keywords: environmental impact evaluation, Minor additional constituent, MSWI residues, X-ray diffraction crystallography

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Authors: Victoria Molina, Wendy Franco, Sergio Benavides, José M. Troncoso, Ricardo Luna, Jose R. PéRez-Correa

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Emamectin Benzoate (EB) is a crystal antiparasitic that belongs to the avermectin family. It is one of the most common treatments used in Chile to control Caligus rogercresseyi in Atlantic salmon. However, the sea lice acquired resistance to EB when it is exposed at sublethal EB doses. The low solubility rate of EB and its degradation at the acidic pH in the fish digestive tract are the causes of the slow absorption of EB in the intestine. To protect EB from degradation and enhance its absorption, specific microencapsulation technologies must be developed. Amorphous Solid Dispersion techniques such as Spray Drying (SD) and Ionic Gelation (IG) seem adequate for this purpose. Recently, Soluplus® (SOL) has been used to increase the solubility rate of several drugs with similar characteristics than EB. In addition, alginate (ALG) is a widely used polymer in IG for biomedical applications. Regardless of the encapsulation technique, the quality of the obtained microparticles is evaluated with the following responses, yield (Y%), encapsulation efficiency (EE%) and loading capacity (LC%). In addition, it is important to know the percentage of EB released from the microparticles in gastric (GD%) and intestinal (ID%) digestions. In this work, we microencapsulated EB with SOL (EB-SD) and with ALG (EB-IG) using SD and IG, respectively. Quality microencapsulation responses and in vitro gastric and intestinal digestions at pH 3.35 and 7.8, respectively, were obtained. A central composite design was used to find the optimum microencapsulation variables (amount of EB, amount of polymer and feed flow). In each formulation, the behavior of these variables was predicted with statistical models. Then, the response surface methodology was used to find the best combination of the factors that allowed a lower EB release in gastric conditions, while permitting a major release at intestinal digestion. Two approaches were used to determine this. The desirability approach (DA) and multi-objective optimization (MOO) with multi-criteria decision making (MCDM). Both microencapsulation techniques allowed to maintain the integrity of EB in acid pH, given the small amount of EB released in gastric medium, while EB-IG microparticles showed greater EB release at intestinal digestion. For EB-SD, optimal conditions obtained with MOO plus MCDM yielded a good compromise among the microencapsulation responses. In addition, using these conditions, it is possible to reduce microparticles costs due to the reduction of 60% of BE regard the optimal BE proposed by (DA). For EB-GI, the optimization techniques used (DA and MOO) yielded solutions with different advantages and limitations. Applying DA costs can be reduced 21%, while Y, GD and ID showed 9.5%, 84.8% and 2.6% lower values than the best condition. In turn, MOO yielded better microencapsulation responses, but at a higher cost. Overall, EB-SD with operating conditions selected by MOO seems the best option, since a good compromise between costs and encapsulation responses was obtained.

Keywords: microencapsulation, multiple decision-making criteria, multi-objective optimization, Soluplus®

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Authors: Xiaoling Ren, Guidong Yang

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Ammonia, as one of the largest-volume industrial chemicals, is mostly produced by century-old Haber-Bosch process with extreme conditionsand high-cost. Under the circumstance, researchersarededicated in finding new ways to replace the Haber-Bosch process. Photocatalytic nitrogen fixation is a promising sustainable, clear and green strategy for ammonia synthesis, butit is still a big challenge due to the high activation energy for nitrogen. It is essential to develop an efficient photocatalyst for making this approach industrial application. Constructing chemisorption active sites through defect engineering can be defined as an effective and reliable means to improve nitrogen activation by forming the extraordinary coordination environment and electronic structure. Besides, the construction of three-dimensionally orderdmacroporous (3DOM) structured photocatalyst is considered to be one of effectivestrategiesto improve the activity due to it canincrease the diffusion rate of reactants in the interior, which isbeneficial to the mass transfer process of nitrogen molecules in photocatalytic nitrogen reduction. Herein, Fe doped 3DOM WO₃(Fe-3DOM WO₃) without noble metal cocatalysts is synthesized by a polystyrene-template strategy, which is firstly used for photocatalytic nitrogen fixation. To elucidate the chemical nature of the dopant, the X-ray diffraction (XRD) analysiswas conducted. The pure 3DOM WO₃ has a monoclinic type crystal structure. And no additional peak is observed in Fe doped 3DOM WO₃, indicating that the incorporation of Fe atoms did not result in a secondary phase formation. In order to confirm the morphologies of Fe-3DOM WO₃and 3DOM WO₃, scanning electron microscopy (SEM) was employed. The synthesized Fe-3DOM WO₃and 3DOM WO₃ both exhibit a highly ordered three dimensional inverse opal structure with interconnected pores. From high-resolution TEM image of Fe-3DOM WO₃, the ordered lattice fringes with a spacing of 3.84 Å can be assigned to the (001) plane of WO₃, which is consistent with the XRD results. Finally, the photocatalytic nitrogen reduction performance of 3DOM WO₃ and Fe doped 3DOM WO₃with various Fe contents were examined. As a result, both Fe-3DOM WO₃ samples achieve higher ammonia production rate than that of pure 3DOM WO₃, indicating that the doped Fe plays a critical role in the photocatalytic nitrogen fixation performance. To verify the reaction process upon N2 reduction on the Fe-3DOM WO₃, in-situ diffuse reflectance infrared Fourier-transform spectroscopy was employed to monitor the intermediates. The in-situ DRIFTS spectra of Fe-3DOM WO₃ exhibit the increased signals with the irradiation time from 0–60min in the N2 atmosphere. The above results prove that nitrogen is gradually hydrogenated to produce ammonia over Fe-3DOM WO₃. Thiswork would enrich our knowledge in designing efficient photocatalystsfor photocatalytic nitrogen reduction.

Keywords: ammonia, photocatalytic, nitrogen fixation, Fe doped 3DOM WO₃

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Authors: Nikolai A. Khlebnikov, Vladimir N. Krasilnikov, Evgenii V. Polyakov, Anastasia A. Maltceva

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Carbon materials with advanced surfaces are widely used both in modern industry and in environmental protection. The physical-chemical nature of these materials is determined by the morphology of primary atomic and molecular carbon structures, which are the basis for synthesizing the following materials: zero-dimensional (fullerenes), one-dimensional (fiber, tubes), two-dimensional (graphene) carbon nanostructures, three-dimensional (multi-layer graphene, graphite, foams) with unique physical-chemical and functional properties. Experience shows that the microscopic morphological level is the basis for the creation of the next mesoscopic morphological level. The dependence of the morphology on the chemical way and process prehistory (crystallization, colloids formation, liquid crystal state and other) is the peculiarity of the last called level. These factors determine the consumer properties of carbon materials, such as specific surface area, porosity, chemical resistance in corrosive environments, catalytic and adsorption activities. Based on the developed ideology of thin precursor synthesis, the authors discuss one of the approaches of the porosity control of carbon-containing materials with a given aggregates morphology. The low-temperature thermolysis of precursors in a gas environment of a given composition is the basis of the above-mentioned idea. The processes of carbothermic precursor synthesis of two different compounds: tungsten carbide WC:nC and zinc oxide ZnO:nC containing an impurity phase in the form of free carbon were selected as subjects of the research. In the first case, the transition metal (tungsten) forming carbides was the object of the synthesis. In the second case, there was selected zinc that does not form carbides. The synthesis of both kinds of transition metals compounds was conducted by the method of precursor carbothermic synthesis from the organic solution. ZnO:nC composites were obtained by thermolysis of succinate Zn(OO(CH2)2OO), formate glycolate Zn(HCOO)(OCH2CH2O)1/2, glycerolate Zn(OCH2CHOCH2OH), and tartrate Zn(OOCCH(OH)CH(OH)COO). WC:nC composite was synthesized from ammonium paratungstate and glycerol. In all cases, carbon structures that are specific for diamond- like carbon forms appeared on the surface of WC and ZnO particles after the heat treatment. Tungsten carbide and zinc oxide were removed from the composites by selective chemical dissolution preserving the amorphous carbon phase. This work presents the results of investigating WC:nC and ZnO:nC composites and carbon nanopowders with tubular, tape, plate and onion morphologies of aggregates that are separated by chemical dissolution of WC and ZnO from the composites by the following methods: SEM, TEM, XPA, Raman spectroscopy, and BET. The connection between the carbon morphology under the conditions of synthesis and chemical nature of the precursor and the possibility of regulation of the morphology with the specific surface area up to 1700-2000 m2/g of carbon-structured materials are discussed.

Keywords: carbon morphology, composite materials, precursor synthesis, tungsten carbide, zinc oxide

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Authors: Adela Diepoltova, Klara Konecna, Ondrej Jandourek, Petr Nachtigal

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A loss of control over antibiotic-resistant pathogens has become a global issue due to severe and often untreatable infections. This state is reflected in complicated treatment, health costs, and higher mortality. All these factors emphasize the urgent need for the discovery and development of new anti-infectives. One of the most common pathogens mentioned in the phenomenon of antibiotic resistance are bacteria of the genus Staphylococcus. These bacterial agents have developed several mechanisms against the effect of antibiotics. One of them is biofilm formation. In staphylococci, biofilms are associated with infections such as endocarditis, osteomyelitis, catheter-related bloodstream infections, etc. To author's best knowledge, no validated and standardized methodology evaluating candidate compound activity against staphylococcal biofilms exists. However, a variety of protocols for in vitro drug activity testing has been suggested, yet there are often fundamental differences. Based on our experience, a key methodological step that leads to credible results is to form a robust biofilm with appropriate attributes such as firm adherence to the substrate, a complex arrangement in layers, and the presence of extracellular polysaccharide matrix. At first, for the purpose of drug antibiofilm activity evaluation, the focus was put on various conditions (supplementation of cultivation media by human plasma/fetal bovine serum, shaking mode, the density of initial inoculum) that should lead to reproducible and robust in vitro staphylococcal biofilm formation in microtiter plate model. Three model staphylococcal reference strains were included in the study: Staphylococcus aureus (ATCC 29213), methicillin-resistant Staphylococcus aureus (ATCC 43300), and Staphylococcus epidermidis (ATCC 35983). The total biofilm biomass was quantified using the Christensen method with crystal violet, and results obtained from at least three independent experiments were statistically processed. Attention was also paid to the viability of the biofilm-forming staphylococcal cells and the presence of extracellular polysaccharide matrix. The conditions that led to robust biofilm biomass formation with attributes for biofilms mentioned above were then applied by introducing an alternative method analogous to the commercially available test system, the Calgary Biofilm Device. In this test system, biofilms are formed on pegs that are incorporated into the lid of the microtiter plate. This system provides several advantages (in situ detection and quantification of biofilm microbial cells that have retained their viability after drug exposure). Based on our preliminary studies, it was found that the attention to the peg surface and substrate on which the bacterial biofilms are formed should also be paid to. Therefore, further steps leading to the optimization were introduced. The surface of pegs was coated by human plasma, fetal bovine serum, and L-polylysine. Subsequently, the willingness of bacteria to adhere and form biofilm was monitored. In conclusion, suitable conditions were revealed, leading to the formation of reproducible, robust staphylococcal biofilms in vitro for the microtiter model and the system analogous to the Calgary biofilm device, as well. The robustness and typical slime texture could be detected visually. Likewise, an analysis by confocal laser scanning microscopy revealed a complex three-dimensional arrangement of biofilm forming organisms surrounded by an extracellular polysaccharide matrix.

Keywords: anti-biofilm drug activity screening, in vitro biofilm formation, microtiter plate model, the Calgary biofilm device, staphylococcal infections, substrate modification, surface coating

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Authors: Biswaranjan D. Mohapatra, Ipsha Hota, Swarna P. Mantry, Nibedita Behera, Kumar S. K. Varadwaj

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Designing highly active and low-cost oxygen evolution (2H₂O → 4H⁺ + 4e⁻ + O₂) electrocatalyst is one of the most active areas of advanced energy research. Some precious metal-based electrocatalysts, such as IrO₂ and RuO₂, have shown excellent performance for oxygen evolution reaction (OER); however, they suffer from high-cost and low abundance which limits their applications. Recently, layered double hydroxides (LDHs), composed of layers of divalent and trivalent transition metal cations coordinated to hydroxide anions, have gathered attention as an alternative OER catalyst. However, LDHs are insulators and coupled with carbon materials for the electrocatalytic applications. Graphene covalently doped with nitrogen has been demonstrated to be an excellent electrocatalyst for energy conversion technologies such as; oxygen reduction reaction (ORR), oxygen evolution reaction (OER) & hydrogen evolution reaction (HER). However, they operate at high overpotentials, significantly above the thermodynamic standard potentials. Recently, we reported remarkably enhanced catalytic activity of benzoate or 1-pyrenebutyrate functionalized N-doped graphene towards the ORR in alkaline medium. The molecular and heteroatom co-doping on graphene is expected to tune the electronic structure of graphene. Therefore, an innovative catalyst architecture, in which LDHs are anchored on aromatic acid functionalized ‘N’ doped graphene may presumably boost the OER activity to a new benchmark. Herein, we report fabrication of Co₂Fe-LDH on aromatic acid (AA) functionalized ‘N’ doped reduced graphene oxide (NG) and studied their OER activities in alkaline medium. In the first step, a novel polyol method is applied for synthesis of AA functionalized NG, which is well dispersed in aqueous medium. In the second step, Co₂Fe LDH were grown on AA functionalized NG by co-precipitation method. The hybrid samples are abbreviated as Co₂Fe LDH/AA-NG, where AA is either Benzoic acid or 1, 3-Benzene dicarboxylic acid (BDA) or 1, 3, 5 Benzene tricarboxylic acid (BTA). The crystal structure and morphology of the samples were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM) and transmission electron microscope (TEM). These studies confirmed the growth of layered single phase LDH. The electrocatalytic OER activity of these hybrid materials was investigated by rotating disc electrode (RDE) technique on a glassy carbon electrode. The linear sweep voltammetry (LSV) on these catalyst samples were taken at 1600rpm. We observed significant OER performance enhancement in terms of onset potential and current density on Co₂Fe LDH/BTA-NG hybrid, indicating the synergic effect. This exploration of molecular functionalization effect in doped graphene and LDH system may provide an excellent platform for innovative design of OER catalysts.

Keywords: π-π functionalization, layered double hydroxide, oxygen evolution reaction, reduced graphene oxide

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Authors: Zubair Ahmed, Andrea Barbieri

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The need to reduce energy consumption has prompted a considerable research effort for developing alternative energy-efficient lighting systems to replace conventional light sources (i.e., incandescent and fluorescent lamps). Organic light emitting device (OLED) technology offers the distinctive possibility to fabricate large area flat devices by vacuum or solution processing. Lanthanide β-diketonates complexes, due to unique photophysical properties of Ln(III) ions, have been explored as emitting layers in OLED displays and in solid-state lighting (SSL) in order to achieve high efficiency and color purity. For such applications, the excellent photoluminescence quantum yield (PLQY) and stability are the two key points that can be achieved simply by selecting the proper organic ligands around the Ln ion in a coordination sphere. Regarding the strategies to enhance the PLQY, the most common is the suppression of the radiationless deactivation pathways due to the presence of high-frequency oscillators (e.g., OH, –CH groups) around the Ln centre. Recently, a different approach to maximize the PLQY of Ln(β-DKs) has been proposed (named 'Escalate Coordination Anisotropy', ECA). It is based on the assumption that coordinating the Ln ion with different ligands will break the centrosymmetry of the molecule leading to less forbidden transitions (loosening the constraints of the Laporte rule). The OLEDs based on such complexes are available, but with low efficiency and stability. In order to get efficient devices, there is a need to develop some new Ln complexes with enhanced PLQYs and stabilities. For this purpose, the Ln complexes, both visible and (NIR) emitting, of variant coordination structures based on the various fluorinated/non-fluorinated β-diketones and O/N-donor neutral ligands were synthesized using a one step in situ method. In this method, the β-diketones, base, LnCl₃.nH₂O and neutral ligands were mixed in a 3:3:1:1 M ratio in ethanol that gave air and moisture stable complexes. Further, they were characterized by means of elemental analysis, NMR spectroscopy and single crystal X-ray diffraction. Thereafter, their photophysical properties were studied to select the best complexes for the fabrication of stable and efficient OLEDs. Finally, the OLEDs were fabricated and investigated using these complexes as emitting layers along with other organic layers like NPB,N,N′-Di(1-naphthyl)-N,N′-diphenyl-(1,1′-biphenyl)-4,4′-diamine (hole-transporting layer), BCP, 2,9-Dimethyl-4,7-diphenyl-1,10-phenanthroline (hole-blocker) and Alq3 (electron-transporting layer). The layers were sequentially deposited under high vacuum environment by thermal evaporation onto ITO glass substrates. Moreover, co-deposition techniques were used to improve charge transport in the devices and to avoid quenching phenomena. The devices show strong electroluminescence at 612, 998, 1064 and 1534 nm corresponding to ⁵D₀ →⁷F₂(Eu), ²F₅/₂ → ²F₇/₂ (Yb), ⁴F₃/₂→ ⁴I₉/₂ (Nd) and ⁴I1₃/₂→ ⁴I1₅/₂ (Er). All the devices fabricated show good efficiency as well as stability.

Keywords: electroluminescence, lanthanides, paramagnetic NMR, photoluminescence

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Authors: Mustapha A. Tijjani, Fanna I. Abdulrahman, Irfan Z. Khan, Umar K. Sandabe, Cong Li

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Air dried sample V. doniana after collection and identification was extracted with ethanol and further partition with chloroform, ethyl acetate and n-butanol. Ethanolic extract (11.9g) was fractionated on a silica gel accelerated column chromatography using solvents such as n-hexane, ethyl acetate and methanol. Each eluent fractions (150ml aliquots) were collected and monitored with thin layer chromatography. Fractions with similar Rf values from same solvents system were pooled together. Phytochemical test of all the fractions were performed using standard procedure. Complete elution yielded 48 fractions (150ml/fraction) which were pooled to 24 fractions base on the Rf values. It was further recombined and 12 fractions were obtained on the basis on Rf values and coded Vd1 to Vd12 fractions. Vd8 was further eluted with ethylacetate and methanol and gave fourteen sub fractions Vd8-a, -Vd8-m. Fraction Vd8-a (56mg) gave a white crystal compound coded V1. It was further checked on TLC and observed under ultraviolet lamp and was found to give a single spot. The Rf values were calculated to be 0.433. The melting point was determined using Gallenkamp capillary melting point apparatus and found to be 241-243°C uncorrected. Characterization of the isolated compound coded V1 was done using FT-infra-red spectroscopy, HNMR, 13CNMR(1and 2D) and HRESI-MS. The IR spectrum of compound V1 shows prominent peaks that corresponds to OHstr (3365cm-1) and C=0 (1652cm-1) etc. This spectrum suggests that among the functional moiety in compound V1 are the carbonyl and hydroxyl group. The 1H NMR (400 MHz) spectrum of compound V1 in DMSO-d6 displayed five singlet signals at δ 0.72 (3H, s, H-18), 0.79 (3H, s, H-19), 1.03 (3H, s, H-21), 1.04 (3H, s, H-26), 1.06 (3H, s, H-27) each integrating for three protons indicating the five methyl functional groups present in the compound. It further showed a broad singlet at δ 5.58 integrated for 1 H due to an olefinic H-atom adjacent to the carbonyl carbon atom. Three signals at δ 3.10 (d, J = 9.0 Hz, H-22), 3.59 (m, 1H, 2H-a) and 3.72 (m, 1H, 3H-e), each integrating for one proton is due to oxymethine protons indicating that three oxymethine H-atoms are present in the compound. These all signals are characteristic to the ecdysteroid skeletons. The 13C-NMR spectrum showed the presence of 27 carbon atoms, suggesting that may be steroid skeleton. The DEPT-135 experiment showed the presence of five CH3, eight CH2, and seven CH groups, and seven quaternary C-atoms. The molecular formula was established as C27H44O7 by high resolution electron spray ionization-mass spectroscopy (HRESI-MS) positive ion mode m/z 481.3179. The signals in mass spectrum are 463, 445, and 427 peaks corresponding to losses of one, two, three, or four water molecules characteristic for ecdysterone skeleton reported in the literature. Based on the spectral analysis (HNMR, 13CNMR, DEPT, HMQC, IR, HRESI-MS) the compound V1 is thus concluded to have ecdysteriod skeleton and conclusively conforms with 2β, 3β 14α, 20R, 22R, 25-hexahydroxy-5 β cholest-7-ene-6- one, or 2, 3, 14, 20, 22, 25 hexahydroxy cholest-7-ene-6-one commonly known as 20-hydroxyecdysone.

Keywords: vitex, phytochemical, purification, isolation, chromatography, spectroscopy

Procedia PDF Downloads 348

Authors: Radik D. Aglyamov, Alexander K. Naumov, Alexey A. Shavelev, Oleg A. Morozov, Arsenij D. Shishkin, Yury P.Brodnikovsky, Alexander A.Karabutov, Alexander A. Oraevsky, Vadim V. Semashko

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The development of medical optoacoustic tomography with the using human blood as endogenic contrast agent is constrained by the lack of reliable, easy-to-use and inexpensive sources of high-power pulsed laser radiation in the spectral region of 750-900 nm [1-2]. Currently used titanium-sapphire, alexandrite lasers or optical parametric light oscillators do not provide the required and stable output characteristics, they are structurally complex, and their cost is up to half the price of diagnostic optoacoustic systems. Here we are developing the lasers based on Cr:LiCaAlF6 crystals which are free of abovementioned disadvantages and provides intensive ten’s ns-range tunable laser radiation at specific absorption bands of oxy- (~840 nm) and -deoxyhemoglobin (~757 nm) in the blood. Cr:LiCAF (с=3 at.%) crystals were grown in Kazan Federal University by the vertical directional crystallization (Bridgman technique) in graphite crucibles in a fluorinating atmosphere at argon overpressure (P=1500 hPa) [3]. The laser elements have cylinder shape with the diameter of 8 mm and 90 mm in length. The direction of the optical axis of the crystal was normal to the cylinder generatrix, which provides the π-polarized laser action correspondent to maximal stimulated emission cross-section. The flat working surfaces of the active elements were polished and parallel to each other with an error less than 10”. No any antireflection coating was applied. The Q-switched master oscillator-power amplifiers laser system (MOPA) with the dual-Xenon flashlamp pumping scheme in diffuse-reflectivity close-coupled head were realized. A specially designed laser cavity, consisting of dielectric highly reflective reflectors with a 2 m-curvature radius, a flat output mirror, a polarizer and Q-switch sell, makes it possible to operate sequentially in a circle (50 ns - laser one pulse after another) at wavelengths of 757 and 840 nm. The programmable pumping system from Tomowave Laser LLC (Russia) provided independent to each pulses (up to 250 J at 180 μs) pumping to equalize the laser radiation intensity at these wavelengths. The MOPA laser operates at 10 Hz pulse repetition rate with the output energy up to 210 mJ. Taking into account the limitations associated with physiological movements and other characteristics of patient tissues, the duration of laser pulses and their energy allows molecular and functional high-contrast imaging to depths of 5-6 cm with a spatial resolution of at least 1 mm. Highly likely the further comprehensive design of laser allows improving the output properties and realizing better spatial resolution of medical multispectral optoacoustic tomography systems.

Keywords: medical optoacoustic, endogenic contrast agent, multiwavelength tunable pulse lasers, MOPA laser system

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Authors: Laura Kocsor, Laszlo Peter, Laszlo Kovacs, Zsolt Kis

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The aim of our research is to prepare rare-earth-doped lithium niobate (LiNbO3) nanocrystals, having only a few dopant ions in the focal point of an exciting laser beam. These samples will be used to achieve individual addressing of the dopant ions by light beams in a confocal microscope setup. One method for the preparation of nanocrystalline materials is to reduce the particle size by mechanical grinding. High-energy ball-milling was used in several works to produce nano lithium niobate. Previously, it was reported that dry high-energy ball-milling of lithium niobate in a shaker mill results in the partial reduction of the material, which leads to a balanced formation of bipolarons and polarons yielding gray color together with oxygen release and Li2O segregation on the open surfaces. In the present work we focus on preparing LiNbO3 nanocrystals by high-energy ball-milling using a Fritsch Pulverisette 7 planetary mill. Every ball-milling process was carried out in zirconia vial with zirconia balls of different sizes (from 3 mm to 0.1 mm), wet grinding with water, and the grinding time being less than an hour. Gradually decreasing the ball size to 0.1 mm, an average particle size of about 10 nm could be obtained determined by dynamic light scattering and verified by scanning electron microscopy. High-energy ball-milling resulted in sample darkening evidenced by optical absorption spectroscopy measurements indicating that the material underwent partial reduction. The unwanted lithium oxide loss decreases the Li/Nb ratio in the crystal, strongly influencing the spectroscopic properties of lithium niobate. Zirconia contamination was found in ground samples proved by energy-dispersive X-ray spectroscopy measurements; however, it cannot be explained based on the hardness properties of the materials involved in the ball-milling process. It can be understood taking into account the presence of lithium hydroxide formed the segregated lithium oxide and water during the ball-milling process, through chemically induced abrasion. The quantity of the segregated Li2O was measured by coulometric titration. During the wet milling process in the planetary mill, it was found that the lithium oxide loss increases linearly in the early phase of the milling process, then a saturation of the Li2O loss can be seen. This change goes along with the disappearance of the relatively large particles until a relatively narrow size distribution is achieved in accord with the dynamic light scattering measurements. With the 3 mm ball size and 1100 rpm rotation rate, the mean particle size achieved is 100 nm, and the total Li2O loss is about 1.2 wt.% of the original LiNbO3. Further investigations have been done to minimize the Li2O segregation during the ball-milling process. Since the Li2O loss was observed to increase with the growing total surface of the particles, the influence of ball-milling parameters on its quantity has also been studied.

Keywords: high-energy ball-milling, lithium niobate, mechanochemical reaction, nanocrystals

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Authors: Mojtaba Eshraghi Arani

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Ship financing is the vital element in the development of shipping industry because while the ship constitutes the owners’ main asset, she is considered a reliable security in the financiers’ viewpoint as well. However, it is most probable that a financier who has accepted a ship as security will face many creditors who are privileged and rank before him for collecting, out of the ship, the money that they are owed. In fact, according to the current rule of maritime law, which was established by “Convention Internationale pour l’Unification de Certaines Règles Relatives aux Privilèges et Hypothèques Maritimes, Brussels, 10 April 1926”, the mortgages, hypotheques, and other charges on vessels rank after several secured claims referred to as “maritime liens”. Such maritime liens are an exhaustive list of claims including but not limited to “expenses incurred in the common interest of the creditors to preserve the vessel or to procure its sale and the distribution of the proceeds of sale”, “tonnage dues, light or harbour dues, and other public taxes and charges of the same character”, “claims arising out of the contract of engagement of the master, crew and other persons hired on board”, “remuneration for assistance and salvage”, “the contribution of the vessel in general average”, “indemnities for collision or other damage caused to works forming part of harbours, docks, etc,” “indemnities for personal injury to passengers or crew or for loss of or damage to cargo”, “claims resulting form contracts entered into or acts done by the master”. The same rule survived with only some minor change in the categories of maritime liens in the substitute conventions 1967 and 1993. The status que in maritime law have always been considered as a major obstacle to the development of shipping market and has inevitably led to increase in the interest rates and other related costs of ship financing. It seems that the national and international policy makers have yet to change their mind being worried about the deviation from the old marine traditions. However, it is crystal clear that the continuation of status que will harm, to a great extent, the shipowners and, consequently, the international merchants as a whole. It is argued in this article that the raison d'être for many categories of maritime liens cease to exist anymore, in view of which, the international community has to recognize only a minimum category of maritime liens which are created in the common interests of all creditors; to this effect, only two category of “compensation due for the salvage of ship” and “extraordinary expenses indispensable for the preservation of the ship” can be declared as taking priority over the mortgagee rights, in anology with the Geneva Convention on the International Recognition of Rights in Aircrafts (1948). A qualitative method with the concept of interpretation of data collection has been used in this manuscript. The source of the data is the analysis of international conventions and domestic laws.

Keywords: ship finance, mortgage, maritime liens, brussels convenion, geneva convention 1948

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Authors: Melanie Francois, Gilles Caboche, Frederic Demoisson, Francois Maeght, Maria Paola Carpanese, Lionel Combemale, Pascal Briois

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Finding new clean, and efficient way for energy production is one of the actual global challenges. Advances in fuel cell technology have shown that, for few years, Protonic Ceramic Fuel Cell (PCFC) has attracted much attention in the field of new hydrogen energy thanks to their lower working temperature, possible higher efficiency, and better durability than classical SOFC. On the contrary of SOFC, where O²⁻ oxygen ion is the charge carrier, PCFC works with H⁺ proton as a charge carrier. Consequently, the lower activation energy of proton diffusion compared to the one of oxygen ion explains those benefits and allows PCFC to work in the 400-600°C temperature range. Doped-BaCeO₃ is currently the most chosen material for this application because of its high protonic conductivity; for example, BaCe₀.₉Y₀.₁O₃ δ exhibits a total conductivity of 1.5×10⁻² S.cm⁻¹ at 600°C in wet H₂. However, BaCeO₃ based perovskite has low stability in H₂O and/or CO₂ containing atmosphere, which limits their practical application. On the contrary, BaZrO₃ based perovskite exhibits good chemical stability but lower total conductivity than BaCeO₃ due to its larger grain boundary resistance. By substituting zirconium with 20% of yttrium, it is possible to achieve a total conductivity of 2.5×10⁻² S.cm⁻¹ at 600°C in wet H₂. However, the high refractory property of BaZr₀.₈Y₀.₂O₃-δ (noted BZY20) causes problems to obtain a dense membrane with large grains. Thereby, using a synthesis process that gives fine particles could allow better sinterability and thus decrease the number of grain boundaries leading to a higher total conductivity. In this work, BaZr₀.₈Y₀.₂O₃-δ have been synthesized by classical batch hydrothermal device and by a continuous hydrothermal device developed at ICB laboratory. The two variants of this process are able to work in supercritical conditions, leading to the formation of nanoparticles, which could be sintered at a lower temperature. The as-synthesized powder exhibits the right composition for the perovskite phase, impurities such as BaCO₃ and YO-OH were detected at very low concentration. Microstructural investigation and densification rate measurement showed that the addition of 1 wt% of ZnO as sintering aid and a sintering at 1550°C for 5 hours give high densified electrolyte material. Furthermore, it is necessary to heat the synthesized powder prior to the sintering to prevent the formation of secondary phases. It is assumed that this thermal treatment homogenizes the crystal structure of the powder and reduces the number of defects into the bulk grains. Electrochemical impedance spectroscopy investigations in various atmospheres and a large range of temperature (200-700°C) were then performed on sintered samples, and the protonic conductivity of BZY20 has been highlighted. Further experiments on half-cell, NiO-BZY20 as anode and BZY20 as electrolyte, are in progress.

Keywords: hydrothermal synthesis, impedance measurement, Y-doped BaZrO₃, proton conductor

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

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

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

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Authors: Yohann R. J. Thomas, Sébastien Solan

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Conventional battery technology includes the assembly of electrode/separator/electrode by standard techniques such as stacking or winding, depending on the format size. In that type of batteries, coating or pasting techniques are only used for the electrode process. The processes are suited for large scale production of batteries and perfectly adapted to plenty of application requirements. Nevertheless, as the demand for both easier and cost-efficient production modes, flexible, custom-shaped and efficient small sized batteries is rising. Thin-film, printable batteries are one of the key areas for printed electronics. In the frame of European BASMATI project, we are investigating the feasibility of a new design of lithium-ion battery: interdigitated planar core design. Polymer substrate is used to produce bendable and flexible rechargeable accumulators. Direct fully printed batteries lead to interconnect the accumulator with other electronic functions for example organic solar cells (harvesting function), printed sensors (autonomous sensors) or RFID (communication function) on a common substrate to produce fully integrated, thin and flexible new devices. To fulfill those specifications, a high resolution printing process have been selected: Aerosol jet printing. In order to fit with this process parameters, we worked on nanomaterials formulation for current collectors and electrodes. In addition, an advanced printed polymer-electrolyte is developed to be implemented directly in the printing process in order to avoid the liquid electrolyte filling step and to improve safety and flexibility. Results: Three different current collectors has been studied and printed successfully. An ink of commercial copper nanoparticles has been formulated and printed, then a flash sintering was applied to the interdigitated design. A gold ink was also printed, the resulting material was partially self-sintered and did not require any high temperature post treatment. Finally, carbon nanotubes were also printed with a high resolution and well defined patterns. Different electrode materials were formulated and printed according to the interdigitated design. For cathodes, NMC and LFP were efficaciously printed. For anodes, LTO and graphite have shown to be good candidates for the fully printed battery. The electrochemical performances of those materials have been evaluated in a standard coin cell with lithium-metal counter electrode and the results are similar with those of a traditional ink formulation and process. A jellified plastic crystal solid state electrolyte has been developed and showed comparable performances to classical liquid carbonate electrolytes with two different materials. In our future developments, focus will be put on several tasks. In a first place, we will synthesize and formulate new specific nano-materials based on metal-oxyde. Then a fully printed device will be produced and its electrochemical performance will be evaluated.

Keywords: high resolution digital printing, lithium-ion battery, nanomaterials, solid-state electrolytes

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Authors: Guenther Schuh, Michael Riesener, Jan Kantelberg

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Due to the fugacity of markets and the reduction of product lifecycles, manufacturing companies from high-wage countries are nowadays faced with the challenge to place more innovative products within even shorter development time on the market. At the same time, volatile customer requirements have to be satisfied in order to successfully differentiate from market competitors. One potential approach to address the explained challenges is provided by agile values and principles. These agile values and principles already proofed their success within software development projects in the form of management frameworks like Scrum or concrete procedure models such as Extreme Programming or Crystal Clear. Those models lead to significant improvements regarding quality, costs and development time and are therefore used within most software development projects. Motivated by the success within the software industry, manufacturing companies have tried to transfer agile mechanisms of action to the development of hardware products ever since. Though first empirical studies show similar effects in the agile development of hardware products, no comprehensive procedure model for the design of development iterations has been developed for hardware development yet due to different constraints of the domains. For this reason, this paper focusses on the design of agile product development processes by transferring mechanisms of action used in agile software development towards product development. This is conducted by decomposing the individual systems 'product development' and 'agile software development' into relevant elements and symbiotically composing the elements of both systems in respect of the design of agile product development processes afterwards. In a first step, existing product development processes are described following existing approaches of the system theory. By analyzing existing case studies from industrial companies as well as academic approaches, characteristic objectives, activities and artefacts are identified within a target-, action- and object-system. In partial model two, mechanisms of action are derived from existing procedure models of agile software development. These mechanisms of action are classified in a superior strategy level, in a system level comprising characteristic, domain-independent activities and their cause-effect relationships as well as in an activity-based element level. Within partial model three, the influence of the identified agile mechanism of action towards the characteristic system elements of product development processes is analyzed. For this reason, target-, action- and object-system of the product development are compared with the strategy-, system- and element-level of agile mechanism of action by using the graph theory. Furthermore, the necessity of existence of activities within iteration can be determined by defining activity-specific degrees of freedom. Based on this analysis, agile product development processes are designed in form of different types of iterations within a last step. By defining iteration-differentiating characteristics and their interdependencies, a logic for the configuration of activities, their form of execution as well as relevant artefacts for the specific iteration is developed. Furthermore, characteristic types of iteration for the agile product development are identified.

Keywords: activity-based process model, agile mechanisms of action, agile product development, degrees of freedom

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Authors: Nivedita T. Patil, M. T. Patil, M. S. Shashidhar, R. G. Gonnade

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Cyclitols are cycloalkane polyols which have raise attention since they have numerous biological and pharmaceutical properties. Among these, inositols are important cyclitols, which constitute a group of naturally occurring polyhydric alcohols. Myo, scyllo, allo, neo, D-chiro- are naturally occurring structural isomer of inositol while other four isomers (L-chiro, allo, epi-, and cis-inositol) are derived from myo-inositol by chemical synthesis. Myo-inositol, most abundant isomer, plays an important role in signal transduction process and for the treatment of type 2 diabetes, bacterial infections, stimulation of menstruation, ovulation in polycystic ovary syndrome, improvement of osteogenesis, and in treatment of neurological disorders. Considering the vast application of the derivatives, it becomes important to supply these compounds for further studies in quantitative amounts, but the synthesis of suitably protected chiral inositol derivatives is the key intermediates in most of the synthesis which is difficult. Chiral inositol derivatives could also be of interest to synthetic organic chemists as they could serve as potential starting materials for the synthesis of several natural products and their analogs. Thus, obtaining chiral myo-inositol derivatives in a more eco-friendly way is need for current inositol chemistry. Thus, the resolution of nonracemates by preferential crystallization of enantiomers has not been reported as a method for inositol derivatives. We are optimistic that this work might lead to the development of the two tosylate enantiomers as synthetic chiral pool molecules for organic synthesis. Resolution of racemic 4-O-benzyl 6-O-tosyl myo-inositol 1, 3, 5 orthoformate was successfully achieved on multigram scale by preferential crystallization, which is more scalable, eco-friendly method of separation than other reported methods. The separation of the conglomeric mixture of tosylate was achieved by suspending the mixture in ethyl acetate till the level of saturation is obtained. To this saturated clear solution was added seed crystal of the desired enantiomers. The filtration of the precipitated seed was carried out at its filtration window to get enantiomerically enriched tosylate, and the process was repeated alternatively. These enantiomerically enriched samples were recrystallized to get tosylate as pure enantiomers. The configuration of the resolved enantiomers was determined by converting it to previously reported dibenzyl ether myo-inositol, which is an important precursor for mono- and tetraphosphates. We have also developed a convenient and practical method for the preparation of enantiomeric 4-O and 6-O-allyl myo-inositol orthoesters by resolution of diastereomeric allyl dicamphante orthoesters on multigram scale. These allyl ethers can be converted to other chiral protected myo-inositol derivatives using routine synthetic transformations. The chiral allyl ethers can be obtained in gram quantities, and the methods are amenable to further scale-up due to the simple procedures involved. We believe that the work described enhances the pace of research to understand the intricacies of the myo-inositol cycle as the methods described provide efficient access to enantiomeric phosphoinositols, cyclitols, and their derivatives from the abundantly available myo-inositol as a starting material.

Keywords: cyclitols, diastereomers, enantiomers, myo-inositol, preferential crystallization, signal transduction

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Authors: Marta Malo, Carlota Soto, Carmen García-Rosales, Teresa Hernández

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SiC based composites are candidates for possible use as structural and functional materials in the future fusion reactors, the main role is intended for the blanket modules. In the blanket, the neutrons produced in the fusion reaction slow down and their energy is transformed into heat in order to finally generate electrical power. In the blanket design named Dual Coolant Lead Lithium (DCLL), a PbLi alloy for power conversion and tritium breeding circulates inside hollow channels called Flow Channel Inserts (FCIs). These FCI must protect the steel structures against the highly corrosive PbLi liquid and the high temperatures, but also provide electrical insulation in order to minimize magnetohydrodynamic interactions of the flowing liquid metal with the high magnetic field present in a magnetically confined fusion environment. Due to their nominally high temperature and radiation stability as well as corrosion resistance, SiC is the main choice for the flow channel inserts. The significantly lower manufacturing cost presents porous SiC (dense coating is required in order to assure protection against corrosion and as a tritium barrier) as a firm alternative to SiC/SiC composites for this purpose. This application requires the materials to be exposed to high radiation levels and extreme temperatures, conditions for which previous studies have shown noticeable changes in both the microstructure and the electrical properties of different types of silicon carbide. Both initial properties and radiation/temperature induced damage strongly depend on the crystal structure, polytype, impurities/additives that are determined by the fabrication process, so the development of a suitable material requires full control of these variables. For this work, several SiC samples with different percentage of porosity and sintering additives have been manufactured by the so-called sacrificial template method at the Ceit-IK4 Technology Center (San Sebastián, Spain), and characterized at Ciemat (Madrid, Spain). Electrical conductivity was measured as a function of temperature before and after irradiation with 1.8 MeV electrons in the Ciemat HVEC Van de Graaff accelerator up to 140 MGy (~ 2·10 -5 dpa). Radiation-induced conductivity (RIC) was also examined during irradiation at 550 ºC for different dose rates (from 0.5 to 5 kGy/s). Although no significant RIC was found in general for any of the samples, electrical conductivity increase with irradiation dose was observed to occur for some compositions with a linear tendency. However, first results indicate enhanced radiation resistance for coated samples. Preliminary thermogravimetric tests of selected samples, together with posterior XRD analysis allowed interpret radiation-induced modification of the electrical conductivity in terms of changes in the SiC crystalline structure. Further analysis is needed in order to confirm this.

Keywords: DCLL blanket, electrical conductivity, flow channel insert, porous SiC, radiation damage, thermal stability

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Authors: Alena Cejkova, Martina Paldrychova, Jana Michailidu, Olga Matatkova, Jan Masak

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Increasing the resistance of pathogenic microorganisms to many antibiotics is a serious threat to the treatment of infectious diseases and cleaning medical instruments. It should be added that the resistance of microbial populations growing in biofilms is often up to 1000 times higher compared to planktonic cells. Biofilm formation in a number of microorganisms is largely influenced by the quorum sensing regulatory mechanism. Finding external factors such as natural substances or physical processes that can interfere effectively with quorum sensing signal molecules should reduce the ability of the cell population to form biofilm and increase the effectiveness of antibiotics. The present work is devoted to the effect of chitosan as a representative of natural substances with anti-biofilm activity and non- thermal plasma (NTP) alone or in combination with polymyxin B on biofilm formation of Pseudomonas aeruginosa. Particular attention was paid to the influence of these agents on the level of quorum sensing signal molecules (acyl-homoserine lactones) during planktonic and biofilm cultivations. Opportunistic pathogenic strains of Pseudomonas aeruginosa (DBM 3081, DBM 3777, ATCC 10145, ATCC 15442) were used as model microorganisms. Cultivations of planktonic and biofilm populations in 96-well microtiter plates on horizontal shaker were used for determination of antibiotic and anti-biofilm activity of chitosan and polymyxin B. Biofilm-growing cells on titanium alloy, which is used for preparation of joint replacement, were exposed to non-thermal plasma generated by cometary corona with a metallic grid for 15 and 30 minutes. Cultivation followed in fresh LB medium with or without chitosan or polymyxin B for next 24 h. Biofilms were quantified by crystal violet assay. Metabolic activity of the cells in biofilm was measured using MTT (3-[4,5-dimethylthiazol-2-yl]-2,5 diphenyl tetrazolium bromide) colorimetric test based on the reduction of MTT into formazan by the dehydrogenase system of living cells. Activity of N-acyl homoserine lactones (AHLs) compounds involved in the regulation of biofilm formation was determined using Agrobacterium tumefaciens strain harboring a traG::lacZ/traR reporter gene responsive to AHLs. The experiments showed that both chitosan and non-thermal plasma reduce the AHLs level and thus the biofilm formation and stability. The effectiveness of both agents was somewhat strain dependent. During the eradication of P. aeruginosa DBM 3081 biofilm on titanium alloy induced by chitosan (45 mg / l) there was an 80% decrease in AHLs. Applying chitosan or NTP on the P. aeruginosa DBM 3777 biofilm did not cause a significant decrease in AHLs, however, in combination with both (chitosan 55 mg / l and NTP 30 min), resulted in a 70% decrease in AHLs. Combined application of NTP and polymyxin B allowed reduce antibiotic concentration to achieve the same level of AHLs inhibition in P. aeruginosa ATCC 15442. The results shown that non-thermal plasma and chitosan have considerable potential for the eradication of highly resistant P. aeruginosa biofilms, for example on medical instruments or joint implants.

Keywords: anti-biofilm activity, chitosan, non-thermal plasma, opportunistic pathogens

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Authors: Omolola Ojetayo, Emmanuel Garuba, Obinna Ajunwa, Abiodun A. Onilude

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Introduction: Biofilm is a functional community of microorganisms that are associated with a surface or an interface. These adherent cells become embedded within an extracellular matrix composed of polymeric substances, i.e., biofilms refer to biological deposits consisting of both microbes and their extracellular products on biotic and abiotic surfaces. Despite their detrimental effects in medicine, biofilms as natural cell immobilization have found several applications in biotechnology, such as in the treatment of wastewater, bioremediation and biodegradation, desulfurization of gas, and conversion of agro-derived materials into alcohols and organic acids. The means of enhancing immobilized cells have been chemical-inductive, and this affects the medium composition and final product. Physical factors including electrical, magnetic, and electromagnetic flux have shown potential for enhancing biofilms depending on the bacterial species, nature, and intensity of emitted signals, the duration of exposure, and substratum used. However, the concept of cell immobilisation by electrical and magnetic induction is still underexplored. Methods: To assess the effects of physical factors on biofilm formation, six American typed culture collection (Acetobacter aceti ATCC15973, Pseudomonas aeruginosa ATCC9027, Serratia marcescens ATCC14756, Gluconobacter oxydans ATCC19357, Rhodobacter sphaeroides ATCC17023, and Bacillus subtilis ATCC6633) were used. Standard culture techniques for bacterial cells were adopted. Natural autoimmobilisation potentials of test bacteria were carried out by simple biofilms ring formation on tubes, while crystal violet binding assay techniques were adopted in the characterisation of biofilm quantity. Electroinduction of bacterial cells by direct current (DC) application in cell broth, static magnetic field exposure, and electromagnetic flux were carried out, and autoimmobilisation of cells in a biofilm pattern was determined on various substrata tested, including wood, glass, steel, polyvinylchloride (PVC) and polyethylene terephthalate. Biot Savart law was used in quantifying magnetic field intensity, and statistical analyses of data obtained were carried out using the analyses of variance (ANOVA) as well as other statistical tools. Results: Biofilm formation by the selected test bacteria was enhanced by the physical factors applied. Electromagnetic induction had the greatest effect on biofilm formation, with magnetic induction producing the least effect across all substrata used. Microbial cell-cell communication could be a possible means via which physical signals affected the cells in a polarisable manner. Conclusion: The enhancement of biofilm formation by bacteria using physical factors has shown that their inherent capability as a cell immobilization method can be further optimised for industrial applications. A possible relationship between the presence of voltage-dependent channels, mechanosensitive channels, and bacterial biofilms could shed more light on this phenomenon.

Keywords: bacteria, biofilm, cell immobilization, electromagnetic induction, substrata

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Authors: Suphaporn Rattanaphinanchai

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The purpose of this study is to 1) describe and analyze the travel motivations of tourists visiting Phi Phi Islands after the Tsunami in 2004 and 2) to better understand whether there are significant differences in the tourists’ motivations in visiting Phi Phi Island after the Tsunami hit across tourists with different demographic profile. This study used Phi Phi Islands, which was damaged by the 2004 Indian Ocean tsunami as a case study. The instrument used in the present study is a self-administered questionnaire. A survey with 200 questionnaires was collected in May - December, 2015. Descriptive statistics, Independent Sample Mean T-tests, and Analysis of Variances was used to analyze the data. The result of the study showed that beauty of nature, good climate, and relaxing atmosphere motivated tourists in visiting Phi Phi Islands after the tsunami.

Keywords: motivation, Thailand, Thai tourism, Thai beaches

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Authors: J. Hajri, H. Hrizi, N. Sboui, H. Baudrand

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This paper presents a study of SIW circuits (Substrate Integrated Waveguide) with a rigorous and fast original approach based on Iterative process (WCIP). The theoretical suggested study is validated by the simulation of two different examples of SIW circuits. The obtained results are in good agreement with those of measurement and with software HFSS.

Keywords: convergence study, HFSS, modal decomposition, SIW circuits, WCIP method

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Authors: Juliana A. B. Silva, Caio H. T. L. Albuquerque, Leonardo L. dos Santos, Cristiane K. Oliveira, Ivani Malvestiti, Fernando Hallwass, Ricardo L. Longo

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Complexes with lanthanide ions have been extensively studied due to their applications as luminescent, magnetic and catalytic materials as molecular or extended crystals, thin films, glasses, polymeric matrices, ionic liquids, and in solution. NMR chemical shift data in solution have been reported and suggest fluxional structures in a wide range of coordination compounds with rare earth ions. However, the fluxional mechanisms for these compounds are still not established. This structural fluxionality may affect the photophysical, catalytic and magnetic properties in solution. Thus, understanding the structural interconversion mechanisms may aid the design of coordination compounds with, for instance, improved (electro)luminescence, catalytic and magnetic behaviors. The [Eu(btfa)₃bipy] complex, where btfa= 4,4,4-trifluoro-1-phenyl-1,3-butanedionate and bipy= 2,2’-bipiridyl, has a well-defined X-ray crystallographic structure and preliminary 1H NMR data suggested a structural fluxionality. Thus, we have investigated a series of coordination compounds with lanthanide ions [Ln(btfa)₃L], where Ln = La, Eu, Gd or Yb and L= bipy or phen (phen=1,10-phenanthroline) using a combined theoretical-experimental approach. These complexes were synthesized and fully characterized, and detailed NMR measurements were obtained. They were also studied by quantum chemical computational methods (DFT-PBE0). The aim was to determine the relevant factors in the structure of these compounds that favor or not the fluxional behavior. Measurements of the 1H NMR signals at variable temperature in CD₂Cl₂ of the [Eu(btfa)₃L] complexes suggest that these compounds have a fluxional structure, because the crystal structure has non-equivalent btfa ligands that should lead to non-equivalent hydrogen atoms and thus to more signals in the NMR spectra than those obtained at room temperature, where all hydrogen atoms of the btfa ligands are equivalent, and phen ligand has an effective vertical symmetry plane. For the [Eu(btfa)₃bipy] complex, the broadening of the signals at –70°C provides a lower bound for the coalescence temperature, which indicates the energy barriers involved in the structural interconversion mechanisms are quite small. These barriers and, consequently, the coalescence temperature are dependent upon the radii of the lanthanide ion as well as to their paramagnetic effects. The PBE0 calculated structures are in very good agreement with the crystallographic data and, for the [Eu(btfa)₃bipy] complex, this method provided several distinct structures with almost the same energy. However, the energy barrier for structural interconversion via dissociative pathways were found to be quite high and could not explain the experimental observations. Whereas the pseudo-rotation pathways, involving the btfa and bipy ligands, have very small activation barriers, in excellent agreement with the NMR data. The results also showed an increase in the activation barrier along the lanthanide series due to the decrease of the ionic radii and consequent increase of the steric effects. TD-DFT calculations showed a dependence of the ligand donor state energy with different structures of the complex [Eu(btfa)₃phen], which can affect the energy transfer rates and the luminescence. The energy required to promote the structural fluxionality may also enhance the luminescence quenching in solution. These results can aid in the design of more luminescent compounds and more efficient devices.

Keywords: computational chemistry, lanthanide-based compounds, NMR, structural fluxionality

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Authors: K. Pandey

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The present study is a functional analysis of the relationship between castes which indicates the dynamics of the caste structure in the rural setting. The researcher has tried to show both the cooperation and competition on important ceremonial and social occasions. The real India exists in the villages, so we need to know about their solidarity and also what the village life is and has been shaping into. We need to emphasize a microcosmic study of Indian rural life. Furthermore, caste integration is an acute problem country faces today. To resolve this we are required to know the dynamics of behavior of the people of different castes and for the study of the caste dynamics a study of caste relations are needed. The present study is an attempt in this direction.

Keywords: hierarchial groups, jajmani system, functional dependence, commensalities

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Authors: Saqib Mehmood, Naveed Iqbal Chaudhry, Asif Mehmood

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This study intends to investigate the information asymmetry theories of IPO and under-pricing in Pakistan. The purpose of the study is to validate the information asymmetry about firm value which leads to under-pricing. A total of 55 IPOs listed from 2000-2011 were included in this study. OLS multiple regression was applied to achieve the objectives of this study. The findings of the study confirm the significance of information asymmetry on under-pricing in Pakistan. The findings have implications for issuing firms and prospective investors.

Keywords: information asymmetry, initial public offerings, under-pricing, firm value

Procedia PDF Downloads 468