Search results for: MeV electron irradiation
Commenced in January 2007
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Edition: International
Paper Count: 2864

Search results for: MeV electron irradiation

134 Preliminary Design, Production and Characterization of a Coral and Alginate Composite for Bone Engineering

Authors: Sthephanie A. Colmenares, Fabio A. Rojas, Pablo A. Arbeláez, Johann F. Osma, Diana Narvaez

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The loss of functional tissue is a ubiquitous and expensive health care problem, with very limited treatment options for these patients. The golden standard for large bone damage is a cadaveric bone as an allograft with stainless steel support; however, this solution only applies to bones with simple morphologies (long bones), has a limited material supply and presents long term problems regarding mechanical strength, integration, differentiation and induction of native bone tissue. Therefore, the fabrication of a scaffold with biological, physical and chemical properties similar to the human bone with a fabrication method for morphology manipulation is the focus of this investigation. Towards this goal, an alginate and coral matrix was created using two production techniques; the coral was chosen because of its chemical composition and the alginate due to its compatibility and mechanical properties. In order to construct the coral alginate scaffold the following methodology was employed; cleaning of the coral, its pulverization, scaffold fabrication and finally the mechanical and biological characterization. The experimental design had: mill method and proportion of alginate and coral, as the two factors, with two and three levels each, using 5 replicates. The coral was cleaned with sodium hypochlorite and hydrogen peroxide in an ultrasonic bath. Then, it was milled with both a horizontal and a ball mill in order to evaluate the morphology of the particles obtained. After this, using a combination of alginate and coral powder and water as a binder, scaffolds of 1cm3 were printed with a SpectrumTM Z510 3D printer. This resulted in solid cubes that were resistant to small compression stress. Then, using a ESQUIM DP-143 silicon mold, constructs used for the mechanical and biological assays were made. An INSTRON 2267® was implemented for the compression tests; the density and porosity were calculated with an analytical balance and the biological tests were performed using cell cultures with VERO fibroblast, and Scanning Electron Microscope (SEM) as visualization tool. The Young’s moduli were dependent of the pulverization method, the proportion of coral and alginate and the interaction between these factors. The maximum value was 5,4MPa for the 50/50 proportion of alginate and horizontally milled coral. The biological assay showed more extracellular matrix in the scaffolds consisting of more alginate and less coral. The density and porosity were proportional to the amount of coral in the powder mix. These results showed that this composite has potential as a biomaterial, but its behavior is elastic with a small Young’s Modulus, which leads to the conclusion that the application may not be for long bones but for tissues similar to cartilage.

Keywords: alginate, biomaterial, bone engineering, coral, Porites asteroids, SEM

Procedia PDF Downloads 233
133 Cotton Fabrics Functionalized with Green and Commercial Ag Nanoparticles

Authors: Laura Gonzalez, Santiago Benavides, Martha Elena Londono, Ana Elisa Casas, Adriana Restrepo-Osorio

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Cotton products are sensitive to microorganisms due to its ability to retain moisture, which might cause change into the coloration, mechanical properties reduction or foul odor generation; consequently, this represents risks to the health of users. Nowadays, have been carried out researches to give antibacterial properties to textiles using different strategies, which included the use of silver nanoparticles (AgNPs). The antibacterial behavior can be affected by laundering process reducing its effectiveness. In the other way, the environmental impact generated for the synthetic antibacterial agents has motivated to seek new and more ecological ways for produce AgNPs. The aims of this work are to determine the antibacterial activity of cotton fabric functionalized with green (G) and commercial (C) AgNPs after twenty washing cycles, also to evaluate morphological and color changes. A plain weave cotton fabric suitable for dyeing and two AgNPs solutions were use. C a commercial product and G produced using an ecological method, both solutions with 0.5 mM concentration were impregnated on cotton fabric without stabilizer, at a liquor to fabric ratio of 1:20 in constant agitation during 30min and then dried at 70 °C by 10 min. After that the samples were subjected to twenty washing cycles using phosphate-free detergent simulated on agitated flask at 150 rpm, then were centrifuged and dried on a tumble. The samples were characterized using Kirby-Bauer test determine antibacterial activity against E. coli y S. aureus microorganisms, the results were registered by photographs establishing the inhibition halo before and after the washing cycles, the tests were conducted in triplicate. Scanning electron microscope (SEM) was used to observe the morphologies of cotton fabric and treated samples. The color changes of cotton fabrics in relation to the untreated samples were obtained by spectrophotometer analysis. The images, reveals the presence of inhibition halo in the samples treated with C and G AgNPs solutions, even after twenty washing cycles, which indicated a good antibacterial activity and washing durability, with a tendency to better results against to S. aureus bacteria. The presence of AgNPs on the surface of cotton fiber and morphological changes were observed through SEM, after and before washing cycles. The own color of the cotton fiber has been significantly altered with both antibacterial solutions. According to the colorimetric results, the samples treated with C lead to yellowing while the samples modified with G to red yellowing Cotton fabrics treated AgNPs C and G from 0.5 mM solutions exhibited excellent antimicrobial activity against E. coli and S. aureus with good laundering durability effects. The surface of the cotton fibers was modified with the presence of AgNPs C and G due to the presence of NPs and its agglomerates. There are significant changes in the natural color of cotton fabric due to deposition of AgNPs C and G which were maintained after laundering process.

Keywords: antibacterial property, cotton fabric, fastness to wash, Kirby-Bauer test, silver nanoparticles

Procedia PDF Downloads 217
132 Stimulation of Nerve Tissue Differentiation and Development Using Scaffold-Based Cell Culture in Bioreactors

Authors: Simon Grossemy, Peggy P. Y. Chan, Pauline M. Doran

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Nerve tissue engineering is the main field of research aimed at finding an alternative to autografts as a treatment for nerve injuries. Scaffolds are used as a support to enhance nerve regeneration. In order to successfully design novel scaffolds and in vitro cell culture systems, a deep understanding of the factors affecting nerve regeneration processes is needed. Physical and biological parameters associated with the culture environment have been identified as potentially influential in nerve cell differentiation, including electrical stimulation, exposure to extracellular-matrix (ECM) proteins, dynamic medium conditions and co-culture with glial cells. The mechanisms involved in driving the cell to differentiation in the presence of these factors are poorly understood; the complexity of each of them raises the possibility that they may strongly influence each other. Some questions that arise in investigating nerve regeneration include: What are the best protein coatings to promote neural cell attachment? Is the scaffold design suitable for providing all the required factors combined? What is the influence of dynamic stimulation on cell viability and differentiation? In order to study these effects, scaffolds adaptable to bioreactor culture conditions were designed to allow electrical stimulation of cells exposed to ECM proteins, all within a dynamic medium environment. Gold coatings were used to make the surface of viscose rayon microfiber scaffolds (VRMS) conductive, and poly-L-lysine (PLL) and laminin (LN) surface coatings were used to mimic the ECM environment and allow the attachment of rat PC12 neural cells. The robustness of the coatings was analyzed by surface resistivity measurements, scanning electron microscope (SEM) observation and immunocytochemistry. Cell attachment to protein coatings of PLL, LN and PLL+LN was studied using DNA quantification with Hoechst. The double coating of PLL+LN was selected based on high levels of PC12 cell attachment and the reported advantages of laminin for neural differentiation. The underlying gold coatings were shown to be biocompatible using cell proliferation and live/dead staining assays. Coatings exhibiting stable properties over time under dynamic fluid conditions were developed; indeed, cell attachment and the conductive power of the scaffolds were maintained over 2 weeks of bioreactor operation. These scaffolds are promising research tools for understanding complex neural cell behavior. They have been used to investigate major factors in the physical culture environment that affect nerve cell viability and differentiation, including electrical stimulation, bioreactor hydrodynamic conditions, and combinations of these parameters. The cell and tissue differentiation response was evaluated using DNA quantification, immunocytochemistry, RT-qPCR and functional analyses.

Keywords: bioreactor, electrical stimulation, nerve differentiation, PC12 cells, scaffold

Procedia PDF Downloads 214
131 An Automated Magnetic Dispersive Solid-Phase Extraction Method for Detection of Cocaine in Human Urine

Authors: Feiyu Yang, Chunfang Ni, Rong Wang, Yun Zou, Wenbin Liu, Chenggong Zhang, Fenjin Sun, Chun Wang

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Cocaine is the most frequently used illegal drug globally, with the global annual prevalence of cocaine used ranging from 0.3% to 0.4 % of the adult population aged 15–64 years. Growing consumption trend of abused cocaine and drug crimes are a great concern, therefore urine sample testing has become an important noninvasive sampling whereas cocaine and its metabolites (COCs) are usually present in high concentrations and relatively long detection windows. However, direct analysis of urine samples is not feasible because urine complex medium often causes low sensitivity and selectivity of the determination. On the other hand, presence of low doses of analytes in urine makes an extraction and pretreatment step important before determination. Especially, in gathered taking drug cases, the pretreatment step becomes more tedious and time-consuming. So developing a sensitive, rapid and high-throughput method for detection of COCs in human body is indispensable for law enforcement officers, treatment specialists and health officials. In this work, a new automated magnetic dispersive solid-phase extraction (MDSPE) sampling method followed by high performance liquid chromatography-mass spectrometry (HPLC-MS) was developed for quantitative enrichment of COCs from human urine, using prepared magnetic nanoparticles as absorbants. The nanoparticles were prepared by silanizing magnetic Fe3O4 nanoparticles and modifying them with divinyl benzene and vinyl pyrrolidone, which possesses the ability for specific adsorption of COCs. And this kind of magnetic particle facilitated the pretreatment steps by electromagnetically controlled extraction to achieve full automation. The proposed device significantly improved the sampling preparation efficiency with 32 samples in one batch within 40mins. Optimization of the preparation procedure for the magnetic nanoparticles was explored and the performances of magnetic nanoparticles were characterized by scanning electron microscopy, vibrating sample magnetometer and infrared spectra measurements. Several analytical experimental parameters were studied, including amount of particles, adsorption time, elution solvent, extraction and desorption kinetics, and the verification of the proposed method was accomplished. The limits of detection for the cocaine and cocaine metabolites were 0.09-1.1 ng·mL-1 with recoveries ranging from 75.1 to 105.7%. Compared to traditional sampling method, this method is time-saving and environmentally friendly. It was confirmed that the proposed automated method was a kind of highly effective way for the trace cocaine and cocaine metabolites analyses in human urine.

Keywords: automatic magnetic dispersive solid-phase extraction, cocaine detection, magnetic nanoparticles, urine sample testing

Procedia PDF Downloads 174
130 Cytotoxic Effects of Ag/TiO2 Nanoparticles on the Unicellular Organism Paramecium tetraurelia

Authors: Juan Bernal-Martinez, Zoe Quinones-Jurado, Miguel Waldo-Mendoza, Elias Perez

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Introduction and Objective: Ag-TiO2 nanoparticles (NP) have been characterized as effective antibacterial compounds against E. aureous, E. coli, Salmonella and others. Because these nanoparticles have been used in plastic-food containers, there is a concern about the toxicity of Ag-TiO2 NP for higher organisms from protozoan, invertebrates, and mammals. The objective of this study is to evaluate the cytotoxic effect of Ag-TiO2 NP on the survival and swimming behavior of the unicellular organism Paramecium tetraurelia. Material and Methods: Preparation of metallic silver on TiO2 surface was based on chemical reduction route of AgNO3. Aqueous suspension of TiO2 nanoparticles was preparing by adding 5 g of TiO2 to 250 ml of deionized water and followed by sonication for 10 min. The required amount of AgNO3 solutions was added to TiO2 suspension, maintaining heating and stirring. Silver concentration was 0.5, 1.5, 5.0, 25, 35 and 45 % w/w versus TiO2. Paramecium tetraurelia (Carolina Biological, Cat. # 131560) was used as a biological preparation. It was cultured in artificial culture media made as follows: Stigmasterol 5 mg/ml of ethanol, Caseaminoacids 0.3 gr/lt.; KCl 4mM; CaCl2 1mM; MgCl2 100uM and MOPS 1mM, pH 7.3. This media was inoculated with Enterobacter-sp. Paramecium was concentrated after 24 hours of incubation by centrifugation. The pellet of cells was resuspended in 4.1.1 solution prepared as follows (in mM): KCl, 4 mM; CaCl2, 1mM and Trizma, 1mM; pH 7.3. Transmission electron microscopy (TEM) studies were performed to evaluate the appropriate dispersion and topographic distribution AgNPs deposited on TiO2. The experimental solutions were prepared as follows: 50 mg of Polyvinyhlpirolidone were added to 5 ml of 4.1.1. solution. Then, 50 mg of powder 25-Ag-TiO2 was added, mixing for 10 min and sonicated for 60 min. Survival of Paramecium and possible toxic effects after 25-Ag-TiO2 treatment was observed through an inverted microscope. The Paramecium swimming behavior and possible dead cells were recorded for periods of approximately 20-50 seconds by using a digital USB camera adapted to the microscope. Results and Discussion: TEM micrographs demonstrated the topographic distribution of AgNPs deposited on TiO2. 25Ag-TiO2 NP was efficiently dissolved and dispersed in 4.1.1 solution at concentrations from 0.1, 1 and 10 mg/ml. When Paramecium were treated with 25Ag-TiO2 NP at 100 ug/ml, it was observed that cells started swimming backwards. This backward swimming behavior is the typical avoiding reaction of the ciliate in response to a noxious stimulus. After 10 min of incubation, it was observed that Paramecium stopped swimming backwards and exploited. We can argue that this toxic effect of 25Ag-TiO2 NP is probably due to the calcium influx and calcium accumulation during the long-lasting swimming backwards. Conclusions: Here we have demonstrated that 25Ag-TiO2 NP has a specific toxic effect on an organism higher than bacteria such as the protozoan Paremecium. Probably these toxic phenomena could be expected to be observed in a higher organism such as invertebrates and mammals.

Keywords: Ag-TiO2, calcium permeability, cytotoxicity, paramecium

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129 Melt–Electrospun Polyprophylene Fabrics Functionalized with TiO2 Nanoparticles for Effective Photocatalytic Decolorization

Authors: Z. Karahaliloğlu, C. Hacker, M. Demirbilek, G. Seide, E. B. Denkbaş, T. Gries

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Currently, textile industry has played an important role in world’s economy, especially in developing countries. Dyes and pigments used in textile industry are significant pollutants. Most of theirs are azo dyes that have chromophore (-N=N-) in their structure. There are many methods for removal of the dyes from wastewater such as chemical coagulation, flocculation, precipitation and ozonation. But these methods have numerous disadvantages and alternative methods are needed for wastewater decolorization. Titanium-mediated photodegradation has been used generally due to non-toxic, insoluble, inexpensive, and highly reactive properties of titanium dioxide semiconductor (TiO2). Melt electrospinning is an attractive manufacturing process for thin fiber production through electrospinning from PP (Polyprophylene). PP fibers have been widely used in the filtration due to theirs unique properties such as hydrophobicity, good mechanical strength, chemical resistance and low-cost production. In this study, we aimed to investigate the effect of titanium nanoparticle localization and amine modification on the dye degradation. The applicability of the prepared chemical activated composite and pristine fabrics for a novel treatment of dyeing wastewater were evaluated.In this study, a photocatalyzer material was prepared from nTi (titanium dioxide nanoparticles) and PP by a melt-electrospinning technique. The electrospinning parameters of pristine PP and PP/nTi nanocomposite fabrics were optimized. Before functionalization with nTi, the surface of fabrics was activated by a technique using glutaraldehyde (GA) and polyethyleneimine to promote the dye degredation. Pristine PP and PP/nTi nanocomposite melt-electrospun fabrics were characterized using scanning electron microscopy (SEM) and X-Ray Photon Spectroscopy (XPS). Methyl orange (MO) was used as a model compound for the decolorization experiments. Photocatalytic performance of nTi-loaded pristine and nanocomposite melt-electrospun filters was investigated by varying initial dye concentration 10, 20, 40 mg/L). nTi-PP composite fabrics were successfully processed into a uniform, fibrous network of beadless fibers with diameters of 800±0.4 nm. The process parameters were determined as a voltage of 30 kV, a working distance of 5 cm, a temperature of the thermocouple and hotcoil of 260–300 ºC and a flow rate of 0.07 mL/h. SEM results indicated that TiO2 nanoparticles were deposited uniformly on the nanofibers and XPS results confirmed the presence of titanium nanoparticles and generation of amine groups after modification. According to photocatalytic decolarization test results, nTi-loaded GA-treated pristine or nTi-PP nanocomposite fabric filtern have superior properties, especially over 90% decolorization efficiency at GA-treated pristine and nTi-PP composite PP fabrics. In this work, as a photocatalyzer for wastewater treatment, surface functionalized with nTi melt-electrospun fabrics from PP were prepared. Results showed melt-electrospun nTi-loaded GA-tretaed composite or pristine PP fabrics have a great potential for use as a photocatalytic filter to decolorization of wastewater and thus, requires further investigation.

Keywords: titanium oxide nanoparticles, polyprophylene, melt-electrospinning

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128 Biodsorption as an Efficient Technology for the Removal of Phosphate, Nitrate and Sulphate Anions in Industrial Wastewater

Authors: Angel Villabona-Ortíz, Candelaria Tejada-Tovar, Andrea Viera-Devoz

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Wastewater treatment is an issue of vital importance in these times where the impacts of human activities are most evident, which have become essential tasks for the normal functioning of society. However, they put entire ecosystems at risk by time destroying the possibility of sustainable development. Various conventional technologies are used to remove pollutants from water. Agroindustrial waste is the product with the potential to be used as a renewable raw material for the production of energy and chemical products, and their use is beneficial since products with added value are generated from materials that were not used before. Considering the benefits that the use of residual biomass brings, this project proposes the use of agro-industrial residues from corn crops for the production of natural adsorbents whose purpose is aimed at the remediation of contaminated water bodies with large loads of nutrients. The adsorption capacity of two biomaterials obtained from the processing of corn stalks was evaluated by batch system tests. Biochar impregnated with sulfuric acid and thermally activated was synthesized. On the other hand, the cellulose was extracted from the corn stalks and chemically modified with cetyltrimethylammonium chloride in order to quaternize the surface of the adsorbent. The adsorbents obtained were characterized by thermogravimetric analysis (TGA), scanning electron microscopy (SEM), infrared spectrometry with Fourier Transform (FTIR), analysis by Brunauer, Emmett and Teller method (BET) and X-ray Diffraction analysis ( XRD), which showed favorable characteristics for the cellulose extraction process. Higher adsorption capacities of the nutrients were obtained with the use of biochar, with phosphate being the anion with the best removal percentages. The effect of the initial adsorbate concentration was evaluated, with which it was shown that the Freundlich isotherm better describes the adsorption process in most systems. The adsorbent-phosphate / nitrate systems fit better to the Pseudo Primer Order kinetic model, while the adsorbent-sulfate systems showed a better fit to the Pseudo second-order model, which indicates that there are both physical and chemical interactions in the process. Multicomponent adsorption tests revealed that phosphate anions have a higher affinity for both adsorbents. On the other hand, the thermodynamic parameters standard enthalpy (ΔH °) and standard entropy (ΔS °) with negative results indicate the exothermic nature of the process, whereas the ascending values of standard Gibbs free energy (ΔG °). The adsorption process of anions with biocarbon and modified cellulose is spontaneous and exothermic. The use of the evaluated biomateriles is recommended for the treatment of industrial effluents contaminated with sulfate, nitrate and phosphate anions.

Keywords: adsorption, biochar, modified cellulose, corn stalks

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127 The Effect of Nanocomposite on the Release of Imipenem on Bacteria Causing Infections with Implants

Authors: Mohammad Hossein Pazandeh, Monir Doudi, Sona Rostampour Yasouri

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—Results The prudent administration of antibiotics aims to avoid the side effects and the microbes' resistance to antibiotics. An approach developing methods of local administration of antibiotics is especially required for localized infections caused by bacterial colonization of medical devices or implant materials. Among the wide variety of materials used as drug delivery systems, bioactive glasses (BG) have large utilization in regenerative medicine . firstly, the production of bioactive glass/nickel oxide/tin dioxide nanocomposite using sol-gel method, and then, the controlled release of imipenem from the double metal oxide/bioactive glass nanocomposite, and finally, the investigation of the antibacterial property of the nanocomposite. against a number of implant-related infectious agents. In this study, BG/SnO2 and BG/NiO single systema with different metal oxide present and BG/NiO/SnO2 nanocomposites were synthesized by sol-gel as drug carriers for tetracycline and imepinem. These two antibiotics were widely used for osteomyelitis because of its favorable penetration and bactericidal effect on all the probable osteomyelitis pathogens. The antibacterial activity of synthesized samples were evaluated against Staphylococcus aureus, Escherichia coli, Pseudomonas aeruginosa as bacteria model using disk diffusion method. The BG modification using metal oxides results to antibacterial property of samples containing metal oxide with highest efficiency for nancomposite. bioactivity of all samples was assessed by determining the surface morphology, structural and composition changes using scanning electron microscopy (SEM), FTIR and X-ray diffraction (XRD) spectroscopy, respectively, after soaking in simulated body fluid (SBF) for 28 days. The hydroxyapatite formation was clearly observed as a bioactivity measurement. Then, BG nanocomposite sample was loaded using two antibiotics, separately and their release profiles were studied. The BG nancomposite sample was shown the slow and continuous drug releasing for a period of 72 hours which is desirable for a drug delivery system. The loaded antibiotic nanocomposite sample retaining antibacterial property and showing inactivation effect against bacteria under test. The modified bioactive glass forming hydroxyapatite with controlled release drug and effective against bacterial infections can be introduced as scaffolds for bone implants after clinical trials for biomedical applications . Considering the formation of biofilm by infectious bacteria after sticking on the surfaces of implants, medical devices, etc. Also, considering the complications of traditional methods, solving the problems caused by the above-mentioned microorganisms in technical and biomedical industries was one of the necessities of this research.

Keywords: antibacterial, bioglass, drug delivery system, sol- gel

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126 Bioflavonoids Derived from Mandarin Processing Wastes: Functional Hydrogels as a Sustainable Food Systems

Authors: Niharika Kaushal, Minni Singh

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Fruit crops are widely cultivated throughout the World, with citrus being one of the most common. Mandarins, oranges, grapefruits, lemons, and limes are among the most frequently grown varieties. Citrus cultivars are industrially processed into juice, resulting in approx. 25-40% by wt. of biomass in the form of peels and seeds, generally considered as waste. In consequence, a significant amount of this nutraceutical-enriched biomass goes to waste, which, if utilized wisely, could revolutionize the functional food industry, as this biomass possesses a wide range of bioactive compounds, mainly within the class of polyphenols and terpenoids, making them an abundant source of functional bioactive. Mandarin is a potential source of bioflavonoids with putative antioxidative properties, and its potential application for developing value-added products is obvious. In this study, ‘kinnow’ mandarin (Citrus nobilis X Citrus deliciosa) biomass was studied for its flavonoid profile. For this, dried and pulverized peels were subjected to green and sustainable extraction techniques, namely, supercritical fluid extraction carried out under conditions pressure: 330 bar, temperature: 40 ̊ C and co-solvent: 10% ethanol. The obtained extract was observed to contain 47.3±1.06 mg/ml rutin equivalents as total flavonoids. Mass spectral analysis revealed the prevalence of polymethoxyflavones (PMFs), chiefly tangeretin and nobiletin. Furthermore, the antioxidant potential was analyzed by the 2,2-diphenyl-1-picrylhydrazyl (DPPH) method, which was estimated to be at an IC₅₀ of 0.55μg/ml. The pre-systemic metabolism of flavonoids limits their functionality, as was observed in this study through in vitro gastrointestinal studies where nearly 50.0% of the flavonoids were degraded within 2 hours of gastric exposure. We proposed nanoencapsulation as a means to overcome this problem, and flavonoids-laden polylactic-co-glycolic acid (PLGA) nano encapsulates were bioengineered using solvent evaporation method, and these were furnished to a particle size between 200-250nm, which exhibited protection of flavonoids in the gastric environment, allowing only 20% to be released in 2h. A further step involved impregnating the nano encapsulates within alginate hydrogels which were fabricated by ionic cross-linking, which would act as delivery vehicles within the gastrointestinal (GI) tract. As a result, 100% protection was achieved from the pre-systemic release of bioflavonoids. These alginate hydrogels had key significant features, i.e., less porosity of nearly 20.0%, and Cryo-SEM (Cryo-scanning electron microscopy) images of the composite corroborate the packing ability of the alginate hydrogel. As a result of this work, it is concluded that the waste can be used to develop functional biomaterials while retaining the functionality of the bioactive itself.

Keywords: bioflavonoids, gastrointestinal, hydrogels, mandarins

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125 p-Type Multilayer MoS₂ Enabled by Plasma Doping for Ultraviolet Photodetectors Application

Authors: Xiao-Mei Zhang, Sian-Hong Tseng, Ming-Yen Lu

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Two-dimensional (2D) transition metal dichalcogenides (TMDCs), such as MoS₂, have attracted considerable attention owing to the unique optical and electronic properties related to its 2D ultrathin atomic layer structure. MoS₂ is becoming prevalent in post-silicon digital electronics and in highly efficient optoelectronics due to its extremely low thickness and its tunable band gap (Eg = 1-2 eV). For low-power, high-performance complementary logic applications, both p- and n-type MoS₂ FETs (NFETs and PFETs) must be developed. NFETs with an electron accumulation channel can be obtained using unintentionally doped n-type MoS₂. However, the fabrication of MoS₂ FETs with complementary p-type characteristics is challenging due to the significant difficulty of injecting holes into its inversion channel. Plasma treatments with different species (including CF₄, SF₆, O₂, and CHF₃) have also been found to achieve the desired property modifications of MoS₂. In this work, we demonstrated a p-type multilayer MoS₂ enabled by selective-area doping using CHF₃ plasma treatment. Compared with single layer MoS₂, multilayer MoS₂ can carry a higher drive current due to its lower bandgap and multiple conduction channels. Moreover, it has three times the density of states at its minimum conduction band. Large-area growth of MoS₂ films on 300 nm thick SiO₂/Si substrate is carried out by thermal decomposition of ammonium tetrathiomolybdate, (NH₄)₂MoS₄, in a tube furnace. A two-step annealing process is conducted to synthesize MoS₂ films. For the first step, the temperature is set to 280 °C for 30 min in an N₂ rich environment at 1.8 Torr. This is done to transform (NH₄)₂MoS₄ into MoS₃. To further reduce MoS₃ into MoS₂, the second step of annealing is performed. For the second step, the temperature is set to 750 °C for 30 min in a reducing atmosphere consisting of 90% Ar and 10% H₂ at 1.8 Torr. The grown MoS₂ films are subjected to out-of-plane doping by CHF₃ plasma treatment using a Dry-etching system (ULVAC original NLD-570). The radiofrequency power of this dry-etching system is set to 100 W and the pressure is set to 7.5 mTorr. The final thickness of the treated samples is obtained by etching for 30 s. Back-gated MoS₂ PFETs were presented with an on/off current ratio in the order of 10³ and a field-effect mobility of 65.2 cm²V⁻¹s⁻¹. The MoS₂ PFETs photodetector exhibited ultraviolet (UV) photodetection capability with a rapid response time of 37 ms and exhibited modulation of the generated photocurrent by back-gate voltage. This work suggests the potential application of the mild plasma-doped p-type multilayer MoS₂ in UV photodetectors for environmental monitoring, human health monitoring, and biological analysis.

Keywords: photodetection, p-type doping, multilayers, MoS₂

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124 Comparison of Gestational Diabetes Influence on the Ultrastructure of Rectus Abdominis Muscle in Women and Rats

Authors: Giovana Vesentini, Fernanda Piculo, Gabriela Marini, Debora Damasceno, Angelica Barbosa, Selma Martheus, Marilza Rudge

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Problem statement: Skeletal muscle is highly adaptable, muscle fiber composition and size can respond to a variety of stimuli, such physiologic, as pregnancy, and metabolic abnormalities, as Diabetes mellitus. This study aimed to analyze the effects of pregnancy-associated diabetes on the rectus abdominis muscle (RA), and to compare this changes in rats and women. Methods: Female Wistar rats were maintained under controlled conditions and distributed in Pregnant (P) and Long-term mild pregnant diabetic (LTMd) (n=3 r/group). Diabetes in rats was induced by streptozotocin (100mg/Kg, sc) on the first day of life, for a hyperglycemic state between 120-300 mg/dL in adult life. Female rats were mated overnight, at day 21 of pregnancy were anesthetized, and killed for the harvesting of maternal RA. Pregnant women who attended the Diabetes Prenatal Care Clinic of Botucatu Medical School were distributed in Pregnant non-diabetic (Pnd) and Gestational Diabetic (GDM) (n=3 w/group). The diagnosis of GDM was established according to ADA’s criteria (2016). The harvesting of RA was during the cesarean section. Transversal cross-sections of the RA of both women and rats were analyzed by transmission electron microscopy. All procedures were approved by the Ethics Committee on Animal Experiments of the Botucatu Medical School (Protocol Number 1003/2013) and by the Botucatu Medical School Ethical Committee for Human Research in Medical Sciences (CAAE: 41570815.0.0000.5411). Results: The photomicrographs of the RA of rats revealed disorganized Z lines, thinning sarcomeres, and a usual quantity of intermyofibrillar mitochondria in the P group. The LTMd group showed swollen sarcoplasmic reticulum, dilated T tubes and areas with sarcomere disruption. The ultrastructural analysis of Pnd non-diabetic women in the RA showed well-organized myofibrils forming intact sarcomeres, organized Z lines and a normal distribution of intermyofibrillar mitochondria. The GDM group revealed increase in intermyofibrillar mitochondria, areas with sarcomere disruption and increased lipid droplets. Conclusion: Pregnancy and diabetes induce adaptations in the ultrastructure of the rectus abdominis muscle for both women and rats, changing the architectural design of these tissues. However, in rats these changes are more severe maybe because, besides the high blood glucose levels, the quadrupedal animal may suffer an excessive mechanical tension during pregnancy by gravity. Probably, these findings may suggest that these alterations are a risk factor that contributes to the development of muscle dysfunction in women with GDM and may motivate treatment strategies in these patients.

Keywords: gestational diabetes, muscle dysfunction, pregnancy, rectus abdominis

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123 Development of 3D Printed Natural Fiber Reinforced Composite Scaffolds for Maxillofacial Reconstruction

Authors: Sri Sai Ramya Bojedla, Falguni Pati

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Nature provides the best of solutions to humans. One such incredible gift to regenerative medicine is silk. The literature has publicized a long appreciation for silk owing to its incredible physical and biological assets. Its bioactive nature, unique mechanical strength, and processing flexibility make us curious to explore further to apply it in the clinics for the welfare of mankind. In this study, Antheraea mylitta and Bombyx mori silk fibroin microfibers are developed by two economical and straightforward steps via degumming and hydrolysis for the first time, and a bioactive composite is manufactured by mixing silk fibroin microfibers at various concentrations with polycaprolactone (PCL), a biocompatible, aliphatic semi-crystalline synthetic polymer. Reconstructive surgery in any part of the body except for the maxillofacial region deals with replacing its function. But answering both the aesthetics and function is of utmost importance when it comes to facial reconstruction as it plays a critical role in the psychological and social well-being of the patient. The main concern in developing adequate bone graft substitutes or a scaffold is the noteworthy variation in each patient's bone anatomy. Additionally, the anatomical shape and size will vary based on the type of defect. The advent of additive manufacturing (AM) or 3D printing techniques to bone tissue engineering has facilitated overcoming many of the restraints of conventional fabrication techniques. The acquired patient's CT data is converted into a stereolithographic (STL)-file which is further utilized by the 3D printer to create a 3D scaffold structure in an interconnected layer-by-layer fashion. This study aims to address the limitations of currently available materials and fabrication technologies and develop a customized biomaterial implant via 3D printing technology to reconstruct complex form, function, and aesthetics of the facial anatomy. These composite scaffolds underwent structural and mechanical characterization. Atomic force microscopic (AFM) and field emission scanning electron microscopic (FESEM) images showed the uniform dispersion of the silk fibroin microfibers in the PCL matrix. With the addition of silk, there is improvement in the compressive strength of the hybrid scaffolds. The scaffolds with Antheraea mylitta silk revealed higher compressive modulus than that of Bombyx mori silk. The above results of PCL-silk scaffolds strongly recommend their utilization in bone regenerative applications. Successful completion of this research will provide a great weapon in the maxillofacial reconstructive armamentarium.

Keywords: compressive modulus, 3d printing, maxillofacial reconstruction, natural fiber reinforced composites, silk fibroin microfibers

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122 The Role of Piceatannol in Counteracting Glyceraldehyde-3-Phosphate Dehydrogenase Aggregation and Nuclear Translocation

Authors: Joanna Gerszon, Aleksandra Rodacka

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In the pathogenesis of neurodegenerative diseases such as Alzheimer's disease and Parkinson's disease, protein and peptide aggregation processes play a vital role in contributing to the formation of intracellular and extracellular protein deposits. One of the major components of these deposits is the oxidatively modified glyceraldehyde-3-phosphate dehydrogenase (GAPDH). Therefore, the purpose of this research was to answer the question whether piceatannol, a stilbene derivative, counteracts and/or slows down oxidative stress-induced GAPDH aggregation. The study also aimed to determine if this natural occurring compound prevents unfavorable nuclear translocation of GAPDH in hippocampal cells. The isothermal titration calorimetry (ITC) analysis indicated that one molecule of GAPDH can bind up to 8 molecules of piceatannol (7.3 ± 0.9). As a consequence of piceatannol binding to the enzyme, the loss of activity was observed. Parallel with GAPDH inactivation the changes in zeta potential, and loss of free thiol groups were noted. Nevertheless, the ligand-protein binding does not influence the secondary structure of the GAPDH. Precise molecular docking analysis of the interactions inside the active center allowed to presume that these effects are due to piceatannol ability to assemble a covalent binding with nucleophilic cysteine residue (Cys149) which is directly involved in the catalytic reaction. Molecular docking also showed that simultaneously 11 molecules of ligand can be bound to dehydrogenase. Taking into consideration obtained data, the influence of piceatannol on level of GAPDH aggregation induced by excessive oxidative stress was examined. The applied methods (thioflavin-T binding-dependent fluorescence as well as microscopy methods - transmission electron microscopy, Congo Red staining) revealed that piceatannol significantly diminishes level of GAPDH aggregation. Finally, studies involving cellular model (Western blot analyses of nuclear and cytosolic fractions and confocal microscopy) indicated that piceatannol-GAPDH binding prevents GAPDH from nuclear translocation induced by excessive oxidative stress in hippocampal cells. In consequence, it counteracts cell apoptosis. These studies demonstrate that by binding with GAPDH, piceatannol blocks cysteine residue and counteracts its oxidative modifications, that induce oligomerization and GAPDH aggregation as well as it prevents hippocampal cells from apoptosis by retaining GAPDH in the cytoplasm. All these findings provide a new insight into the role of piceatannol interaction with GAPDH and present a potential therapeutic strategy for some neurological disorders related to GAPDH aggregation. This work was supported by the by National Science Centre, Poland (grant number 2017/25/N/NZ1/02849).

Keywords: glyceraldehyde-3-phosphate dehydrogenase, neurodegenerative disease, neuroprotection, piceatannol, protein aggregation

Procedia PDF Downloads 138
121 Fractional, Component and Morphological Composition of Ambient Air Dust in the Areas of Mining Industry

Authors: S.V. Kleyn, S.Yu. Zagorodnov, А.А. Kokoulina

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Technogenic emissions of the mining and processing complex are characterized by a high content of chemical components and solid dust particles. However, each industrial enterprise and the surrounding area have features that require refinement and parameterization. Numerous studies have shown the negative impact of fine dust PM10 and PM2.5 on the health, as well as the possibility of toxic components absorption, including heavy metals by dust particles. The target of the study was the quantitative assessment of the fractional and particle size composition of ambient air dust in the area of impact by primary magnesium production complex. Also, we tried to describe the morphology features of dust particles. Study methods. To identify the dust emission sources, the analysis of the production process has been carried out. The particulate composition of the emissions was measured using laser particle analyzer Microtrac S3500 (covered range of particle size is 20 nm to 2000 km). Particle morphology and the component composition were established by electron microscopy by scanning microscope of high resolution (magnification rate - 5 to 300 000 times) with X-ray fluorescence device S3400N ‘HITACHI’. The chemical composition was identified by X-ray analysis of the samples using an X-ray diffractometer XRD-700 ‘Shimadzu’. Determination of the dust pollution level was carried out using model calculations of emissions in the atmosphere dispersion. The calculations were verified by instrumental studies. Results of the study. The results demonstrated that the dust emissions of different technical processes are heterogeneous and fractional structure is complicated. The percentage of particle sizes up to 2.5 micrometres inclusive was ranged from 0.00 to 56.70%; particle sizes less than 10 microns inclusive – 0.00 - 85.60%; particle sizes greater than 10 microns - 14.40% -100.00%. During microscopy, the presence of nanoscale size particles has been detected. Studied dust particles are round, irregular, cubic and integral shapes. The composition of the dust includes magnesium, sodium, potassium, calcium, iron, chlorine. On the base of obtained results, it was performed the model calculations of dust emissions dispersion and establishment of the areas of fine dust РМ 10 and РМ 2.5 distribution. It was found that the dust emissions of fine powder fractions PM10 and PM2.5 are dispersed over large distances and beyond the border of the industrial site of the enterprise. The population living near the enterprise is exposed to the risk of diseases associated with dust exposure. Data are transferred to the economic entity to make decisions on the measures to minimize the risks. Exposure and risks indicators on the health are used to provide named patient health and preventive care to the citizens living in the area of negative impact of the facility.

Keywords: dust emissions, еxposure assessment, PM 10, PM 2.5

Procedia PDF Downloads 236
120 Bioresorbable Medicament-Eluting Grommet Tube for Otitis Media with Effusion

Authors: Chee Wee Gan, Anthony Herr Cheun Ng, Yee Shan Wong, Subbu Venkatraman, Lynne Hsueh Yee Lim

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Otitis media with effusion (OME) is the leading cause of hearing loss in children worldwide. Surgery to insert grommet tube into the eardrum is usually indicated for OME unresponsive to antimicrobial therapy. It is the most common surgery for children. However, current commercially available grommet tubes are non-bioresorbable, not drug-treated, with unpredictable duration of retention on the eardrum to ventilate middle ear. Their functionality is impaired when clogged or chronically infected, requiring additional surgery to remove/reinsert grommet tubes. We envisaged that a novel fully bioresorbable grommet tube with sustained antibiotic release technology could address these drawbacks. In this study, drug-loaded bioresorbable poly(L-lactide-co-ε-caprolactone)(PLC) copolymer grommet tubes were fabricated by microinjection moulding technique. In vitro drug release and degradation model of PLC tubes were studied. Antibacterial property was evaluated by incubating PLC tubes with P. aeruginosa broth. Surface morphology was analyzed using scanning electron microscopy. A preliminary animal study was conducted using guinea pigs as an in vivo model to evaluate PLC tubes with and without drug, with commercial Mini Shah grommet tube as comparison. Our in vitro data showed sustained drug release over 3 months. All PLC tubes revealed exponential degradation profiles over time. Modeling predicted loss of tube functionality in water to be approximately 14 weeks and 17 weeks for PLC with and without drug, respectively. Generally, PLC tubes had less bacteria adherence, which were attributed to the much smoother tube surfaces compared to Mini Shah. Antibiotic from PLC tube further made bacteria adherence on surface negligible. They showed neither inflammation nor otorrhea after 18 weeks post-insertion in the eardrums of guinea pigs, but had demonstrated severe degree of bioresorption. Histology confirmed the new PLC tubes were biocompatible. Analyses on the PLC tubes in the eardrums showed bioresorption profiles close to our in vitro degradation models. The bioresorbable antibiotic-loaded grommet tubes showed good predictability in functionality. The smooth surface and sustained release technology reduced the risk of tube infection. Tube functional duration of 18 weeks allowed sufficient ventilation period to treat OME. Our ongoing studies include modifying the surface properties with protein coating, optimizing the drug dosage in the tubes to enhance their performances, evaluating their functional outcome on hearing after full resoption of grommet tube and healing of eardrums, and developing animal model with OME to further validate our in vitro models.

Keywords: bioresorbable polymer, drug release, grommet tube, guinea pigs, otitis media with effusion

Procedia PDF Downloads 426
119 Effect of Ti, Nb, and Zr Additives on Biocompatibility of Injection Molded 316L Stainless Steel for Biomedical Applications

Authors: Busra Gundede, Ozal Mutlu, Nagihan Gulsoy

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Background: Over the years, material research has led to the development of numerous metals and alloys for using in biomedical applications. One of the major tasks of biomaterial research is the functionalization of the material surface to improve the biocompatibility according to a specific application. 316L and 316L alloys are excellent for various bio-applications. This research was investigated the effect of titanium (Ti), niobium (Nb), and zirconium (Zr) additives on injection molded austenitic grade 316L stainless steels in vitro biocompatibility. For this purpose, cytotoxic tests were performed to evaluate the potential biocompatibility of the specimens. Materials and Methods: 3T3 fibroblast were cultivated in DMEM supplemented with 10% fetal bovine serum and %1 penicillin-streptomycin at 37°C with 5% CO2 and 95%humidity. Trypsin/EDTA solution was used to remove cells from the culture flask. Cells were reseeded at a density of 1×105cell in 25T flasks. The medium change took place every 3 days. The trypan blue assay was used to determine cell viability. Cell viability is calculated as the number of viable cells divided by the total number of cells within the grids on the cell counter machine counted the number of blue staining cells and the number of total cells. Cell viability should be at least 95% for healthy log-phase cultures. MTT assay was assessed for 96-hours. Cells were cultivated in 6-well flask within 5 ml DMEM and incubated as same conditions. 0,5mg/ml MTT was added for 4-hours and then acid-isoprohanol was added for solubilize to formazan crystals. Cell morphology after 96h was investigated by SEM. The medium was removed, samples were washed with 0.15 M PBS buffer and fixed for 12h at 4- 8°C with %2,5 gluteraldehyte. Samples were treated with 1% osmium tetroxide. Samples were then dehydrated and dried, mounted on appropriate stubs with colloidal silver and sputter-coated with gold. Images were collected using a scanning electron microscope. ROS assay is a cell viability test for in vitro studies. Cells were grown for 96h, ROS solution added on cells in 6 well plate flask and incubated for 1h. Fluorescence signal indicates ROS generation by cells. Results: Trypan Blue exclusion assay results were 96%, 92%, 95%, 90%, 91% for negative control group, 316L, 316L-Ti, 316L-Nb and 316L-Zr, respectively. Results were found nearly similar to each other when compared with control group. Cell viability from MTT analysis was found to be 100%, 108%, 103%, 107%, and 105% for the control group, 316L, 316L-Ti, 316L-Nb and 316L-Zr, respectively. Fluorescence microscopy analysis indicated that all test groups were same as the control group in ROS assay. SEM images demonstrated that the attachment of 3T3 cells on biomaterials. Conclusion: We, therefore, concluded that Ti, Nb and Zr additives improved physical properties of 316L stainless. In our in vitro experiments showed that these new additives did not modify the cytocompatibility of stainless steel and these additives on 316L might be useful for biomedical applications.

Keywords: 316L stainles steel, biocompatibility, cell culture, Ti, Nb, Zr

Procedia PDF Downloads 487
118 Recycling the Lanthanides from Permanent Magnets by Electrochemistry in Ionic Liquid

Authors: Celine Bonnaud, Isabelle Billard, Nicolas Papaiconomou, Eric Chainet

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Thanks to their high magnetization and low mass, permanent magnets (NdFeB and SmCo) have quickly became essential for new energies (wind turbines, electrical vehicles…). They contain large quantities of neodymium, samarium and dysprosium, that have been recently classified as critical elements and that therefore need to be recycled. Electrochemical processes including electrodissolution followed by electrodeposition are an elegant and environmentally friendly solution for the recycling of such lanthanides contained in permanent magnets. However, electrochemistry of the lanthanides is a real challenge as their standard potentials are highly negative (around -2.5V vs ENH). Consequently, non-aqueous solvents are required. Ionic liquids (IL) are novel electrolytes exhibiting physico-chemical properties that fulfill many requirements of the sustainable chemistry principles, such as extremely low volatility and non-flammability. Furthermore, their chemical and electrochemical properties (solvation of metallic ions, large electrochemical windows, etc.) render them very attractive media to implement alternative and sustainable processes in view of integrated processes. All experiments that will be presented were carried out using butyl-methylpyrrolidinium bis(trifluoromethanesulfonyl)imide. Linear sweep, cyclic voltammetry and potentiostatic electrochemical techniques were used. The reliability of electrochemical experiments, performed without glove box, for the classic three electrodes cell used in this study has been assessed. Deposits were obtained by chronoamperometry and were characterized by scanning electron microscopy and energy-dispersive X-ray spectroscopy. The IL cathodic behavior under different constraints (argon, nitrogen, oxygen atmosphere or water content) and using several electrode materials (Pt, Au, GC) shows that with argon gas flow and gold as a working electrode, the cathodic potential can reach the maximum value of -3V vs Fc+/Fc; thus allowing a possible reduction of lanthanides. On a gold working electrode, the reduction potential of samarium and neodymium was found to be -1.8V vs Fc+/Fc while that of dysprosium was -2.1V vs Fc+/Fc. The individual deposits obtained were found to be porous and presented some significant amounts of C, N, F, S and O atoms. Selective deposition of neodymium in presence of dysprosium was also studied and will be discussed. Next, metallic Sm, Nd and Dy electrodes were used in replacement of Au, which induced changes in the reduction potential values and the deposit structures of lanthanides. The individual corrosion potentials were also measured in order to determine the parameters influencing the electrodissolution of these metals. Finally, a full recycling process was investigated. Electrodissolution of a real permanent magnet sample was monitored kinetically. Then, the sequential electrodeposition of all lanthanides contained in the IL was investigated. Yields, quality of the deposits and consumption of chemicals will be discussed in depth, in view of the industrial feasibility of this process for real permanent magnets recycling.

Keywords: electrodeposition, electrodissolution, ionic liquids, lanthanides, rcycling

Procedia PDF Downloads 243
117 Performance Improvement of Piston Engine in Aeronautics by Means of Additive Manufacturing Technologies

Authors: G. Andreutti, G. Saccone, D. Lucariello, C. Pirozzi, S. Franchitti, R. Borrelli, C. Toscano, P. Caso, G. Ferraro, C. Pascarella

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The reduction of greenhouse gases and pollution emissions is a worldwide environmental issue. The amount of CO₂ released by an aircraft is associated with the amount of fuel burned, so the improvement of engine thermo-mechanical efficiency and specific fuel consumption is a significant technological driver for aviation. Moreover, with the prospect that avgas will be phased out, an engine able to use more available and cheaper fuels is an evident advantage. An advanced aeronautical Diesel engine, because of its high efficiency and ability to use widely available and low-cost jet and diesel fuels, is a promising solution to achieve a more fuel-efficient aircraft. On the other hand, a Diesel engine has generally a higher overall weight, if compared with a gasoline one of same power performances. Fixing the MTOW, Max Take-Off Weight, and the operational payload, this extra-weight reduces the aircraft fuel fraction, partially vinifying the associated benefits. Therefore, an effort in weight saving manufacturing technologies is likely desirable. In this work, in order to achieve the mentioned goals, innovative Electron Beam Melting – EBM, Additive Manufacturing – AM technologies were applied to a two-stroke, common rail, GF56 Diesel engine, developed by the CMD Company for aeronautic applications. For this purpose, a consortium of academic, research and industrial partners, including CMD Company, Italian Aerospace Research Centre – CIRA, University of Naples Federico II and the University of Salerno carried out a technological project, funded by the Italian Minister of Education and Research – MIUR. The project aimed to optimize the baseline engine in order to improve its performance and increase its airworthiness features. This project was focused on the definition, design, development, and application of enabling technologies for performance improvement of GF56. Weight saving of this engine was pursued through the application of EBM-AM technologies and in particular using Arcam AB A2X machine, available at CIRA. The 3D printer processes titanium alloy micro-powders and it was employed to realize new connecting rods of the GF56 engine with an additive-oriented design approach. After a preliminary investigation of EBM process parameters and a thermo-mechanical characterization of titanium alloy samples, additive manufactured, innovative connecting rods were fabricated. These engine elements were structurally verified, topologically optimized, 3D printed and suitably post-processed. Finally, the overall performance improvement, on a typical General Aviation aircraft, was estimated, substituting the conventional engine with the optimized GF56 propulsion system.

Keywords: aeronautic propulsion, additive manufacturing, performance improvement, weight saving, piston engine

Procedia PDF Downloads 114
116 Optimization of Cobalt Oxide Conversion to Co-Based Metal-Organic Frameworks

Authors: Aleksander Ejsmont, Stefan Wuttke, Joanna Goscianska

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Gaining control over particle shape, size and crystallinity is an ongoing challenge for many materials. Especially metalorganic frameworks (MOFs) are recently widely studied. Besides their remarkable porosity and interesting topologies, morphology has proven to be a significant feature. It can affect the further material application. Thus seeking new approaches that enable MOF morphology modulation is important. MOFs are reticular structures, where building blocks are made up of organic linkers and metallic nodes. The most common strategy of ensuring metal source is using salts, which usually exhibit high solubility and hinder morphology control. However, there has been a growing interest in using metal oxides as structure-directing agents towards MOFs due to their very low solubility and shape preservation. Metal oxides can be treated as a metal reservoir during MOF synthesis. Up to now, reports in which receiving MOFs from metal oxides mostly present ZnO conversion to ZIF-8. However, there are other oxides, for instance, Co₃O₄, which often is overlooked due to their structural stability and insolubility in aqueous solutions. Cobalt-based materials are famed for catalytic activity. Therefore the development of their efficient synthesis is worth attention. In the presented work, an optimized Co₃O₄transition to Co-MOFviaa solvothermal approach was proposed. The starting point of the research was the synthesis of Co₃O₄ flower petals and needles under hydrothermal conditions using different cobalt salts (e.g., cobalt(II) chloride and cobalt(II) nitrate), in the presence of urea, and hexadecyltrimethylammonium bromide (CTAB) surfactant as a capping agent. After receiving cobalt hydroxide, the calcination process was performed at various temperatures (300–500 °C). Then cobalt oxides as a source of cobalt cations were subjected to reaction with trimesic acid in solvothermal environment and temperature of 120 °C leading to Co-MOF fabrication. The solution maintained in the system was a mixture of water, dimethylformamide, and ethanol, with the addition of strong acids (HF and HNO₃). To establish how solvents affect metal oxide conversion, several different solvent ratios were also applied. The materials received were characterized with analytical techniques, including X-ray powder diffraction, energy dispersive spectroscopy,low-temperature nitrogen adsorption/desorption, scanning, and transmission electron microscopy. It was confirmed that the synthetic routes have led to the formation of Co₃O₄ and Co-based MOF varied in shape and size of particles. The diffractograms showed receiving crystalline phase for Co₃O₄, and also for Co-MOF. The Co₃O₄ obtained from nitrates and with using low-temperature calcination resulted in smaller particles. The study indicated that cobalt oxide particles of different size influence the efficiency of conversion and morphology of Co-MOF. The highest conversion was achieved using metal oxides with small crystallites.

Keywords: Co-MOF, solvothermal synthesis, morphology control, core-shell

Procedia PDF Downloads 126
115 Processing of Flexible Dielectric Nanocomposites Using Nanocellulose and Recycled Alum Sludge for Wearable Technology Applications

Authors: D. Sun, L. Saw, A. Onyianta, D. O’Rourke, Z. Lu, C. See, C. Wilson, C. Popescu, M. Dorris

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With the rapid development of wearable technology (e.g., smartwatch, activity trackers and health monitor devices), flexible dielectric materials with environmental-friendly, low-cost and high-energy efficiency characteristics are in increasing demand. In this work, a flexible dielectric nanocomposite was processed by incorporating two components: cellulose nanofibrils and alum sludge in a polymer matrix. The two components were used in the reinforcement phase as well as for enhancing the dielectric properties; they were processed using waste materials that would otherwise be disposed to landfills. Alum sludge is a by-product of the water treatment process in which aluminum sulfate is prevalently used as the primary coagulant. According to the data from a project partner-Scottish Water: there are approximately 10k tons of alum sludge generated as a waste from the water treatment work to be landfilled every year in Scotland. The industry has been facing escalating financial and environmental pressure to develop more sustainable strategies to deal with alum sludge wastes. In the available literature, some work on reusing alum sludge has been reported (e.g., aluminum recovery or agriculture and land reclamation). However, little work can be found in applying it to processing energy materials (e.g., dielectrics) for enhanced energy density and efficiency. The alum sludge was collected directly from a water treatment plant of Scottish Water and heat-treated and refined before being used in preparing composites. Cellulose nanofibrils were derived from water hyacinth, an invasive aquatic weed that causes significant ecological issues in tropical regions. The harvested water hyacinth was dried and processed using a cost-effective method, including a chemical extraction followed by a homogenization process in order to extract cellulose nanofibrils. Biodegradable elastomer polydimethylsiloxane (PDMS) was used as the polymer matrix and the nanocomposites were processed by casting raw materials in Petri dishes. The processed composites were characterized using various methods, including scanning electron microscopy (SEM), rheological analysis, thermogravimetric and X-ray diffraction analysis. The SEM result showed that cellulose nanofibrils of approximately 20nm in diameter and 100nm in length were obtained and the alum sludge particles were of approximately 200um in diameters. The TGA/DSC analysis result showed that a weight loss of up to 48% can be seen in the raw material of alum sludge and its crystallization process has been started at approximately 800°C. This observation coincides with the XRD result. Other experiments also showed that the composites exhibit comprehensive mechanical and dielectric performances. This work depicts that it is a sustainable practice of reusing such waste materials in preparing flexible, lightweight and miniature dielectric materials for wearable technology applications.

Keywords: cellulose, biodegradable, sustainable, alum sludge, nanocomposite, wearable technology, dielectric

Procedia PDF Downloads 57
114 Pesticides Monitoring in Surface Waters of the São Paulo State, Brazil

Authors: Fabio N. Moreno, Letícia B. Marinho, Beatriz D. Ruiz, Maria Helena R. B. Martins

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Brazil is a top consumer of pesticides worldwide, and the São Paulo State is one of the highest consumers among the Brazilian federative states. However, representative data about the occurrence of pesticides in surface waters of the São Paulo State is scarce. This paper aims to present the results of pesticides monitoring executed within the Water Quality Monitoring Network of CETESB (The Environmental Agency of the São Paulo State) between the 2018-2022 period. Surface water sampling points (21 to 25) were selected within basins of predominantly agricultural land-use (5 to 85% of cultivated areas). The samples were collected throughout the year, including high-flow and low-flow conditions. The frequency of sampling varied between 6 to 4 times per year. Selection of pesticide molecules for monitoring followed a prioritizing process from EMBRAPA (Brazilian Agricultural Research Corporation) databases of pesticide use. Pesticides extractions in aqueous samples were performed according to USEPA 3510C and 3546 methods following quality assurance and quality control procedures. Determination of pesticides in water (ng L-1) extracts were performed by high-performance liquid chromatography coupled with mass spectrometry (HPLC-MS) and by gas chromatography with nitrogen phosphorus (GC-NPD) and electron capture detectors (GC-ECD). The results showed higher frequencies (20- 65%) in surface water samples for Carbendazim (fungicide), Diuron/Tebuthiuron (herbicides) and Fipronil/Imidaclopride (insecticides). The frequency of observations for these pesticides were generally higher in monitoring points located in sugarcane cultivated areas. The following pesticides were most frequently quantified above the Aquatic life benchmarks for freshwater (USEPA Office of Pesticide Programs, 2023) or Brazilian Federal Regulatory Standards (CONAMA Resolution no. 357/2005): Atrazine, Imidaclopride, Carbendazim, 2,4D, Fipronil, and Chlorpiryfos. Higher median concentrations for Diuron and Tebuthiuron in the rainy months (october to march) indicated pesticide transport through surface runoff. However, measurable concentrations in the dry season (april to september) for Fipronil and Imidaclopride also indicates pathways related to subsurface or base flow discharge after pesticide soil infiltration and leaching or dry deposition following pesticide air spraying. With exception to Diuron, no temporal trends related to median concentrations of the most frequently quantified pesticides were observed. These results are important to assist policymakers in the development of strategies aiming at reducing pesticides migration to surface waters from agricultural areas. Further studies will be carried out in selected points to investigate potential risks as a result of pesticides exposure on aquatic biota.

Keywords: pesticides monitoring, são paulo state, water quality, surface waters

Procedia PDF Downloads 35
113 Changes of Chemical Composition and Physicochemical Properties of Banana during Ethylene-Induced Ripening

Authors: Chiun-C.R. Wang, Po-Wen Yen, Chien-Chun Huang

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Banana is produced in large quantities in tropical and subtropical areas. Banana is one of the important fruits which constitute a valuable source of energy, vitamins and minerals. The ripening and maturity standards of banana vary from country to country depending on the expected shelf life of market. The compositions of bananas change dramatically during ethylene-induced ripening that are categorized as nutritive values and commercial utilization. Nevertheless, there is few study reporting the changes of physicochemical properties of banana starch during ethylene-induced ripening of green banana. The objectives of this study were to investigate the changes of chemical composition and enzyme activity of banana and physicochemical properties of banana starch during ethylene-induced ripening. Green bananas were harvested and ripened by ethylene gas at low temperature (15℃) for seven stages. At each stage, banana was sliced and freeze-dried for banana flour preparation. The changes of total starch, resistant starch, chemical compositions, physicochemical properties, activity of amylase, polyphenolic oxidase (PPO) and phenylalanine ammonia lyase (PAL) of banana were analyzed each stage during ripening. The banana starch was isolated and analyzed for gelatinization properties, pasting properties and microscopic appearance each stage of ripening. The results indicated that the highest total starch and resistant starch content of green banana were 76.2% and 34.6%, respectively at the harvest stage. Both total starch and resistant starch content were significantly declined to 25.3% and 8.8%, respectively at the seventh stage. Soluble sugars content of banana increased from 1.21% at harvest stage to 37.72% at seventh stage during ethylene-induced ripening. Swelling power of banana flour decreased with the progress of ripening stage, but solubility increased. These results strongly related with the decreases of starch content of banana flour during ethylene-induced ripening. Both water insoluble and alcohol insoluble solids of banana flour decreased with the progress of ripening stage. Both activity of PPO and PAL increased, but the total free phenolics content decreased, with the increases of ripening stages. As ripening stage extended, the gelatinization enthalpy of banana starch significantly decreased from 15.31 J/g at the harvest stage to 10.55 J/g at the seventh stage. The peak viscosity and setback increased with the progress of ripening stages in the pasting properties of banana starch. The highest final viscosity, 5701 RVU, of banana starch slurry was found at the seventh stage. The scanning electron micrograph of banana starch showed the shapes of banana starch appeared to be round and elongated forms, ranging in 10-50 μm at the harvest stage. As the banana closed to ripe status, some parallel striations were observed on the surface of banana starch granular which could be caused by enzyme reaction during ripening. These results inferred that the highest resistant starch was found in the green banana at the harvest stage could be considered as a potential application of healthy foods. The changes of chemical composition and physicochemical properties of banana could be caused by the hydrolysis of enzymes during the ethylene-induced ripening treatment.

Keywords: ethylene-induced ripening, banana starch, resistant starch, soluble sugars, physicochemical properties, gelatinization enthalpy, pasting characteristics, microscopic appearance

Procedia PDF Downloads 446
112 Developing a Tissue-Engineered Aortic Heart Valve Based on an Electrospun Scaffold

Authors: Sara R. Knigge, Sugat R. Tuladhar, Alexander Becker, Tobias Schilling, Birgit Glasmacher

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Commercially available mechanical or biological heart valve prostheses both tend to fail long-term due to thrombosis, calcific degeneration, infection, or immunogenic rejection. Moreover, these prostheses are non-viable and do not grow with the patients, which is a problem for young patients. As a result, patients often need to undergo redo-operations. Tissue-engineered (TE) heart valves based on degradable electrospun fiber scaffolds represent a promising approach to overcome these limitations. Such scaffolds need sufficient mechanical properties to withstand the hydrodynamic stress of intracardiac hemodynamics. Additionally, the scaffolds should be colonized by autologous or homologous cells to facilitate the in vivo remodeling of the scaffolds to a viable structure. This study investigates how process parameters of electrospinning and degradation affect the mechanical properties of electrospun scaffolds made of FDA-approved, biodegradable polymer polycaprolactone (PCL). Fiber mats were produced from a PCL/tetrafluoroethylene solution by electrospinning. The e-spinning process was varied in terms of scaffold thickness, fiber diameter, fiber orientation, and fiber interconnectivity. The morphology of the fiber mats was characterized with a scanning electron microscope (SEM). The mats were degraded in different solutions (cell culture media, SBF, PBS and 10 M NaOH-Solution). At different time points of degradation (2, 4 and 6 weeks), tensile and cyclic loading tests were performed. Fresh porcine pericardium and heart valves served as a control for the mechanical assessment. The progression of polymer degradation was quantified by SEM and differential scanning calorimetry (DSC). Primary Human aortic endothelial cells (HAECs) and Human induced pluripotent stem cell-derived endothelial cells (iPSC-ECs) were seeded on the fiber mats to investigate the cell colonization potential. The results showed that both the electrospinning parameters and the degradation significantly influenced the mechanical properties. Especially the fiber orientation has a considerable impact and leads to a pronounced anisotropic behavior of the scaffold. Preliminary results showed that the polymer became strongly more brittle over time. However, the embrittlement can initially only be detected in the mechanical test. In the SEM and DSC investigations, neither morphological nor thermodynamic changes are significantly detectable. Live/Dead staining and SEM imaging of the cell-seeded scaffolds showed that HAECs and iPSC-ECs were able to grow on the surface of the polymer. In summary, this study's results indicate a promising approach to the development of a TE aortic heart valve based on an electrospun scaffold.

Keywords: electrospun scaffolds, long-term polymer degradation, mechanical behavior of electrospun PCL, tissue engineered aortic heart valve

Procedia PDF Downloads 115
111 Combustion Characteristics and Pollutant Emissions in Gasoline/Ethanol Mixed Fuels

Authors: Shin Woo Kim, Eui Ju Lee

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The recent development of biofuel production technology facilitates the use of bioethanol and biodiesel on automobile. Bioethanol, especially, can be used as a fuel for gasoline vehicles because the addition of ethanol has been known to increase octane number and reduce soot emissions. However, the wide application of biofuel has been still limited because of lack of detailed combustion properties such as auto-ignition temperature and pollutant emissions such as NOx and soot, which has been concerned mainly on the vehicle fire safety and environmental safety. In this study, the combustion characteristics of gasoline/ethanol fuel were investigated both numerically and experimentally. For auto-ignition temperature and NOx emission, the numerical simulation was performed on the well-stirred reactor (WSR) to simulate the homogeneous gasoline engine and to clarify the effect of ethanol addition in the gasoline fuel. Also, the response surface method (RSM) was introduced as a design of experiment (DOE), which enables the various combustion properties to be predicted and optimized systematically with respect to three independent variables, i.e., ethanol mole fraction, equivalence ratio and residence time. The results of stoichiometric gasoline surrogate show that the auto-ignition temperature increases but NOx yields decrease with increasing ethanol mole fraction. This implies that the bioethanol added gasoline is an eco-friendly fuel on engine running condition. However, unburned hydrocarbon is increased dramatically with increasing ethanol content, which results from the incomplete combustion and hence needs to adjust combustion itself rather than an after-treatment system. RSM results analyzed with three independent variables predict the auto-ignition temperature accurately. However, NOx emission had a big difference between the calculated values and the predicted values using conventional RSM because NOx emission varies very steeply and hence the obtained second order polynomial cannot follow the rates. To relax the increasing rate of dependent variable, NOx emission is taken as common logarithms and worked again with RSM. NOx emission predicted through logarithm transformation is in a fairly good agreement with the experimental results. For more tangible understanding of gasoline/ethanol fuel on pollutant emissions, experimental measurements of combustion products were performed in gasoline/ethanol pool fires, which is widely used as a fire source of laboratory scale experiments. Three measurement methods were introduced to clarify the pollutant emissions, i.e., various gas concentrations including NOx, gravimetric soot filter sampling for elements analysis and pyrolysis, thermophoretic soot sampling with transmission electron microscopy (TEM). Soot yield by gravimetric sampling was decreased dramatically as ethanol was added, but NOx emission was almost comparable regardless of ethanol mole fraction. The morphology of the soot particle was investigated to address the degree of soot maturing. The incipient soot such as a liquid like PAHs was observed clearly on the soot of higher ethanol containing gasoline, and the soot might be matured under the undiluted gasoline fuel.

Keywords: gasoline/ethanol fuel, NOx, pool fire, soot, well-stirred reactor (WSR)

Procedia PDF Downloads 191
110 Spectroscopic Autoradiography of Alpha Particles on Geologic Samples at the Thin Section Scale Using a Parallel Ionization Multiplier Gaseous Detector

Authors: Hugo Lefeuvre, Jerôme Donnard, Michael Descostes, Sophie Billon, Samuel Duval, Tugdual Oger, Herve Toubon, Paul Sardini

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Spectroscopic autoradiography is a method of interest for geological sample analysis. Indeed, researchers may face different issues such as radioelement identification and quantification in the field of environmental studies. Imaging gaseous ionization detectors find their place in geosciences for conducting specific measurements of radioactivity to improve the monitoring of natural processes using naturally-occurring radioactive tracers, but also for the nuclear industry linked to the mining sector. In geological samples, the location and identification of the radioactive-bearing minerals at the thin-section scale remains a major challenge as the detection limit of the usual elementary microprobe techniques is far higher than the concentration of most of the natural radioactive decay products. The spatial distribution of each decay product in the case of uranium in a geomaterial is interesting for relating radionuclides concentration to the mineralogy. The present study aims to provide spectroscopic autoradiography analysis method for measuring the initial energy of alpha particles with a parallel ionization multiplier gaseous detector. The analysis method has been developed thanks to Geant4 modelling of the detector. The track of alpha particles recorded in the gas detector allow the simultaneous measurement of the initial point of emission and the reconstruction of the initial particle energy by a selection based on the linear energy distribution. This spectroscopic autoradiography method was successfully used to reproduce the alpha spectra from a 238U decay chain on a geological sample at the thin-section scale. The characteristics of this measurement are an energy spectrum resolution of 17.2% (FWHM) at 4647 keV and a spatial resolution of at least 50 µm. Even if the efficiency of energy spectrum reconstruction is low (4.4%) compared to the efficiency of a simple autoradiograph (50%), this novel measurement approach offers the opportunity to select areas on an autoradiograph to perform an energy spectrum analysis within that area. This opens up possibilities for the detailed analysis of heterogeneous geological samples containing natural alpha emitters such as uranium-238 and radium-226. This measurement will allow the study of the spatial distribution of uranium and its descendants in geo-materials by coupling scanning electron microscope characterizations. The direct application of this dual modality (energy-position) of analysis will be the subject of future developments. The measurement of the radioactive equilibrium state of heterogeneous geological structures, and the quantitative mapping of 226Ra radioactivity are now being actively studied.

Keywords: alpha spectroscopy, digital autoradiography, mining activities, natural decay products

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109 The Power of in situ Characterization Techniques in Heterogeneous Catalysis: A Case Study of Deacon Reaction

Authors: Ramzi Farra, Detre Teschner, Marc Willinger, Robert Schlögl

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Introduction: The conventional approach of characterizing solid catalysts under static conditions, i.e., before and after reaction, does not provide sufficient knowledge on the physicochemical processes occurring under dynamic conditions at the molecular level. Hence, the necessity of improving new in situ characterizing techniques with the potential of being used under real catalytic reaction conditions is highly desirable. In situ Prompt Gamma Activation Analysis (PGAA) is a rapidly developing chemical analytical technique that enables us experimentally to assess the coverage of surface species under catalytic turnover and correlate these with the reactivity. The catalytic HCl oxidation (Deacon reaction) over bulk ceria will serve as our example. Furthermore, the in situ Transmission Electron Microscopy is a powerful technique that can contribute to the study of atmosphere and temperature induced morphological or compositional changes of a catalyst at atomic resolution. The application of such techniques (PGAA and TEM) will pave the way to a greater and deeper understanding of the dynamic nature of active catalysts. Experimental/Methodology: In situ Prompt Gamma Activation Analysis (PGAA) experiments were carried out to determine the Cl uptake and the degree of surface chlorination under reaction conditions by varying p(O2), p(HCl), p(Cl2), and the reaction temperature. The abundance and dynamic evolution of OH groups on working catalyst under various steady-state conditions were studied by means of in situ FTIR with a specially designed homemade transmission cell. For real in situ TEM we use a commercial in situ holder with a home built gas feeding system and gas analytics. Conclusions: Two complimentary in situ techniques, namely in situ PGAA and in situ FTIR were utilities to investigate the surface coverage of the two most abundant species (Cl and OH). The OH density and Cl uptake were followed under multiple steady-state conditions as a function of p(O2), p(HCl), p(Cl2), and temperature. These experiments have shown that, the OH density positively correlates with the reactivity whereas Cl negatively. The p(HCl) experiments give rise to increased activity accompanied by Cl-coverage increase (opposite trend to p(O2) and T). Cl2 strongly inhibits the reaction, but no measurable increase of the Cl uptake was found. After considering all previous observations we conclude that only a minority of the available adsorption sites contribute to the reactivity. In addition, the mechanism of the catalysed reaction was proposed. The chlorine-oxygen competition for the available active sites renders re-oxidation as the rate-determining step of the catalysed reaction. Further investigations using in situ TEM are planned and will be conducted in the near future. Such experiments allow us to monitor active catalysts at the atomic scale under the most realistic conditions of temperature and pressure. The talk will shed a light on the potential and limitations of in situ PGAA and in situ TEM in the study of catalyst dynamics.

Keywords: CeO2, deacon process, in situ PGAA, in situ TEM, in situ FTIR

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108 Influence of Torrefied Biomass on Co-Combustion Behaviors of Biomass/Lignite Blends

Authors: Aysen Caliskan, Hanzade Haykiri-Acma, Serdar Yaman

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Co-firing of coal and biomass blends is an effective method to reduce carbon dioxide emissions released by burning coals, thanks to the carbon-neutral nature of biomass. Besides, usage of biomass that is renewable and sustainable energy resource mitigates the dependency on fossil fuels for power generation. However, most of the biomass species has negative aspects such as low calorific value, high moisture and volatile matter contents compared to coal. Torrefaction is a promising technique in order to upgrade the fuel properties of biomass through thermal treatment. That is, this technique improves the calorific value of biomass along with serious reductions in the moisture and volatile matter contents. In this context, several woody biomass materials including Rhododendron, hybrid poplar, and ash-tree were subjected to torrefaction process in a horizontal tube furnace at 200°C under nitrogen flow. In this way, the solid residue obtained from torrefaction that is also called as 'biochar' was obtained and analyzed to monitor the variations taking place in biomass properties. On the other hand, some Turkish lignites from Elbistan, Adıyaman-Gölbaşı and Çorum-Dodurga deposits were chosen as coal samples since these lignites are of great importance in lignite-fired power stations in Turkey. These lignites were blended with the obtained biochars for which the blending ratio of biochars was kept at 10 wt% and the lignites were the dominant constituents in the fuel blends. Burning tests of the lignites, biomasses, biochars, and blends were performed using a thermogravimetric analyzer up to 900°C with a heating rate of 40°C/min under dry air atmosphere. Based on these burning tests, properties relevant to burning characteristics such as the burning reactivity and burnout yields etc. could be compared to justify the effects of torrefaction and blending. Besides, some characterization techniques including X-Ray Diffraction (XRD), Fourier Transform Infrared (FTIR) spectroscopy and Scanning Electron Microscopy (SEM) were also conducted for the untreated biomass and torrefied biomass (biochar) samples, lignites and their blends to examine the co-combustion characteristics elaborately. Results of this study revealed the fact that blending of lignite with 10 wt% biochar created synergistic behaviors during co-combustion in comparison to the individual burning of the ingredient fuels in the blends. Burnout and ignition performances of each blend were compared by taking into account the lignite and biomass structures and characteristics. The blend that has the best co-combustion profile and ignition properties was selected. Even though final burnouts of the lignites were decreased due to the addition of biomass, co-combustion process acts as a reasonable and sustainable solution due to its environmentally friendly benefits such as reductions in net carbon dioxide (CO2), SOx and hazardous organic chemicals derived from volatiles.

Keywords: burnout performance, co-combustion, thermal analysis, torrefaction pretreatment

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107 Elaboration and Characterization of in-situ CrC- Ni(Al, Cr) Composites Elaborated from Ni and Cr₂AlC Precursors

Authors: A. Chiker, A. Benamor, A. Haddad, Y. Hadji, M. Hadji

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Metal matrix composites (MMCs) have been of big interest for a few decades. Their major drawback lies in their enhanced mechanical performance over unreinforced alloys. They found ground in many engineering fields, such as aeronautics, aerospace, automotive, and other structural applications. One of the most used alloys as a matrix is nickel alloys, which meet the need for high-temperature mechanical properties; some attempts have been made to develop nickel base composites reinforced by high melt point and high modulus particulates. Among the carbides used as reinforcing particulates, chromium carbide is interesting for wear applications; it is widely used as a tribological coating material in high-temperature applications requiring high wear resistance and hardness. Moreover, a set of properties make it suitable for use in MMCs, such as toughness, the good corrosion and oxidation resistance of its three polymorphs -the cubic (Cr23C6), the hexagonal (Cr7C3), and the orthorhombic (Cr3C2)-, and it’s coefficient of thermal expansion that is almost equal to that of metals. The in-situ synthesis of CrC-reinforced Ni matrix composites could be achieved by the powder metallurgy route. To ensure the in-situ reactions during the sintering process, the use of phase precursors is necessary. Recently, new precursor materials have been proposed; these materials are called MAX phases. The MAX phases are thermodynamically stable nano-laminated materials displaying unusual and sometimes unique properties. These novel phases possess Mn+1AXn chemistry, where n is 1, 2, or 3, M is an early transition metal element, A is an A-group element, and X is C or N. Herein, the pressureless sintering method is used to elaborate Ni/Cr2AlC composites. Four composites were elaborated from 5, 10, 15 and 20 wt% of Cr2AlC MAX phase precursor which fully reacted with Ni-matrix at 1100 °C sintering temperature for 4 h in argon atmosphere. XRD results showed that Cr2AlC MAX phase was totally decomposed forming chromium carbide Cr7C3, and the released Al and Cr atoms diffused in Ni matrix giving rise to γ-Ni(Al,Cr) solid solution and γ’-Ni3(Al,Cr) intermetallic. Scanning Electron Microscopy (SEM) of the elaborated samples showed the presence of nanosized Cr7C3 reinforcing particles embedded in the Ni metal matrix, which have a direct impact on the tribological properties of the composites and their hardness. All the composites exhibited higher hardness than pure Ni; whereas adding 15 wt% of Cr2AlC gives the highest hardness (1.85 GPa). Using a ball-on-disc tribometer, dry sliding tests for the elaborated composites against 100Cr6 steel ball were studied under different applied loads. The microstructures and worn surface characteristics were then analyzed using SEM and Raman spectroscopy. The results show that all the composites exhibited better wear resistance compared to pure Ni, which could be explained by the formation of a lubricious tribo-layer during sliding and the good bonding between the Ni matrix and the reinforcing phases.

Keywords: composites, microscopy, sintering, wear

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106 Synthesis of Carbon Nanotubes from Coconut Oil and Fabrication of a Non Enzymatic Cholesterol Biosensor

Authors: Mitali Saha, Soma Das

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The fabrication of nanoscale materials for use in chemical sensing, biosensing and biological analyses has proven a promising avenue in the last few years. Cholesterol has aroused considerable interest in recent years on account of its being an important parameter in clinical diagnosis. There is a strong positive correlation between high serum cholesterol level and arteriosclerosis, hypertension, and myocardial infarction. Enzyme-based electrochemical biosensors have shown high selectivity and excellent sensitivity, but the enzyme is easily denatured during its immobilization procedure and its activity is also affected by temperature, pH, and toxic chemicals. Besides, the reproducibility of enzyme-based sensors is not very good which further restrict the application of cholesterol biosensor. It has been demonstrated that carbon nanotubes could promote electron transfer with various redox active proteins, ranging from cytochrome c to glucose oxidase with a deeply embedded redox center. In continuation of our earlier work on the synthesis and applications of carbon and metal based nanoparticles, we have reported here the synthesis of carbon nanotubes (CCNT) by burning coconut oil under insufficient flow of air using an oil lamp. The soot was collected from the top portion of the flame, where the temperature was around 6500C which was purified, functionalized and then characterized by SEM, p-XRD and Raman spectroscopy. The SEM micrographs showed the formation of tubular structure of CCNT having diameter below 100 nm. The XRD pattern indicated the presence of two predominant peaks at 25.20 and 43.80, which corresponded to (002) and (100) planes of CCNT respectively. The Raman spectrum (514 nm excitation) showed the presence of 1600 cm-1 (G-band) related to the vibration of sp2-bonded carbon and at 1350 cm-1 (D-band) responsible for the vibrations of sp3-bonded carbon. A nonenzymatic cholesterol biosensor was then fabricated on an insulating Teflon material containing three silver wires at the surface, covered by CCNT, obtained from coconut oil. Here, CCNTs worked as working as well as counter electrodes whereas reference electrode and electric contacts were made of silver. The dimensions of the electrode was 3.5 cm×1.0 cm×0.5 cm (length× width × height) and it is ideal for working with 50 µL volume like the standard screen printed electrodes. The voltammetric behavior of cholesterol at CCNT electrode was investigated by cyclic voltammeter and differential pulse voltammeter using 0.001 M H2SO4 as electrolyte. The influence of the experimental parameters on the peak currents of cholesterol like pH, accumulation time, and scan rates were optimized. Under optimum conditions, the peak current was found to be linear in the cholesterol concentration range from 1 µM to 50 µM with a sensitivity of ~15.31 μAμM−1cm−2 with lower detection limit of 0.017 µM and response time of about 6s. The long-term storage stability of the sensor was tested for 30 days and the current response was found to be ~85% of its initial response after 30 days.

Keywords: coconut oil, CCNT, cholesterol, biosensor

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105 Various Shaped ZnO and ZnO/Graphene Oxide Nanocomposites and Their Use in Water Splitting Reaction

Authors: Sundaram Chandrasekaran, Seung Hyun Hur

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Exploring strategies for oxygen vacancy engineering under mild conditions and understanding the relationship between dislocations and photoelectrochemical (PEC) cell performance are challenging issues for designing high performance PEC devices. Therefore, it is very important to understand that how the oxygen vacancies (VO) or other defect states affect the performance of the photocatalyst in photoelectric transfer. So far, it has been found that defects in nano or micro crystals can have two possible significances on the PEC performance. Firstly, an electron-hole pair produced at the interface of photoelectrode and electrolyte can recombine at the defect centers under illumination of light, thereby reducing the PEC performances. On the other hand, the defects could lead to a higher light absorption in the longer wavelength region and may act as energy centers for the water splitting reaction that can improve the PEC performances. Even if the dislocation growth of ZnO has been verified by the full density functional theory (DFT) calculations and local density approximation calculations (LDA), it requires further studies to correlate the structures of ZnO and PEC performances. Exploring the hybrid structures composed of graphene oxide (GO) and ZnO nanostructures offer not only the vision of how the complex structure form from a simple starting materials but also the tools to improve PEC performances by understanding the underlying mechanisms of mutual interactions. As there are few studies for the ZnO growth with other materials and the growth mechanism in those cases has not been clearly explored yet, it is very important to understand the fundamental growth process of nanomaterials with the specific materials, so that rational and controllable syntheses of efficient ZnO-based hybrid materials can be designed to prepare nanostructures that can exhibit significant PEC performances. Herein, we fabricated various ZnO nanostructures such as hollow sphere, bucky bowl, nanorod and triangle, investigated their pH dependent growth mechanism, and correlated the PEC performances with them. Especially, the origin of well-controlled dislocation-driven growth and its transformation mechanism of ZnO nanorods to triangles on the GO surface were discussed in detail. Surprisingly, the addition of GO during the synthesis process not only tunes the morphology of ZnO nanocrystals and also creates more oxygen vacancies (oxygen defects) in the lattice of ZnO, which obviously suggest that the oxygen vacancies be created by the redox reaction between GO and ZnO in which the surface oxygen is extracted from the surface of ZnO by the functional groups of GO. On the basis of our experimental and theoretical analysis, the detailed mechanism for the formation of specific structural shapes and oxygen vacancies via dislocation, and its impact in PEC performances are explored. In water splitting performance, the maximum photocurrent density of GO-ZnO triangles was 1.517mA/cm-2 (under UV light ~ 360 nm) vs. RHE with high incident photon to current conversion Efficiency (IPCE) of 10.41%, which is the highest among all samples fabricated in this study and also one of the highest IPCE reported so far obtained from GO-ZnO triangular shaped photocatalyst.

Keywords: dislocation driven growth, zinc oxide, graphene oxide, water splitting

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