Search results for: diffraction

Authors: Luís F. da Silva, Ariadne C. Catto, Osmando F. Lopes, Khalifa Aguir, Valmor R. Mastelaro, Caue Ribeiro, Elson Longo

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Gas detection is important for controlling industrial, and vehicle emissions, agricultural residues, and environmental control. In last decades, several semiconducting oxides have been used to detect dangerous or toxic gases. The excellent gas-sensing performance of these devices have been observed at high temperatures (~250 °C), which forbids the use for the detection of flammable and explosive gases. In this way, ultraviolet light activated gas sensors have been a simple and promising alternative to achieve room temperature sensitivity. Among the semiconductor oxides which exhibit a good performance as gas sensor, the zinc oxide (ZnO) and tin oxide (SnO2) have been highlighted. Nevertheless, their poor selectivity is the main disadvantage for application as gas sensor devices. Recently, heterostructures combining these two semiconductors (ZnO-SnO2) have been studied as an alternative way to enhance the gas sensor performance (sensitivity, selectivity, and stability). In this work, we investigated the influence of mass ratio Zn:Sn on the properties of ZnO-SnO2 nanocomposites prepared by hydrothermal treatment for 4 hours at 200 °C. The crystalline phase, surface, and morphological features were characterized by X-ray diffraction (XRD), high-resolution transmission electron (HR-TEM), and X-ray photoelectron spectroscopy (XPS) measurements. The gas sensor measurements were carried out at room-temperature under ultraviolet (UV) light irradiation using different ozone levels (0.06 to 0.61 ppm). The XRD measurements indicate the presence of ZnO and SnO2 crystalline phases, without the evidence of solid solution formation. HR-TEM analysis revealed that a good contact between the SnO2 nanoparticles and the ZnO nanorods, which are very important since interface characteristics between nanostructures are considered as challenge to development new and efficient heterostructures. Electrical measurements proved that the best ozone gas-sensing performance is obtained for ZnO:SnO2 (50:50) nanocomposite under UV light irradiation. Its sensitivity was around 6 times higher when compared to SnO2 pure, a traditional ozone gas sensor. These results demonstrate the potential of ZnO-SnO2 heterojunctions for the detection of ozone gas at room-temperature when irradiated with UV light irradiation.

Keywords: hydrothermal, zno-sno2, ozone sensor, uv-activation, room-temperature

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Authors: Sohini Manna, Jong Woo Kim, Oleg Shpyrko, Eric E. Fullerton

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CVD techniques have emerged as a promising approach in the formation of a broad range of nanostructured materials. The realization of many practical applications will require efficient and economical synthesis techniques that preferably avoid the need for templates or costly single-crystal substrates and also afford process adaptability. Towards this end, we have developed a single-step route for the reduction-type synthesis of nanostructured Ni materials using a thermal CVD method. By tuning the CVD growth parameters, we can synthesize morphologically dissimilar nanostructures including single-crystal cubes and Au nanostructures which form atop untreated amorphous SiO2||Si substrates. An understanding of the new properties that emerge in these nanostructures materials and their relationship to function will lead to for a broad range of magnetostrictive devices as well as other catalysis, fuel cell, sensor, and battery applications based on high-surface-area transition-metal nanostructures. We use coherent X-ray diffraction imaging technique to obtain 3-D image and strain maps of individual nanocrystals. Coherent x-ray diffractive imaging (CXDI) is a technique that provides the overall shape of a nanostructure and the lattice distortion based on the combination of highly brilliant coherent x-ray sources and phase retrieval algorithm. We observe a fine interplay of reduction of surface energy vs internal stress, which plays an important role in the morphology of nano-crystals. The strain distribution is influenced by the metal-substrate interface and metal-air interface, which arise due to differences in their thermal expansion. We find the lattice strain at the surface of the octahedral gold nanocrystal agrees well with the predictions of the Young-Laplace equation quantitatively, but exhibits a discrepancy near the nanocrystal-substrate interface resulting from the interface. The strain in the bottom side of the Ni nanocube, which is contacted on the substrate surface is compressive. This is caused by dissimilar thermal expansion coefficients between Ni nanocube and Si substrate. Research at UCSD support by NSF DMR Award # 1411335.

Keywords: CVD, nanostructures, strain, CXRD

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Authors: H. Ferfera-Harrar, T. Benhalima, D. Lerari

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Contamination of water, due to the discharge of untreated industrial wastewaters into the ecosystem, has become a serious problem for many countries. In this study, bioadsorbents based on chitosan-g-poly(acrylamide) and montmorillonite (MMt) clay (CTS-g-PAAm/MMt) hydrogel nanocomposites were prepared via free‐radical grafting copolymerization and crosslinking of acrylamide monomer (AAm) onto natural polysaccharide chitosan (CTS) as backbone, in presence of various contents of MMt clay as nanofiller. Then, they were hydrolyzed to obtain highly functionalized pH‐sensitive nanomaterials with uppermost swelling properties. Their structure characterization was conducted by X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM) analyses. The adsorption performances of the developed nanohybrids were examined for removal of methylene blue (MB) cationic dye from aqueous solutions. The factors affecting the removal of MB, such as clay content, pH medium, adsorbent dose, initial dye concentration and temperature were explored. The adsorption process was found to be highly pH dependent. From adsorption kinetic results, the prepared adsorbents showed remarkable adsorption capacity and fast adsorption rate, mainly more than 88% of MB removal efficiency was reached after 50 min in 200 mg L^-1 of dye solution. In addition, the incorporating of various content of clay has enhanced adsorption capacity of CTS-g-PAAm matrix from 1685 to a highest value of 1749 mg g^-1 for the optimized nanocomposite containing 2 wt.% of MMt. The experimental kinetic data were well described by the pseudo-second-order model, while the equilibrium data were represented perfectly by Langmuir isotherm model. The maximum Langmuir equilibrium adsorption capacity (q_m) was found to increase from 2173 mg g⁻¹ until 2221 mg g⁻¹ by adding 2 wt.% of clay nanofiller. Thermodynamic parameters revealed the spontaneous and endothermic nature of the process. In addition, the reusability study revealed that these bioadsorbents could be well regenerated with desorption efficiency overhead 87% and without any obvious decrease of removal efficiency as compared to starting ones even after four consecutive adsorption/desorption cycles, which exceeded 64%. These results suggest that the optimized nanocomposites are promising as low cost bioadsorbents.

Keywords: chitosan, clay, dye adsorption, hydrogels nanocomposites

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Authors: Uttam Kumar Ghorai, Madhupriya Samanta, Subhajit Saha, Swati Das, Nilesh Mazumder, Kalyan Kumar Chattopadhyay

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Organic semiconductors have gained potential interest in the last few decades for their significant contributions in the various fields such as solar cell, non-volatile memory devices, field effect transistors and light emitting diodes etc. The most important advantages of using organic materials are mechanically flexible, light weight and low temperature depositing techniques. Recently with the advancement of nanoscience and technology, one dimensional organic and inorganic nanostructures such as nanowires, nanorods, nanotubes have gained tremendous interests due to their very high aspect ratio and large surface area for electron transport etc. Among them, self-assembled organic nanostructures like Copper, Zinc Phthalocyanine have shown good transport property and thermal stability due to their π conjugated bonds and π-π stacking respectively. Field emission properties of inorganic and carbon based nanostructures are reported in literatures mostly. But there are few reports in case of cold cathode emission characteristics of organic semiconductor nanostructures. In this work, the authors report the field emission characteristics of chemically and physically synthesized Copper Phthalocyanine (CuPc) nanostructures such as nanowires, nanotubes and nanotips. The as prepared samples were characterized by X-Ray diffraction (XRD), Ultra Violet Visible Spectrometer (UV-Vis), Fourier Transform Infra-red Spectroscopy (FTIR), and Field Emission Scanning Electron Microscope (FESEM) and Transmission Electron Microscope (TEM). The field emission characteristics were measured in our home designed field emission set up. The registered turn-on field and local field enhancement factor are found to be less than 5 V/μm and greater than 1000 respectively. The field emission behaviour is also stable for 200 minute. The experimental results are further verified by theoretically using by a finite displacement method as implemented in ANSYS Maxwell simulation package. The obtained results strongly indicate CuPc nanostructures to be the potential candidate as an electron emitter for field emission based display device applications.

Keywords: organic semiconductor, phthalocyanine, nanowires, nanotubes, field emission

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Authors: Hanaa A. Al-Gaoudi, Hassan Ebeid

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The research investigates the materials and processes used in the manufacturing of an Egyptian polychrome cartonnage mummy mask with the aim of dating this object and establishing trade patterns of certain materials that were used and available at the time of ancient Egypt. This anonymous-source object was held in the basement storage of the Egyptian Museum in Cairo (EMC) and has never been on display. Furthermore, there is no information available regarding its owner, provenance, date, and even the time of its possession by the museum. Moreover, the object is in a very poor condition where almost two-thirds of the mask was bent and has never received any previous conservation treatment. This research has utilized well-established multi-analytical methods to identify the considerable diversity of materials that have been used in the manufacturing of this object. These methods include Computed Tomography Scan (CT scan) to acquire detailed pictures of the inside physical structure and condition of the bended layers. Dino-Lite portable digital microscope, scanning electron microscopy with energy dispersive X-ray spectrometer (SEM-EDX), and the non-invasive imaging technique of multispectral imaging (MSI) to obtain information about the physical characteristics and condition of the painted layers and to examine the microstructure of the materials. Portable XRF Spectrometer (PXRF) and X-Ray powder diffraction (XRD) to identify mineral phases and the bulk element composition in the gilded layer, ground, and pigments; Fourier-transform infrared (FTIR) to identify organic compounds and their molecular characterization; accelerator mass spectrometry (AMS 14C) to date the object. Preliminary results suggest that there are no human remains inside the object, and the textile support is linen fibres with tabby weave 1/1 and these fibres are in a very bad condition. Several pigments have been identified, such as Egyptian blue, Magnetite, Egyptian green frit, Hematite, Calcite, and Cinnabar; moreover, the gilded layers are pure gold and the binding media in the pigments is Arabic gum and animal glue in the textile support layer.

Keywords: analytical methods, Egyptian museum, mummy mask, pigments, textile

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Authors: A. Elsayed, M. H. Dewaidar, M. Ghali, M. Elkemary

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The high production cost of the conventional solar cells requires the search for economic methods suitable for solar energy conversion. Cadmium Sulfide (CdS) is one of the most important semiconductors used in photovoltaics, especially in large area solar cells; and can be prepared in a thin film form by a wide variety of deposition techniques. The preparation techniques include vacuum evaporation, sputtering and molecular beam epitaxy. Other techniques, based on chemical solutions, are also used for depositing CdS films with dramatically low-cost compared to other vacuum-based methods. Although this technique is widely used during the last decades, due to simplicity and low-deposition temperature (~100°C), there is still a strong need for more information on the growth process and its relation with the quality of the deposited films. Here, we report on deposition of high-quality CdS thin films; with low-surface roughness ( < 3.0 nm) and sharp optical absorption edge; on low-temperature glass substrates (70°C) using a new method based on the room-temperature chemical solution. In this method, a mixture solution of cadmium acetate and thiourea at room temperature was used under special growth conditions for deposition of CdS films. X-ray diffraction (XRD) measurements were used to examine the crystal structure properties of the deposited CdS films. In addition, UV-VIS transmittance and low-temperature (4K) photoluminescence (PL) measurements were performed for quantifying optical properties of the deposited films. The deposited films show high optical quality as confirmed by observation of both, sharp edge in the transmittance spectra and strong PL intensity at room temperature. Furthermore, we found a strong effect of the growth conditions on the optical band gap of the deposited films; where remarkable red-shift in the absorption edge with temperature is clearly seen in both transmission and PL spectra. Such tuning of both optical band gap of the deposited CdS films can be utilized for tuning the electronic bands' alignments between CdS and other light-harvesting materials, like CuInGaSe or CdTe, for potential improvement in the efficiency of solar cells devices based on these heterostructures.

Keywords: chemical deposition, CdS, optical properties, surface, thin film

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Authors: Sospeter P. Maganga, Alphonce Wikedzi, Mussa D. Budeba, Samwel V. Manyele

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This study characterizes complex gold ores (elemental and mineralogical composition, gold distribution, ore grindability, and mineral liberation) for preliminary process selection. About 200 kg of ore samples were collected from each location using systematic sampling by mass interval. Ores were dried, crushed, milled, and split into representative sub-samples (about 1 kg) for elemental and mineralogical composition analyses using X-ray fluorescence (XRF), fire assay finished with Atomic Absorption Spectrometer (AAS), and X-ray Diffraction (XRD) methods, respectively. The gold distribution was studied on size-by-size fractions, while ore grindability was determined using the standard Bond test. The mineral liberation analysis was conducted using ThermoFisher Scientific Mineral Liberation Analyzer (MLA) 650, where unsieved polished grain mounts (80% passing 700 µm) were used as MLA feed. Two MLA measurement modes, X-ray modal analysis (XMOD) and sparse phase liberation-grain X-ray mapping analysis (SPL-GXMAP), were employed. At least two cyanide consumers (Cu, Fe, Pb, and Zn) and kinetics impeders (Mn, S, As, and Bi) were present in all locations investigated. Copper content at Kapanda (0.77% Cu) and Ibindi (7.48% Cu) exceeded the recommended threshold of 0.5% Cu for direct cyanidation. The gold ore at Ibindi indicated a higher rate of grinding compared to other locations. This could be explained by the highest grindability (2.119 g/rev.) and lowest Bond work index (10.213 kWh/t) values. The pyrite-marcasite, chalcopyrite, galena, and siderite were identified as major gold, copper, lead, and iron-bearing minerals, respectively, with potential for economic extraction. However, only gold and copper can be recovered under conventional milling because of grain size issues (galena is exposed by 10%) and process complexity (difficult to concentrate and smelt iron from siderite). Therefore, the preliminary process selection is copper flotation followed by gold cyanidation for Kapanda and Ibindi ores, whereas gold cyanidation with additives such as glycine or ammonia is selected for Mawemeru and Itumbi ores because of low concentrations of Cu, Pb, Fe, and Zn minerals.

Keywords: complex gold ores, mineral liberation, ore characterization, ore grindability

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Authors: Jyoti Yadav, Rini Singh, Anoop M.D, Nisha Yadav, N. Srinivasa Rao, Fouran Singh, Takayuki Ichikawa, Ankur Jain, Kamlendra Awasthi, Manoj Kumar

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Nanocrystalline films exhibit defects and strain induced by its grain boundaries. Defects and strain affect the physical as well as topological insulating properties of the Bi2Te3 thin films by changing their electronic structure. In the present studies, the effect of Ni7+ ion irradiation on the physical and electrical properties of Bi2Te3 thin films was studied. The films were irradiated at five different fluences (5x1011, 1x1012, 3x1012, 5x1012, 1x1013 ions/cm2). Thin films synthesized using the e-beam technique possess a rhombohedral crystal structure with the R-3m space group. The average crystallite size, as determined by x-ray diffraction (XRD) peak broadening, was found to be 18.5 ± 5 (nm). It was also observed that irradiation increases the induced strain. Raman Spectra of the films demonstrate the splitting of A_1u^1 modes originating from the vibrations along the c-axis. This is by the variation in the lattice parameter ‘c,’ as observed through XRD. The atomic force microscopy study indicates the decrease in surface roughness up to the fluence of 3x1012 ions/cm2 and further increasing the fluence increases the roughness. The decrease in roughness may be due to the growth of smaller nano-crystallites on the surface of thin films due to irradiation-induced annealing. X-ray photoelectron spectroscopy studies reveal the composition to be in close agreement to the nominal values i.e. Bi2Te3. The resistivity v/s temperature measurements revealed an increase in resistivity up to the fluence 3x1012 ions/cm2 and a decrease on further increasing the fluence. The variation in electrical resistivity is corroborated with the change in the carrier concentration as studied through low-temperature Hall measurements. A crossover from the n-type to p-type carriers was achieved in the irradiated films. Interestingly, tuning of the Fermi level by compensating the bulk carriers using ion-irradiation could be achieved.

Keywords: Annealing, Irradiation, Fermi level, Tuning

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Authors: Oyindamola Kayode, Sarah George, Roberto Borrageiro, Mike Shirran

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A phenomenon identified by our industrial partner has experienced sag on AA3104 can body stock (CBS) transfer bar during transportation of the slab from the breakdown mill to the finishing mill. Excessive sag results in bottom scuffing of the slab onto the roller table, resulting in surface defects on the final product. It has been found that increasing the strain rate on the breakdown mill final pass results in a slab resistant to sag. The creep response for materials hot deformed at different Zener–Holloman parameter values needs to be evaluated experimentally to gain better understanding of the operating mechanism. This study investigates this identified phenomenon through laboratory simulation of the breakdown mill conditions for various strain rates by utilizing the Gleeble at UCT Centre for Materials Engineering. The experiment will determine the creep response for a range of conditions as well as quantifying the associated material microstructure (sub-grain size, grain structure etc). The experimental matrices were determined based on experimental conditions approximate to industrial hot breakdown rolling and carried out on the Gleeble 3800 at the Centre for Materials Engineering, University of Cape Town. Plane strain compression samples were used for this series of tests at an applied load that allow for better contact and exaggerated creep displacement. A tantalum barrier layer was used for increased conductivity and decreased risk of anvil welding. One set of tests with no in-situ hold time was performed, where the samples were quenched after deformation. The samples were retained for microstructure analysis of the micrographs from the light microscopy (LM), quantitative data and images from scanning electron microscopy (SEM) and energy dispersive X-ray (EDX), sub-grain size and grain structure from electron back scattered diffraction (EBSD).

Keywords: aluminium alloy, can-body stock, hot rolling, creep response, Zener-Hollomon parameter

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Authors: L. Mentar, O. Baka, A. Azizi

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Zinc oxide as a wide band semiconductor materials, especially nanostructured materials, have potential applications in large-area such as electronics, sensors, photovoltaic cells, photonics, optical devices and optoelectronics due to their unique electrical and optical properties and surface properties. The feasibility of ZnO for these applications is due to the successful synthesis of diverse ZnO nanostructures, including nanorings, nanobows, nanohelixes, nanosprings, nanobelts, nanotubes, nanopropellers, nanodisks, and nanocombs, by different method. Among various synthesis methods, electrochemical deposition represents a simple and inexpensive solution based method for synthesis of semiconductor nanostructures. In this study, the electrodeposition method was used to produce zinc oxide (ZnO) nanostructures on fluorine-doped tin oxide (FTO)-coated conducting glass substrate as TCO from chloride bath. We present a systematic study on the effects of the concentration of chloride anion on the properties of ZnO. The influence of KCl concentrations on the electrodeposition process, morphological, structural and optical properties of ZnO nanostructures was examined. In this research electrochemical deposition of ZnO nanostructures is investigated using conventional electrochemical measurements (cyclic voltammetry and Mott-Schottky), scanning electron microscopy (SEM), and X-ray diffraction (XRD) techniques. The potentials of electrodeposition of ZnO were determined using the cyclic voltammetry. From the Mott-Schottky measurements, the flat-band potential and the donor density for the ZnO nanostructure are determined. SEM images shows different size and morphology of the nanostructures and depends greatly on the KCl concentrations. The morphology of ZnO nanostructures is determined by the corporated action between [Zn(NO3)2] and [Cl-].Very netted hexagonal grains are observed for the nanostructures deposited at 0.1M of KCl. XRD studies revealed that the all deposited films were polycrystalline in nature with wurtzite phase. The electrodeposited thin films are found to have preferred oriented along (002) plane of the wurtzite structure of ZnO with c-axis normal to the substrate surface for sample at different concentrations of KCl. UV-Visible spectra showed a significant optical transmission (~80%), which decreased with low Cl-1 concentrations. The energy band gap values have been estimated to be between 3.52 and 3.80 eV.

Keywords: electrodeposition, ZnO, chloride ions, Mott-Schottky, SEM, XRD

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Authors: Magdy Torab

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Ancient Egyptians built their temples purposefully close to the River Nile to use it for transporting construction stones from far away quarries to building sites in river-boats. Most temples, therefore, have river-harbors associated with their geometric designs. The paleoriver channel remapped by using this idea, besides other geomorphological and geoarchaeological indicators/evidence located between Aswan and Luxor cities. In this sense, this paper defines the characteristics of this ancient course and its associated landforms using paleochannel morphology, paleomeandering, and ancient river dynamics during historic and prehistoric times. Both geomorphological and geoarchaeological approaches used to reconstruct the paleomorphology of the river course. It helps to investigate the ancient river morphology by using the following techniques: comparison and interpretation of multi dates satellite images and historical maps between 1943 and 2004. The results illustrated on maps using GIS (ARC GIS V.10 software) and the field data collected from the western bank of The Nile River at Luxor area and Karnak, Edfu, Esna and Kom Ombo temples. Created both current and paleogeomorphological maps depending upon the results of geoarchaeological surveying and soil analysis and dating, for surface and subsurface soil sampling by handle auger, laser diffraction analysis for 7 soil samples collected from some mounds and Malkata channel in the western bank of The Nile River near Luxor. Paleo-current directions were determined by using standard Brunton compass to use it as an indicator is evidence for the direction of flow of The Nile River during deposition of some accumulated mounds on the western part of the floodplain near Luxor city. C-14 dating was used for two samples collected from these mounds as well as geographical information system (GIS) technique for mapping. The geomorphological and geoarchaeological evidence shows that the Nile River course in Luxor area was around 4.5 km wide and contained many islands and sandbars which separated inside the river channel, now appearing as scattered mounds inside the floodplain. Upper Egypt has migrated during the historic times to the east up to five kilometers and become far away from the ancient temples, quarries, and harbors. It has also become as well as become more meandering and narrower than before.

Keywords: Nile River, ancient harbours, Luxor, paleogeomorphology, geoarchaeology

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Authors: Lahcen Daoudi, Soukaina Elidrissi, Nathalie Fagel

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The calcareous accumulations in the surface formations of the soil, are a very widespread phenomenon in the arid and semi-arid regions. Many aspects of physical and chemical evolution of these soils were debated for more than one century. The last two decades have witnessed a remarkable interest in the study of the calcrete. In Morocco, as in most Mediterranean countries, soils with carbonate accumulation cover large areas of the territory. The isohumic subtropical soils and red Mediterranean soils include always a horizon of calcrete accumulation. In the lowland of Tensift Al Haouz located in the central part of Morocco, the arable lands are underlain by indurate pedogenic calcrete of various thicknesses; this constitutes a serious handicap for agricultural development in the region. Our aims in this study is to analyze the characteristics of the crusts developed in this area in order to identify the various facies, their geographic distribution and the factors that played a significant role in the differentiation of these calcareous accumulations. The characterizations were based on various techniques including field observations, X-ray diffraction analysis (XRD) for both raw materials and clay fractions, SEM analysis, Calcimetry and Loss On Ignition (LOI). The analysis of encrusting calcrete in a rich and varied observation field as the region of Tensift Al Haouz enabled us to specify the important types of accumulations: diffuse, nodular and massive encrusting. The shape of encrusting as well as their consistency and hardness is clearly related to the contents of CaCO3 of the profiles. Among these facies, the hardpan which results from a complex succession of processes is certainly the most morphologically advanced form of encrusting. The vertical and lateral distribution of these forms in the Tensift Al Haouz area indicates that they do not appear randomly but seem related to well defined environmental conditions. The differentiation and evolution of encrusting is under the influence of two major factors: 1) the availability of carbonate rich solution which is controlled by the topography, the nature and texture of underlying host rock and the detrital processes; 2) the climate which is responsible for the evaporation and crystallization of carbonate.

Keywords: soil calcrete, characterization, morphology, Tensift Al Haouz, Morocco

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Authors: Amanda C. Q. M. Vieira, Cybelly M. Melo, Camila B. M. Figueirêdo, Giovanna C. R. M. Schver, Salvana P. M. Costa, Magaly A. M. de Lyra, Ping I. Lee, José L. Soares-Sobrinho, Pedro J. Rolim-Neto, Mônica F. R. Soares

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Epiisopiloturine (EPI) is a drug candidate that is extracted from Pilocarpus microphyllus and isolated from the waste of Pilocarpine. EPI has demonstrated promising schistosomicidal, leishmanicide, anti-inflammatory and antinociceptive activities, according to in vitro studies that have been carried out since 2009. However, this molecule shows poor aqueous solubility, which represents a problem for the release of the drug candidate and its absorption by the organism. The purpose of the present study is to investigate the extent of enhancement of kinetic solubility of a solid solution (SS) of EPI in hipromellose phthalate HP-55 (HPMCP), an enteric polymer carrier. SS was obtained by the solvent evaporation methodology, using acetone/methanol (60:40) as solvent system. Both EPI and polymer (drug loading 10%) were dissolved in this solvent until a clear solution was obtained, and then dried in oven at 60ºC during 12 hours, followed by drying in a vacuum oven for 4 h. The results show a considerable modification in the crystalline structure of the drug candidate. For instance, X-ray diffraction (XRD) shows a crystalline behavior for the EPI, which becomes amorphous for the SS. Polarized light microscopy, a more sensitive technique than XRD, also shows completely absence of crystals in SS sample. Differential Scanning Calorimetric (DSC) curves show no signal of EPI melting point in SS curve, indicating, once more, no presence of crystal in this system. Interaction between the drug candidate and the polymer were found in Infrared microscopy, which shows a carbonyl 43.3 cm-1 band shift, indicating a moderate-strong interaction between them, probably one of the reasons to the SS formation. Under sink conditions (pH 6.8), EPI SS had its dissolution performance increased in 2.8 times when compared with the isolated drug candidate. EPI SS sample provided a release of more than 95% of the drug candidate in 15 min, whereas only 45% of EPI (alone) could be dissolved in 15 min and 70% in 90 min. Thus, HPMCP demonstrates to have a good potential to enhance the kinetic solubility profile of EPI. Future studies to evaluate the stability of SS are required to conclude the benefits of this system.

Keywords: epiisopiloturine, hipromellose phthalate HP-55, pharmaceuticaltechnology, solubility

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Authors: Elena B. Cherepetskaya, Alexander A. Karabutov, Natalia B. Podymova, Ivan Sas

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Nonlinear evolution of broadband ultrasonic pulses passed through the rock specimens is studied using the apparatus ‘GEOSCAN-02M’. Ultrasonic pulses are excited by the pulses of Q-switched Nd:YAG laser with the time duration of 10 ns and with the energy of 260 mJ. This energy can be reduced to 20 mJ by some light filters. The laser beam radius did not exceed 5 mm. As a result of the absorption of the laser pulse in the special material – the optoacoustic generator–the pulses of longitudinal ultrasonic waves are excited with the time duration of 100 ns and with the maximum pressure amplitude of 10 MPa. The immersion technique is used to measure the parameters of these ultrasonic pulses passed through a specimen, the immersion liquid is distilled water. The reference pulse passed through the cell with water has the compression and the rarefaction phases. The amplitude of the rarefaction phase is five times lower than that of the compression phase. The spectral range of the reference pulse reaches 10 MHz. The cubic-shaped specimens of the Karelian gabbro are studied with the rib length 3 cm. The ultimate strength of the specimens by the uniaxial compression is (300±10) MPa. As the reference pulse passes through the area of the specimen without cracks the compression phase decreases and the rarefaction one increases due to diffraction and scattering of ultrasound, so the ratio of these phases becomes 2.3:1. After preloading some horizontal cracks appear in the specimens. Their location is found by one-sided scanning of the specimen using the backward mode detection of the ultrasonic pulses reflected from the structure defects. Using the computer processing of these signals the images are obtained of the cross-sections of the specimens with cracks. By the increase of the reference pulse amplitude from 0.1 MPa to 5 MPa the nonlinear transformation of the ultrasonic pulse passed through the specimen with horizontal cracks results in the decrease by 2.5 times of the amplitude of the rarefaction phase and in the increase of its duration by 2.1 times. By the increase of the reference pulse amplitude from 5 MPa to 10 MPa the time splitting of the phases is observed for the bipolar pulse passed through the specimen. The compression and rarefaction phases propagate with different velocities. These features of the powerful broadband ultrasonic pulses passed through the rock specimens can be described by the hysteresis model of Preisach-Mayergoyz and can be used for the location of cracks in the optically opaque materials.

Keywords: cracks, geological materials, nonlinear evolution of ultrasonic pulses, rock

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Authors: Yuvraj S. Malghe, Atul B. Lavand

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In recent years, semiconductor photocatalytic degradation processes have attracted a lot of attention and are used widely for the destruction of organic pollutants present in waste water. Among various semiconductors, titanium dioxide (TiO2) is the most popular photocatalyst due to its excellent chemical stability, non-toxicity, relatively low cost and high photo-oxidation power. It has been known that zinc oxide (ZnO) with band gap energy 3.2 eV is a suitable alternative to TiO2 due to its high quantum efficiency, however it corrodes in acidic medium. Unfortunately TiO2 and ZnO both are active only in UV light due to their wide band gaps. Sunlight consist about 5-7% UV light, 46% visible light and 47% infrared radiation. In order to utilize major portion of sunlight (visible spectrum), it is necessary to modify the band gap of TiO2 as well as ZnO. This can be done by several ways such as semiconductor coupling, doping the material with metals/non metals. Doping of TiO2 using transition metals like Fe, Co and non-metals such as N, C or S extends its absorption wavelengths from UV to visible region. In the present work, we have synthesized ZnO-TiO2 nanocomposite using reverse microemulsion method. Visible light photocatalytic activity of synthesized nanocomposite was investigated for degradation of aqueous solution of malachite green (MG). To increase the photocatalytic activity of ZnO-TiO2 nanocomposite, it is decorated with C and Fe. Pure, carbon (C) doped and carbon, iron(C, Fe) co-doped nanosized ZnO-TiO2 nanocomposites were synthesized using reverse microemulsion method. These composites were characterized using, X-ray diffraction (XRD), Energy dispersive X-ray spectroscopy (EDX), Scanning electron microscopy (SEM), UV visible spectrophotometery and X-ray photoelectron spectroscopy (XPS). Visible light photocatalytic activities of synthesized nanocomposites were investigated for degradation of aqueous malachite green (MG) solution. C, Fe co-doped ZnO-TiO2 nanocomposite exhibit better photocatalytic activity and showed threefold increase in photocatalytic activity. Effect of amount of catalyst, pH and concentration of MG solution on the photodegradation rate is studied. Stability and reusability of photocatalyst is also studied. C, Fe decorated ZnO-TiO2 nanocomposite shows threefold increase in photocatalytic activity.

Keywords: malachite green, nanocomposite, photocatalysis, titanium dioxide, zinc oxide

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Authors: Gonzalo Reyes, Magdalena Walczak, Esteban Ramos-Moore, Jorge Ramos-Grez

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Metal additive manufacture technologies have gained strong support and acceptance as a promising and alternative method to manufacture high performance complex geometry products. The main purpose of the present work is to study the microstructure and phase transformation temperatures of Cu-Al-Ni shape memory alloys fabricated from a direct laser additive process using metallic powders as precursors. The potential application is to manufacture self-centering seismic dampers for earthquake protection of buildings out of a copper based alloy by an additive process. In this process, the Cu-Al-Ni alloy is melted, inside of a high temperature and vacuum chamber with the aid of a high power fiber laser under inert atmosphere. The laser provides the energy to melt the alloy powder layer. The process allows fabricating fully dense, oxygen-free Cu-Al-Ni specimens using different laser power levels, laser powder interaction times, furnace ambient temperatures, and cooling rates as well as modifying concentration of the alloying elements. Two sets of specimens were fabricated with a nominal composition of Cu-13Al-3Ni and Cu-13Al-4Ni in wt.%, however, semi-quantitative chemical analysis using EDX examination showed that the specimens’ resulting composition was closer to Cu-12Al-5Ni and Cu-11Al-8Ni, respectively. In spite of that fact, it is expected that the specimens should still possess shape memory behavior. To confirm this hypothesis, phase transformation temperatures will be measured using DSC technique, to look for martensitic and austenitic phase transformations at 150°C. So far, metallographic analysis of the specimens showed defined martensitic microstructures. Moreover, XRD technique revealed diffraction peaks corresponding to (0 0 18) and (1 2 8) planes, which are too associated with the presence of martensitic phase. We conclude that it would be possible to obtain fully dense Cu-Al-Ni alloys having shape memory effect behavior by direct laser fabrication process, and to advance into fabrication of self centering seismic dampers by a controllable metal additive manufacturing process.

Keywords: Cu-Al-Ni alloys, direct laser fabrication, shape memory alloy, self-centering seismic dampers

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Authors: Mardin Abdalqadir, Paul Adzakro, Tannaz Pak, Sina Rezaei Gomari

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Climate change and global warming recently became significant concerns due to the massive emissions of greenhouse gases into the atmosphere, predominantly CO2 gases. Therefore, it is necessary to find sustainable and inexpensive methods to capture the greenhouse gasses and protect the environment for live species. The application of naturally available and cheap adsorbents of carbon such as clay minerals became a great interest. However, the minerals prone to low storage capacity despite their high affinity to adsorb carbon. This paper aims to explore ways to improve the pore volume and surface area of two selected clay minerals, ‘montmorillonite and kaolinite’ by acid treatment to overcome their low storage capacity. Montmorillonite and kaolinite samples were treated with different sulfuric acid concentrations (0.5, 1.2 and 2.5 M) at 40 °C for 8 hours to achieve the above aim. The grain size distribution and morphology of clay minerals before and after acid treatment were explored with Scanning Electron Microscope to evaluate surface area improvement. The ImageJ software was used to find the porosity and pore volume of treated and untreated clay samples. The structure of the clay minerals was also analyzed using an X-ray Diffraction machine. The results showed that the pore volume and surface area were increased substantially through acid treatment, which speeded up the rate of carbon dioxide adsorption. XRD pattern of kaolinite did not change after sulfuric acid treatment, which indicates that acid treatment would not affect the structure of kaolinite. It was also discovered that kaolinite had a higher pore volume and porosity than montmorillonite before and after acid treatment. For example, the pore volume of untreated kaolinite was equal to 30.498 um3 with a porosity of 23.49%. Raising the concentration of acid from 0.5 M to 2.5 M in 8 hours’ time reaction led to increased pore volume from 30.498 um3 to 34.73 um3. The pore volume of raw montmorillonite was equal to 15.610 um3 with a porosity of 12.7%. When the acid concentration was raised from 0.5 M to 2.5 M for the same reaction time, pore volume also increased from 15.610 um3 to 20.538 um3. However, montmorillonite had a higher specific surface area than kaolinite. This study concludes that clay minerals are inexpensive and available material sources to model the realistic conditions and apply the results of carbon capture to prevent global warming, which is one of the most critical and urgent problems in the world.

Keywords: acid treatment, kaolinite, montmorillonite, pore volume, porosity, surface area

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Authors: Md. Shoffikul Islam, Hongqing Hu

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Reducing trace elements' mobility and bioavailability through amendment addition, especially biochar (BC), is a cost-effective and efficient method to address their toxicity in the soil environment. However, the low molecular weight organic acids (LMWOAs) in the rhizosphere could affect BC's efficiency to stabilize trace metals as the LMWOAs could either mobilize or fix metals in the soils. Therefore, understanding the BC's and LMWOAs' interaction mechanisms on metals stabilization in the rhizosphere is crucial. The present study explored the impact of BC derived from rice husk and citric acid (CA) and the combination of BC and CA on the redistribution of cadmium (Cd), lead (Pb), and zinc (Zn) among their geochemical forms through incubation experiment. The changes of zeta potential and X-ray diffraction (XRD) pattern of BC and BC-amended soils to investigate the probable mechanisms of trace elements' immobilization by BC under the CA attack were also examined. The rice husk BC at 5% (w/w) was mixed with the air-dry soil (an Anthrosols) contaminated with Cd, Pb, and Zn in the plastic pot. The 2, 5, 10, and 20 mM kg-1 (w/v) of CA were added separately into the pot. All the ingredients were mixed thoroughly with the soil. A control (CK) treatment was also prepared without BC and CA addition. After 7, 15, and 60 days of incubation with 60% (w/v) moisture level at 25 °C, the incubated soils were determined for pH and EC and were sequentially extracted to assess the metals' transformation in soil. The electronegative charges and XRD peaks of BC and BC-amended soils were also measured. Compared to CK, the application of BC, low level of CA (2 mM kg-1 soil) (CA2), and BC plus the low concentration of CA (BC-CA2) considerably declined the acid-soluble Cd, Pb, and Zn in which BC-CA2 was found to be the most effective treatment. The reversed trends were observed concerning the high levels of CA (>5-20 mM kg-1 soil) and the BC plus high concentrations of CA treatments. BC-CA2 changed the highest amounts of acid-soluble and reducible metals to the oxidizable and residual forms with time. The most increased electronegative charges of BC-CA2 indicate its (BC-CA2) highest Cd, Pb, and Zn immobilizing efficiency, probably through metals adsorption and fixation with the negative charge sites. The XRD study revealed the presence of P, O, CO32-, and Cl1- in BC, which might be responsible for the precipitation of CdCO3, pyromorphite, and hopeite in the case of Cd, Pb, and Zn immobilization, respectively. The findings depicted that the low concentration of CA increased metals' stabilization, whereas the high levels of CA enhanced their mobilization. The BC-CA2 emerged as the best amendment among treatments for metals stabilization in contaminated soils.

Keywords: Biochar, citric acid, immobilization, trace elements contaminated soil

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Authors: M. Vadivel, R. Ramesh Babu

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Spinel ferrite magnetic nanomaterials have received a great deal of attention in recent years due to their wide range of potential applications in various fields such as magnetic data storage and microwave device applications. Among the family of spinel ferrites, cobalt ferrite (CoFe2O4) has been widely used in the field of high-frequency applications because of its remarkable material qualities such as moderate saturation magnetization, high coercivity, large permeability at higher frequency and high electrical resistivity. For aforementioned applications, the materials should have an improved electrical property, especially enhancement in the dielectric properties. It is well known that the substitution of rare earth metal cations in Fe3+ site of CoFe2O4 nanoparticles leads to structural distortion and thus significantly influences the structural and morphological properties whereas greatly modifies the electrical and magnetic properties of a material. In the present investigation, we report on the influence of lanthanum (La3+) ion substitution on the structural, morphological, dielectric and magnetic properties of CoFe2O4 magnetic nanoparticles prepared by co-precipitation method. Powder X-ray diffraction patterns reveal the formation of inverse cubic spinel structure with the signature of LaFeO3 phase at higher La3+ ion concentrations. Raman and Fourier transform infrared spectral analysis also confirms the formation of inverse cubic spinel structure and Fe-O symmetrical stretching vibrations of CoFe2O4 nanoparticles, respectively. Transmission electron microscopy study reveals that the size of the particles gradually increases with increasing La3+ ion concentrations whereas the agglomeration gets slightly reduced for La3+ ion substituted CoFe2O4 nanoparticles than that of undoped CoFe2O4 nanoparticles. Dielectric properties such as dielectric constant and dielectric loss were recorded as a function of frequency and temperature which reveals that the dielectric constant gradually increases with increasing temperatures as well as La3+ ion concentrations. The increased dielectric constant might be the reason that the formation of LaFeO3 secondary phase at higher La3+ ion concentrations. Magnetic measurement demonstrates that the saturation magnetization gradually decreases from 61.45 to 25.13 emu/g with increasing La3+ ion concentrations which is due to the nonmagnetic nature of La3+ ions substitution.

Keywords: cobalt ferrite, co-precipitation, dielectric properties, saturation magnetization

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Authors: Özge Alptoğa, Nuray Uçar, Nilgün Karatepe Yavuz, Ayşen Önen

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Sulfur dioxide (SO₂) is a very toxic air pollutant gas and it causes the greenhouse effect, photochemical smog, and acid rain, which threaten human health severely. Thus, the capture of SO₂ gas is very important for the environment. Graphene which is two-dimensional material has excellent mechanical, chemical, thermal properties, and many application areas such as energy storage devices, gas adsorption, sensing devices, and optical electronics. Further, graphene oxide (GO) is examined as a good adsorbent because of its important features such as functional groups (epoxy, carboxyl and hydroxyl) on the surface and layered structure. The SO₂ adsorption properties of the fibers are usually investigated on carbon fibers. In this study, potential adsorption capacity of GO fibers was researched. GO dispersion was first obtained with Hummers’ method from graphite, and then GO fibers were obtained via wet spinning process. These fibers were converted into a disc shape, dried, and then subjected to SO₂ gas adsorption test. The SO₂ gas adsorption capacity of GO fiber discs was investigated in the fields of utilization of different coagulation baths and reduction by hydrazine hydrate. As coagulation baths, single and triple baths were used. In single bath, only ethanol and CaCl₂ (calcium chloride) salt were added. In triple bath, each bath has a different concentration of water/ethanol and CaCl₂ salt, and the disc obtained from triple bath has been called as reference disk. The fibers which were produced with single bath were flexible and rough, and the analyses show that they had higher SO₂ adsorption capacity than triple bath fibers (reference disk). However, the reduction process did not increase the adsorption capacity, because the SEM images showed that the layers and uniform structure in the fiber form were damaged, and reduction decreased the functional groups which SO₂ will be attached. Scanning Electron Microscopy (SEM), Fourier Transform Infrared Spectroscopy (FTIR), X-Ray Diffraction (XRD) analyzes were performed on the fibers and discs, and the effects on the results were interpreted. In the future applications of the study, it is aimed that subjects such as pH and additives will be examined.

Keywords: coagulation bath, graphene oxide fiber, reduction, SO2 gas adsorption

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Authors: Hussein M. Etmimi, Peter E. Mallon

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Electrospinning uses an electrical charge to draw very fine fibers (typically on the micro or nano scale) from a liquid or molten precursor. Over the years, this method has become a widely used and a successful technique to process polymer materials and their composites into nanofibers. The main focus of this work is to study the electrospinning of multi-phase amphiphilic copolymers and their nanocomposites, which contain graphene as the nanofiller material. In such amphiphilic materials, the constituents segments are incompatible and thus the solid state morphology will be determined by the composition of the various constituents as well as the method of preparation. In this study, amphiphilic block copolymers of poly(dimethyl siloxane) and poly(methyl methacrylate) (PDMS-b-PMMA) with well-defined structures were synthesized and the solution electrospinning of these materials and their properties were investigated. Atom transfer radical polymerization (ATRP) was used to obtain the controlled block copolymers with relatively high molar masses and narrow dispersity. First, PDMS macroinitiators with different chain length of 1000, 5000 and 10000 g/mol were synthesized by the reaction of monocarbinol terminated PDMS with α-bromoisobutyryl bromide initiator. The obtained macroinitiators were used for the polymerization of methyl methacrylate monomer to obtain the desired block copolymers using the ATRP process. Graphene oxide (GO) of different loading was then added to the copolymer solution and the resultant nanocomposites were successfully electrospun into nanofibers. The electrospinning was achieved using dimethylformamide/chloroform mixture (60:40 vl%) as electrospinning solution medium. Scanning electron microscopy (SEM) showed the successful formation of the electrospun fibers with dimensions in the nanometer range. X-ray diffraction indicated that the GO nanosheets were of an exfoliated structure, irrespective of the filler loading. Thermogravimetric analysis also showed that the thermal stability of the nanofibers was improved in the presence of GO, which was not a function of the filler loading. Differential scanning calorimetry also showed that the mechanical properties (measured as glass transition temperature) of the nanofibers was improved significantly in the presence of GO, which was a function of the filler loading.

Keywords: elctrospinning, graphene oxide, nanofibers, polymethyl methacrylate (PMMA)

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Authors: Pouyan Motamedi, Ken Bosnick, Ken Cadien, James Hogan

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Growth of conformal ultrathin metal films has attracted a considerable amount of attention recently. Plasma-enhanced atomic layer deposition (PEALD) is a method capable of growing conformal thin films at low temperatures, with an exemplary control over thickness. The authors have recently reported on growth of metastable epitaxial nickel thin films via PEALD, along with a comprehensive characterization of the films and a study on the relationship between the growth parameters and the film characteristics. The goal of the current study is to use the mentioned films as a case study to investigate the temperature-activated phase transformation and agglomeration in ultrathin metallic films. For this purpose, metastable hexagonal nickel thin films were annealed using a controlled heating/cooling apparatus. The transformations in the crystal structure were observed via in-situ synchrotron x-ray diffraction. The samples were annealed to various temperatures in the range of 400-1100° C. The onset and progression of particle formation were studied in-situ via laser measurements. In addition, a four-point probe measurement tool was used to record the changes in the resistivity of the films, which is affected by phase transformation, as well as roughening and agglomeration. Thin films annealed at various temperature steps were then studied via atomic force microscopy, scanning electron microscopy and high-resolution transmission electron microscopy, in order to get a better understanding of the correlated mechanisms, through which phase transformation and particle formation occur. The results indicate that the onset of hcp-to-bcc transformation is at 400°C, while particle formations commences at 590° C. If the annealed films are quenched after transformation, but prior to agglomeration, they show a noticeable drop in resistivity. This can be attributed to the fact that the hcp films are grown epitaxially, and are under severe tensile strain, and annealing leads to relaxation of the mismatch strain. In general, the results shed light on the nature of structural transformation in nickel thin films, as well as metallic thin films, in general.

Keywords: atomic layer deposition, metastable, nickel, phase transformation, thin film

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Authors: Zh. Saffari, A. Naeimi, M. S. Ekrami-Kakhki, Kh. Khandan-Barani

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The textile industries are becoming a major source of environmental contamination because an alarming amount of dye pollutants are generated during the dyeing processes. Organic dyes are one of the largest pollutants released into wastewater from textile and other industrial processes, which have shown severe impacts on human physiology. Nano-structure compounds have gained importance in this category due their anticipated high surface area and improved reactive sites. In recent years several novel adsorbents have been reported to possess great adsorption potential due to their enhanced adsorptive capacity. Nano-MnO2 has great potential applications in environment protection field and has gained importance in this category because it has a wide variety of structure with large surface area. The diverse structures, chemical properties of manganese oxides are taken advantage of in potential applications such as adsorbents, sensor catalysis and it is also used for wide catalytic applications, such as degradation of dyes. In this study, adsorption of Methyl Violet (MV) dye from aqueous solutions onto MnO2 nanoparticles (MNP) has been investigated. The surface characterization of these nano particles was examined by Particle size analysis, Scanning Electron Microscopy (SEM), Fourier Transform Infrared (FTIR) spectroscopy and X-Ray Diffraction (XRD). The effects of process parameters such as initial concentration, pH, temperature and contact duration on the adsorption capacities have been evaluated, in which pH has been found to be most effective parameter among all. The data were analyzed using the Langmuir and Freundlich for explaining the equilibrium characteristics of adsorption. And kinetic models like pseudo first- order, second-order model and Elovich equation were utilized to describe the kinetic data. The experimental data were well fitted with Langmuir adsorption isotherm model and pseudo second order kinetic model. The thermodynamic parameters, such as Free energy of adsorption (ΔG°), enthalpy change (ΔH°) and entropy change (ΔS°) were also determined and evaluated.

Keywords: MnO2 nanoparticles, adsorption, methyl violet, isotherm models, kinetic models, surface chemistry

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Authors: Wighens Ngoie Ilunga, Pamela J. Welz, Olewaseun O. Oyekola, Daniel Ikhu-Omoregbe

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Currently, most sludge from the wastewater treatment plants of edible oil factories is disposed to landfills, but landfill sites are finite and potential sources of environmental pollution. Production of biodiesel from wastewater sludge can contribute to energy production and waste minimization. However, conventional biodiesel production is energy and waste intensive. Generally, biodiesel is produced from the transesterification reaction of oils with alcohol (i.e., Methanol, ethanol) in the presence of a catalyst. Homogeneously catalysed transesterification is the conventional approach for large-scale production of biodiesel as reaction times are relatively short. Nevertheless, homogenous catalysis presents several challenges such as high probability of soap. The current study aimed to reuse wastewater sludge from the edible oil industry as a novel feedstock for both monounsaturated fats and bioethanol for the production of biodiesel. Preliminary results have shown that the fatty acid profile of the oilseed wastewater sludge is favourable for biodiesel production with 48% (w/w) monounsaturated fats and that the residue left after the extraction of fats from the sludge contains sufficient fermentable sugars after steam explosion followed by an enzymatic hydrolysis for the successful production of bioethanol [29% (w/w)] using a commercial strain of Saccharomyces cerevisiae. A novel nano-magnetic catalyst was synthesised from mineral processing alkaline tailings, mainly containing dolomite originating from cupriferous ores using a modified sol-gel. The catalyst elemental chemical compositions and structural properties were characterised by X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infra-red (FTIR) and the BET for the surface area with 14.3 m²/g and 34.1 nm average pore diameter. The mass magnetization of the nano-magnetic catalyst was 170 emu/g. Both the catalytic properties and reusability of the catalyst were investigated. A maximum biodiesel yield of 78% was obtained, which dropped to 52% after the fourth transesterification reaction cycle. The proposed approach has the potential to reduce material costs, energy consumption and water usage associated with conventional biodiesel production technologies. It may also mitigate the impact of conventional biodiesel production on food and land security, while simultaneously reducing waste.

Keywords: biodiesel, bioethanol, edible oil wastewater sludge, nano-magnetism

Procedia PDF Downloads 145

Authors: S. K. M. Nzaba, H. H. Nyoni, B. Ntsendwana, B. B. Mamba, A. T. Kuvarega

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Azo dye effluents, released into water bodies are not only toxic to the ecosystem but also pose a serious impact on human health due to the carcinogenic and mutagenic effects of the compounds present in the dye discharge. Conventional water treatment methods such as adsorption, flocculation/coagulation and biological processes are not effective in completely removing most of the dyes and their natural degradation by-products. Advanced oxidation processes (AOPs) have proven to be effective technologies for complete mineralization of these recalcitrant pollutants. Therefore, there is a need for new technology that can solve the problem. Thus, this study examined the photocatalytic degradation of an azo dye brilliant black (BB) using non-metal/metal codoped TiO₂. N, Pt co-doped TiO₂ photocatalysts were prepared by a modified sol-gel method using amine-terminated polyamidoamine dendrimer generation 0 (PAMAM G0), amine-terminated polyamidoamine dendrimer generation 1 ( PAMAM G1) and hyperbranched polyethyleneimine (HPEI) as templates and source of nitrogen. Structural, morphological, and textural properties were evaluated using scanning electron microscopy coupled to energy dispersive X-ray spectroscopy (SEM/EDX), high-resolution transmission electron microscopy (HRTEM), X-ray diffraction spectroscopy (XRD), X-ray photoelectron spectroscopy (XPS), thermal gravimetric analysis (TGA), Fourier- transform infrared (FTIR), Raman spectroscopy (RS), photoluminescence (PL) and ultra-violet /visible spectroscopy (UV-Vis). The synthesized photocatalysts exhibited lower band gap energies as compared to the Degussa P-25 revealing a red shift in band gap towards the visible light absorption region. Photocatalytic activity of N, Pt co-doped TiO₂ was measured by the reaction of photocatalytic degradation of brilliant black (BB) dye. The N, metal codoped TiO₂ containing 0.5 wt. % of the metal consisted mainly of the anatase phase as confirmed by XRD results of all three samples, with a particle size range of 13–30 nm. The particles were largely spherical and shifted the absorption edge well into the visible region. Band gap reduction was more pronounced for the N, Pt HPEI (Pt 0.5 wt. %) codoped TiO₂ compared to PAMAM G0 and PAMAM G1. Consequently, codoping led to an enhancement in the photocatalytic activity of the materials for the degradation of brilliant black (BB).

Keywords: codoped TiO₂, dendrimer, photodegradation, wastewater

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Authors: Ehsan Alishahi, Chuang Deng

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Materials with microstructural heterogeneity have recently attracted dramatic attention in the materials science community. Although most of the metals are identified as crystalline, the new class of amorphous alloys, sometimes are known as metallic glasses (MGs), exhibited remarkable properties, particularly high mechanical strength and elastic limit. The unique properties of MGs led to the wide range of studies in developing and characterizing of new alloys or composites which met the commercial desires. In spite of applicable properties of MGs, commercializing of metallic glasses was limited due to a major drawback, the lack of ductility and sudden brittle failure mode. Hence, crystalline-amorphous (C-A) composites were introduced almost in 2000s as a toughening strategy to improve the ductility of MGs. Despite the considerable progress reported in previous studies, there are still challenges in both synthesis and characterization of metallic C-A composites. In this study, accumulative roll bonding (ARB) was used to synthesize bulk crystalline-amorphous composites starting from crystalline Cu-Zr multilayers. Due to the severe plastic deformation state, new CuZr phases were formed during the rolling process which was reflected in SEM-EDS analysis. EDS elemental analysis showed the variation in the composition of CuZr phases such as 38-62, 50-50 to 68-32 at Cu-Zr % respectively. Moreover, TEM with electron diffraction analysis indicated the presence of both crystalline and amorphous structures for the new formed CuZr phases. In addition to the microstructural analysis, the mechanical properties of the synthesized composites were studied using the nanoindentation technique. Hysitron Nanoindentation instrument was used to conduct nanoindentation tests with cube corner tip. The maximum load of 5000 µN was applied in load control mode to measure the elastic modulus and hardness of different phases. The trend of results indicated three distinct regimes of hardness and elastic modulus including pure Cu, pure Zr, and new formed CuZr phases. More specifically, pure Cu regions showed the lowest values for both nanoindentation hardness and elastic modulus while the CuZr phases take the highest values. Consequently, pure Zr was placed in the intermediate range which is harder than pure Cu but softer than CuZr phases. In overall, it was found that CuZr phases with higher hardness were nucleated during ARB process as a result of mechanical alloying phenomenon.

Keywords: ARB, crystalline-amorphous composites, mechanical alloying, nanoindentation hardness

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Authors: Mohd Maniruzzaman, Md. Monjurul Alam, Md. Hafezur Rahaman, Anika Amir Mohona

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The consumption of water by various industries is increasing day by day, and the wastewaters from them are increasing as well. These wastewaters consist of various kinds of color, dissolved solids, toxic heavy metals, residual chlorine, and other non-degradable organic materials. If these wastewaters are exposed directly to the environment, it will be hazardous for the environment and personal health. So, it is very necessary to treat these wastewaters before exposing into the environment. In this research, we have demonstrated the successful processing and utilization of fully bio-based cellulose micro crystal (CMC) composite for the removal of heavy metals, dyes, and salinity from industrial wastewaters. Banana rachis micro-cellulose were prepared by acid hydrolysis (H₂SO₄) of banana (Musa acuminata L.) rachis fiber, and Bijoypur raw clay were treated by organic solvent tri-ethyl amine. Composites were prepared with varying different composition of banana rachis nano-cellulose and modified Bijoypur (north-east part in Bangladesh) clay. After the successful characterization of cellulose micro crystal (CMC) and modified clay, our targeted filter was fabricated with different composition of cellulose micro crystal and clay in the locally fabricated packing column with 7.5 cm as thickness of composites fraction. Waste-water was collected from local small textile industries containing basic yellow 2 as dye, lead (II) nitrate [Pb(NO₃)₂] and chromium (III) nitrate [Cr(NO₃)₃] as heavy metals and saline water was collected from Khulna to test the efficiency of banana rachis cellulose micro crystal-clay composite for removing the above impurities. The filtering efficiency of wastewater purification was characterized by Fourier transforms infrared spectroscopy (FTIR), X-ray diffraction (X-RD), thermo gravimetric analysis (TGA), atomic absorption spectrometry (AAS), scanning electron microscopy (SEM) analyses. Finally, our all characterizations data are shown with very high expected results for in industrial application of our fabricated filter.

Keywords: banana rachis, bio-based filter, cellulose micro crystal-clay composite, wastewaters, synthetic dyes, heavy metal, water salinity

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Authors: Celestine Mbakaan, Iorkyaa Ahemen, A. D. Onoja, A. N. Amah, Emmanuel Barki

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Rice husk (RH) is a natural sheath that forms and covers the grain of rice. The husk composed of hard materials, including opaline silica and lignin. It separates from its grain during rice milling. RH also contains approximately 15 to 28 wt % of silica in hydrated amorphous form. Nanosilica was derived from the husk of different rice varieties after pre-treating the husk (RH) with HCl and calcination at 550°C. Nanosilica derived from the husk of Osi rice variety produced the highest silica yield, and further pretreatment with 0.8 M H₃PO₄ acid removed more mineral impurities. The silica obtained from this rice variety was selected as a host matrix for doping with Sm³⁺ ions. Rice husk silica (RH-SiO₂) doped with samarium (RH-SiO₂: xSm³⁺ (x=0.01, 0.05, and 0.1 molar ratios) nanophosphors were synthesized via the sol-gel method. The structural analysis by X-ray diffraction analysis (XRD) reveals amorphous structure while the surface morphology, as revealed by SEM and TEM, indicates agglomerates of nano-sized spherical particles with an average particle size measuring 21 nm. The nanophosphor has a large surface area measuring 198.0 m²/g, and Fourier transform infrared spectroscopy (FT-IR) shows only a single absorption band which is strong and broad with a valley at 1063 cm⁻¹. Diffuse reflectance spectroscopy (DRS) shows strong absorptions at 319, 345, 362, 375, 401, and 474 nm, which can be exclusively assigned to the 6H5/2→4F11/2, 3H7/2, 4F9/2, 4D5/2, 4K11/2, and 4M15/2 + 4I11/2, transitions of Sm³⁺ respectively. The photoluminescence excitation spectra show that near UV and blue LEDs can effectively be used as excitation sources to produce red-orange and yellow-orange emission from Sm³⁺ ion-doped RH-SiO₂ nanophosphors. The photoluminescence (PL) of the nanophosphors gives three main lines; 568, 605, and 652 nm, which are attributed to the intra-4f shell transitions from the excited level to ground levels, respectively under excitation wavelengths of 365 and 400 nm. The result, as confirmed from the 1931 CIE coordinates diagram, indicates the emission of red-orange light by RH-SiO₂: xSm³⁺ (x=0.01 and 0.1 molar ratios) and yellow-orange light from RH-SiO₂: 0.05 Sm³⁺. Finally, the result shows that RH-SiO₂ doped with samarium (Sm³⁺) ions can be applicable in display applications.

Keywords: luminescence, nanosilica, nanophosphors, Sm³⁺

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Authors: Gulshan Mammadova

Abstract:

This paper presents the results of studying the surface microrelief in 2D and 3D models and analyzing the spectroscopy of a three-junction TlInSe₂ crystal. Analysis of the results obtained showed that with a change in the composition of the TlInSe₂ crystal, sharp changes occur in the microrelief of its surface. An X-ray optical diffraction analysis of the TlInSe₂ crystal was experimentally carried out. Based on ellipsometric data, optical functions were determined - the real and imaginary parts of the dielectric permittivity of crystals, the coefficients of optical absorption and reflection, the dependence of energy losses and electric field power on the effective density, the spectral dependences of the real (σᵣ) and imaginary (σᵢ) parts, optical electrical conductivity were experimentally studied. The fluorescence spectra of the ternary compound TlInSe₂ were isolated and analyzed when excited by light with a wavelength of 532 nm. X-ray studies of TlInSe₂ showed that this phase crystallizes into tetragonal systems. Ellipsometric measurements showed that the real (ε₁) and imaginary (ε₂) parts of the dielectric constant are components of the dielectric constant tensor of the uniaxial joints under consideration and do not depend on the angle. Analysis of the dependence of the real and imaginary parts of the refractive index of the TlInSe₂ crystal on photon energy showed that the nature of the change in the real and imaginary parts of the dielectric constant does not differ significantly. When analyzing the spectral dependences of the real (σr) and imaginary (σi) parts of the optical electrical conductivity, it was noticed that the real part of the optical electrical conductivity increases exponentially in the energy range 0.894-3.505 eV. In the energy range of 0.654-2.91 eV, the imaginary part of the optical electrical conductivity increases linearly, reaches a maximum value, and decreases at an energy of 2.91 eV. At 3.6 eV, an inversion of the imaginary part of the optical electrical conductivity of the TlInSe₂ compound is observed. From the graphs of the effective power density versus electric field energy losses, it is known that the effective power density increases significantly in the energy range of 0.805–3.52 eV. The fluorescence spectrum of the ternary compound TlInSe₂ upon excitation with light with a wavelength of 532 nm has been studied and it has been established that this phase has luminescent properties.

Keywords: optical properties, dielectric permittivity, real and imaginary dielectric permittivity, optical electrical conductivity

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Authors: Hristina Šalipur, Jasmina Dostanić, Davor Lončarević, Matej Huš

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Photocatalytic water splitting/alcohol photoreforming has been used for the conversion of sunlight energy in the process of hydrogen production due to its sustainability, environmental safety, effectiveness and simplicity. Titanate nanotubes are frequently studied materials since they combine the properties of photo-active semiconductors with the properties of layered titanates, such as the ion-exchange ability. Platinum (Pt) doping into titanate structure has been considered an effective strategy in better separation efficiency of electron-hole pairs and lowering the overpotential for hydrogen production, which results in higher photocatalytic activity. In our work, Pt doped titanate catalysts were synthesized via simple alkaline hydrothermal treatment, incipient wetness impregnation method and temperature-programmed reduction. The structural, morphological and optical properties of the prepared catalysts were investigated using various characterization techniques such as X-ray diffraction (XRD), scanning electron microscopy (SEM), N2 physisorption, and diffuse reflectance spectroscopy (DRS). The activities of the prepared Pt-doped titanate photocatalysts were tested for hydrogen production via photocatalytic water splitting/alcohol photoreforming process under simulated solar light irradiation. Characterization of synthesized Pt doped titanate catalysts showed crystalline anatase phase, preserved nanotubular structure and high specific surface area. The result showed enhancement of activity in photocatalytic water splitting/alcohol photoreforming in the following order 2-butanol>1-butanol>tert-butanol, with obtained maximal hydrogen production rate of 7.5, 5.3 and 2 mmol g-1 h-1, respectively. Different possible factors influencing the hole scavenging ability, such as hole scavenger redox potential and diffusivity, adsorption and desorption rate of the hole scavenger on the surface and stability of the alcohol radical species generated via hole scavenging, were investigated. The theoretical evaluation using density functional theory (DFT) further elucidated the reaction kinetics and detailed mechanism of photocatalytic water splitting/alcohol photoreforming.

Keywords: hydrogen production, platinum, semiconductor, water splitting, density functional theory

Procedia PDF Downloads 113