Search results for: Scanning Electron Microscopy (SEM)
775 Collision Induced Dissociation of Transition Metal Fluoride Complexes and the Multiply Charged Anions
Authors: Ruqia Nazir, Robin Perutz
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Collision-induced dissociation (CID) can be used to study the intrinsic properties of ions in the gas phase.1 Decay pathways of transition metal difluoride complexes of titanium, zirconium, hafnium, and ruthenium were studied by CID in an ESI-Ion trap mass spectrometer. Furthermore, the decay pathways of multiply charged anions (MCAs) of titanium and zirconium were also studied. The CID results are illustrated by the behaviour of (Cp*)₂TiF₂, which initially forms the ions [M-F-]⁺, [M+Na]⁺, and [M+K]⁺. The [(Cp*₂)TiF⁺ ion decays on resonant excitation to lose HF forming [Cp*(C₅Me₄CH₂)Ti]⁺ (Figure). The other major ion, [(Cp*)₂TiF₂+Na]⁺, decays on resonant excitation with production of [(Cp*)₂TiF₂]⁺ and [C₅Me₄CH₂]⁺. We also report the behaviour of Cp₂MF₂ (M = Zr, Hf) and Ru(PMe₃)₄F₂. The decay pathway of the multiply charged anions (MCAs), notably TiF₆²⁻ and ZrF₆²⁻ was concluded to be ionic fragmentation with loss of F⁻ rather than electron detachment.Keywords: collision induced dissociation, transition metal difluoride comolexes, multiply charged anions, mass spectrometry
Procedia PDF Downloads 107774 Improved Morphology in Sequential Deposition of the Inverted Type Planar Heterojunction Solar Cells Using Cheap Additive (DI-H₂O)
Authors: Asmat Nawaz, Ceylan Zafer, Ali K. Erdinc, Kaiying Wang, M. Nadeem Akram
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Hybrid halide Perovskites with the general formula ABX₃, where X = Cl, Br or I, are considered as an ideal candidates for the preparation of photovoltaic devices. The most commonly and successfully used hybrid halide perovskite for photovoltaic applications is CH₃NH₃PbI₃ and its analogue prepared from lead chloride, commonly symbolized as CH₃NH₃PbI₃_ₓClₓ. Some researcher groups are using lead free (Sn replaces Pb) and mixed halide perovskites for the fabrication of the devices. Both mesoporous and planar structures have been developed. By Comparing mesoporous structure in which the perovskite materials infiltrate into mesoporous metal oxide scaffold, the planar architecture is much simpler and easy for device fabrication. In a typical perovskite solar cell, a perovskite absorber layer is sandwiched between the hole and electron transport. Upon the irradiation, carriers are created in the absorber layer that can travel through hole and electron transport layers and the interface in between. We fabricated inverted planar heterojunction structure ITO/PEDOT/ Perovskite/PCBM/Al, based solar cell via two-step spin coating method. This is also called Sequential deposition method. A small amount of cheap additive H₂O was added into PbI₂/DMF to make a homogeneous solution. We prepared four different solution such as (W/O H₂O, 1% H₂O, 2% H₂O, 3% H₂O). After preparing, the whole night stirring at 60℃ is essential for the homogenous precursor solutions. We observed that the solution with 1% H₂O was much more homogenous at room temperature as compared to others. The solution with 3% H₂O was precipitated at once at room temperature. The four different films of PbI₂ were formed on PEDOT substrates by spin coating and after that immediately (before drying the PbI₂) the substrates were immersed in the methyl ammonium iodide solution (prepared in isopropanol) for the completion of the desired perovskite film. After getting desired films, rinse the substrates with isopropanol to remove the excess amount of methyl ammonium iodide and finally dried it on hot plate only for 1-2 minutes. In this study, we added H₂O in the PbI₂/DMF precursor solution. The concept of additive is widely used in the bulk- heterojunction solar cells to manipulate the surface morphology, leading to the enhancement of the photovoltaic performance. There are two most important parameters for the selection of additives. (a) Higher boiling point w.r.t host material (b) good interaction with the precursor materials. We observed that the morphology of the films was improved and we achieved a denser, uniform with less cavities and almost full surface coverage films but only using precursor solution having 1% H₂O. Therefore, we fabricated the complete perovskite solar cell by sequential deposition technique with precursor solution having 1% H₂O. We concluded that with the addition of additives in the precursor solutions one can easily be manipulate the morphology of the perovskite film. In the sequential deposition method, thickness of perovskite film is in µm and the charge diffusion length of PbI₂ is in nm. Therefore, by controlling the thickness using other deposition methods for the fabrication of solar cells, we can achieve the better efficiency.Keywords: methylammonium lead iodide, perovskite solar cell, precursor composition, sequential deposition
Procedia PDF Downloads 246773 Characterization of Nanoemulsion Incorporating Crude Cocoa Polyphenol
Authors: Suzannah Sharif, Aznie Aida Ahmad, Maznah Ismail
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Cocoa bean is the raw material for products such as cocoa powder and chocolate. Cocoa bean contains polyphenol which has been shown in several clinical studies to confer beneficial health effects. However studies showed that cocoa polyphenol absorption in the human intestinal tracts are very low. Therefore nanoemulsion may be one way to increase the bioavailability of cocoa polyphenol. This study aim to characterize nanoemulsion incorporating crude cocoa polyphenol produced using high energy technique. Cocoa polyphenol was extracted from fresh freeze-dried cocoa beans from Malaysia. The particle distribution, particle size, and zeta potential were determined. The emulsion was also analysed using transmission electron microscope to visualize the particles. Solubilization study was conducted by titrating the nanoemulsion into distilled water or 1% surfactant solution. Result showed that the nanoemulsion contains particle which have narrow size distribution. The particles size average at 112nm with zeta potential of -45mV. The nanoemulsions behave differently in distilled water and surfactant solution.Keywords: cocoa, nanoemulsion, cocoa polyphenol, solubilisation study
Procedia PDF Downloads 466772 Physicochemical Attributes of Pectin Hydrogel and Its Wound Healing Activity
Authors: Nor Khaizan Anuar, Nur Karimah Aziz, Tin Wui Wong, Ahmad Sazali Hamzah, Wan Rozita Wan Engah
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The physicochemical attributes and wound healing activity of pectin hydrogel in rat models, following partial thickness thermal injury were investigated. The pectin hydrogel was prepared by solvent evaporation method with the aid of glutaraldehyde as crosslinking agent and glycerol as plasticizer. The physicochemical properties were mainly evaluated using differential scanning calorimetry (DSC) and Fourier transform infrared (FTIR) spectroscopy, while the wound healing activity was examined by the macroscopic images, wound size reduction and histological evaluation using haematoxylin and eosin (H&E) stain for 14 days. The DSC and FTIR analysis suggested that pectin hydrogel exhibited higher extent of polymer-polymer interaction at O-H functional group in comparison to the unprocessed pectin. This was indicated by the increase of endothermic enthalpy values from 139.35 ± 13.06 J/g of unprocessed pectin to 156.23 ± 2.86 J/g of pectin hydrogel, as well as the decrease of FTIR wavenumber corresponding to O-H at 3432.07 ± 0.49 cm-1 of unprocessed pectin to 3412.62 ± 13.06 cm-1 of pectin hydrogel. Rats treated with pectin hydrogel had significantly smaller wound size (Student’s t-test, p<0.05) when compared to the untreated group starting from day 7 until day 14. H&E staining indicated that wounds received pectin hydrogel had more fibroblasts, blood vessels and collagen bundles on day 14 in comparison to the untreated rats.Keywords: pectin, physicochemical, rats, wound
Procedia PDF Downloads 360771 Air-Coupled Ultrasonic Testing for Non-Destructive Evaluation of Various Aerospace Composite Materials by Laser Vibrometry
Authors: J. Vyas, R. Kazys, J. Sestoke
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Air-coupled ultrasonic is the contactless ultrasonic measurement approach which has become widespread for material characterization in Aerospace industry. It is always essential for the requirement of lightest weight, without compromising the durability. To archive the requirements, composite materials are widely used. This paper yields analysis of the air-coupled ultrasonics for composite materials such as CFRP (Carbon Fibre Reinforced Polymer) and GLARE (Glass Fiber Metal Laminate) and honeycombs for the design of modern aircrafts. Laser vibrometry could be the key source of characterization for the aerospace components. The air-coupled ultrasonics fundamentals, including principles, working modes and transducer arrangements used for this purpose is also recounted in brief. The emphasis of this paper is to approach the developed NDT techniques based on the ultrasonic guided waves applications and the possibilities of use of laser vibrometry in different materials with non-contact measurement of guided waves. 3D assessment technique which employs the single point laser head using, automatic scanning relocation of the material to assess the mechanical displacement including pros and cons of the composite materials for aerospace applications with defects and delaminations.Keywords: air-coupled ultrasonics, contactless measurement, laser interferometry, NDT, ultrasonic guided waves
Procedia PDF Downloads 239770 First Principle Calculations of the Structural and Optoelectronic Properties of Cubic Perovskite CsSrF3
Authors: Meriem Harmel, Houari Khachai
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We have investigated the structural, electronic and optical properties of a compound perovskite CsSrF3 using the full-potential linearized augmented plane wave (FP-LAPW) method within density functional theory (DFT). In this approach, both the local density approximation (LDA) and the generalized gradient approximation (GGA) were used for exchange-correlation potential calculation. The ground state properties such as lattice parameter, bulk modulus and its pressure derivative were calculated and the results are compared whit experimental and theoretical data. Electronic and bonding properties are discussed from the calculations of band structure, density of states and electron charge density, where the fundamental energy gap is direct under ambient conditions. The contribution of the different bands was analyzed from the total and partial density of states curves. The optical properties (namely: the real and the imaginary parts of the dielectric function ε(ω), the refractive index n(ω) and the extinction coefficient k(ω)) were calculated for radiation up to 35.0 eV. This is the first quantitative theoretical prediction of the optical properties for the investigated compound and still awaits experimental confirmations.Keywords: DFT, fluoroperovskite, electronic structure, optical properties
Procedia PDF Downloads 477769 Wetting Properties of Silver Based Alloys
Authors: Zoltán Weltsch, József Hlinka, Eszter Kókai
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The temperature dependence of wettability (wetting angle, Θ (T)) for Ag-based melts on graphite and Al2O3 substrates is compared. Typical alloying effects are found, as the Ag host metal is gradually replaced by various metallic elements. The essence of alloying lies in the change of the electron/atom (e/a) ratio. This ratio is also manifested in the shift of wetting angles on the same substrate. Nevertheless, the effects are partially smeared by other (metallurgical) factors, like the interaction between the oxygen-alloying elements and by the graphite substrate-oxygen interaction. In contrast, such effects are not pronounced in the case of Al2O3 substrates. As a consequence, Θ(T) exhibits an opposite trend in the case of two substrates. Crossovers of the Θ(T) curves were often found. The positions of crossovers depend on the chemical character and concentration of solute atoms. Segregation and epitaxial texture formation after solidification were also observed in certain alloy drops, especially in high concentration range. This phenomenon is not yet explained in every detail.Keywords: contact angle, graphite, silver, soldering, solid solubility, substrate, temperature dependence, wetting
Procedia PDF Downloads 413768 The Optical Properties of CdS and Conjugated Cadmium Sulphide-Cowpea Chlorotic Mottle Virus
Authors: Afiqah Shafify Amran, Siti Aisyah Shamsudin, Nurul Yuziana Mohd Yusof
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Cadmium Sulphide (CdS) from group II-IV quantum dots with good optical properties was successfully synthesized by using the simple colloidal method. Capping them with ligand Polyethylinamine (PEI) alters the surface defect of CdS while, thioglycolic acid (TGA) was added to the reaction as a stabilizer. Due to their cytotoxicity, we decided to conjugate them with the protein cage nanoparticles. In this research, we used capsid of Cowpea Chlorotic Mottle Virus (CCMV) to package the CdS because they have the potential to serve in drug delivery, cell targeting and imaging. Adding Sodium Hydroxide (NaOH) changes the pH of the systems hence the isoelectric charge is adjusted. We have characterized and studied the morphology and the optical properties of CdS and CdS-CCMV by transmitted electron microscopic (TEM), UV-Vis spectroscopy, photoluminescence spectroscopy, UV lamp and Fourier transform infrared spectroscopy (FTIR), respectively. The results obtained suggest that the protein cage nanoparticles do not affect the optical properties of CdS.Keywords: cadmium sulphide, cowpea chlorotic mottle virus, protein cage nanoparticles, quantum dots
Procedia PDF Downloads 338767 Elaboration and Characterization of PVDF/TiO2 Nanocomposites
Authors: F. Z. Benabid, S. Kridi, F. Zouai, D. Benachour
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The aim of present work is to characterize the PVDF/TiO2 blends as nanocomposites, and study the effect of TiO2 on properties of different compositions and the evaluation of the effectiveness of the method used for filler treatment. Nanocomposite samples were synthesized by molten route in an internal mixer. The TiO2 nanoparticles were treated with stearic acid in order to obtain a good dispersion, and the demonstration of the effectiveness of the treatment on the morphology and roughness of the nanofiller was established by microstructural analysis by FTIR and AFM. The various developed nanocomposite compositions were characterized by different methods; i.e. FTIR, XRD, SEM and optical microscopy. Rheological, dielectric and mechanical studies were also performed. The results showed a remarkable increase in the crystallinity of the PVDF/neat TiO2 nanocomposite containing 1 wt% loading of filler, due to the nucleation effect of TiO2 nanoparticles. A good dispersion was obtained in PVDF/treated TiO2 nanocomposites. The rheological study showed an increase in the fluidity in all developed nanocomposite compositions, involved by the orientation of TiO2 nanoparticles in the flow direction. The dielectric study revealed an increase in electrical conductivity in PVDF/neat TiO2 nanocomposites. However, in PVDF/ treated TiO2 nanocomposites, the electrical conductivity was decreased by the addition of 0.5 and 2 wt% loading of filler.Keywords: nanocomposites, PVDF, TiO2, comixing, mechanical treatment
Procedia PDF Downloads 318766 Design, Synthesis and In-Vitro Antibacterial and Antifungal Activities of Some Novel Spiro[Azetidine-2, 3’-Indole]-2, 4(1’H)-Dione
Authors: Ravi J. Shah
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The present study deals with the synthesis of novel spiro[azetidine-2, 3’-indole]-2’, 4(1’H)-dione derivative from the reactions of 3-(phenylimino)-1,3-dihydro-2H-indol-2-one derivatives with chloracetyl chloride in presence of triethyl amine (TEA). All the compounds were characterized using IR, 1H NMR, MS and elemental analysis. They were screened for their antibacterial and antifungal activities. Results revealed that, compounds (7a), (7b), (7c), (7d) and (7e) showed very good activity with MIC value of 6.25-12.5 μg/ml against three evaluated bacterial strains and the remaining compounds showed good to moderate activity comparable to standard drugs as antibacterial agents. Compounds (7c) and (7h) displayed equipotent antifungal activity in comparison to standard drugs. Structure-activity relationship study of the compounds showed that the presence of electron withdrawing group substitution at 5’ and 7’ positions of indoline ring and on ortho or para position of phenyl ring increases both antibacterial and antifungal activity of the compound. Henceforth, our findings will have a good impact on chemists and biochemists for further investigations in search of bromine containing spiro fused antimicrobial agents.Keywords: antibacterial activity, antifungal activity, 2-Azetidinone, indoline
Procedia PDF Downloads 491765 Study of the Microstructure and Mechanical Properties of Locally Developed Carbon Fibers-Silica Sand Nanoparticles Aluminium Based Hybrid Composites
Authors: Tahir Ahmad, M. Kamran, R. Ahmad, M. T. Z. Butt
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Hybrid aluminum metal matrix composites with 1, 2, 3 and 4 wt. % of silica sand nanoparticles and electro-less nickel coated carbon fibers were successfully developed using sand casting technique. Epoxy coating of carbon fibers was removed and phosphorous-nickel coating was successfully applied via electro-less route. The developed hybrid composites were characterized using micro hardness tester, tensile testing, and optical microscopy. The gradual increase of reinforcing phases yielded improved mechanical properties such as hardness and tensile strength. The increase in hardness was attributed to the presence of silica sand nanoparticles whereas electro-less nickel coated carbon fibers enhanced the tensile properties of developed hybrid composites. The microstructure of the developed hybrid composites revealed the homogeneous distribution of both carbon fibers and silica sand nanoparticles in aluminum based hybrid composites. The formation of dendrite microstructure is the main cause of improving mechanical properties.Keywords: aluminum based hybrid composites, mechanical properties, microstructure, microstructure and mechanical properties relationship
Procedia PDF Downloads 411764 Synthesis and Characterization of Partially Oxidized Graphite Oxide for Solar Energy Storage Applications
Authors: Ghada Ben Hamad, Zohir Younsi, Fabien Salaun, Hassane Naji, Noureddine Lebaz
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The graphene oxide (GO) material has attracted much attention for solar energy applications. This paper reports the synthesis and characterization of partially oxidized graphite oxide (GTO). GTO was obtained by modified Hummers method, which is based on the chemical oxidation of natural graphite. Several samples were prepared with different oxidation degree by an adjustment of the oxidizing agent’s amount. The effect of the oxidation degree on the chemical structure and on the morphology of GTO was determined by using Fourier transform infrared (FT-IR) spectroscopy, Energy Dispersive X-ray Spectroscopy (EDS), and scanning electronic microscope (SEM). The thermal stability of GTO was evaluated by using thermogravimetric analyzer (TGA) in Nitrogen atmosphere. The results indicate high degree oxidation of graphite oxide for each sample, proving that the process is efficient. The GTO synthesized by modified Hummers method shows promising characteristics. Graphene oxide (GO) obtained by exfoliation of GTO are recognized as a good candidate for thermal energy storage, and it will be used as solid shell material in the encapsulation of phase change materials (PCM).Keywords: modified hummers method, graphite oxide, oxidation degree, solar energy storage
Procedia PDF Downloads 118763 Development of Strategic Cooperation in Managing Thailand-Myanmar Borders: Roles of Education in Enhancing Sustainability
Authors: Rungrot Trongsakul
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This paper was aimed to study the strategic cooperation development of Thailand in accordance with the door open policy of Myanmar, by use of DIMES Model: Diplomacy, Information, Military and Economics, Socio-Culture. This research employed qualitative method, aiming to study, analyze and synthesize the content of laws, policies, relevant research papers and documents, and relevant theories, and to study external environment and national power based on DIMES Model. The five steps of strategic development utilized in this study included (1) conceptual framework and definition; (2) environmental scanning; (3) assessing; (4) determining; and (5) drafting strategic plan. The suggested strategies were based on the concept of 'Soft Power'. Therefore, the determination of measures, action plans or projects as strategic means of public and private organizations should be based on sincere participation among people and communities living on the borders shared by both countries. Adoption of education, learning and sharing process is a key to building sustainability of the countries’ strategic cooperation, while an application of 'Soft Power' in all dimensions of the cooperation between the two countries was suggested.Keywords: education, strategic cooperation, Thailand-Myanmar borders, sustainability
Procedia PDF Downloads 352762 Orthodontic Treatment Using CAD/CAM System
Authors: Cristiane C. B. Alves, Livia Eisler, Gustavo Mota, Kurt Faltin Jr., Cristina L. F. Ortolani
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The correct positioning of the brackets is essential for the success of orthodontic treatment. Indirect bracket placing technique has the main objective of eliminating the positioning errors, which commonly occur in the technique of direct system of brackets. The objective of this study is to demonstrate that the exact positioning of the brackets is of extreme relevance for the success of the treatment. The present work shows a case report of an adult female patient who attended the clinic with the complaint of being in orthodontic treatment for more than 5 years without noticing any progress. As a result of the intra-oral clinical examination and documentation analysis, a class III malocclusion, an anterior open bite, and absence of all third molars and first upper and lower bilateral premolars were observed. For the treatment, the indirect bonding technique with self-ligating ceramic braces was applied. The preparation of the trays was done after the intraoral digital scanning and printing of models with a 3D printer. Brackets were positioned virtually, using a specialized software. After twelve months of treatment, correction of the malocclusion was observed, as well as the closing of the anterior open bite. It is concluded that the adequate and precise positioning of brackets is necessary for a successful treatment.Keywords: anterior open-bite, CAD/CAM, orthodontics, malocclusion, angle class III
Procedia PDF Downloads 194761 Phase Transition in Iron Storage Protein Ferritin
Authors: Navneet Kaur, S. D. Tiwari
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Ferritin is a protein which present in the blood of mammals. It maintains the need of iron inside the body. It has an antiferromagnetic iron core, 7-8 nm in size, which is encapsulated inside a protein cage. The thickness of this protein shell is about 2-3 nm. This protein shell reduces the interaction among particles and make ferritin a model superparamagnet. The major composition of ferritin core is mineral ferrihydrite. The molecular formula of ferritin core is (FeOOH)8[FeOOPO3H2]. In this study, we discuss the phase transition of ferritin. We characterized ferritin using x-ray diffractometer, transmission electron micrograph, thermogravimetric analyzer and vibrating sample magnetometer. It is found that ferritin core is amorphous in nature with average particle size of 8 nm. The thermogravimetric and differential thermogravimetric analysis curves shows mass loss at different temperatures. We heated ferritin at these temperatures. It is found that ferritin core starts decomposing after 390^o C. At 1020^o C, the ferritin core is finally converted to alpha phase of iron oxide. Magnetization behavior of final sample clearly shows the iron oxyhydroxide core is completely converted to alpha iron oxide.Keywords: Antiferromagnetic, Ferritin, Phase, Superparamagnetic
Procedia PDF Downloads 119760 Increased Retention of Nanoparticle by Small Molecule Inhibitor in Cancer Cells
Authors: Neha Singh
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Background: Nowadays, the nanoparticle is gaining unexceptional attention in targeted drug delivery. But before proceeding to this episode of accomplishment, the journey and closure of these nanoparticles inside the cells should be disentangle. Being foreign for the cells, nanoparticles will easily getcleared off without any effective outcome. As the cancer cells withhold these nanoparticles for a longer period of time, more will be the drug’s effect. Chlorpromazine is a cationic amphiphilic drug which is believed to inhibit clathrin-coated pit formation by a reversible translocation of clathrin and its adapter proteins from the plasma membrane to intracellular vesicles. Chlorpromazine has a role in increasing the retention of nanoparticles in cancer cells. The mechanism of action how this small molecule increases the retention of nanoparticles is still uncovered. Method: Polymeric nanoparticle (PLGA) with Cyanine3.5 dye were synthesized by solvent evaporation method and characterized for size and zeta potential. FTIR was also done. Pulse and chase studies with and without inhibitor were done to check the retention of nanoparticle using fluorescence microscopy. Mean fluorescence intensity was measured by ImageJ software. Results: Increased retention of nanoparticle with inhibitor was observed in both pulse and chase studies. Conclusion: Our results demonstrate that by repurposing these small molecule inhibitor, we can increase the retention of nanoparticle at the targeted site.Keywords: nanoparticle, endocytosis, clathrin inhibitor, cancer cell
Procedia PDF Downloads 105759 A 1.8 GHz to 43 GHz Low Noise Amplifier with 4 dB Noise Figure in 0.1 µm Galium Arsenide Technology
Authors: Mantas Sakalas, Paulius Sakalas
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This paper presents an analysis and design of a ultrawideband 1.8GHz to 43GHz Low Noise Amplifier (LNA) in 0.1 μm Galium Arsenide (GaAs) pseudomorphic High Electron Mobility Transistor (pHEMT) technology. The feedback based bandwidth extension techniques is analyzed and based on the outcome, a two stage LNA is designed. The impedance fine tuning is implemented by using Transmission Line (TL) structures. The measured performance shows a good agreement with simulation results and an outstanding wideband noise matching. The measured small signal gain was 12 dB, whereas a 3 dB gain flatness in range from 1.8 - 43 GHz was reached. The noise figure was below 4 dB almost all over the entire frequency band of 1.8GHz to 43GHz, the output power at 1 dB compression point was 6 dBm and the DC power consumption was 95 mW. To the best knowledge of the authors the designed LNA outperforms the State of the Art (SotA) reported LNA designs in terms of combined parameters of noise figure within the addressed ultra-wide 3 dB bandwidth, linearity and DC power consumption.Keywords: feedback amplifiers, GaAs pHEMT, monolithic microwave integrated circuit, LNA, noise matching
Procedia PDF Downloads 216758 Development of One-Pot Sequential Cyclizations and Photocatalyzed Decarboxylative Radical Cyclization: Application Towards Aspidospermatan Alkaloids
Authors: Guillaume Bélanger, Jean-Philippe Fontaine, Clémence Hauduc
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There is an undeniable thirst from organic chemists and from the pharmaceutical industry to access complex alkaloids with short syntheses. While medicinal chemists are interested in the fascinating wide range of biological properties of alkaloids, synthetic chemists are rather interested in finding new routes to access these challenging natural products of often low availability from nature. To synthesize complex polycyclic cores of natural products, reaction cascades or sequences performed one-pot offer a neat advantage over classical methods for their rapid increase in molecular complexity in a single operation. In counterpart, reaction cascades need to be run on substrates bearing all the required functional groups necessary for the key cyclizations. Chemoselectivity is thus a major issue associated with such a strategy, in addition to diastereocontrol and regiocontrol for the overall transformation. In the pursuit of synthetic efficiency, our research group developed an innovative one-pot transformation of linear substrates into bi- and tricyclic adducts applied to the construction of Aspidospermatan-type alkaloids. The latter is a rich class of indole alkaloids bearing a unique bridged azatricyclic core. Despite many efforts toward the synthesis of members of this family, efficient and versatile synthetic routes are still coveted. Indeed, very short, non-racemic approaches are rather scarce: for example, in the cases of aspidospermidine and aspidospermine, syntheses are all fifteen steps and over. We envisaged a unified approach to access several members of the Aspidospermatan alkaloids family. The key sequence features a highly chemoselective formamide activation that triggers a Vilsmeier-Haack cyclization, followed by an azomethine ylide generation and intramolecular cycloaddition. Despite the high density and variety of functional groups on the substrates (electron-rich and electron-poor alkenes, nitrile, amide, ester, enol ether), the sequence generated three new carbon-carbon bonds and three rings in a single operation with good yield and high chemoselectivity. A detailed study of amide, nucleophile, and dipolarophile variations to finally get to the successful combination required for the key transformation will be presented. To complete the indoline fragment of the natural products, we developed an original approach. Indeed, all reported routes to Aspidospermatan alkaloids introduce the indoline or indole early in the synthesis. In our work, the indoline needs to be installed on the azatricyclic core after the key cyclization sequence. As a result, typical Fischer indolization is not suited since this reaction is known to fail on such substrates. We thus envisaged a unique photocatalyzed decarboxylative radical cyclization. The development of this reaction as well as the scope and limitations of the methodology, will also be presented. The original Vilsmeier-Haack and azomethine ylide cyclization sequence as well as the new photocatalyzed decarboxylative radical cyclization will undoubtedly open access to new routes toward polycyclic indole alkaloids and derivatives of pharmaceutical interest in general.Keywords: Aspidospermatan alkaloids, azomethine ylide cycloaddition, decarboxylative radical cyclization, indole and indoline synthesis, one-pot sequential cyclizations, photocatalysis, Vilsmeier-Haack Cyclization
Procedia PDF Downloads 81757 Effect of Different Parameters in the Preparation of Antidiabetic Microparticules by Coacervation
Authors: Nawel Ouennoughi, Kamel Daoud
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During recent years, new pharmaceutical dosage forms were developed in the research laboratories and which consists of encapsulating one or more active molecules in a polymeric envelope. Several techniques of encapsulation allow obtaining the microparticles or the nanoparticles containing one or several polymers. In the industry, microencapsulation is implemented to fill the following objectives: to ensure protection, the compatibility and the stabilization of an active matter in a formulation, to carry out an adapted working, to improve the presentation of a product, to mask a taste or an odor, to modify and control the profile of release of an active matter to obtain, for example, prolonged or started effect. To this end, we focus ourselves on the encapsulation of the antidiabetic. It is an oral hypoglycemic agent belonging to the second generation of sulfonylurea’s commonly employed in the treatment of type II non-insulin-dependent diabetes in order to improve profile them dissolution. Our choice was made on the technique of encapsulation by complex coacervation with two types of polymers (gelatin and the gum Arabic) which is a physicochemical process. Several parameters were studied at the time of the formulation of the microparticles and the nanoparticles: temperature, pH, ratio of polymers etc. The microparticles and the nanoparticles obtained were characterized by microscopy, laser granulometry, FTIR and UV-visible spectrophotometry. The profile of dissolution obtained for the microparticles showed an improvement of the kinetics of dissolution compared to that obtained for the active ingredient.Keywords: coacervation, gum Arabic, microencapsulation, gelatin
Procedia PDF Downloads 269756 Solid Dispersions of Cefixime Using β-Cyclodextrin: Characterization and in vitro Evaluation
Authors: Nagasamy Venkatesh Dhandapani, Amged Awad El-Gied
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Cefixime, a BCS class II drug, is insoluble in water but freely soluble in acetone and in alcohol. The aqueous solubility of cefixime in water is poor and exhibits exceptionally slow and intrinsic dissolution rate. In the present study, cefixime and β-Cyclodextrin (β-CD) solid dispersions were prepared with a view to study the effect and influence of β-CD on the solubility and dissolution rate of this poorly aqueous soluble drug. Phase solubility profile revealed that the solubility of cefixime was increased in the presence of β-CD and was classified as AL-type. Effect of variable, such as drug:carrier ratio, was studied. Physical characterization of the solid dispersion was characterized by Fourier transform infrared spectroscopy (FT-IR) and Differential scanning calorimetry (DSC). These studies revealed that a distinct loss of drug crystallinity in the solid molecular dispersions is ostensibly accounting for enhancement of dissolution rate in distilled water. The drug release from the prepared solid dispersion exhibited a first order kinetics. Solid dispersions of cefixime showed a 6.77 times fold increase in dissolution rate over the pure drug.Keywords: β-cyclodextrin, cefixime, dissolution, Kneading method, solid dispersions, release kinetics
Procedia PDF Downloads 316755 Development of pH Responsive Nanoparticles for Colon Targeted Drug Delivery System
Authors: V. Balamuralidhara
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The aim of the present work was to develop Paclitaxel loaded polyacrylamide grafted guar gum nanoparticles as pH responsive nanoparticle systems for targeting colon. The pH sensitive nanoparticles were prepared by modified ionotropic gelation technique. The prepared nanoparticles showed mean diameters in the range of 264±0.676 nm to 726±0.671nm, and a negative net charge 10.8 mV to 35.4mV. Fourier Transformed Infrared Spectroscopy (FT-IR) and Differential Scanning Calorimetry (DSC) studies suggested that there was no chemical interaction between drug and polymers. The encapsulation efficiency of the drug was found to be 40.92% to 48.14%. The suitability of the polyacrylamide grafted guar gum ERN’s for the release of Paclitaxel was studied by in vitro release at pH 1.2 and 7.4. It was observed that, there was no significant amount of drug release at gastric pH and 97.63% of drug release at pH 7.4 was obtained for optimized formulation F3 at the end of 12 hrs. In vivo drug targeting performance for the prepared optimized formulation (F3) and pure drug Paclitaxel was evaluated by HPLC. It was observed that the polyacrylamide grafted guar gum can be used to prepare nanoparticles for targeting the drug to the colon. The release performance was greatly affected by the materials used in ERN’s preparation, which allows maximum release at colon’s pH. It may be concluded that polyacrylamide grafted guar gum nanoparticles loaded with paclitaxel have desirable release responsive to specific pH. Hence it is a unique approach for colonic delivery of drug having appropriate site specificity and feasibility and controlled release of drug.Keywords: colon targeting, polyacrylamide grafted guar gum nanoparticles, paclitaxel, nanoparticles
Procedia PDF Downloads 354754 Left to Right-Right Most Parsing Algorithm with Lookahead
Authors: Jamil Ahmed
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Left to Right-Right Most (LR) parsing algorithm is a widely used algorithm of syntax analysis. It is contingent on a parsing table, whereas the parsing tables are extracted from the grammar. The parsing table specifies the actions to be taken during parsing. It requires that the parsing table should have no action conflicts for the same input symbol. This requirement imposes a condition on the class of grammars over which the LR algorithms work. However, there are grammars for which the parsing tables hold action conflicts. In such cases, the algorithm needs a capability of scanning (looking-ahead) next input symbols ahead of the current input symbol. In this paper, a ‘Left to Right’-‘Right Most’ parsing algorithm with lookahead capability is introduced. The 'look-ahead' capability in the LR parsing algorithm is the major contribution of this paper. The practicality of the proposed algorithm is substantiated by the parser implementation of the Context Free Grammar (CFG) of an already proposed programming language 'State Controlled Object Oriented Programming' (SCOOP). SCOOP’s Context Free Grammar has 125 productions and 192 item sets. This algorithm parses SCOOP while the grammar requires to ‘look ahead’ the input symbols due to action conflicts in its parsing table. Proposed LR parsing algorithm with lookahead capability can be viewed as an optimization of ‘Simple Left to Right’-‘Right Most’ (SLR) parsing algorithm.Keywords: left to right-right most parsing, syntax analysis, bottom-up parsing algorithm
Procedia PDF Downloads 126753 Tin and Tin-Copper Composite Nanorod Anodes for Rechargeable Lithium Applications
Authors: B. D. Polat, Ö. Keleş
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Physical vapor deposition under conditions of an obliquely incident flux results in a film formation with an inclined columnar structure. These columns will be oriented toward the vapor source because of the self-shadowing effect, and they are homogenously distributed on the substrate surface because of the limited surface diffusion ability of ad-atoms when there is no additional substrate heating. In this work, the oblique angle electron beam evaporation technique is used to fabricate thin films containing inclined nanorods. The results demonstrate that depending on the thin film composition, the morphology of the nanorods changed as well. The galvanostatic analysis of these thin film anodes reveals that a composite CuSn nanorods having approximately 900mAhg-1 of initial discharge capacity, performs higher electrochemical performance compared to pure Sn nanorods containing anode material. The long cycle life and the advanced electrochemical properties of the nano-structured composite electrode might be attributed to its improved mechanical tolerance and enhanced electrical conductivity depending on the Cu presence in the nanorods.Keywords: Cu-Sn thin film, oblique angle deposition, lithium ion batteries, anode
Procedia PDF Downloads 347752 Cell-free Bioconversion of n-Octane to n-Octanol via a Heterogeneous and Bio-Catalytic Approach
Authors: Shanna Swart, Caryn Fenner, Athanasios Kotsiopoulos, Susan Harrison
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Linear alkanes are produced as by-products from the increasing use of gas-to-liquid fuel technologies for synthetic fuel production and offer great potential for value addition. Their current use as low-value fuels and solvents do not maximize this potential. Therefore, attention has been drawn towards direct activation of these aliphatic alkanes to more useful products such as alcohols, aldehydes, carboxylic acids and derivatives. Cytochrome P450 monooxygenases (P450s) can be used for activation of these aliphatic alkanes using whole-cells or cell-free systems. Some limitations of whole-cell systems include reduced mass transfer, stability and possible side reactions. Since the P450 systems are little studied as cell-free systems, they form the focus of this study. Challenges of a cell-free system include co-factor regeneration, substrate availability and enzyme stability. Enzyme immobilization offers a positive outlook on this dilemma, as it may enhance stability of the enzyme. In the present study, 2 different P450s (CYP153A6 and CYP102A1) as well as the relevant accessory enzymes required for electron transfer (ferredoxin and ferredoxin reductase) and co-factor regeneration (glucose dehydrogenase) have been expressed in E. coli and purified by metal affinity chromatography. Glucose dehydrogenase (GDH), was used as a model enzyme to assess the potential of various enzyme immobilization strategies including; surface attachment on MagReSyn® microspheres with various functionalities and on electrospun nanofibers, using self-assembly based methods forming Cross Linked Enzymes (CLE), Cross Linked Enzyme Aggregates (CLEAs) and spherezymes as well as in a sol gel. The nanofibers were synthesized by electrospinning, which required the building of an electrospinning machine. The nanofiber morphology has been analyzed by SEM and binding will be further verified by FT-IR. Covalent attachment based methods showed limitations where only ferredoxin reductase and GDH retained activity after immobilization which were largely attributed to insufficient electron transfer and inactivation caused by the crosslinkers (60% and 90% relative activity loss for the free enzyme when using 0.5% glutaraldehyde and glutaraldehyde/ethylenediamine (1:1 v/v), respectively). So far, initial experiments with GDH have shown the most potential when immobilized via their His-tag onto the surface of MagReSyn® microspheres functionalized with Ni-NTA. It was found that Crude GDH could be simultaneously purified and immobilized with sufficient activity retention. Immobilized pure and crude GDH could be recycled 9 and 10 times, respectively, with approximately 10% activity remaining. The immobilized GDH was also more stable than the free enzyme after storage for 14 days at 4˚C. This immobilization strategy will also be applied to the P450s and optimized with regards to enzyme loading and immobilization time, as well as characterized and compared with the free enzymes. It is anticipated that the proposed immobilization set-up will offer enhanced enzyme stability (as well as reusability and easy recovery), minimal mass transfer limitation, with continuous co-factor regeneration and minimal enzyme leaching. All of which provide a positive outlook on this robust multi-enzyme system for efficient activation of linear alkanes as well as the potential for immobilization of various multiple enzymes, including multimeric enzymes for different bio-catalytic applications beyond alkane activation.Keywords: alkane activation, cytochrome P450 monooxygenase, enzyme catalysis, enzyme immobilization
Procedia PDF Downloads 227751 Ordered Mesoporous WO₃-TiO₂ Nanocomposites for Enhanced Xylene Gas Detection
Authors: Vijay K. Tomer, Ritu Malik, Satya P. Nehra, Anshu Sharma
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Highly ordered mesoporous WO₃-TiO₂ nanohybrids with large intrinsic surface area and highly ordered pore channels were synthesized using mesoporous silica, KIT-6 as hard template using a nanocasting strategy. The nanohybrid samples were characterized by a variety of physico-chemical techniques including X-ray diffraction, Nitrogen adsorption-desorption isotherms, and high resolution transmission electron microscope. The nanohybrids were tested for detection of important indoor Volatile Organic Compounds (VOCs) including acetone, ethanol, n-butanol, toluene, and xylene. The sensing result illustrates that the nanocomposite sensor was highly responsive towards xylene gas at relatively lower operating temperature. A rapid response and recovery time, highly linear response and excellent stability in the concentration ranges from 1 to 100 ppm was observed for xylene gas. It is believed that the promising results of this study can be utilized in the synthesis of ordered mesoporous nanostructures which can extend its configuration for the development of new age e-nose type sensors with enhanced gas-sensing performance.Keywords: nanohybrids, response, sensor, VOCs, xylene
Procedia PDF Downloads 331750 Study of Aerosol Deposition and Shielding Effects on Fluorescent Imaging Quantitative Evaluation in Protective Equipment Validation
Authors: Shinhao Yang, Hsiao-Chien Huang, Chin-Hsiang Luo
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The leakage of protective clothing is an important issue in the occupational health field. There is no quantitative method for measuring the leakage of personal protective equipment. This work aims to measure the quantitative leakage of the personal protective equipment by using the fluorochrome aerosol tracer. The fluorescent aerosols were employed as airborne particulates in a controlled chamber with ultraviolet (UV) light-detectable stickers. After an exposure-and-leakage test, the protective equipment was removed and photographed with UV-scanning to evaluate areas, color depth ratio, and aerosol deposition and shielding effects of the areas where fluorescent aerosols had adhered to the body through the protective equipment. Thus, this work built a calculation software for quantitative leakage ratio of protective clothing based on fluorescent illumination depth/aerosol concentration ratio, illumination/Fa ratio, aerosol deposition and shielding effects, and the leakage area ratio on the segmentation. The results indicated that the two-repetition total leakage rate of the X, Y, and Z type protective clothing for subject T were about 3.05, 4.21, and 3.52 (mg/m2). For five-repetition, the leakage rate of T were about 4.12, 4.52, and 5.11 (mg/m2).Keywords: fluorochrome, deposition, shielding effects, digital image processing, leakage ratio, personal protective equipment
Procedia PDF Downloads 323749 Rare Earth Doped Alkali Halide Crystals for Thermoluminescence Dosimetry Application
Authors: Pooja Seth, Shruti Aggarwal
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The Europium (Eu) doped (0.02-0.1 wt %) lithium fluoride (LiF) crystal in the form of multicrystalline sheet was gown by the edge defined film fed growth (EFG) technique. Crystals were grown in argon gas atmosphere using graphite crucible and stainless steel die. The systematic incorporation of Eu inside the host LiF lattice was confirmed by X-ray diffractometry. Thermoluminescence (TL) glow curve was recorded on annealed (AN) crystals after irradiation with a gamma dose of 15 Gy. The effect of different concentration of Eu in enhancing the thermoluminescence (TL) intensity of LiF was studied. The normalized peak height of the Eu-doped LiF crystal was nearly 12 times that of the LiF crystals. The optimized concentration of Eu in LiF was found to be 0.05wt% at which maximum TL intensity was observed with main TL peak positioned at 185 °C. At higher concentration TL intensity decreases due to the formation of precipitates in the form of clusters or aggregates. The nature of the energy traps in Eu doped LiF was analysed through glow curve deconvolution. The trap depth was found to be in the range of 0.2 – 0.5 eV. These results showed that doping with Eu enhances the TL intensity by creating more defect sites for capturing of electron and holes during irradiation which might be useful for dosimetry application.Keywords: thermoluminescence, defects, gamma radiation, crystals
Procedia PDF Downloads 330748 Investigating Anti-bacterial and Anti-Covid-19 Virus Properties and Mode of Action of Mg(Oh)₂ and Copper-Infused Mg(Oh)₂ Nanoparticles on Coated Polypropylene Surfaces
Authors: Saleh Alkarri, Melinda Frame, Dimple Sharma, John Cairney, Lee Maddan, Jin H. Kim, Jonathan O. Rayner, Teresa M. Bergholz, Muhammad Rabnawaz
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Reported herein is an investigation of anti-bacterial and anti-virus properties, mode of action of Mg(OH)₂ and copper-infused Mg(OH)₂ nanoplatelets (NPs) on melt-compounded and thermally embossed polypropylene (PP) surfaces. The anti-viral activity for the NPs was studied in aqueous liquid suspensions against SARS-CoV-2, and the mode of action was investigated on neat NPs and PP samples that were thermally embossed with NPs. Anti-bacterial studies for melt-compounded NPs in PP confirmed approximately 1 log reduction of E. coli populations in 24 h, while for thermally embossed NPs, an 8 log reduction of E. coli populations was observed. In addition, the NPs exhibit anti-viral activity against SARS-CoV-2. Fluorescence microscopy revealed that reactive oxygen species (ROS) is the main mode of action through which Mg(OH)₂ and Cu-Infused Mg(OH)₂act against microbes. Plastics with anti-microbial surfaces from where biocides are non-leachable are highly desirable. This work provides a general fabrication strategy for developing anti-microbial plastic surfaces.Keywords: anti-microbial activity, E. coli K-12 MG1655, anti-viral activity, SARS-CoV-2, copper-infused magnesium hydroxide, non-leachable, ROS, compounding, surface embossing, dyes
Procedia PDF Downloads 66747 Optical Characterization of Anisotropic Thiophene-Phenylene Co-Oligomer Micro Crystals by Spectroscopic Imaging Ellipsometry
Authors: Christian Röling, Elena Y. Poimanova, Vladimir V. Bruevich
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Here we demonstrate a non-destructive optical technique to localize and characterize single crystals of semiconductive organic materials – Spectroscopic Imaging Ellipsometry. With a combination of microscopy and ellipsometry, it is possible to characterize even micro-sized thin film crystals on plane surface regarding anisotropy, optical properties, crystalline domains and thickness. The semiconducting thiophene-phenylene co-oligomer 1,4-bis(5'-hexyl-[2,2'-bithiophen]-5-yl)benzene (dHex-TTPTT) crystals were grown by solvent based self-assembly technique on silicon substrate with 300 nm thermally silicon dioxide. The ellipsometric measurements were performed with an Ep4-SE (Accurion). In an ellipsometric high-contrast image of the complete sample, we have localized high-quality single crystals. After demonstrating the uniaxial anisotropy of the crystal by using Müller-Matrix imaging ellipsometry, we determined the optical axes by rotating the sample and performed spectroscopic measurements (λ = 400-700 nm) in 5 nm intervals. The optical properties were described by using a Lorentz term in the Ep4-Model. After determining the dispersion of the crystals, we converted a recorded Delta and Psi-map into a 2D thickness image. Based on a quantitative analysis of the resulting thickness map, we have calculated the height of a molecular layer (3.49 nm).Keywords: anisotropy, ellipsometry, SCFET, thin film
Procedia PDF Downloads 251746 Metallic Coating for Carbon Fiber Reinforced Polymer Matrix Composite Substrate
Authors: Amine Rezzoug, Said Abdi, Nadjet Bouhelal, Ismail Daoud
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This paper investigates the application of metallic coatings on high fiber volume fraction carbon/epoxy polymer matrix composites. For the grip of the metallic layer, a method of modifying the surface of the composite by introducing a mixture of copper and steel powder (filler powders) which can reduce the impact of thermal spray particles. The powder was introduced to the surface at the time of the forming. Arc spray was used to project the zinc coating layer. The substrate was grit blasted to avoid poor adherence. The porosity, microstructure, and morphology of layers are characterized by optical microscopy, SEM and image analysis. The samples were studied also in terms of hardness and erosion resistance. This investigation did not reveal any visible evidence damage to the substrates. The hardness of zinc layer was about 25.94 MPa and the porosity was around (∼6.70%). The erosion test showed that the zinc coating improves the resistance to erosion. Based on the results obtained, we can conclude that thermal spraying allows the production of protective coating on PMC. Zinc coating has been identified as a compatible material with the substrate. The filler powders layer protects the substrate from the impact of hot particles and allows avoiding the rupture of brittle carbon fibers.Keywords: arc spray, coating, composite, erosion
Procedia PDF Downloads 451