Search results for: Scanning Tunneling Spectroscopy

Authors: O. Gsib, U. Peirera, C. Egles, S. A. Bencherif

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In skin regenerative medicine, one of the critical issues is to produce a three-dimensional scaffold with optimized porosity for dermal fibroblast infiltration and neovascularization, which exhibits high mechanical properties and displays sufficient wound healing characteristics. In this study, we report on the synthesis and characterization of macroporous sequential interpenetrating polymer networks (IPNs) combining skin wound healing properties of fibrin with the excellent physical properties of polyethylene glycol (PEG). Fibrin fibers serve as a provisional biologically active network to promote cell adhesion and proliferation while PEG provides the mechanical stability to maintain the entire 3D construct. After having modified both PEG and Serum Albumin (used for promoting enzymatic degradability) by adding methacrylate residues (PEGDM and SAM, respectively), Fibrin/PEGDM-SAM sequential IPNs were synthesized as follows: Macroporous sponges were first produced from PEGDM-SAM hydrogels by a freeze-drying technique and then rehydrated by adding the fibrin precursors. Environmental Scanning Electron Microscopy (ESEM) and Confocal Laser Scanning Microscopy (CLSM) were used to characterize their microstructure. Human dermal fibroblasts were cultivated during one week in the constructs and different cell culture parameters (viability, morphology, proliferation) were evaluated. Subcutaneous implantations of the scaffolds were conducted on five-week old male nude mice to investigate their biocompatibility in vivo. We successfully synthesized interconnected and macroporous Fibrin/PEGDM-SAM sequential IPNs. The viability of primary dermal fibroblasts was well maintained (above 90%) after 2 days of culture. Cells were able to adhere, spread and proliferate in the scaffolds suggesting the suitable porosity and intrinsic biologic properties of the constructs. The fibrin network adopted a spider web shape that covered partially the pores allowing easier cell infiltration into the macroporous structure. To further characterize the in vitro cell behavior, cell proliferation (EdU incorporation, MTS assay) is being studied. Preliminary histological analysis of animal studies indicated the persistence of hydrogels even after one-month post implantation and confirmed the absence of inflammation response, good biocompatibility and biointegration of our scaffolds within the surrounding tissues. These results suggest that our Fibrin/PEGDM-SAM IPNs could be considered as potential candidates for dermis regenerative medicine. Histological analysis will be completed to further assess scaffold remodeling including de novo extracellular matrix protein synthesis and early stage angiogenesis analysis. Compression measurements will be conducted to investigate the mechanical properties.

Keywords: fibrin, hydrogels for dermal reconstruction, polyethylene glycol, semi-interpenetrating polymer network

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Authors: S. Nigri, R. Oumeddour, F. Djazi

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The inhibition of the corrosion of copper in 1 M HNO3 solution by oleic acid was investigated by weight loss measurement, potentiodynamic polarization and scanning electron microscope (SEM) studies. The experimental results have showed that this compound revealed a good corrosion inhibition and the inhibition efficiency is increased with the inhibitor concentration to reach 98%. The results obtained revealed that the adsorption of the inhibitor molecule onto metal surface is found to obey Langmuir adsorption isotherm. The temperature effect on the corrosion behavior of copper in 1 M HNO3 without and with inhibitor at different concentration was studied in the temperature range from 303 to 333 K and the kinetic parameters activation such as Ea, ∆Ha and ∆Sa were evaluated. Tafel plot analysis revealed that oleic acid acts as a mixed type inhibitor. SEM analysis substantiated the formation of protective layer over the copper surface.

Keywords: oleic acid, weight loss, electrochemical measurement, SEM analysis

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Authors: Azna Zuberi

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Biofilm is a sessile bacterial accretion in which bacteria adapts different physiological and morphological behavior from planktonic form. It is the root cause of about 80% microbial infections in human. Among them, E. coli biofilms are most prevalent in medical devices associated nosocomial infections. The objective of this study was to inhibit biofilm formation by targeting LuxS gene, involved in quorum sensing using CRISPRi. luxS is a synthase, involved in the synthesis of Autoinducer-2(AI-2), which in turn guides the initial stage of biofilm formation. To implement CRISPRi system, we have synthesized complementary sgRNA to target gene sequence and co-expressed with dCas9. Suppression of luxS was confirmed through qRT-PCR. The effect of luxS gene on biofilm inhibition was studied through crystal violet assay, XTT reduction assay and scanning electron microscopy. We conclude that CRISPRi system could be a potential strategy to inhibit bacterial biofilm through mechanism base approach.

Keywords: biofilm, CRISPRi, luxS, microbial

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Authors: B. D. Patni, Ashwani Jain, Arindom Chakraborty

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The world’s highest mountain range has been forming since the collision of Indian Plate with Asian Plate 40-50 million years ago. The Indian subcontinent has been deeper and deeper in to the rest of Asia resulting upliftment of Himalaya & Tibetan Plateau. The complex domain has become a major challenge for construction of hydro electric projects. The Himalayas are geologically complex & seismically active. Shifting of Indian Plate northwardly and increasing the amount of stresses in the fragile domain which leads to deformation in the form of several fold, faults and upliftment. It is difficult to undergo extensive geological investigation to ascertain the geological problems to be encountered during construction. Inaccessibility of the terrain, high rock cover, unpredictable ground water condition etc. are the main constraints. The hydroelectric projects located in Himalayas have faced many geological and geo-hydrological problems while construction of surface and subsurface works. Based on the experience, efforts have been made to identify the expected geological problems during and after construction of the projects. These have been classified into surface and subsurface problems which include existence of inhomogeneous deep overburden in the river bed or buried valley, abrupt change in bed rock profile, Occurrences of fault zones/shear zones/fractured rock in dam foundation and slope instability in the abutments. The tunneling difficulties are many such as squeezing ground condition, popping, rock bursting, high temperature gradient, heavy ingress of water, existence of shear seams/shear zones and emission of obnoxious gases. However, these problems were mitigated by adopting suitable remedial measures as per site requirement. The support system includes shotcrete, wire mesh, rock bolts, steel ribs, fore-poling, pre-grouting, pipe-roofing, MAI anchors, toe wall, retaining walls, reinforced concrete dowels, drainage drifts, anchorage cum drainage shafts, soil nails, concrete cladding and shear keys. Controlled drilling & blasting, heading & benching, proper drainage network and ventilation system are other remedial measures adopted to overcome such adverse situations. The paper highlights the geological uncertainties and its remedial measures in Himalaya, based on the analysis and evaluation of 20 hydroelectric projects during construction.

Keywords: geological problems, shear seams, slope, drilling & blasting, shear zones

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Authors: Ahmet Yonetken, Ayhan Erol

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The microstructure, mechanical properties and corrosion characteristics of Ni plated %10Al2O3-%40Co-%20Cr and %10Ti powders were investigated using specimens produced by tube furnace sintering at 800-1200°C temperature. A uniform nickel layer on Al2O3-Co-Cr and Ti powders was deposited prior to sintering using electroless plating technique. A composite consisting of quintet additions, a metallic phase, Ti,Cr and Co including a ceramic phase, alumina, within a matrix of Ni has been prepared under Ar shroud and then tube furnace sintered. XRD, SEM (Scanning Electron Microscope), corrosion behavior in acidic media were investigated to characterize the properties of the specimens. Experimental results carried out for composition (%10Al2O3-%40Co-%20Cr- %10Ti)20Ni at 1200°C suggest that the best properties as 312.18HV were obtained at 1200°C.

Keywords: sintering, intermetallic, Electroless nickel plating, composite

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Authors: Samira Gharehkhani, Seyed Farid Seyed Shirazi, Abdolreza Gharehkhani, Hooman Yarmand, Ahmad Badarudin, Rushdan Ibrahim, Salim Newaz Kazi

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Nanocrystalline cellulose (NCC) were prepared by acid hydrolysis and ultrasound treatment of bleached Acacia mangium fibers. The obtained rod-shaped nanocrystals showed a uniform size. The results showed that NCC with high crystallinity can be obtained using 64 wt% sulfuric acid. The effect of synthesis condition was investigated. Different reaction times were examined to produce the NCC and the results revealed that an optimum reaction time has to be used for preparing the NCC. Morphological investigation was performed using the transmission electron microscopy (TEM). Fourier transform infrared (FTIR) spectroscopy and thermogravimetric analysis (TGA) were performed. X-ray diffraction (XRD) analysis revealed that the crystallinity increased with successive treatments. The NCC suspension was homogeneous and stable and no sedimentation was observed for a long time.

Keywords: acid hydrolysis, nanocrystalline cellulose, nano material, reaction time

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Authors: Souha Bouagila, Soufiene Ilahi, Noureddine Yacoubi

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We have used Photothermal deflection spectroscopy PTD to investigate the impact of thermal annealing on electronics properties of GaInAsSb/GaSb.GaInAsSb used as an active layer for Vertical Cavity Surface Emitting laser (VCSEL). We have remarked that surface recombination velocity (SRV) from 7963 m / s (± 6.3%) to 1450 m / s (± 3.6) for as grown to sample annealed for 60 min. Accordingly, Force Microscopy images analyses agree well with the measure of surface recombination velocity. We have found that Root-Mean-Square Roughness (RMS) decreases as respect of annealing time. In addition, we have that the diffusion length and minority carrier mobility have been enhanced according to annealing time. However, due to annealing effects, the interface recombination velocity (IRV) is increased from 1196 m / s (± 5) to 6000 m/s (5%) for GaInAsSb in respect of annealed times.

Keywords: nonradiative lifetime, mobility of minority carrier, diffusion length, Surface and interface recombination velocity

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Authors: Awni H. Alkhazaleh, Baljinder K. Kandola

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In this study, a form-stable composite Paraffin/Nanoclay (PA-NC) has been prepared by absorbing PA into porous particles of NC to be used for low-temperature latent heat thermal energy storage. The leakage test shows that the maximum mass fraction of PA that can be incorporated in NC without leakage is 60 wt.%. Differential scanning calorimetry (DSC) has been used to measure the thermal properties of the PA and PA-NC both before and after incorporation in plasterboard (PL). The mechanical performance of the samples has been evaluated in flexural mode. The thermal energy storage performance has been studied using a small test chamber (100 mm × 100 mm × 100 mm) made from 10 mm thick PL and measuring the temperatures using thermocouples. The flammability of the PL+PL-NC has been discussed using a cone calorimeter. The results indicate that the form composite PA has good potential for use as thermal energy storage materials in building applications.

Keywords: building materials, flammability, phase change materials, thermal energy storage

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Authors: Farid Amidi-Fazli

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Problems and disadvantages of using conventional plastics are more apparent in recent years and have attracted researchers' attention. Polymers from natural resources or bio polymers represent a suitable replacement to overcome to the disadvantages of plastics. But due to the some flaws of bio polymers, using suitable filler almost seems necessary. Nanocrystalline cellulose with low cost and availability can be applied as appropriate filler. In this study nanocrystalline cellulose was produced from cotton Linter and was characterized. The cotton Linter was hydrolyzed in sulfuric acid then neutralized by the two different concentrations of NaOH. The resulted suspension was treated by ultrasound waves. Process efficiency was determined as 90%. The final product was studied using scanning electron microscopy and x-ray diffraction technique. The obtained diagram of XRD experiment confirmed that the produced material was nanocrystalline cellulose. Also percentage of crystallinity was calculated as 84% in the obtained material as well as the size of crystals. It can be said that the applied method is a rapid and easy method for the production of nanocrystalline cellulose.

Keywords: nanocrystalline cellulose, crystallinity, XRD, cotton linter

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Authors: Eduardo Padilla, Luis Daniel Rodriguez, Ivan Sanchez, Angelica Sofia Go

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The synthesis and application of metallic nanoparticles have increased in recent years. Biological methods go beyond the chemical and physical synthesis that is expensive and not friendly to the environment. Therefore, in this study, silver nanoparticles were synthesized biologically in an environmentally friendly way by Handroanthus chrysanthus flower aqueous extract (AgNPs) that contains phytochemicals capable of reducing silver nitrate. AgNPs were characterized visually by UV-visible spectroscopy and TEM. The antimicrobial activity of the AgNPs was tested by determining the minimum inhibitory concentration (MIC), and minimal bactericidal concentration (MBC) in Escherichia coli and Staphylococcus aureus strains AgNPs showed potent antimicrobial activity against gram-negative and gram-positive bacteria. MIC and MBC values were as low as 41.6, and 83.2 ug/mL using AgNPs biosynthesized by H. chrysanthus flower extract. This nanoparticle could be the basis for the formulation of disinfectants for use in the food and pharmaceutical industry.

Keywords: antimicrobial, silver nanoparticles, flower extract, Handroanthus

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Authors: Mohamed H. El-Newehy, Sameh M. Osman, Moamen S. Refat, Salem S. Al-Deyab, Ayman El-Faham

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The two copolymers itaconic acid-methyl methacrylate and itaconic acid-acrylamide have been prepared in different ratio by radical copolymerization in the presence of azobisisobutyronitrile (AIBN) as initiator and using 2-butanone as reaction medium using microwave irradiation. The microwave technique is safe, fast, and gives high yield of the products with high purity in an optimum time, comparing to the traditional conventional heating. All the prepared copolymers were characterized by FT-IR, thermal analysis and elemental microanalysis. The itaconic acid-based copolymers showed a good sensitivity in alkaline media for scavenging Cu (II) and Pb (II). The chelation behavior of both Cu (II) and Pb (II) complexes were checked using FT-IR, thermogravimetric analysis (TGA), and differential scanning calorimetery (DSC). The infrared data are in a good agreement with the coordination through carboxylate-to-metal, in which the copolymers acting as a bidentate ligand.

Keywords: microwave synthesis, itaconic acid, copolymerization, scavenging, thermal stability

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Authors: Abdulrahman Sumayli

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Natural Zinc has many significant biological functions, including developments and sustainable of bones and wound healing. Metallic zinc has recently been explored as potential biomaterials that have preferable biodegradable, biocompatible, and mechanical properties. Pure metal zinc has a preferable physical and mechanical properties for biodegradable and biocompatible applications such as density and modulus of elasticity. The aim of the research is to make different Zn-based metallic alloys and test them effectively to be used as biocompatible and biodegradable materials in the field biomedical application. Microstructure study of the as-cast alloys will be examined using SEM (scanning electron microscope) followed by X-ray diffraction investigated so as to evaluate phase constitution of the designed alloys. After that, immersion test and electrochemical test will be applied to the designed alloys so as to study bio corrosion behaviour of the proposed alloys. Finally, in vitro cytocompatibility well conducted to study biocompatibility of the made alloys.

Keywords: Zn-based alloys, biodegradable and biocompatible materials, cytotoxicity test, neutron synchrotron imaging

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Authors: N. Webb, A. Buchanan

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Digital and virtual heritage is often associated with the recreation of lost artefacts and architecture; however, we can also investigate works that were not completed, using digital tools and techniques. Here we explore physical evidence of a fourteenth-century Gothic vault located in the north transept of St Mary’s church in Nantwich, Cheshire, using existing springer stones that are built into the walls as a starting point. Digital surveying tools are used to document the architecture, followed by an analysis process to hypothesise and simulate possible design solutions, had the vault been completed. A number of options, both two-dimensionally and three-dimensionally, are discussed based on comparison with examples of other contemporary vaults, thus adding another specimen to the corpus of vault designs. Dissemination methods such as digital models and 3D prints are also explored as possible resources for demonstrating what the finished vault might have looked like for heritage interpretation and other purposes.

Keywords: digital simulation, heritage interpretation, medieval vaults, virtual heritage, 3d scanning

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Authors: Altoumi Alndalusi

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The work examines the aqueous corrosion behavior of grades of stain less steel which are used as corrosion resistant castings for applications such as valve and pump bodies. The corrosion behavior of steels in the as-cast condition has been examined using potentiostatic studies to illustrate the need for correct thermal treatment. A metallurgical examination and chemical analysis were carried out to establish the morphology of the steel structure. Heat treatment was carried out in order to compare damage in relation to microstructure. Optical and scanning electron microscopy examinations confirmed that the austenitic steels suffers from severe localized inter-dendritic pitting attack, while non homogenized castings highly alloyed duplex steels gave inferior corrosion resistance. Through the heat treatment conditions a significant of phase transformation of the duplex steel C were occurred (from ferrite to austenite and sigma plus carbides) and were gave reduction resistance.

Keywords: cast, corrosion, duplex stainless, heat treatment, material, steel

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Authors: Mohamed Elbehery

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Historical textiles in the burial environment or in museums are exposed to many types of stains and dirt that are associated with historical textiles by multiple chemical bonds that cause damage to historical textiles. The cleaning process must be carried out with great care, with no irreversible damage, and sediments removed without affecting the original material of the surface being cleaned. Science and technology continue to provide innovative systems in the bio-cleaning process (using pure enzymes) of historical textiles and artistic surfaces. Lipase and α-amylase were immobilized on nanoparticles of alginate/κ-carrageenan nanoparticle complex and used in historical textiles cleaning. Preparation of nanoparticles, activation, and enzymes immobilization were characterized. Optimization of loading time and units of the two enzymes were done. It was found that, the optimum time and units of amylase were 4 hrs and 25U, respectively. While, the optimum time and units of lipase were 3 hrs and 15U, respectively. The methods used to examine the fibers using a scanning electron microscope equipped with an X-ray energy dispersal unit: SEM with EDX unit.

Keywords: nanoparticles, enzymes, immobilization, textiles

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Authors: Randa Slatnia

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In this study, the nanostructured stable phase identification elaborated by nickel nitrate hyxahydrate and thiourea compounds. After the preparation of the solution (Stirred mixture with methanol as solvent), a deposition of eight layers of this solution on a glass substrate and annealed at 300 °C for energy applications. The annealed sample was analyzed by X-ray Grazing incidence diffraction (GID) with a Bruker D8 Advance diffractometer using Cu Kα1 radiation at 40 kV and 40 mA (1600 W) and Scanning electron microscopy (Thermo Fisher environmental SEM). The results of XRD-GID analysis for the prepared sample showed the formation of an identified stable phase NiS2 and the XRD-GID pattern of the elaborated sample with eight layers prepared solution and annealed show wide and characteristic peaks of the NiS2 with cubic structure (ICDD card no. PDF 01-078-4702). The morphology of the NiS2 thin films confirmed by XRD-GID analysis was investigated by ESEM showed a surface with a uniform and homogeneous distribution nanostructure.

Keywords: nickel sulfide, thin films, XRD, ESEM

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Authors: Huseyin Kavas

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Oleic acid (OA) capped superparamagnetic iron oxide nanoparticles (SPION) were synthesized by a thermal decomposition method. The composition of nanoparticles was confirmed by X-ray powder diffraction, and the morphology of particles was investigated by Atomic Force Microscopy (AFM), Scanning Electron Microscopy (SEM), and Transmission electron microscopy (TEM). The crystalline and particle size distribution of SPIONS capped with OA were investigated with a mean size of 6.99 nm and 8.9 nm, respectively. It was found that SPIONS have superparamagnetic characteristics with a saturation magnetization value of 64 emu/g. The thin film form of self-assembled SPIONS was fabricated by coating techniques of spin coating and dip coating. SQUID-VSM magnetometer and FMR techniques were performed in order to evaluate the magnetic properties of thin films, especially the existence of magnetic anisotropy. The thin films with magnetic anisotropy were obtained by self-assembled monolayers of SPION.

Keywords: magnetic materials, nanostructures, self-assembly, FMR

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Authors: Amrei Voelkner, Nils Peters, Thomas Mannheim

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The worldwide exponential growth of the population and the simultaneous increasing food production requires the strategic realization of sustainable and improved cultivation systems to ensure the fertility of arable land and to guarantee the food supply for the whole world. To fulfill this target, large quantities of fertilizers have to be applied to the field, but the long-term environmental impacts remain uncertain. Thus, a combined system would be necessary to increase the nutrient availability for plants while reducing nutrient losses (e.g. NO3- by leaching) to the environment. To enhance the nutrient efficiency, polymer coated fertilizer with a controlled release behavior have been developed. This kind of fertilizer ensures a delayed release of nutrients to synchronize the nutrient supply with the demand of different crops. In the last decades, research focused primarily on semi-permeable polyurethane coatings, which remain in the soil for a long period after the complete solvation of the fertilizer core. Within the implementation of the new European Regulation Directive the replacement of non-degradable synthetic polymers by degradable coatings is necessary. It was, therefore, the objective of this study to develop a total biodegradable polymer (to CO2 and H2O) coating according to ISO 17556 and to compare the retarding effect of the biodegradable coatings with commercially available non-degradable products. To investigate the effect of ten selected coated urea fertilizer on the yield of annual ryegrass and maize, the fresh and dry mass, the percentage of total nitrogen and main nutrients were analyzed in greenhouse experiments in sixfold replications using near-infrared spectroscopy. For the experiments, a homogenized and air-dried loamy sand (Cambic Luvisol) was equipped with a basic fertilization of P, K, Mg and S. To investigate the effect of nitrogen level increase, three levels (80%, 100%, 120%) were established, whereas the impact of CRF granules was determined using a N-level of 100%. Additionally, leaching of NO3- from pots planted with annual ryegrass was examined to evaluate the retention capacity of urea by the polymer coating. For this, leachate from Kick-Brauckmann-Pots was collected daily and analyzed for total nitrogen, NO3- and NH4+ in twofold repetition once a week using near-infrared spectroscopy. We summarize from the results that the coated fertilizer have a clear impact on the yield of annual ryegrass and maize. Compared to the control, an increase of fresh and dry mass could be recognized. Partially, the non-degradable coatings showed a retarding effect for a longer period, which was however reflected by a lower fresh and dry mass. It was ascertained that the percentage of leached-out nitrate could be reduced markedly. As a conclusion, it could be pointed out that the impact of coated fertilizer of all polymer types might contribute to a reduction of negative environmental impacts in addition to their fertilizing effect.

Keywords: biodegradable polymers, coating, enhanced efficiency fertilizers, nitrate leaching

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Authors: Dilip K. Paul

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The most popular mesoporous molecular sieves, Mobil Composition of Matter (MCM) are keenly studied by researchers because of these materials possess amorphous silica wall and have a long range of ordered framework with uniform mesopores. These materials also possess large surface area, which can be up to more than 1000 m2g−1. Herein the investigation is focused upon the synthesis and characterization of chromium and aluminum doped MCM-41 using XRD and FTIR. Acid-base properties of Cr-Al-MCM 41 was investigated by molecularly sensitive transmission FT-IR spectroscopy by adsorbing pyridine. In addition, these MCM nanomaterial was used to catalyze C-C bond formation from acetaldehyde adsorption. The assignment of all infrared peaks during adsorption of pyridine provided detail information on the presence of acid-base sites which in turn helped us to explain the roles of these in the condensation reaction of aldehyde. Reaction mechanisms of C-C bond formation is therefore explored to shed some light on this elusive reaction detail.

Keywords: mesoporous nanomaterial, MCM 41, FTIR studies, acid-base studies

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Authors: Emmanuel Ogundimu, Esther Akinlabi, Mutiu Erinosho

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The aim of this paper is to study the effect of welding current on the microstructure and the mechanical properties. Material characterizations were conducted on a 6 mm thick plates of type-304 austenite stainless steel, welded by TIG welding process at two different welding currents of 150 A (Sample F3) and 170 A (Sample F4). The tensile strength and the elongation obtained from sample F4 weld were approximately 584 MPa and 19.3 %; which were higher than sample F3 weld. The average microhardness value of sample F4 weld was found to be 235.7 HV, while that of sample F3 weld was 233.4 HV respectively. Homogenous distribution of iron (Fe), chromium (Cr) and nickel (Ni) were observed at the welded joint of the two samples. The energy dispersive spectroscopy (EDS) analysis revealed that Fe, Cr, and Ni made up the composition formed in the weld zone. The optimum welding current of 170 A for TIG welding of type-304 austenite stainless steel can be recommended for high-tech industrial applications.

Keywords: microhardness, microstructure, tensile, MIG welding, process, tensile, shear stress TIG welding, TIG-MIG welding

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Authors: Gerd Wilsch, Tobias Guenther, Tobias Voelker

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In view of the ageing of vital infrastructure facilities, a reliable condition assessment of concrete structures is becoming of increasing interest for asset owners to plan timely and appropriate maintenance and repair interventions. For concrete structures, reinforcement corrosion induced by penetrating chlorides is the dominant deterioration mechanism affecting the serviceability and, eventually, structural performance. The determination of the quantitative chloride ingress is required not only to provide valuable information on the present condition of a structure, but the data obtained can also be used for the prediction of its future development and associated risks. At present, wet chemical analysis of ground concrete samples by a laboratory is the most common test procedure for the determination of the chloride content. As the chloride content is expressed by the mass of the binder, the analysis should involve determination of both the amount of binder and the amount of chloride contained in a concrete sample. This procedure is laborious, time-consuming, and costly. The chloride profile obtained is based on depth intervals of 10 mm. LIBS is an economically viable alternative providing chloride contents at depth intervals of 1 mm or less. It provides two-dimensional maps of quantitative element distributions and can locate spots of higher concentrations like in a crack. The results are correlated directly to the mass of the binder, and it can be applied on-site to deliver instantaneous results for the evaluation of the structure. Examples for the application of the method in the laboratory for the investigation of diffusion and migration of chlorides, sulfates, and alkalis are presented. An example for the visualization of the Li transport in concrete is also shown. These examples show the potential of the method for a fast, reliable, and automated two-dimensional investigation of transport processes. Due to the better spatial resolution, more accurate input parameters for model calculations are determined. By the simultaneous detection of elements such as carbon, chlorine, sodium, and potassium, the mutual influence of the different processes can be determined in only one measurement. Furthermore, the application of a mobile LIBS system in a parking garage is demonstrated. It uses a diode-pumped low energy laser (3 mJ, 1.5 ns, 100 Hz) and a compact NIR spectrometer. A portable scanner allows a two-dimensional quantitative element mapping. Results show the quantitative chloride analysis on wall and floor surfaces. To determine the 2-D distribution of harmful elements (Cl, C), concrete cores were drilled, split, and analyzed directly on-site. Results obtained were compared and verified with laboratory measurements. The results presented show that the LIBS method is a valuable addition to the standard procedures - the wet chemical analysis of ground concrete samples. Currently, work is underway to develop a technical code of practice for the application of the method for the determination of chloride concentration in concrete.

Keywords: chemical analysis, concrete, LIBS, spectroscopy

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Authors: Yeshona Sewsynker

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This study presents three microwave-assisted alkalic salt pretreatments to enhance delignification and enzymatic saccharification of corn cobs. The effects of process parameters of salt concentration (0-15%), microwave power intensity (0-800 W) and pretreatment time (2-8 min) on reducing sugar yield from corn cobs were investigated. Pretreatment models were developed with the high coefficient of determination values (R2>0.85). Optimization gave a maximum reducing sugar yield of 0.76 g/g. Scanning electron microscopy (SEM) and Fourier Transform Infrared analysis (FTIR) showed major changes in the lignocellulosic structure after pretreatment. A 7-fold increase in the sugar yield was observed compared to previous reports on the same substrate. The developed pretreatment strategy was effective for enhancing enzymatic saccharification from lignocellulosic wastes for microbial biofuel production processes and value-added products.

Keywords: pretreatment, lignocellulosic biomass, enzymatic hydrolysis, delignification

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Authors: A. Saurabh Singh, B. Raghvendra, C. Prabhakar Singh

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Solid Oxide Fuel Cells (SOFCs) are one of the most attractive electrochemical energy conversion systems, as these devices present a clean energy production, thus promising high efficiencies and low environmental impact. The electrodes are the main components that decisively control the performance of a SOFC. Conventional, anode materials (like Ni-YSZ) are operates at very high temperature. Therefore, cost-effective materials which operate at relatively lower temperatures are still required. In present study, we have synthesized La doped Strontium Titanate via solid state reaction route. The structural, microstructural and density of the pellet have been investigated employing XRD, SEM and Archimedes Principle, respectively. The electrical conductivity of the systems has been determined by impedance spectroscopy techniques. The electrical conductivity of the Lanthanum Strontium Titanate (LST) has been found to be higher than the composite Ni-YSZ system at 700 °C.

Keywords: IT-SOFC, LST, Lanthanum Strontium Titanate, electrical conductivity

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Authors: Darren A. Whitaker, Dan Palmer, Jens Wesholowski, James Flaherty, John Mack, Ahmad B. Albadarin, Gavin Walker

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Traditional mechanosynthesis has been performed by either ball milling or manual grinding. However, neither of these techniques allow the easy application of process control. The temperature may change unpredictably due to friction in the process. Hence the amount of energy transferred to the reactants is intrinsically non-uniform. Recently, it has been shown that the use of Twin-Screw extrusion (TSE) can overcome these limitations. Additionally, TSE enables a platform for continuous synthesis or manufacturing as it is an open-ended process, with feedstocks at one end and product at the other. Several materials including metal-organic frameworks (MOFs), co-crystals and small organic molecules have been produced mechanochemically using TSE. The described advantages of TSE are offset by drawbacks such as increased process complexity (a large number of process parameters) and variation in feedstock flow impacting on product quality. To handle the above-mentioned drawbacks, this study utilizes UV-Vis spectrophotometry (InSpectroX, ColVisTec) as an online tool to gain real-time information about the quality of the product. Additionally, this is combined with real-time process information in an Advanced Process Control system (PharmaMV, Perceptive Engineering) allowing full supervision and control of the TSE process. Further, by characterizing the dynamic behavior of the TSE, a model predictive controller (MPC) can be employed to ensure the process remains under control when perturbed by external disturbances. Two reactions were studied; a Knoevenagel condensation reaction of barbituric acid and vanillin and, the direct amidation of hydroquinone by ammonium acetate to form N-Acetyl-para-aminophenol (APAP) commonly known as paracetamol. Both reactions could be carried out continuously using TSE, nuclear magnetic resonance (NMR) spectroscopy was used to confirm the percentage conversion of starting materials to product. This information was used to construct partial least squares (PLS) calibration models within the PharmaMV development system, which relates the percent conversion to product to the acquired UV-Vis spectrum. Once this was complete, the model was deployed within the PharmaMV Real-Time System to carry out automated optimization experiments to maximize the percentage conversion based on a set of process parameters in a design of experiments (DoE) style methodology. With the optimum set of process parameters established, a series of PRBS process response tests (i.e. Pseudo-Random Binary Sequences) around the optimum were conducted. The resultant dataset was used to build a statistical model and associated MPC. The controller maximizes product quality whilst ensuring the process remains at the optimum even as disturbances such as raw material variability are introduced into the system. To summarize, a combination of online spectral monitoring and advanced process control was used to develop a robust system for optimization and control of two TSE based mechanosynthetic processes.

Keywords: continuous synthesis, pharmaceutical, spectroscopy, advanced process control

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Authors: Leslie Raphael de M. Ferraz, Salvana Priscylla M. Costa, Tarcyla de A. Gomes, Giovanna Christinne R. M. Schver, Cristóvão R. da Silva, Magaly Andreza M. de Lyra, Danilo Augusto F. Fontes, Larissa A. Rolim, Amanda Carla Q. M. Vieira, Miracy M. de Albuquerque, Pedro J. Rolim-Neto

Abstract:

Efavirenz (EFV) is a drug used as first-line treatment of AIDS. However, it has poor aqueous solubility and wettability, presenting problems in the gastrointestinal tract absorption and bioavailability. One of the most promising strategies to improve the solubility is the use of solid dispersions (SD). Therefore, this study aimed to characterize SD EFZ with the polymers: PVP-K30, PVPVA 64 and SOLUPLUS in order to find an optimal formulation to compose a future pharmaceutical product for AIDS therapy. Initially, Physical Mixtures (PM) and SD with the polymers were obtained containing 10, 20, 50 and 80% of drug (w/w) by the solvent method. The best formulation obtained between the SD was selected by in vitro dissolution test. Finally, the drug-carrier system chosen, in all ratios obtained, were analyzed by the following techniques: Differential Scanning Calorimetry (DSC), polarization microscopy, Scanning Electron Microscopy (SEM) and spectrophotometry of absorption in the region of infrared (IR). From the dissolution profiles of EFV, PM and SD, the values of area Under The Curve (AUC) were calculated. The data showed that the AUC of all PM is greater than the isolated EFV, this result is derived from the hydrophilic properties of the polymers thus favoring a decrease in surface tension between the drug and the dissolution medium. In adittion, this ensures an increasing of wettability of the drug. In parallel, it was found that SD whom had higher AUC values, were those who have the greatest amount of polymer (with only 10% drug). As the amount of drug increases, it was noticed that these results either decrease or are statistically similar. The AUC values of the SD using the three different polymers, followed this decreasing order: SD PVPVA 64-EFV 10% > SD PVP-K30-EFV 10% > SD Soluplus®-EFV 10%. The DSC curves of SD’s did not show the characteristic endothermic event of drug melt process, suggesting that the EFV was converted to its amorphous state. The analysis of polarized light microscopy showed significant birefringence of the PM’s, but this was not observed in films of SD’s, thus suggesting the conversion of the drug from the crystalline to the amorphous state. In electron micrographs of all PM, independently of the percentage of the drug, the crystal structure of EFV was clearly detectable. Moreover, electron micrographs of the SD with the two polymers in different ratios investigated, we observed the presence of particles with irregular size and morphology, also occurring an extensive change in the appearance of the polymer, not being possible to differentiate the two components. IR spectra of PM corresponds to the overlapping of polymer and EFV bands indicating thereby that there is no interaction between them, unlike the spectra of all SD that showed complete disappearance of the band related to the axial deformation of the NH group of EFV. Therefore, this study was able to obtain a suitable formulation to overcome the solubility limitations of the EFV, since SD PVPVA 64-EFZ 10% was chosen as the best system in delay crystallization of the prototype, reaching higher levels of super saturation.

Keywords: characterization, dissolution, Efavirenz, solid dispersions

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Authors: R. R. Galiev, I. I. Lykov, A. E. Shitikov, I. A. Bilenko

Abstract:

Dual-comb interferometry is based on the mixing of two optical frequency combs with slightly different lines spacing which results in the mapping of the optical spectrum into the radio-frequency domain for future digitizing and numerical processing. The dual-comb approach enables diverse applications, including metrology, fast high-precision spectroscopy, and distance range. Ordinary frequency-modulated continuous-wave (FMCW) laser-based Light Identification Detection and Ranging systems (LIDARs) suffer from two main disadvantages: slow and unreliable mechanical, spatial scan and a rather wide linewidth of conventional lasers, which limits speed measurement resolution. Dual-comb distance measurements with Allan deviations down to 12 nanometers at averaging times of 13 microseconds, along with ultrafast ranging at acquisition rates of 100 megahertz, allowing for an in-flight sampling of gun projectiles moving at 150 meters per second, was previously demonstrated. Nevertheless, pump lasers with EDFA amplifiers made the device bulky and expensive. An alternative approach is a direct coupling of the laser to a reference microring cavity. Backscattering can tune the laser to the eigenfrequency of the cavity via the so-called self-injection locked (SIL) effect. Moreover, the nonlinearity of the cavity allows a solitonic frequency comb generation in the very same cavity. In this work, we developed a fully integrated, power-efficient, electrically driven dual-micro comb source based on the semiconductor lasers SIL to high-quality integrated Si3N4 microresonators. We managed to obtain robust 1400-1700 nm combs generation with a 150 GHz or 1 THz lines spacing and measure less than a 1 kHz Lorentzian withs of stable, MHz spaced beat notes in a GHz band using two separated chips, each pumped by its own, self-injection locked laser. A deep investigation of the SIL dynamic allows us to find out the turn-key operation regime even for affordable Fabry-Perot multifrequency lasers used as a pump. It is important that such lasers are usually more powerful than DFB ones, which were also tested in our experiments. In order to test the advantages of the proposed techniques, we experimentally measured a minimum detectable speed of a reflective object. It has been shown that the narrow line of the laser locked to the microresonator provides markedly better velocity accuracy, showing velocity resolution down to 16 nm/s, while the no-SIL diode laser only allowed 160 nm/s with good accuracy. The results obtained are in agreement with the estimations and open up ways to develop LIDARs based on compact and cheap lasers. Our implementation uses affordable components, including semiconductor laser diodes and commercially available silicon nitride photonic circuits with microresonators.

Keywords: dual-comb spectroscopy, LIDAR, optical microresonator, self-injection locking

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Authors: L. Achou, A. Doghmane

Abstract:

Elastic performances, as an essential property of nanowires (NWs), play a significant role in the design and fabrication of modern nanodevices. In this paper, our interest is focused on ZnO NWs to investigate wire diameter (D_wire ≤ 400 nm) effects on elastic properties. The plotted data reveal that a strong size dependence of the elastic constants exists when the wire diameter is smaller than ~ 100 nm. For larger diameters (D_wire > 100 nm), these ones approach their corresponding bulk values. To enrich this study, we make use of the scanning acoustic microscopy simulation technique. The calculation methodology consists of several steps: determination of longitudinal and transverse wave velocities, calculation of refection coefficients, calculation of acoustic signatures and Rayleigh velocity determination. Quantitatively, it was found that changes in ZnO diameters over the ranges 1 nm ≤ D_wire ≤ 100 nm lead to similar exponential variations, for all elastic parameters, of the from: A = a + b exp(-D_wire/c) where a, b, and c are characteristic constants of a given parameter. The developed relation can be used to predict elastic properties of such NW by just knowing its diameter and vice versa.

Keywords: elastic properties, nanowires, semiconductors, theoretical model, ZnO

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Authors: Josef Sepitka, Petr Vlcak, Tomas Horazdovsky, Vratislav Perina

Abstract:

An ion implantation technique was used for designing the surface area of a titanium alloy and for irradiation-enhanced hardening of the surface. The Ti6Al4V alloy was treated by nitrogen ion implantation at fluences of 2·10¹⁷ and 4·10¹⁷ cm^-2 and at ion energy 90 keV. The depth distribution of the nitrogen was investigated by Rutherford Backscattering Spectroscopy. The gradient of mechanical properties was investigated by nanoindentation. The continuous measurement mode was used to obtain depth profiles of the indentation hardness and the reduced storage modulus of the modified surface area. The reduced storage modulus and the hardness increase with increasing fluence. Increased fluence shifts the peak of the mechanical properties as well as the peak of nitrogen concentration towards to the surface. This effect suggests a direct relationship between mechanical properties and nitrogen distribution.

Keywords: nitrogen ion implantation, titanium-based nanolayer, storage modulus, hardness, microstructure

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Authors: Jose Gonzalez, Fai Cheng, Ivy Fan

Abstract:

Shipping has a mature and ever expanding worldwide market. The future of the marine industry itself is not only irrevocably linked with the global economic, social, and political landscape; it is also subject to the technological developments in different fields. Some of them may have never been linked to the marine industry before. Companies in the marine sector are getting more dependent on technologies to achieve competitive advantage in an increasing open market. Technologies can be fused across different business functions and geopolitical influences. A successful marine business should be prepared to embrace such potential changes that lie ahead. The present paper intends to articulate long-term marine technology strategies from an industrial perspective. Methodology and current development are introduced. The paper will also provide insight into future technological trends demand for major commercial ship types. It may also assist different stakeholders in tailoring their long-term strategies to achieve a Sea Change and to uncap opportunity.

Keywords: commercial sector, marine, trends, technology

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Authors: Devender Mandala, Paul Watts

Abstract:

Cis-Nucleosides mainly lamivudine (3TC) and emtricitabine (FTC) are an important tool in the treatment of Human immune deficiency virus (HIV), Hepatitis B virus (HBV) and Human T-Lymotropoic virus (HTLV). Lamivudine and emtricitabine are potent nucleoside analog reverse transcriptase inhibitors (nRTI). These two drugs are synthesized by a four-stage process from the starting materials: menthyl glyoxylate hydrate and 1,4-dithane-2,5-diol to produce the 5-hydroxy oxathiolane which upon acetylation with acetic anhydride to yield 5-acetoxy oxathiolane. Then glycosylation of this acetyl product with silyl protected nucleoside to produce the intermediate. The reduction of this intermediates can provide the final targets. Although there are several different methods reported for the synthesis of lamivudine and emtricitabine as a single enantiomer, we required an efficient route, which was suitable for large-scale synthesis to support the development of these compounds. In this process, we successfully prepared the intermediates of lamivudine and emtricitabine without using any solvents and catalyst, thus promoting the green synthesis. All the synthesized compound were confirmed by TLC, GC, Mass, NMR and 13C NMR spectroscopy.

Keywords: emtricitabine, green synthesis, lamivudine, nucleoside

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