Search results for: in-situ synchrotron X-ray diffraction

Authors: M.F. Elkady, Sahar Zaki, Desouky Abd-El-Haleem

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Silver nanoparticles (AgNPs) are already widely prepared using different technologies. However, there are limited data on the effects of hydrogen ion concentration on nano-silver production. In this investigation, the impact of the pH reaction medium toward the particle size, agglomeration and the yield of the produced bio-synthesized silver were established. Quasi-spherical silver nanoparticles were synthesized through the biosynthesis green production process using the Egyptian E. coli bacterial strain 23N at different pH values. The formation of AgNPs has been confirmed with ultraviolet–visible spectra through identification of their characteristic peak at 410 nm. The quantitative production yield and the orientation planes of the produced nano-silver were examined using X-ray spectroscopy (EDS) and X-ray diffraction (XRD). Quantitative analyses indicated that the silver production yield was promoted at elevated pH regarded to increase the reduction rate of silver precursor through both chemical and biological processes. As a result, number of the nucleus and thus the size of the silver nanoparticles were tunable through changing pH of the reaction system. Accordingly, the morphological structure and size of the produced silver and its aggregates were determined using scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images. It was considered that the increment in pH value of the reaction media progress the aggregation of silver clusters. However, the presence of stain 23N biomass decreases the possibility of silver aggregation at the pH 7.

Keywords: silver nanoparticles, biosynthesis, reaction media pH, nano-silver characterization

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Authors: Magdalena Hałupka-Bryl, Magdalena Bednarowicz, Ryszard Krzyminiewski, Yukio Nagasaki

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Due to their unique physical properties, superparamagnetic iron oxide nanoparticles are increasingly used in medical applications. They are very useful carriers for delivering antitumor drugs in targeted cancer treatment. Magnetic nanoparticles (PEG-PIONs/DOX) with chemotherapeutic were synthesized by coprecipitation method followed by coating with biocompatible polymer PEG-derivative (poly(ethylene glycol)-block-poly(4-vinylbenzylphosphonate). Complete physicochemical characterization was carried out (ESR, HRTEM, X-ray diffraction, SQUID analysis) to evaluate the magnetic properties of obtained PEG-PIONs/DOX. Nanoparticles were investigated also in terms of their stability, drug loading efficiency, drug release and antiproliferative effect on cancer cells. PEG-PIONs/DOX have been successfully used for the efficient delivery of an anticancer drug into the tumor region. Fluorescent imaging showed the internalization of PEG-PIONs/DOX in the cytoplasm. Biodistribution studies demonstrated that PEG-PIONs/DOX preferentially accumulate in tumor region via the enhanced permeability and retention effect. The present findings show that synthesized nanosystem is promising tool for potential magnetic drug delivery.

Keywords: targeted drug delivery, magnetic properties, iron oxide nanoparticles, biodistribution

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Authors: Joy Marie Mora, Mark Daniel De Luna, Tsair-Wang Chung

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Transesterification reaction of soybean oil with methanol was carried out to produce fatty acid methyl esters (FAME) using calcined alkali metal (Na and Li) supported by pumice silica as the solid base catalyst. Pumice silica catalyst was activated by loading alkali metal ions to its surface via an ion-exchange method. Response surface methodology (RSM) in combination with Box-Behnken design (BBD) was used to optimize the operating parameters in biodiesel production, namely: reaction temperature, methanol to oil molar ratio, reaction time, and catalyst concentration. Using the optimized sets of parameters, FAME yields using sodium and lithium silicate catalysts were 98.80% and 98.77%, respectively. A pseudo-first order kinetic equation was applied to evaluate the kinetic parameters of the reaction. The prepared catalysts were characterized by several techniques such as X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Brunauer-Emmett-Teller (BET) sorptometer, and scanning electron microscopy (SEM). In addition, the reusability of the catalysts was successfully tested in two subsequent cycles.

Keywords: alkali metal, biodiesel, Box-Behnken design, heterogeneous catalyst, kinetics, optimization, pumice, transesterification

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Authors: Burak Bal

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Mechanical characterization tests might come with a remarkable cost of time and money for both companies and academics. The inquiry to transform laboratory experiments to the computational media is getting a trend; accordingly, the literature supplies many analytical ways to explain the mechanics of deformation. In our work, we focused on the crystal plasticity finite element modeling (CPFEM) analysis on various materials in various crystal structures to predict the stress-strain curve without tensile tests. For FEM analysis, which we used in this study was ABAQUS, a standard user-defined material subroutine (UMAT) was prepared. The geometry of a specimen was created via DREAM 3D software with the inputs of Euler angles taken by Electron Back-Scattered Diffraction (EBSD) technique as orientation, or misorientation angles. The synthetic crystal created with DREAM 3D is also meshed in a way the grains inside the crystal meshed separately, and the computer can realize interaction of inter, and intra grain structures. The mechanical deformation parameters obtained from the literature put into the Fortran based UMAT code to describe how material will response to the load applied from specific direction. The mechanical response of a synthetic crystal created with DREAM 3D agrees well with the material response in the literature.

Keywords: crystal plasticity finite element modeling, ABAQUS, Dream.3D, microstructure

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Authors: Krishnamoorthy Sathiyan, Shanti Gopal Patra, Ronen Bar-Ziv, Tomer Zidki

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Developing efficient non-noble metal catalysts that are cheap and durable for oxygen evolution reaction (OER) is a great challenge. Moreover, altering the electronic structure of the catalyst and structural engineering of the materials provide a new direction for enhancing the OER. Herein, we have successfully synthesized Fe and Co incorporated MoS₂ catalysts, which show improved catalytic activity for OER when compared with MoS₂, Fe-MoS₂, and Co-MoS₂. It was found that at an optimal ratio of Fe and Co, the electronic and structural modification of MoS₂ occurs, which leads to change in orientation and thereby enhances the active catalytic sites on the edges, which are more exposed for OER. The nanocomposites have been well characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), and energy dispersive X-ray analysis (EDX), Elemental Mapping, transmission electron microscope (TEM), and high-resolution transmission electron microscope (HR-TEM) analysis. Among all, a particular ratio of FeCo-MoS₂ exhibits a much smaller onset with better catalytic current density. The remarkable catalytic activity is mainly attributed to the synergistic effect from the Fe and Co. Most importantly, our work provides an essential insight in altering the electronic structure of MoS₂ based materials by incorporating promoters such as Co and Fe in an optimal amount, which enhances OER activity.

Keywords: electrocatalysts, molybdenum disulfide, oxygen evolution reaction, transition metals

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Authors: Hamid Merzouk, Djahida Touati-Talantikite, Amina Zaabar

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New nanosized materials are in huge expansion worldwide. They play a fundamental role in various industrial applications thanks their unique and functional properties. Moreover, in recent years, a great effort has been made to the design and control fabrication of nanostructured semiconductors such zinc sulphide. In recent years, much attention has been accorded in doped and co-doped ZnS to improve the ZnS films quality. We present in this work the preparation and characterization of ZnS and Al doped ZnS thin films. Nanoparticles ZnS and Al doped ZnS films are prepared by chemical bath deposition method (CBD), for various dopant concentrations. Thin films are deposed onto commercial microscope glass slides substrates. Thiourea is used as sulfide ion source, zinc acetate as zinc ion source and manganese acetate as manganese ion source in alkaline bath at 90 °C. X-ray diffraction (XRD) analyses are carried out at room temperature on films and powders with a powder diffractometer, using CuKα radiation. The average grain size obtained from the Debye–Scherrer’s formula is around 10 nm. Films morphology is examined by scanning electron microscopy. IR spectra of representative sample are recorded with the FTIR between 400 and 4000 cm-1.The transmittance (70 %) is performed with the UV–VIS spectrometer in the wavelength range 200–800 nm. This value is enhanced by Al doping.

Keywords: ZnS, nanostructured semiconductors, thin films, chemical bath deposition

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Authors: Eman Alzahrani

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Magnetic nanoparticles (MNPs) were fabricated using the chemical co-precipitation method followed by coating the surface of magnetic Fe3O4 nanoparticles with gum arabic (GA). The fabricated magnetic nanoparticles were characterised using transmission electron microscopy (TEM) which showed that the Fe3O4 nanoparticles and GA-MNPs nanoparticles had a mean diameter of 33 nm, and 38 nm, respectively. Scanning electron microscopy (SEM) images showed that the MNPs modified with GA had homogeneous structure and agglomerated. The energy dispersive X-ray spectroscopy (EDAX) spectrum showed strong peaks of Fe and O. X-ray diffraction patterns (XRD) indicated that the naked magnetic nanoparticles were pure Fe3O4 with a spinel structure and the covering of GA did not result in a phase change. The covering of GA on the magnetic nanoparticles was also studied by BET analysis, and Fourier transform infrared spectroscopy. Moreover, the present study reports a fast and simple method for removal and recovery of methylene blue dye (MB) from aqueous solutions by using the synthesised magnetic nanoparticles modified with gum arabic as adsorbent. The experimental results show that the adsorption process attains equilibrium within five minutes. The data fit the Langmuir isotherm equation and the maximum adsorption capacities were 8.77 mg mg-1 and 14.3 mg mg-1 for MNPs and GA-MNPs, respectively. The results indicated that the homemade magnetic nanoparticles were quite efficient for removing MB and will be a promising adsorbent for the removal of harmful dyes from waste-water.

Keywords: Fe3O4 magnetic nanoparticles, gum arabic, co-precipitation, adsorption dye, methylene blue, adsorption isotherm

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Authors: Gul Afreen, Sreedevi Upadhyayula, Mahendra K. Sunkara

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One-dimensional (1D) nanostructures like nanowires, nanotubes, and nanorods find variety of practical application owing to their unique physico-chemical properties. In this work, TiO₂ nanowires were synthesized by direct oxidation of titanium particles in a unique microwave plasma jet reactor. The prepared TiO₂ nanowires manifested the flexible features, and were characterized by using X-ray diffraction, Brunauer-Emmett-Teller (BET) surface area analyzer, UV-Visible and FTIR spectrophotometers, Scanning electron microscope, and Transmission electron microscope. Further, the photodegradation efficiency of these nanowires were tested against toxic organic dye like methylene blue (MB) and the results were compared with the commercial TiO₂. It was found that TiO₂ nanowires exhibited superior photocatalytic performance (89%) as compared to commercial TiO₂ (75%) after 60 min of reaction. This is attributed to the lower recombination rate and increased interfacial charge transfer in TiO₂ nanowire. Pseudo-first order kinetic modelling performed with the experimental results revealed that the rate constant of photodegradation in case of TiO₂ nanowire was 1.3 times higher than that of commercial TiO₂. Superoxide radical (O₂˙⁻) was found to be the major contributor in the photodegradation mechanism. Based on the trapping experiments, a plausible mechanism of the photocatalytic reaction is discussed.

Keywords: heterogeneous catalysis, photodegradation, reactive oxygen species, TiO₂ nanowires

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Authors: Sakshi Tomar, Renu Chadha

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Cocrystallization comprises a selective route to the intensive design of pharmaceutical products with desired physiochemical and pharmacokinetic properties. The present study is focused on the preparation, characterization, and evaluation of etodolac (ET) co-crystals with coformers nicotinamide (ETNI) and Glutaric acid (ETGA), using cocrystallization approach. Preliminarily examination of the prepared co-crystal was done by differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FT-IR), powder X-ray diffraction (PXRD). DSC thermographs of ETNI and ETGA cocrystals showed single sharp melting endotherms at 144°C and 135°C, respectively, which were different from the melting of drugs and coformers. FT-IR study points towards carbonyl-acid interaction sandwiched between the involving molecules. The emergence of new peaks in the PXRD pattern confirms the formation of new crystalline solid forms. Both the cocrystals exhibited better apparent solubility, and 3.8-5.0 folds increase in IDR were established, as compared to pure etodolac. Evaluations of these solid forms were done using anti-osteoarthritic activities. All the results indicate that etodolac cocrystals possess better anti-osteoarthritic efficacy than free drug. Thus loom of cocrystallization has been found to be a viable approach to resolve the solubility and bioavailability issues that circumvent the use of potential antiosteoarthritic molecules.

Keywords: bioavailability, etodolac, nicotinamide, osteoarthritis

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Authors: Uchenna Sydney Mbamara, Bolu Olofinjana, Ezekiel Oladele B. Ajayi

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Elaborate surface metrology of undoped ZnO thin films, deposited by organometallic chemical vapour deposition (OMCVD) technique at different precursor flow rates, was carried out. Dicarbomethyl-zinc precursor was used. The films were deposited on AISI304L steel and soda-lime glass substrates. Ultraviolet-visible-near-infrared (UV-Vis-NIR) spectroscopy showed that all the thin films were over 80% transparent, with an average bandgap of 3.39 eV, X-ray diffraction (XRD) results showed that the thin films were crystalline with a hexagonal structure, while Rutherford backscattering spectroscopy (RBS) results identified the elements present in each thin film as zinc and oxygen in the ratio of 1:1. Microscope and contactless profilometer results gave images with characteristic colours. The profilometer also gave the surface roughness data in both 2D and 3D. The asperity distribution of the thin film surfaces was Gaussian, while the average fractal dimension Da was in the range of 2.5 ≤ Da. The metrology proved the surfaces good for ‘touch electronics’ and coating mechanical parts for low friction.

Keywords: undoped ZnO, precursor flow rate, OMCVD, thin films, surface texture, tribology

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Authors: Radia Bagtache, Karima Boudjedien, Ahmed Malek Djaballah, Mohamed Trari

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The compounds with a spinel structure have received special attention because of their numerous applications in electronics, magnetism, catalysis, electrocatalysis, photocatalysis, etc. Among these oxides, CuCo₂O₄ was selected because of its optimal band gap, very close to the ideal value for solar devices, its low cost, and a potential candidate in the field of energy storage. Herein, we reported the junction Ag/CuCo₂O₄ (5/95 % wt.) prepared by co-precipitation, characterized physically and photo electrochemically. Moreover, its performance was evaluated for the oxidation of methyl orange (MO) under solar light. The X-ray diffraction exhibited narrow peaks ascribed to the spinel CuCo₂O₄ and Ag. The SEM analysis displayed grains with regular shapes. The band gap of CuCo₂O₄ (1.38 eV) was deducted from the diffuse reflectance, and this value decreased down to 1.15 eV due to the synergy effect in the junction. The current-potential (J-E) curve plotted in Na₂SO₄ electrolyte showed a medium hysteresis, characteristic of good chemical stability. The capacitance-2 – potential (C⁻² – E) graph displayed that the spinel behaves as a p-type semiconductor, a property supported by chrono-amperometry. The conduction band, located at 4.05 eV (-0.94 VNHE), was made up of Co³⁺: 3d orbital. The result showed a total discoloration of MO after 2 h of illumination under solar light.

Keywords: junction Ag/CuCo₂O₄, semiconductor, environment, sunlight, characterization, depollution

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Authors: Hoda Aleali, Nastran Mansour, Maryam Mirzaie

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In this paper, we study the optical nonlinearities of Silver sulfide (Ag2S) nanostructures dispersed in the Dimethyl sulfoxide (DMSO) under exposure to 532 nm, 15 nanosecond (ns) pulsed laser irradiation. Ultraviolet–visible absorption spectrometry (UV-Vis), X-ray diffraction (XRD), and transmission electron microscopy (TEM) are used to characterize the obtained nanocrystal samples. The band gap energy of colloid is determined by analyzing the UV–Vis absorption spectra of the Ag2S NPs using the band theory of semiconductors. Z-scan technique is used to characterize the optical nonlinear properties of the Ag2S nanoparticles (NPs). Large enhancement of two photon absorption effect is observed with increase in concentration of the Ag2S nanoparticles using open Z-scan measurements in the ns laser regime. The values of the nonlinear absorption coefficients are determined based on the local nonlinear responses including two photon absorption. The observed aperture dependence of the Ag2S NP limiting performance indicates that the nonlinear scattering plays an important role in the limiting action of the sample.The concentration dependence of the optical liming is also investigated. Our results demonstrate that the optical limiting threshold decreases with increasing the silver sulfide NPs in DMSO.

Keywords: nanoscale materials, silver sulfide nanoparticles, nonlinear absorption, nonlinear scattering, optical limiting

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Authors: Hannatu Abubakar Sani, Abubakar Umar Birnin Yauri, Aliyu Muhammad, Mujahid Salau, Aminu Musa, Hadiza Adamu Kwazo

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The increase in the global population and advances in technology have made plastic materials to have wide applications in every aspect of life. However, the non-biodegradability of these petrochemical-based materials and their increasing accumulation in the environment has been a threat to the planet and has been a source of environmental concerns and hence, the driving force in the search for ‘green’ alternatives for which agricultural waste remains the front liner. Sorghum husk, an agricultural waste with potentials as a raw material in the production of bioplastic, was used in this research to prepare bioplastic using sulphuric acid-catalyzed acetylation process. The prepared bioplastic was characterized by X-ray diffraction and Fourier transform infrared spectroscopy (FTIR), and the structure of the prepared bioplastic was confirmed. The Fourier transform infrared spectroscopy (FTIR) spectra of the product displayed the presence of OH, C-H, C=O, and C-O absorption peaks. The bioplastic obtained is biodegradable and is affected by acid, salt, and alkali to a lesser extent. Other tests like solubility and swelling studies were carried out to ensure the commercial properties of these bioplastic materials. Therefore, this revealed that new bioplastics with better environmental and sustainable properties could be produced from agricultural waste, which may have applications in many industries.

Keywords: agricultural waste, bioplastic, characterization, Sorghum Husk

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Authors: A. P. Srivastava, D. Srivastava, D. J. Browne

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Relaxation dynamics of Zr44Cu40Al8Ag8 bulk metallic glass (BMG) has been probed using dynamic mechanical analyzer. The BMG sample was casted in the form of a plate of dimension 55 mm x 40 mm x 3 mm using tilt casting technique. X-ray diffraction and transmission electron microscope have been used for the microstructural characterization of as-cast BMG. For the mechanical spectroscopy study, samples in the form of a bar of size 55 mm X 2 mm X 3 mm were machined from the BMG plate. The mechanical spectroscopy was performed on dynamic mechanical analyzer (DMA) by 50 mm 3-point bending method in a nitrogen atmosphere. It was observed that two glass transition process were competing in supercooled liquid region around temperature 390°C and 430°C. The supercooled liquid state was completely characterized using DMA and differential scanning calorimeter (DSC). In addition to the main α-relaxation process, presence of β relaxation process around temperature 360°C; below the glass transition temperature was also observed. The β relaxation process could be described by Arrhenius law with the activation energy of 160 kJ/mole. The volume of the flow unit associated with this relaxation process has been estimated. The results from DMA study has been used to characterize the shear transformation zone in terms of activation volume and size. High fragility parameter value of 34 and higher activation volume indicates that this alloy could show good plasticity in supercooled liquid region. The possible mechanism for the relaxation processes has been discussed.

Keywords: DMA, glass transition, metallic glass, thermoplastic forming

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Authors: Kanika Sharma, Shaila Bahl, Birendra Singh, Pratik Kumar, S. P. Lochab, A. Pandey

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In the present investigation, initially nano-particles of CaF2 were prepared by the chemical co-precipitation method and later the prepared salt was activated by thulium (0.1 mol%) using the combustion technique. The final product was characterized and confirmed by X-Ray diffraction (XRD) and transmission electron microscopy (TEM). Further, the thermoluminescence (TL) properties of the nanophosphor were studied by irradiating it with 1.25 MeV of gamma radiation and 65 MeV of carbon (C6+) ion beam. For gamma rays, two prominent TL peaks were observed with a low temperature peak at around 1070C and a high temperature peak at around 1570C. Furthermore, the nanophosphor maintained a linear TL response for the entire range of studied doses i.e. 10 Gy to 2000 Gy for both the temperature peaks. Moreover, when the nanophosphor was irradiated with 65 MeV of C6+ ion beam the shape and structure of the glow curves remained spectacularly similar and the nanophosphor displayed a linear TL response for the full range of studied fluences i.e. 5*1010 ions/cm2 to 1 *1012 ions/ cm2. Finally, various tests like reproducibility test and batch homogeneity were also carried out to define the final product. Thus, co-precipitation method followed by combustion technique was successful in effectively producing dosimetric grade CaF2:Tm for dosimetry of gamma as well as carbon (C6+) beam.

Keywords: gamma radiation, ion beam, nanocrystalline, radiation dosimetry

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Authors: Meryem Imane Babaghayou, Asma Abdelhafidi, Salem Fouad Chabira, Mohammed Sebaa

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A challenge of plastics industries is the realization of materials that resist the degradation in its application environment, and that to guarantee a longer life time therefore an optimal time of use. Blown extruded films of low-density polyethylene (LDPE) supplied by SABIC SAUDI ARABIA blown and extruded in SOFIPLAST company in Setif ALGERIA , have been subjected to climatic ageing in a sub-Saharan facility at Laghouat (Algeria) with direct exposure to sun. Samples were characterized by X-ray diffraction (XRD) and differential scanning calorimetry (DSC) techniques after prescribed amounts of time up to 8 months. It has been shown via these two techniques the impact of UV irradiation on the morphological development of a plastic material, especially the crystallinity degree which increases with exposure time. The reason of these morphological changes is related to photooxidative reactions leading to cross linking in the beginning and to chain scissions for an advanced stage of ageing this last ones are the first responsible. The crystallinity degree change is essentially controlled by the secondary crystallization of the amorphous chains whose mobility is enhanced by the chain scission processes. The diffusion of these short segments integrates the surface of the lamellae increasing in this way their thicknesses. The results presented highlight the complexity of the involved phenomena.

Keywords: Low Density poly (Ethylene), crystallinity, ageing, XRD, DSC

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Authors: Victor Chinecherem Ejeke, Raphael Eze Nnam

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The main objective of this research is to produce biodiesel from waste vegetable oil using activated eggshell waste as solid catalysts. A transesterification reaction was performed for the conversion to biodiesel. Waste eggshells were calcined at 700°C, 800°C and 900°C for a time period of 3hrs for the preparation of the renewable catalyst. The calcined waste eggshell catalyst was characterized using X-Ray Florescence (XRF) Spectroscopy, which revealed CaO as the major constituent (90.86%); this was further confirmed by X-Ray Diffraction (XRD) and Fourier Transform Infrared (FTIR) analyses. The prepared catalyst was used for transesterification reaction and the effects of calcination temperature (700 to 900°C), Deep Eutectic Solvent DES loading (3 to 18 wt. %), Waste Egg Shell (WES) catalyst loading (6 to 14 wt. %) on the conversion to biodiesel were studied. The yield of biodiesel using a waste eggshell catalyst (91%) is comparable to conventional catalyst like sodium hydroxide with a yield of 80-90%. The maximum biodiesel production yield was obtained at a specific oil-to methanol molar ratio of 1:10, a temperature of 65°C and a catalyst loading of 14g-wt%. The biodiesel produced was characterized as being composed of methyl Tetradecanoate (C₁₄H₂₈O₂) 30.92% using the Gas Chromatographic (GC-MS) analysis. The fuel properties of the biodiesel (Flashpoint 138ᵒC) were comparable to commercial diesel, and hence it can be used in compression-ignition engines. The results indicated that the catalysts derived from waste eggshell had high potential to be used as biodiesel production catalysts in transesterification of waste vegetable oil with the advantage of reusability and also not requiring water washing steps.

Keywords: waste vegetable oil, catalyst , biodiesel , waste egg shell

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Authors: Rashad Al-Gaashani

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The physicochemical activation method was used to produce high-quality activated carbon (AC) with a large surface area of about 2000 m2/g from low-cost and abundant biomass wastes in Qatar, namely date seeds. X-Ray diffraction (XRD), scanning electron spectroscopy (SEM), energy dispersive X-Ray spectroscopy (EDS), and Brunauer-Emmett-Teller (BET) surface area analysis was used to evaluate the AC samples. AC produced from date seeds has a wide range of pores available, including micro- and nano-pores. This type of AC with a well-developed pore structure may be very attractive for different applications, including air and water purification from micro and nano pollutants. Heavy metals iron (III) and copper (II) ions were removed from wastewater using the AC produced using a batch adsorption technique. The AC produced from date seeds biomass wastes shows high removal of heavy metals such as iron (III) ions (100%) and copper (II) ions (97.25%). The highest removal of copper (II) ions (100%) with AC produced from date seeds was found at pH 8, whereas the lowest removal (22.63%) occurred at pH 2. The effect of adsorption time, adsorbent dose, and pH on the removal of heavy metals was studied.

Keywords: activated carbon, date seeds, biomass, heavy metals removal, water treatment

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Authors: S. Said, Asmaa A. Abdulrahman

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MoOₓ/Al₂O₃ based catalyst has long been widely used as an active catalyst in oxidative desulfurization reaction due to its high stability under severe reaction conditions and high resistance to sulfur poisoning. In this context, 4 & 9wt.% MoO₃ grafted on mesoporous γ-Al₂O₃ has been synthesized using the modified atomic layer deposition (ALD) method. Another MoO₃/Al₂O₃ sample was prepared by the conventional wetness impregnation (IM) method, for comparison. The effect of the preparation methods on the metal-support interaction was evaluated using different characterization techniques, including X-ray diffraction, X-ray photoelectron spectroscopy (XPS), N₂-physisorption, transmission electron microscopy (TEM), H₂- temperature-programmed reduction and FT-IR. Oxidative desulfurization (ODS) reaction of the model fuel oil was used as a probe reaction to examine the catalytic efficiency of the prepared catalysts. ALD method led to samples with much better physicochemical properties than those of the prepared one via the impregnation method. However, the 9 wt.%MoO₃/Al₂O₃ (ALD) catalyst in the ODS reaction of model fuel oil shows enhanced catalytic performance with ~90%, which has been attributed to the more Mo⁶⁺ surface concentrations relative to Al³⁺ with large pore diameter and surface area. The kinetic study shows that the ODS of DBT follows a pseudo first-order rate reaction.

Keywords: mesoporous Al₂O₃, xMoO₃/Al₂O₃, atomic layer deposition, wetness impregnation, ODS, DBT

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Authors: Nuray Güy, Mahmut Özacar

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In the past few decades, considerable attention has been devoted to the photocatalysts for the photocatalytic degradation of environmental pollutants. Many novel nanostructured photocatalysts for wastewater treatment have been investigated, such as TiO2 and, CdS, ZnO and silver halides (AgX, X = Cl, Br, I). The silver halides are photosensitive materials which can absorb photons in the visible region to produce electron–hole pairs. Silver halides are expensive that restricts their applications in large-scale photocatalytic processes. Tannin contains hydroxyl functional groups, it was employed as a modifier to improve the surface properties and adsorption capacity of the activated carbon towards the metal cations uptake. In this work, we designed a new structure of magnetically separable photocatalyst that combines AgCl/ZnO nanoparticles with Fe3O4 nanoparticles deposited on tannin, which was denoted as (AgI/ZnO)-Fe3O4/Tannin. The as-prepared products are characterized by X-ray diffraction (XRD), field emission scanning electron microscope (FESEM), Fourier transform infrared (FTIR), diffuse reflectance spectra (DRS) and vibrating sample magnetometer (VSM). The photocatalyst exhibited high activity degrading a textile dye under visible light irradiation. Moreover, the excellent magnetic property gives a more convenient way to recycle the photocatalysts.

Keywords: AgI/ZnO-Fe3O4/Tannin, visible light, magnetically separable, photocatalyst

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Authors: Mehdi Rahimi-Nasrabadi, Seied Mahdi Pourmortazavi

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Taguchi robust design as a statistical method was applied for optimization of the process parameters in order to tunable, simple and fast synthesis of europium (III) tungstate nanoparticles. Europium (III) tungstate nanoparticles were synthesized by a chemical precipitation reaction involving direct addition of europium ion aqueous solution to the tungstate reagent solved in aqueous media. Effects of some synthesis procedure variables i.e., europium and tungstate concentrations, flow rate of cation reagent addition, and temperature of reaction reactor on the particle size of europium (III) tungstate nanoparticles were studied experimentally in order to tune particle size of europium (III) tungstate. Analysis of variance shows the importance of controlling tungstate concentration, cation feeding flow rate and temperature for preparation of europium (III) tungstate nanoparticles by the proposed chemical precipitation reaction. Finally, europium (III) tungstate nanoparticles were synthesized at the optimum conditions of the proposed method and the morphology and chemical composition of the prepared nano-material were characterized by means of X-Ray diffraction, scanning electron microscopy, transmission electron microscopy, FT-IR spectroscopy, and fluorescence.

Keywords: europium (III) tungstate, nano-material, particle size control, procedure optimization

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Authors: Christian C. Vaso, Rinlee Butch M. Cervera

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One of the most promising anode materials for solid oxide electrolysis cell (SOEC) application is the Sr-doped LaMnO₃ (LSM) which is known to have a high electronic conductivity but low ionic conductivity. To increase the ionic conductivity or diffusion of ions through the anode, Yttria-stabilized Zirconia (YSZ), which has good ionic conductivity, is proposed to be combined with LSM to create a composite electrode and to obtain a high mixed ionic and electronic conducting anode. In this study, composite of lanthanum strontium manganite and YSZ oxide, La_0.8Sr_0.2MnO₃/Zr_0.92Y_0.08O₂ (LSM/YSZ), with different wt.% compositions of LSM and YSZ were synthesized using solid-state reaction. The obtained prepared composite samples of 60, 50, and 40 wt.% LSM with remaining wt.% of 40, 50, and 60, respectively for YSZ were fully characterized for its microstructure by using powder X-ray diffraction (XRD), Thermogravimetric analysis (TGA), Fourier transform infrared (FTIR), and Scanning electron microscope/Energy dispersive spectroscopy (SEM/EDS) analyses. Surface morphology of the samples via SEM analysis revealed a well-sintered and densified pure LSM, while a more porous composite sample of LSM/YSZ was obtained. Electrochemical impedance measurements at intermediate temperature range (500-700 °C) of the synthesized samples were also performed which revealed that the 50 wt.% LSM with 50 wt.% YSZ (L50Y50) sample showed the highest total conductivity of 8.27x10^-1 S/cm at 600 ^oC with 0.22 eV activation energy.

Keywords: ceramics, microstructure, fuel cells, electrochemical impedance spectroscopy

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Authors: H. Boucheloukh, S. Rouissa, N. Aoun, M. Beloucifa, T. Sehili, F. Parrino, V. Loddo

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To optimize water purification and wastewater treatment by heterogeneous photocatalysis, we used NiFe₂O₄ as a catalyst and solar irradiation as a source of energy. In this concept, an organic substance present in many industrial effluents was chosen: naproxen ((S)-6-methoxy-α-methyl-2-naphthaleneacetic acid or 2-(6-methoxynaphthalenyl) propanoic), a non-steroidal anti-inflammatory drug. The main objective of this study is to degrade naproxen by an iron and nickel catalyst, the degradation of this organic pollutant by nickel ferrite has been studied in a heterogeneous aqueous medium, with the study of the various factors influencing photocatalysis such as the concentration of matter and the acidity of the medium. The photocatalytic activity was followed by HPLC-UV andUV-Vis spectroscopy. A first-order kinetic model appropriately fitted the experimental data. The degradation of naproxen was also studied in the presence of H₂O₂ as well as in an aqueous solution. The new hetero-system NiFe₂O₄/oxalic acid is also discussed. The fastest naproxen degradation was obtained with NiFe₂O₄/H₂O₂. In a first-place, we detailed the characteristics of the material NiFe₂O₄, which was synthesized by the sol-gel methods, using various analytical techniques: visible UV spectrophotometry, X-ray diffraction, FTIR, cyclic voltammetry, luminescent discharge optical emission spectroscopy.

Keywords: naproxen, nickelate, photocatalysis, oxalic acid

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Authors: Friday Godwin Okibe, Christian Chinweuba Onoyima, Edith Bolanle Agbaji, Victor Olatunji Ajibola

Abstract:

Polymer-inorganic nanocomposites are presently impacting diverse areas, specifically in biomedical sciences. In this research, hydroxyapatite-sodium alginate has been prepared, and characterized, with emphasis on the influence of sodium alginate on its characteristics. In situ wet chemical precipitation method was used in the preparation. The prepared nanocomposite was characterized with Fourier Transform Infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM), with image analysis, and X-Ray Diffraction (XRD). The FTIR study shows peaks characteristics of hydroxyapatite and confirmed formation of the nanocomposite via chemical interaction between sodium alginate and hydroxyapatite. Image analysis shows the nanocomposites to be of irregular morphologies which did not show significant change with increasing sodium alginate addition, while particle size decreased with increase in sodium alginate addition (359.46 nm to 109.98 nm). From the XRD data, both the crystallite size and degree of crystallinity also decreased with increasing sodium alginate composition (32.36 nm to 9.47 nm and 72.87% to 1.82% respectively), while the specific surface area and microstrain increased with increasing sodium alginate composition (0.0041 to 0.0139 and 58.99 m²/g to 201.58 m²/g respectively). The results show that the formulation with 50%wt of sodium alginate (HASA-50%wt), possess exceptional characteristics for biomedical applications such as drug delivery.

Keywords: nanocomposite, sodium alginate, hydroxyapatite, biomedical, FTIR, XRD, SEM

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Authors: Mulatu Kassie Birhanu

Abstract:

Electro-oxidation of glycerol is an important process to convert the less price glycerol into other expensive (essential) and energy-rich chemicals. In this study, nickel was electro-deposited on laboratory-made carbon ceramic electrode (CCE) substrate using electrochemical techniques that is cyclic voltammetry (CV) to prepare an electro-catalyst (Ni/CCE) for electro-oxidation of glycerol. Carbon ceramic electrode was prepared from graphite and methyl tri-methoxy silane (MTMOS) through the processes called hydrolysis and condensation with methanol in acidic media (HCl) by a sol-gel technique. Physico-chemical characterization of bare CCE and modified (deposited) CCE (Ni/CCE) was measured and evaluated by Fourier Transform Infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM) and X-ray diffraction (XRD). Electro-oxidation of glycerol was performed in 0.1 M glycerol in alkaline media (0.5 M NaOH). High-Performance Liquid Chromatography (HPLC) technique was used to identify and determine the concentration of glycerol, reaction intermediates and oxidized products of glycerol after its electro-oxidation is performed. The conversion (%) of electro-oxidation of glycerol during 9-hour oxidation was 73% and 36% at 1.8V and 1.6V vs. RHE, respectively. Formate, oxalate, glycolate and glycerate are the main oxidation products of glycerol with selectivity (%) of 75%, 8.6%, 1.1% and 0.95 % at 1.8 V vs. RHE and 55.4%, 2.2%, 1.0% and 0.6% at 1.6 V vs. RHE respectively. The result indicates that formate is the main product in the electro-oxidation of glycerol on Ni/CCE using the indicated applied potentials.

Keywords: carbon-ceramic electrode, electrodeposition, electro-oxidation, Methyltrimethoxysilane

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Authors: Pankaj Verma, Gagandeep Singh Walia, Padma Devi, H. P. Singh

Abstract:

Code Division Multiple Access 2000 operates on various RF channel bandwidths 1.2288 or 3.6864 Mcps. CDMA offers high bandwidth and wireless broadband services but the efficiency gets decreased because of many interfering factors like fading, interference, scattering, diffraction, refraction, reflection etc. To reduce the spectral bandwidth is one of the major concerns in modern day technology and this is achieved by pulse shaping filter. This paper investigates the effect of diversity (MRC), interpolation factor in Root Raised Cosine (RRC) filter for the QPSK and BPSK modulation schemes. It is made possible to send information with minimum inter symbol interference and within limited bandwidth with proper pulse shaping technique. Bit error rate (BER) performance is analyzed by applying diversity technique by varying the interpolation factor for Binary Phase Shift Keying (BPSK) and Quadrature Phase Shift Keying (QPSK). Interpolation factor increases the original sampling rate of a sequence to a higher rate and reduces the interference and diversity reduces the fading.

Keywords: CDMA2000, root raised cosine, roll off factor, ISI, diversity, interference, fading

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Authors: A. M. Metak, T. T. Ajaal, Amal Metak, Tawfik Ajaal

Abstract:

Commercial nanocomposite food packaging type nano-silver containers were characterised using scanning electron microscopy (SEM) and energy-dispersive X-Ray spectroscopy (EDX). The presence of nanoparticles consistent with the incorporation of 1% nano-silver (Ag) and 0.1% titanium dioxide (TiO2) nanoparticle into polymeric materials formed into food containers was confirmed. Both nanomaterials used in this type of packaging appear to be embedded in a layered configuration within the bulk polymer. The dimensions of the incorporated nanoparticles were investigated using X-Ray diffraction (XRD) and determined by calculation using the Scherrer Formula; these were consistent with Ag and TiO2 nanoparticles in the size range 20-70nm both were spherical shape nanoparticles. Antimicrobial assessment of the nanocomposite container has also been performed and the results confirm the antimicrobial activity of Ag and TiO2 nanoparticles in food packaging containers. Migration assessments were performed in a wide range of food matrices to determine the migration of nanoparticles from the packages. The analysis was based on the relevant European safety directives and involved the application of inductively coupled plasma mass spectrometry (ICP-MS) to identify the range of migration risk. The data pertain to insignificance levels of migration of Ag and TiO2 nanoparticles into the selected food matrices.

Keywords: nano-silver, antimicrobial food packaging, migration, titanium dioxide

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Authors: Amine.Harbia, Hicham. Moutaabbidb, Yann. Le Godecb, Said. Benmokhtara, Mouhammed. Moutaabbida

Abstract:

This study explores the structural and magnetic characteristics of newly synthesized double perovskite oxides, La₂NiₓCo1-xMnO₆, with x ranging from 0.2 to 0.8. Utilizing X-ray powder diffraction and SQUID magnetometry, we analyzed the compounds that consistently exhibit a monoclinic structure with the P21/n space group at ambient temperature. it findings reveal that as Ni2+ is progressively substituted by Co2+, there is a corresponding decrease in cell parameters, attributable to the smaller ionic radius of Ni2+ (0.69 Å) compared to Co2+ (0.74 Å). The crystal structure features octahedrally coordinated (Co/Ni)2+ and Mn4+ cations with oxygen, forming (Co/Ni)O6 and MnO6 octahedra linked via oxygen atoms along different crystallographic axes. Magnetic characterization conducted over a temperature range of 2 to 300 K in both DC and AC magnetic fields, showed a predominant paramagnetic to ferromagnetic transition between 232 K and 260 K, with the Curie temperature notably increasing with higher x values. Samples with x=0.2, 0.25, and 0.5 exhibited a secondary PM-FM transition between 200 K and 208 K. Cation ordering was quantitatively assessed, indicating a higher ordering in Ni2+-rich samples (x=0.75 and 0.8) at over 96%, whereas the sample with x=0.25 showed minimal ordering. Furthermore, the out-of-phase component of the AC susceptibility displayed frequency-dependent transitions between 65 K and 110 K, suggesting the presence of superparamagnetic domains across all samples.

Keywords: double perovskite oxides, magnetic transitions, cation ordering, squid magnetometry

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Authors: I. Ben Kaddour, S. Larbaoui

Abstract:

Since their first synthesis, the Silicoaluminophosphates materials have proved their efficiency as a good adsorbent and catalyst in several environmental and energetic applications. In this work, the photocatalytic hydrogen production from water splitting reactions has been conducted under visible radiations in the presence of a series of iron and/or titanium-containing microporous silico-alumino-phosphates materials synthesized by hydrothermal method, using triethylamine as an organic structuring agent to obtain the AFI structure type. These photo-catalysts were then characterized by various physicochemical methods to determine their structural, textural and morphological properties such as X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FTIR), scanning electron microscopy (SEM) coupled with X rays microanalysis, nitrogen adsorption measurements, UV-visible diffuse reflectance spectroscopy (UV-Vis-DRS), and X-rays photoelectron spectroscopy (XPS) and the analysis revealed that these materials have significant photocatalytic properties. The hydrogen production process has been followed by photoelectrochemical characterization (PEC). The results showed that hydrogen is the only gas produced, and the reaction takes place in the conduction band where water is reduced to hydrogen. The electron recombination has also been avoided, as holes are entrapped using hole scavengers. In addition, these catalysts have been shown to remain stable during reuse for up to five cycles.

Keywords: photocatalysis, SAPO-5, hydrothermal synthesis, hydrogen production

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Authors: Mariano Gonzalez Cortina, Pablo Saiz Martinez, Francisco Fernandez Martinez, Antonio Rodriguez Sanchez

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Construction sector incessant activity of the last years preceding the crisis has originated a high waste generation and an increased use of raw materials. The main aim of this research is to compare three types of recycled aggregates and the feasibility to incorporate them into masonry mortar fabrication. The tests were developed using two types of binders: CEM II/B-L 32.5 N and CEM IV/B (V) 32.5 N. 50%, 75% and 100% of natural sand were replaced with three types of recycled aggregates. Cement-to-aggregate by dry weight proportions were 1:3 and 1:4. Physical and chemical characterization of recycled aggregates showed continues particle size distribution curve, lower density and higher absorption, which was the reason to use additive to obtain required mortar consistency. Main crystalline phases determined in the X-Ray diffraction test were calcite, quartz, and gypsum. Performed tests show that cement-based mortars fabricated with CEM IV/B (V) 32. 5 N can incorporate recycled aggregates coming from ceramic, concrete and mixed recycling processes, using 1:3 and 1:4 cement-to-aggregate proportions, complying with the limits established by the Spanish standards. It was concluded that recycled mortar coming from concrete recycling process is the one which presents better characteristics.

Keywords: construction and demolition waste, masonry mortar, mechanical properties, recycled aggregate, waste treatment

Procedia PDF Downloads 423