Search results for: gas chromatography-mass spectroscopy

Authors: Hossein Bayahia, Mohammed Saad Motlaq Al-Gahmdi

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The gas-phase deoxygenation of propionic acid was investigated in the presence of Co-Mo catalysts in N2 or H2 flow at 200-400 °C. In the presence of N2 the main product was 3-pentanone with other deoxygenates and some light gases: ethane and ethene. Using H2 flow, the catalyst was active for decarboxylation and decarbonylation of acid and the yields of ethane and ethene. The decarboxylation and decarbonylation reactions increased with increasing temperature. Cobalt-molybdenum supported on alumina showed better performance than bulk catalyst, especially at 400 °C in the presence of N2 for the ketonisation of propionic acid to form 3-pentanone as the main product. Bulk and supported catalysts were characterized by surface area porosity (BET), thermogravimetric analysis (TGA) and diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) of pyridine adsorption.

Keywords: deoxygenation, propionic acid, gas-phase, catalyst

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Authors: Patrícia Severino, Luciana Nalone, Daniele Martins, Marco Chaud, Classius Ferreira, Cristiane Bani, Ricardo Albuquerque

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Hydrogels produced with polymers have been used in the development of dressings for wound treatment and tissue revitalization. Our study on polymer nanocomposites containing silver nanoparticles shows antimicrobial activity and applications in wound healing. The effects are linked with the slow oxidation and Ag⁺ liberation to the biological environment. Furthermore, bacterial cell membrane penetration and metabolic disruption through cell cycle disarrangement also contribute to microbial cell death. The silver antimicrobial activity has been known for many years, and previous reports show that low silver concentrations are safe for human use. This work aims to develop a hydrogel using natural polymers (sodium alginate and gelatin) combined with silver nanoparticles for wound healing and with antimicrobial properties in cutaneous lesions. The hydrogel development utilized different sodium alginate and gelatin proportions (20:80, 50:50 and 80:20). The silver nanoparticles incorporation was evaluated at the concentrations of 1.0, 2.0 and 4.0 mM. The physico-chemical properties of the formulation were evaluated using ultraviolet-visible (UV-Vis) absorption spectroscopy, Fourier transform infrared (FTIR) spectroscopy, differential scanning calorimetry (DSC), and thermogravimetric (TG) analysis. The morphological characterization was made using transmission electron microscopy (TEM). Human fibroblast (L2929) viability assay was performed with a minimum inhibitory concentration (MIC) assessment as well as an in vivo cicatrizant test. The results suggested that sodium alginate and gelatin in the (80:20) proportion with 4 mM of AgNO₃ in the (UV-Vis) exhibited a better hydrogel formulation. The nanoparticle absorption spectra of this analysis showed a maximum band around 430 - 450 nm, which suggests a spheroidal form. The TG curve exhibited two weight loss events. DSC indicated one endothermic peak at 230-250 °C, due to sample fusion. The polymers acted as stabilizers of a nanoparticle, defining their size and shape. Human fibroblast viability assay L929 gave 105 % cell viability with a negative control, while gelatin presented 96% viability, alginate: gelatin (80:20) 96.66 %, and alginate 100.33 % viability. The sodium alginate:gelatin (80:20) exhibited significant antimicrobial activity, with minimal bacterial growth at a ratio of 1.06 mg.mL⁻¹ in Pseudomonas aeruginosa and 0.53 mg.mL⁻¹ in Staphylococcus aureus. The in vivo results showed a significant reduction in wound surface area. On the seventh day, the hydrogel-nanoparticle formulation reduced the total area of injury by 81.14 %, while control reached a 45.66 % reduction. The results suggest that silver-hydrogel nanoformulation exhibits potential for wound dressing therapeutics.

Keywords: nanocomposite, wound healing, hydrogel, silver nanoparticle

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Authors: Muhammad Mufakkar, Ghulam Hussain Bhatti, Maryem Rana

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The study of the coordination behavior of thiones is of considerable interest due to the similarity of their binding sites to those in living systems. The complexation of thiones towards Copper(I) has also received considerable attraction in view of their variable bonding modes, structural diversity and promising biological implications. Copper (I) complexes of thioureas of the general formula: CuLCl, CuL2Cl and CuL3Cl [where L= Thiourea and its N- and N, N/- mono and di alkyl and phenyl derivatives] have been prepared using Cu(I)CN in the presence of HCl. The complexes have been characterized by thermal, IR and NMR(1H and 13C) spectroscopy. An upfield shift in 13C NMR and downfield shifts in 1H NMR are consistent with the sulfur coordination to Copper(I). The disappearance of a band around 2200 cm⁻¹ in IR and a resonance around 146 ppm in 13C NMR indicates that during the course of reaction the cyanide group of the Copper(I) salt has been replaced by chloride leading to the formation of chlorido complexes.

Keywords: Thiones, complexation, spectra, TGA, thermogram, chemical shifts, deshielding, resonance

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Authors: Gyu-Jin Kim, Hyo-Gyoung Kwak

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In this research, the effect of prestressing force on the nonlinearity of concrete was investigated by an experimental study. For the measurement of ultrasonic nonlinearity, a prestressed concrete beam was prepared and a nonlinear resonant ultrasound method was adopted. When the prestressing force changes, the stress state of the concrete inside the beam is affected, which leads to the occurrence of micro-cracks and changes in mechanical properties. Therefore, it is necessary to introduce nonlinear ultrasonic technology which sensitively reflects microstructural changes. Repetitive prestressing load history, including maximum levels of 45%, 60% and 75%, depending on the compressive strength, is designed to evaluate the impact of loading levels on the nonlinearity. With the experimental results, the possibility of ultrasonic nonlinearity as a trial indicator of stress was evaluated.

Keywords: micro crack, nonlinear ultrasonic resonant spectroscopy, prestressed concrete beam, prestressing force, ultrasonic nonlinearity

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Authors: Yaseen Elhebshi, Abdulkareem Hamid, Nureddin Bin Issa, Xiaonong Chen

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A convenient method of preparing ultrafine polystyrene latex nano-particles with amino groups on the surface is developed. Polystyrene latexes in the size range 50–400 nm were prepared via emulsion polymerization, using sodium dodecyl sulfate (SDS) as surfactant. Polystyrene with amino groups on the surface will be fine to use as organic filler to modify rubber. Transmission electron microscopy (TEM) was used to observe the morphology of silicon dioxide and functionalized polystyrene nano-particles. The nature of bonding between the polymer and the reactive groups on the filler surfaces was analyzed using Fourier transform infrared spectroscopy (FTIR). Scanning electron microscopy (SEM) was employed to examine the filler surface.

Keywords: reactive filler, emulsion polymerization, particle size, polystyrene nanoparticles

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Authors: N. Zoghi, Laleh Maleknia , M. E. Olya

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The nano-Cu particles were produced on cotton fabric substrate by ink-jet printing technology with water-soluble ink, which was based on copper. The surface tension and viscosity of the prepared inks were evaluated. The ink-jet printing process was repeated 1, 3, and 5 times in order to evaluate variations in the optical properties by changing thickness of printed film. Following initial drying of the printed film, the samples were annealed at different temperatures (150 °C, 200 °C and 250 °C) to determine the optimum temperature for the parameters set out in this experiment. The prepared nano-Cu particles were characterized by XRD and UV spectroscopy. The appearance of printed image and the nano-Cu particles morphology were observed by SEM. The results demonstrated that the ink-jet printing technology can be used to produce nano-particles on the cotton fabrics surface.

Keywords: ink-jet printing, nano-cu, fabric ink, in situ production, cotton fabric, water-soluble ink, morphology

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Authors: Gülşah Çelik Gül, Figen Kurtuluş

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Magnesium containing boron compounds with hexagonal structure have been drawn much attention due to their superconductive nature. The main target of this work is new modified microwave oven by on our own has an ability about passing through a gas in the oven medium for attainment of oxygen-free compounds such as c-BN.  Mg containing boride was synthesized by modified-microwave method under nitrogen atmosphere using amorphous boron and magnesium source in appropriate molar ratio. Microwave oven with oxygen free environment has been modified to aimed to obtain magnesium boride without oxygen. Characterizations were done by powder X-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectroscopy. Mg containing boride, generally named magnesium boride, with amorphous character without oxygen is obtained via designed microwave oven system.

Keywords: magnesium containing boron compounds, modified microwave synthesis, powder X-ray diffraction, FTIR

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Authors: Mohan Singh Mehata, R. K. Ratnesh

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CdSe, CdSe/ZnS, and CdSe/CdS core-shell quantum dots (QDs) of 3-4 nm were developed by using chemical route and following successive ion layer adsorption and reaction (SILAR) methods. The prepared QDs have been examined by using X-ray diffraction, high-resolution electron microscopy and optical spectroscopy. The photoluminescence (PL) quantum yield (QY) of core-shell QDs increases with respect to the core, indicating that the radiative rate increases by the formation of shell around core, as evident by the measurement of PL lifetime. Further, the PL of bovine serum albumin is quenched strongly by the presence of core-shall QDs and follow the Stern-Volmer (S-V) relation, whereas the lifetime does not follow the S-V relation, demonstrating that the observed quenching is predominantly static in nature. Among all the QDs, the CdSe/ZnS QDs shows the least cytotoxicity hence most biocompatibility.

Keywords: biocompatibility, core-shell quantum dots, photoluminescence and lifetime, sensing ability

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Authors: Amal M. Nassar, Nehal S. Ahmed, Rasha S. Kamal

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Some lube oil additives improve the base oil performance such as viscosity index improvers and pour point depressants which are the most important type of additives. In the present work, some homopolymeric additives were prepared by esterification of acrylic acid with different alcohols (1-dodecyl, 1-hexadecyl, and 1-octadecyl )and then homopolymerization of the prepared esters with different ratio of benzoyl peroxide catalyst (0.25%& 0.5 % and 1%). Structure of the prepared esters was confirmed by Infra-Red Spectroscopy. The molecular weights of the prepared homopolymers were determined by using Gel Permeation Chromatograph. The efficiency of the prepared homopolymers as viscosity index improvers and pour point depressants for lube oil was the investigation. It was found that all the prepared homopolymers are effective as viscosity index improvers and pour point depressants.

Keywords: lube oil additives, homopolymerization, viscosity index improver, pour point depressant

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Authors: Muhammad Hanif, Muhammad Salik

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In the present research work we present the optical emission studies of the Indium (In)-Tin (Sn) plasma produced by the first (1064 nm) harmonic of an Nd: YAG nanosecond pulsed laser. The experimentally observed line profiles of neutral Indium (InI) and Tin (SnI) are used to extract the electron temperature (Te) using the Boltzmann plot method. Whereas, the electron number density (Ne) has been determined from the Stark broadening line profile method. The Te is calculated by varying the distance from the target surface along the line of propagation of plasma plume and also by varying the laser irradiance. Beside we have studied the variation of Ne as a function of laser irradiance as well as its variation with distance from the target surface.

Keywords: indium-tin plasma, laser ablation, optical emission spectroscopy, electron temperature, electron number density

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Authors: R. L. M. Paiva, M. R. Capri, D. R. Mulinari, C. F. Bandeira, S. R. Montoro

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Natural fibers are used in polymer composites to improve mechanical properties, substituting inorganic reinforcing agents produced by non renewable resources. The present study investigates the tensile, flexural and impact behaviors of sugarcane bagasse fibers-polypropylene composite as a function of volume fraction. The surface of the fibers was modified by mercerization treatments to improve the wetting behavior of the apolar polypropylene. The treatment characterization was obtained by infrared spectroscopy and scanning electron microscopy. Results evidence that a good adhesion interfacial between fibers-matrix causing an increase strength and modulus flexural as well as impact strength in the modified fibers/PP composites when compared to the pure PP and unmodified fibers reinforced composites.

Keywords: sugarcane bagasse, polymer composites, mechanical properties, fibers

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Authors: Lea Lenhardt, Ivana Zeković, Tatjana Dramićanin, Miroslav D. Dramićanin

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Fluorescence spectroscopy coupled with parallel factor analysis (PARAFAC) and artificial neural networks (ANN) were used for characterization and classification of honey. Excitation emission spectra were obtained for 95 honey samples of different botanical origin (acacia, sunflower, linden, meadow, and fake honey) by recording emission from 270 to 640 nm with excitation in the range of 240-500 nm. Fluorescence spectra were described with a six-component PARAFAC model, and PARAFAC scores were further processed with two types of ANN’s (feed-forward network and self-organizing maps) to obtain algorithms for classification of honey on the basis of their botanical origin. Both ANN’s detected fake honey samples with 100% sensitivity and specificity.

Keywords: honey, fluorescence, PARAFAC, artificial neural networks

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Authors: Abderrahmane Hamdi, Julie Chalon, Benoit Dodin, Philippe Champagne

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In this report, we present a simple route to realize robust, hydrophobic, and highly transparent coatings using organic polysilazane (durazane) and zinc oxide nanoparticles (ZnO). These coatings were deposited by spraying the mixture solution on glass slides. Thus, the properties of the films were characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), UV–vis-NIR spectrophotometer, and water contact angle method. This sprayable polymer mixed with ZnO nanoparticles shows high transparency for visible light > 90%, a hydrophobic character (CA > 90°), and good mechanical and chemical stability. The coating also demonstrates excellent self-cleaning properties, which makes it a promising candidate for commercial use.

Keywords: coatings, durability, hydrophobicity, organic polysilazane, self-cleaning, transparence, zinc oxide nanoparticles

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Authors: A. Pourahmad, Sh. Gharipour

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The present work describes the preparation and characterization of nanosized SiO₂@PbS core-shell particles by using a simple wet chemical route. This method utilizes silica spheres formation followed by successive ionic layer adsorption and reaction method assisted lead sulphide shell layer formation. The final product was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), UV–vis spectroscopic, infrared spectroscopy (IR) and transmission electron microscopy (TEM) experiments. The morphological studies revealed the uniformity in size distribution with core size of 250 nm and shell thickness of 18 nm. The electron microscopic images also indicate the irregular morphology of lead sulphide shell layer. The structural studies indicate the face-centered cubic system of PbS shell with no other trace for impurities in the crystal structure.

Keywords: core-shell, nanostructure, semiconductor, optical property, XRD

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Authors: P. J. Sweeney, T. Ahtoniemi, J. Puoliväli, T. Laitinen, K.Lehtimäki, A. Nurmi, D. Wells

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Duchenne muscular dystrophy (DMD) is an X-linked, lethal muscle wasting disease for which there are currently no treatment that effectively prevents the muscle necrosis and progressive muscle loss. DMD is among the most common of inherited diseases affecting around 1/3500 live male births. MDX (X-linked muscular dystrophy) mice only partially encapsulate the disease in humans and display weakness in muscles, muscle damage and edema during a period deemed the “critical period” when these mice go through cycles of muscular degeneration and regeneration. Although the MDX mutant mouse model has been extensively studied as a model for DMD, to-date an extensive temporal, non-invasive imaging profile that utilizes magnetic resonance imaging (MRI) and 1H-magnetic resonance spectroscopy (1H-MRS) has not been performed.. In addition, longitudinal imaging characterization has not coincided with attempts to exacerbate the progressive muscle damage by exercise. In this study we employed an 11.7 T small animal MRI in order to characterize the MRI and MRS profile of MDX mice longitudinally during a 12 month period during which MDX mice were subjected to exercise. Male mutant MDX mice (n=15) and male wild-type mice (n=15) were subjected to a chronic exercise regime of treadmill walking (30 min/ session) bi-weekly over the whole 12 month follow-up period. Mouse gastrocnemius and tibialis anterior muscles were profiled with baseline T2-MRI and 1H-MRS at 6 weeks of age. Imaging and spectroscopy was repeated again at 3 months, 6 months, 9 months and 12 months of age. Plasma creatine kinase (CK) level measurements were coincided with time-points for T2-MRI and 1H-MRS, but also after the “critical period” at 10 weeks of age. The results obtained from this study indicate that chronic exercise extends dystrophic phenotype of MDX mice as evidenced by T2-MRI and1H-MRS. T2-MRI revealed extent and location of the muscle damage in gastrocnemius and tibialis anterior muscles as hyperintensities (lesions and edema) in exercised MDX mice over follow-up period.. The magnitude of the muscle damage remained stable over time in exercised mice. No evident fat infiltration or cumulation to the muscle tissues was seen at any time-point in exercised MDX mice. Creatine, choline and taurine levels evaluated by 1H-MRS from the same muscles were found significantly decreased in each time-point, Extramyocellular (EMCL) and intramyocellular lipids (IMCL) did not change in exercised mice supporting the findings from anatomical T2-MRI scans for fat content. Creatine kinase levels were found to be significantly higher in exercised MDX mice during the follow-up period and importantly CK levels remained stable over the whole follow-up period. Taken together, we have described here longitudinal prophile for muscle damage and muscle metabolic changes in MDX mice subjected to chronic exercised. The extent of the muscle damage by T2-MRI was found to be stable through the follow-up period in muscles examined. In addition, metabolic profile, especially creatine, choline and taurine levels in muscles, was found to be sustained between time-points. The anatomical muscle damage evaluated by T2-MRI was supported by plasma CK levels which remained stable over the follow-up period. These findings show that non-invasive imaging and spectroscopy can be used effectively to evaluate chronic muscle pathology. These techniques can be also used to evaluate the effect of various manipulations, like here exercise, on the phenotype of the mice. Many of the findings we present here are translatable to clinical disease, such as decreased creatine, choline and taurine levels in muscles. Imaging by T2-MRI and 1H-MRS also revealed that fat content or extramyocellar and intramyocellular lipids, respectively, are not changed in MDX mice, which is in contrast to clinical manifestation of the Duchenne’s muscle dystrophy. Findings show that non-invasive imaging can be used to characterize the phenotype of a MDX model and its translatability to clinical disease, and to study events that have traditionally been not examined, like here rigorous exercise related sustained muscle damage after the “critical period”. The ability for this model to display sustained damage beyond the spontaneous “critical period“ and in turn to study drug effects on this extended phenotype will increase the value of the MDX mouse model as a tool to study therapies and treatments aimed at DMD and associated diseases.

Keywords: 1H-MRS, MRI, muscular dystrophy, mouse model

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Authors: Richard E. Miller

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12.7-mm thick plates of 6061-T6511 aluminum alloy and high hardness steel (528 HV) were successfully joined by a friction stir bonding process using a tungsten-rhenium stir tool. Process parameter variation experiments, which included tool design geometry, plunge and traverse rates, tool offset, spindle tilt, and rotation speed, were conducted to develop a parameter set which yielded a defect free joint. Laboratory tensile tests exhibited yield stresses which exceed the strengths of comparable AA6061-to-AA6061 fusion and friction stir weld joints. Scanning electron microscopy and energy dispersive X-ray spectroscopy analysis also show atomic diffusion at the material interface region.

Keywords: dissimilar materials, friction stir, welding, materials science

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Authors: Alain Kusmoko, Druce Dunne, Huijun Li

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Stellite 6 was deposited by laser cladding on a chromium bearing substrate (P91) with energy inputs of 1 kW (P91-1) and 1.8 kW (P91-1.8). The chemical compositions and microstructures of these coatings were characterized by atomic absorption spectroscopy, optical microscopy and scanning electron microscopy. The microhardness of the coatings was measured and the wear mechanism of the coatings was assessed using a pin-on-plate (reciprocating) wear testing machine. The results showed less cracking and pore development for Stellite 6 coatings applied to the P91 steel substrate with the lower heat input (P91-1). Further, the Stellite coating for P91-1 was significantly harder than that obtained for P91-1.8. The wear test results indicated that the weight loss for P91-1 was much lower than for P91-1.8. It is concluded that the lower hardness of the coating for P91-1.8, together with the softer underlying substrate structure, markedly reduced the wear resistance of the Stellite 6 coating.

Keywords: friction and wear, laser cladding, P91 steel, Stellite 6 coating

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Authors: Olga V. Kharchenko

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Applicability of a KTA crystal-based laser system with optical parametric oscillators (OPO) generation to lidar sounding of the atmosphere in the spectral range 3–4 µm is studied in this work. A technique based on differential absorption lidar (DIAL) method and differential optical absorption spectroscopy (DOAS) is developed for lidar sounding of trace atmospheric gases (TAG). The DIAL-DOAS technique is tested to estimate its efficiency for lidar sounding of atmospheric trace gases.

Keywords: atmosphere, lidar sounding, DIAL, DOAS, trace gases, nonlinear crystal

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Authors: P. Hemalatha, Deepalekshmi Ponnamma, Mariam Al Ali Al-Maadeed

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The Poly(vinylideneflouride-hexafluoropropylene) (PVDF-HFP)/ zinc oxide (ZnO) nanocomposites films were successfully prepared by mixing the fine ZnO particles into PVDF-HFP solution followed by film casting and sandwich techniques. Zinc oxide nanoparticles were synthesized by hydrothermal method. Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM) were used to characterize the structure and properties of the obtained nanocomposites. The dielectric properties of the PVDF-HFP/ZnO nanocomposites were analyzed in detail. In comparison with pure PVDF-HFP, the dielectric constant of the nanocomposite (1wt% ZnO) was significantly improved. The piezoelectric co-efficients of the nanocomposites films were measured. Experimental results revealed the influence of filler on the properties of PVDF-HFP and enhancement in the output performance and dielectric properties reflects the ability for energy storage capabilities.

Keywords: dielectric constant, hydrothermal, nanoflowers, organic compounds

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Authors: E. Fereydouni, Laleh Maleknia , M. E. Olya

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The present research, nylon fabric dyed by pressure method with nano-Si, nano-Ti particles and SiO2-TiO2 nancomposite. The influence of the amount of Si, Ti and SiO2-TiO2 on the performance of nylon fabric was investigated by the use of Fourier transform infrared spectrophotometer (FTIR), horizontal flammability apparatus (HFA), scanning electron microscope (SEM), electron dispersive X-ray spectroscope (EDX), water contact angle tester (WCA) and CIE LAB colorimetric system. The possible interactions between particles and nylon fiber were elucidated by the FTIR spectroscopy. Results indicated that the stabilized nanoparticles and nanocomposite enhances flame retardancy of nylon fabrics. Also, the prominet features of nanoparticles and nanocomposite treatment can note increase of adsorption and fixation of dye.

Keywords: nano-Si, nano- Ti, SiO2-TiO2 nancomposite, nylon fabric, flame retardant nylon

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Authors: K. Akhil, J. Jayakumar, S. Sudheer Khan

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Zinc oxide nanoparticles (ZnO NPs) are extensively used in a wide variety of commercial products including sunscreen, textile and paints. The present study evaluated the effect of surface capping agents including polyethylene glycol (EG), gelatin, polyvinyl alcohol(PVA) and poly vinyl pyrrolidone(PVP) on photocatalytic activity of ZnO NPs. The particles were also tested for its antibacterial and antibiofilm activity against Staphylococcus aureus (MTCC 3160) and Pseudomonas aeruginosa (MTCC 1688). Preliminary characterization was done by UV-Visible spectroscopy. Electron microscopic analysis showed that the particles were hexagonal in shape. The hydrodynamic size distribution was analyzed by using dynamic light scattering method and crystalline nature was determined by X-Ray diffraction method.

Keywords: antibacterial, antibiofilm, capping agents, photodegradation, surface coating, zinc oxide nanoparticles

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Authors: Pham-Thi Huong, Byeong-Kyu Lee, Jitae Kim, Chi-Hyeon Lee

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Fe-nano zeolite adsorbent was used for removal of Ni (II) ions from aqueous solution. The adsorbent was characterized by Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and the surface area Brunauer–Emmett–Teller (BET) using for analysis of functional groups, morphology and surface area. Bath adsorption experiments were analyzed on the effect of pH, time, adsorbent doses and initial Ni (II) concentration. The optimum pH for Ni (II) removal using Fe-nano zeolite was found at 5.0 and 90 min of reaction time. The maximum adsorption capacity of Ni (II) was 231.68 mg/g based on the Langmuir isotherm. The kinetics data for the adsorption process was fitted with the pseudo-second-order model. The desorption of Ni (II) from Ni-loaded Fe-nano zeolite was analyzed and even after 10 cycles 72 % desorption was achieved. These finding supported that Fe-nano zeolite with high adsorption capacity, high reuse ability would be utilized for Ni (II) removal from water.

Keywords: Fe-nano zeolite, adsorption, Ni (II) removal, regeneration

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Authors: M. Sari Yilmaz, N. Karamahmut Mermer

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Coal fly ash is formed as a solid waste product from the combustion of coal in coal fired power stations. Huge amounts of fly ash are produced globally every year and are predicted to increase. Nowadays, less than half of the fly ash is used as a raw material for cement manufacturing, construction and the rest of it is disposed as a waste causing yet another environmental concern. For this reason, the recycling of this kind of slurries into useful materials is quite important in terms of economical and environmental aspects. The purpose of this study is to evaluate the Orhaneli and Tuncbilek coal fly ashes for utilization in some industrial applications. Therefore the mineralogical and chemical compositions of these fly ashes were analyzed by X-ray fluorescence (XRF) spectroscopy and X-ray diffraction (XRD). The silicon (Si) and aluminum (Al) in the fly ashes were activated by alkali fusion technique with sodium hydroxide. The obtained extracts were analyzed for Si and Al content by inductively coupled plasma optical emission spectrometry (ICP-OES).

Keywords: extraction, fly ash, fusion, XRD

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Authors: G. Çelik Gül, F. Kurtuluş

Abstract:

Colemanite is the most common borate mineral, and the main source of the boron required by plants, human, and earth. Transition metals exhibit optical and physical properties such as; non-linear optical character, structural diversity, thermal stability, long cycle life and luminescent radiation. The doping of colemanite with a transition metal, bring it very interesting and attractive properties which make them applicable in industry. Iron doped calcium borate was synthesized by conventional solid state method at 1200 °C for 12 h with a systematic pathway. X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy/energy dispersive analyze (SEM/EDS) were used to characterize structural and morphological properties. Also, thermal properties were recorded by thermogravimetric-differential thermal analysis (TG/DTA). 

Keywords: colemanite, conventional synthesis, powder x-ray diffraction, borates

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Authors: K. Selvakumar, J. Kalaiselvimary, B. Jansirani, M. Ramesh Prabhu

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Proton conducting sulphonated poly (vinylidene fluoride- hexafluoro propylene) PVdF-HFP membranes were modified with nano – sized montmorillonite (MMT) through homogeneous dispersive mixing and solution casting technique for fuel cell applications. The prepared composite membranes were characterized using Fourier Transform Infrared Spectroscopy and 1HNMR technique. The suitability of the composite membranes for fuel cell application was evaluated in terms of water uptake, swelling behavior, and proton conductivity. These composites showed good conductivities and durability and expected to be used in the development of proton exchange membrane for fuel cells.

Keywords: composite, proton conduction, sulphonation, water uptake

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Authors: Peter Kus, Anna Ostroverkh, Yurii Yakovlev, Yevheniia Lobko, Roman Fiala, Ivan Khalakhan, Vladimir Matolin

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Hydrogen economy is a concept of low-emission society which harvests most of its energy from renewable sources (e.g., wind and solar) and in case of overproduction, electrochemically turns the excess amount into hydrogen, which serves as an energy carrier. Proton exchange membrane water electrolyzers (PEMWE) are the backbone of this concept. By fast-response electricity to hydrogen conversion, the PEMWEs will not only stabilize the electrical grid but also provide high-purity hydrogen for variety of fuel cell powered devices, ranging from consumer electronics to vehicles. Wider commercialization of PEMWE technology is however hindered by high prices of noble metals which are necessary for catalyzing the redox reactions within the cell. Namely, platinum for hydrogen evolution reaction (HER), running on cathode, and iridium for oxygen evolution reaction (OER) on anode. Possible way of how to lower the loading of Pt and Ir is by using conductive high-surface nanostructures as catalyst supports in conjunction with thin-film catalyst deposition. The presented study discusses unconventional technique of membrane electron assembly (MEA) preparation. Noble metal catalysts (Pt and Ir) were magnetron sputtered in very low loadings onto the surface of porous sublayers (located on gas diffusion layer or directly on membrane), forming so to say localized three-phase boundary. Ultrasonically sprayed corrosion resistant TiC-based sublayer was used as a support material on anode, whereas magnetron sputtered nanostructured etched nitrogenated carbon (CNx) served the same role on cathode. By using this configuration, we were able to significantly decrease the amount of noble metals (to thickness of just tens of nanometers), while keeping the performance comparable to that of average state-of-the-art catalysts. Complex characterization of prepared supported catalysts includes in-cell performance and durability tests, electrochemical impedance spectroscopy (EIS) as well as scanning electron microscopy (SEM) imaging and X-ray photoelectron spectroscopy (XPS) analysis. Our research proves that magnetron sputtering is a suitable method for thin-film deposition of electrocatalysts. Tested set-up of thin-film supported anode and cathode catalysts with combined loading of just 120 ug.cm⁻² yields remarkable values of specific current. Described approach of thin-film low-loading catalyst deposition might be relevant when noble metal reduction is the topmost priority.

Keywords: hydrogen economy, low-loading catalyst, magnetron sputtering, proton exchange membrane water electrolyzer

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Authors: K. Abbas, R. Ahmad, I. A. Khan, S. Saleem, U. Ikhlaq

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Nitriding of p-type Si samples by pulsed DC glow discharge is carried out for different Ar concentrations (30% to 90%) in nitrogen-argon plasma whereas the other parameters like pressure (2 mbar), treatment time (4 hr) and power (175 W) are kept constant. The phase identification, crystal structure, crystallinity, chemical composition, surface morphology and topography of the nitrided layer are studied using X-ray diffraction (XRD), Fourier transform infra-red spectroscopy (FTIR), optical microscopy (OM), scanning electron microscopy (SEM) and atomic force microscopy (AFM) respectively. The XRD patterns reveal the development of different diffraction planes of Si₃N₄ confirming the formation of polycrystalline layer. FTIR spectrum confirms the formation of bond between Si and N. Results reveal that addition of Ar into N₂ plasma plays an important role to enhance the production of active species which facilitate the nitrogen diffusion.

Keywords: crystallinity, glow discharge, nitriding, sputtering

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Authors: R. S. Yadav, J. Havlica, I. Kuřitka, Z. Kozakova, J. Masilko, M. Hajdúchová, V. Enev, J. Wasserbauer

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In this present work, CoFe2-xNdxO4 (0.0 ≤ x ≥0.1) spinel ferrite nanoparticles were synthesized by starch-assisted sol-gel auto-combustion method. Powder X-ray diffraction patterns were revealed the formation of cubic spinel ferrite with the signature of NdFeO3 phase at higher Nd3+ concentration. The field emission scanning electron microscopy study demonstrated the spherical nanoparticle in the size range between 5-15 nm. Raman and Fourier Transform Infrared spectra supported the formation of the spinel ferrite structure in the nanocrystalline form. The X-ray photoelectron spectroscopy (XPS) analysis confirmed the presence of Co2+ and Fe3+ at octahedral as well as a tetrahedral site in CoFe2-xNdxO4 nanoparticles. The change in magnetic properties with a variation of concentration of Nd3+ ions in cobalt ferrite nanoparticles was observed.

Keywords: nanoparticles, spinel ferrites, sol-gel auto-combustion method, CoFe2-xNdxO4

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Authors: Arslan Usman, Abdul Sattar, Hamid Latif, Afshan Ashfaq, Muhammad Rafique, Martin Koch

Abstract:

Two-dimensional materials have promising applications in optoelectronic and photonics; MoS₂ is the pioneer 2D material in the family of transition metal dichalcogenides. Its optical, optoelectronic, and structural properties are of practical importance along with its exciton dynamics. Exciton, along with exciton complexes, plays a vital role in realizing quantum devices. MoS₂ monolayers were synthesized using chemical vapour deposition (CVD) technique on SiO₂ and hBN substrates. Photoluminescence spectroscopy (PL) was used to identify the monolayer, which also reflects the substrate based peak broadening due to screening effects. In-plane and out of plane characteristic vibrational modes E¹₂g and A₁g, respectively, were detected in a different configuration on the substrate. The B-excitons and trions showed a dominant feature at low temperatures due to electron-phonon coupling effects, whereas their energies are separated by 100 meV.

Keywords: 2D materials, photoluminescence, AFM, excitons

Procedia PDF Downloads 146

Authors: Yamina Zouambia, Khadidja Youcef Ettoumi, Mohamed Krea, Nadji Moulai Mostefa

Abstract:

Environment pollution through various wastes (particularly by heavy metals) is a major environmental problem due to industrialization and the development of various human activities. Considerable attention has been focused, in recent years, upon the field of biosorption which represents a biotechnological innovation as well as an excellent tool for removal of metal ions from aqueous effluents. So the purpose of this study is to valorize by-product which are orange peels and an extract of these peels (pectin; a heteropolysaccharide) in treatment of water containing heavy metals. All biosorption experiments were carried out at room temperature, an indicated pH, a precise amount of biosorbent and under continuous stirring. Biosorption kinetic was determined by evaluating the residual concentration of the metal ion at different time intervals using UV spectroscopy. The results obtained show that the orange peels and pectin are interesting biosorbents with maximum biosorption capacity of up to 140 mg/g.

Keywords: orange peels, pectin, heavy metals, biosorption

Procedia PDF Downloads 332