Search results for: two-photon fluorescence microscopy

Authors: Hina Verma, Karine Le Guen, Mohammed H. Modi, Rajnish Dhawan, Philippe Jonnard

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Periodic multilayer mirrors have potential application as optical components in X-ray microscopy, particularly working in the water window region. The water window range, located between the absorption edges of carbon (285 eV) and oxygen (530eV), along with the presence of nitrogen K absorption edge (395 eV), makes it a powerful method for imaging biological samples due to the natural optical contrast between water and carbon. We characterized bilayer, trilayer, quadrilayer, and multilayer systems of Mg/Sc with ZrC thin layers introduced as a barrier layer and capping layer prepared by ion beam sputtering. The introduction of ZrC as a barrier layer is expected to improve the structure of the Mg/Sc system. The ZrC capping layer also prevents the stack from oxidation. The structural analysis of the Mg/Sc systems was carried out by using grazing incidence X-ray reflectivity (GIXRR) to obtain non-destructively a first description of the structural parameters, thickness, roughness, and density of the layers. Resonant soft X-ray reflectivity measurements in the vicinity of Sc L-absorption edge were performed to investigate and quantify the atomic distribution of deposited layers. Near absorption edge, the atomic scattering factor of an element changes sharply depending on its chemical environment inside the structure.

Keywords: buried interfaces, resonant soft X-ray reflectivity, X-ray optics, X-ray reflectivity

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Authors: R. Khrifou, M. Galai, R. Touir, M. Ebn Touhami, Y. Ramli

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A 2-(5-methyl-2-Nitro-1H-imidazol-1-yl)ethyl benzoate (IMDZ-B) was synthesized and characterized using elemental analyses, NMR, and Fourier transform infrared (FTIR) techniques. Its effect on brass corrosion in 1.0 M H₃PO₄ solution was investigated by using electrochemical measurements coupled with X-ray diffraction analysis (XRD), Scanning electron microscopy (SEM) and Energy-dispersive X-ray spectroscopy (EDX). The polarization measurements showed that the IMDZ-B acts as a mixed-type inhibitor. Indeed, it is found that the IMDZ-B compound is a very good inhibitor, and its inhibition efficiency increases with concentration to reach a maximum of 99.5 % at 10-³ M. In addition, the obtained electrochemical parameters from impedance indicated that the IMDZ-B molecules act by adsorption on metallic surfaces. This adsorption was found to obey Langmuir’s adsorption isotherm. However, the temperature effect on the performance of IMDZ-B was also studied. It is found that the IMDZ-B takes its performance at high temperatures. In addition, the obtained kinetic and thermodynamic parameters showed that the IMDZ-B molecules act via two adsorption modes, physisorption and chemisorptions, and its process is endothermic and spontaneous. Finally, the XRD and SEM/EDX analyses confirmed the electrochemical obtained results.

Keywords: low concentration, anti-corrosion brass, IMDZ-B product, phosphoric acid solution, electrochemical, SEM\EDAX analysis

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Authors: Abhishek Kumar Sah, Preeti K. Suresh

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Effective drug delivery to the eye is a massive challenge, due to complicated physiological ocular barriers, rapid washout by tear and nasolachrymal drainage. Thus, most of the conventional ophthalmic formulations face the problem of low ocular bioavailability. Ophthalmic drug therapy can be improved by enhancing the precorneal drug retention along with improved drug penetration. The aim of the present investigation was to develop and evaluate a biodegradable polymer poly (D, L-lactide-co-glycolide) (PLGA) coated nanoparticulate carrier of loteprednol etabonate. PLGA nanoparticles were prepared by modified emulsification/solvent diffusion method using high-speed homogenizer followed by sonication. The nanoparticles were characterized for various parameters such as particle size, zeta potential, polydispersity index, X-ray powder diffraction (XRD), Transmission electron microscopy (TEM), in vitro drug release profile and stability. The prepared nanocarriers displayed mean particle size in the range of 271.7 to 424.4 nm, with zeta potential less than –10 mV. In vitro release in simulated tear fluid (STF) nanocarrier showed an extended release profile of loteprednol etabonate. TEM confirmed the spherical morphology and smooth surface of the particles. All the prepared formulations were found to be stable at varying temperatures.

Keywords: drug delivery, ocular delivery, polymeric nanoparticles, loteprednol etabonate

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Authors: Alok Srivastava, Vidit Gupta, Aparna Singh, Chandra Sekher Yerramalli

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Carbon-fiber epoxy composites show extremely high modulus and strength in the uniaxial direction. However, they are prone to fail under low load in transverse direction due to the weak nature of the interface between the carbon-fiber and epoxy. In the current study, we have coated graphene nano-platelets (GNPs) on the carbon-fibers in an attempt to strengthen the interface/interphase between the fiber and the matrix. Vacuum Assisted Resin Transfer Moulding (VARTM) has been used to make the laminates of eight cross-woven fabrics. Tensile, flexural and fracture toughness tests have been performed on pristine carbon-fiber composite (P-CF), GNP coated carbon-fiber composite (GNP-CF) and functionalized-GNP coated carbon-fiber composite (F-GNP-CF). The tensile strength and flexural strength values are pretty similar for P-CF and GNP-CF. The micro-structural examination of the GNP coated carbon-fibers, as well as the fracture surfaces, have been carried out using scanning electron microscopy (SEM). The micrographs reveal the deposition of GNPs onto the carbon fibers in transverse and longitudinal direction. Fracture surfaces show the debonding and pull outs of the carbon fibers in P-CF and GNP-CF samples.

Keywords: carbon fiber, graphene nanoplatelets, strength, VARTM, Vacuum Assisted Resin Transfer Moulding

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Authors: Raghvendra Singh Yadav, Ivo Kuřitka, Jarmila Vilcakova, Pavel Urbánek, Michal Machovsky, Milan Masař, Martin Holek

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Herein, we reported the influence of La³⁺ substitution on structural, magnetic and dielectric properties of CoFe₂O₄ nanoparticles synthesized by starch-assisted sol-gel combustion method. X-ray diffraction pattern confirmed the formation of cubic spinel structure of La³⁺ ions doped CoFe₂O₄ nanoparticles. Raman and Fourier Transform Infrared spectroscopy study also confirmed cubic spinel structure of La³⁺ substituted CoFe₂O₄ nanoparticles. The field emission scanning electron microscopy study revealed that La³⁺ substituted CoFe2O4 nanoparticles were in the range of 10-40 nm. The magnetic properties of La³⁺ substituted CoFe₂O₄ nanoparticles were investigated by using vibrating sample magnetometer. The variation in saturation magnetization, coercivity and remanent magnetization with La³⁺ concentration in CoFe2O4 nanoparticles was observed. The variation of real and imaginary part of dielectric constant, tan δ, and AC conductivity were studied with change of concentration of La³⁺ ions in CoFe₂O₄ nanoparticles. The variation in optical properties was studied via UV-Vis absorption spectroscopy. Acknowledgment: This work was supported by the Ministry of Education, Youth and Sports of the Czech Republic – Program NPU I (LO1504).

Keywords: starch, sol-gel combustion method, nanoparticles, magnetic properties, dielectric properties

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Authors: Hu-Cheng Weng, Jhen-Ting Huang, Chia-Chia Chang, An-Ya Lo

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In this study, carbon mesoporous material, CMK-3, was adopted as supporting material for electroactive polymerspolyaniline (PANI), polyaniline, for supercapacitor application, where hydroquinone (HQ) was integrated to enhance the redox reaction of PANI. The results show that the addition of PANI improves the capacitance of electrode from 89 F/g (CMK-3) to 337 F/g (PANI/CMK-3), the addition of HQ furtherly improves the capacitance to 463 F/g (PANI/CMK-3/HQ). The PANI provides higher energy density and also acts as binder of the electrode; the CMK-3 provides higher electron double layer capacitance EDLC and stabilize the polyaniline by its highly porosity. With the addition of HQ, the capacitance of PANI/CMK-3 was further enhanced. In-situ analyses including cyclic voltammetry (CV), chronopotentiometry (CP), electron impedance spectrum (EIS) analyses were applied for electrode performance examination. For materials characterization, the crystal structure, morphology, microstructure, and porosity were examined by X-ray diffraction (XRD), scanning electron microscope (SEM), and transmission electron microscopy (TEM), and 77K N2 adsorption/desorption analyses, respectively. The effects of electrolyte pH value, PANI polymerization time, HQ concentration, and PANI/CMK-3 ratio on capacitance were discussed. The durability was also studied by long-term operation test. The results show that PANI/CMK-3/HQ with great potential for supercapacitor application. Finally, the potential of all-solid PANI/CMK-3/HQ based supercapacitor was successfully demonstrated.

Keywords: CMK3, PANI, redox electrolyte, solid supercapacitor

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Authors: N. Rajeswara Rao, T. Venkatappa Rao, K. Sowri Babu, N. Srinivas Rao, P. S. V. Shanmukhi

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Carboxymethyl Starch (CMS) is a biopolymer derived from starch by the substitution method. CMS is proclaimed to have improved physicochemical properties than native starch. The present work deals with the effect of gamma radiation on the physicochemical properties of CMS. The samples were exposed to gamma irradiation of doses 30, 60 and 90 kGy. The resultant properties were studied with electron spin resonance (ESR), fourier transform infrared spectrometer (FTIR), differential scanning calorimeter (DSC), X-ray diffractometer (XRD) and scanning electron microscopy. Irradiation of CMS by gamma rays initiates cleavage of glucosidic bonds producing different types of radicals. Some of these radicals convert to peroxy radicals by abstracting oxygen. The ESR spectrum of CMS is anisotropic and is thought to be due to the superposition of various component spectra. In order to analyze the ESR spectrum, computer simulations were also employed. ESR spectra are also recorded under different conditions like post-irradiation times, variable temperatures and saturation behavior in order to evaluate the stability of free radicals produced on irradiation. Thermal studies from DSC depict that for CMS the gelatization process was absconded at higher doses. Relative crystallinity was reduced significantly after irradiation from XRD Studies. FTIR studies also confirm the same aspect. From ESR studies, it was concluded that irradiated CMS could be a potential reference material in ESR dosimetry.

Keywords: gamma rays, free radicals, ESR simulations, gelatization

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Authors: Kitti Szoke, Laszlo Szoke, Attila Czompa, Arpad Tosaki, Istvan Lekli

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Autophagy plays an important role in cardiac hypertrophy, which is one of the most common causes of heart failure in the world. This self-degradative catabolic process, responsible for protein quality control, balancing sources of energy at critical times, and elimination of damaged organelles. The autophagic activity can be triggered by starvation, oxidative stress, or pharmacological agents, like rapamycin. This induced autophagy can promote cell survival during starvation or pathological stress. In this study, it is investigated the effect of the induced autophagic process on angiotensin induced hypertrophic H9c2 cells. In our study, it is used H9c2 cells as an in vitro model. To induce hypertrophy, cells were treated with 10000 nM angiotensin-II, and to activate autophagy, 100 nM rapamycin treatment was used. The following groups were formed: 1: control, 2: 10000 nM AT-II, 3: 100 nM rapamycin, 4: 100 nM rapamycin pretreatment then 10000 nM AT-II. The cell viability was examined via MTT (cell proliferation assay) assay. The cells were stained with rhodamine-conjugated phalloidin and DAPI to visualize F-actin filaments and cell nuclei then the cell size alteration was examined in a fluorescence microscope. Furthermore, the expression levels of autophagic and apoptotic proteins such as Beclin-1, p62, LC3B-II, Cleaved Caspase-3 were evaluated by Western blot. MTT assay result suggests that the used pharmaceutical agents in the tested concentrations did not have a toxic effect; however, at group 3, a slight decrement was detected in cell viability. In response to AT-II treatment, a significant increase was detected in the cell size; cells became hypertrophic. However, rapamycin pretreatment slightly reduced the cell size compared to group 2. Western blot results showed that AT-II treatment-induced autophagy, because the increased expression of Beclin-1, p62, LC3B-II were observed. However, due to the incomplete autophagy, the apoptotic Cleaved Caspase-3 expression also increased. Rapamycin pretreatment up-regulated Beclin-1 and LC3B-II, down-regulated p62 and Cleaved Caspase-3, indicating that rapamycin-induced autophagy can restore the normal autophagic flux. Taken together, our results suggest that rapamycin activated autophagy reduces angiotensin-II induced hypertrophy.

Keywords: angiotensin-II, autophagy, H9c2 cell line, hypertrophy, rapamycin

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Authors: Marinos Dimitropoulos, George Trakakis, Nikolaus Meyerbröker, Raphael Dalpke, Polina Angelova, Albert Schnieders, Christos Pavlou, Christos Kostaras, Costas Galiotis, Konstantinos Dassios

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Intended for purifying water, water separation technologies are widely employed in a variety of contemporary household and industrial applications. Ultrathin Carbon Nanomembranes (CNMs) offer a highly selective, fast-flow, energy-efficient water separation technology intended for demanding water treatment applications as a technological replacement for biological filtration membranes. The membranes are two-dimensional (2D) materials with sub-nm functional pores and a thickness of roughly 1 nm; they may be generated in large quantities on porous supporting substrates and have customizable properties. The purpose of this work was to investigate and analyze the mechanical characteristics of CNMs and their substrates in order to ensure the structural stability of the membrane during operation. Contrary to macro-materials, it is difficult to measure the mechanical properties of membranes that are only a few nanometers thick. The membranes were supported on atomically flat substrates as well as suspended over patterned substrates, and their inherent mechanical properties were tested with atomic force microscopy. Quantitative experiments under nanomechanical loading, nanoindentation, and nano fatigue demonstrated the membranes' potential for usage in water separation applications.

Keywords: carbon nanomembranes, mechanical properties, AFM

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Authors: I. M. B. Omiogbemi, D. S. Yawas, I. M. Dagwa, F. G. Okibe

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This work present the effects of some gas metal arc welding parameters on the corrosion behavior of austenitic stainless steel, exposed to 0.5M sodium hydroxide at ambient temperatures (298K) using conventional weight loss determination, together with surface morphology evaluation by scanning electron microscopy and the application of factorial design of experiment to determine welding conditions which enhance the integrity of the welded stainless steel. The welding variables evaluated include speed, voltage and current. Different samples of the welded stainless steels were immersed in the corrosion environment for 8, 16, 24, 32 and 40 days and weight loss determined. From the results, it was found that increase in welding current and speed at constant voltage gave the optimum performance of the austenitic stainless steel in the environment. At a of speed 40cm/min, 110Amp current and voltage of 230 volt the welded stainless steel showed only a 0.0015mg loss in weight after 40 days. Pit-like openings were observed on the surface of the metals indicating corrosion but were minimal at the optimum conditions. It was concluded from the research that relatively high welding speed and current at a constant voltage gives a good welded austenitic stainless steel with better integrity.

Keywords: welding, current, speed, austenitic stainless steel, sodium hydroxide

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Authors: Anjali G. Pillai, S. Chadrakaran

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The extensive amount of sludge generated throughout the world, as a part of water treatment works, have caused various social and economic issues, such as a demand on landfill spaces, increase in environmental pollution and raising the waste management cost. With growing social awareness about toxic incinerator emissions and the increasing concern over the disposal of sludge on the agricultural land, the recovery of sewage sludge as a building and construction raw material can be considered as an innovative approach to tackle the sludge disposal problem. The proposed work aims at studying the recycling ability of the sludge, generated from the water treatment process, by incorporating it into the fired clay brick units. The work involves initial study of the geotechnical characteristics of the brick-clay and the sludge. Chemical compatibility of both the materials will be analyzed by X-ray fluorescence technique. The variation in the strength aspects with varying proportions of sludge i.e. 10%, 20%, 30% and 40% in the sludge-clay mix will also be determined by the proctor density test. Based on the optimum moisture content, the sludge-clay bricks will be manufactured in a brick manufacturing plant and the modified brick units will be tested to determine the variation in compressive strength, bulk density, firing shrinkage, shrinkage loss and initial water absorption rate with respect to the conventional clay bricks. The results will be compared with the specifications given in Indian Standards to arrive at the potential use of the new bricks. The durability aspect will be studied by conducting the leachate analysis test using atomic adsorption spectrometry. The lightweight characteristics of the sludge modified bricks will be ascertained with the scanning electron microscope technique which will be indicative of the variation in pore structure with the increase in sludge content within the bricks. The work will determine the suitable proportion of the sludge – clay mix in the brick which can then be effectively implemented. The feasibility aspect of the work will be determined for commercial production of the units. The work involves providing a strategy for conversion of waste to resource. Moreover, it provides an alternative solution to the problem of growing scarcity of brick-clay for the manufacturing of fired clay bricks.

Keywords: eco-bricks, green construction material, sludge amended bricks, sludge disposal, waste management

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Authors: Prashant Parhad, Vinayak Dakre, Ajay Likhite, Jatin Bhatt

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This work mainly focuses on machinability studies of Austempered Ductile Iron (ADI). The Ductile Iron (DI) was austempered at 250 oC for different durations and the process window for austempering was established by studying the microstructure. The microstructural characterization of the material was done using optical microscopy, SEM and XRD. The samples austempered as per the process window were then subjected to turning using a TiAlN-coated tungsten carbide insert to study the effect of cutting parameters, namely the cutting speed and the depth of cut. The effect was investigated in terms of cutting forces required as well as the surface roughness obtained. The turning was conducted on a CNC turning machine and primary (Fx), radial (Fy) and feed (Fz) cutting forces were quantified with a three-component dynamometer. It was observed that the magnitude of radial force was more than that of primary cutting force for all cutting speed and for various depths of cut studied. It has also been seen that increasing the cutting speed improves the surface quality. The observed machinability behaviour was investigated in light of the microstructure of the material obtained under the given austempering conditions and a structure-property- co-relation was established between the two. For all cutting speed and depth of cut, the best machining response in terms of cutting forces and surface quality was obtained towards the centre of process window.

Keywords: process window, cutting speed, depth of cut, surface roughness

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Authors: Nicole Nazario Bayon, Prathima Prabhu Tumkur, Nithin Krisshna Gunasekaran, Krishnan Prabhakaran, Joseph C. Hall, Govindarajan T. Ramesh

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Titanium nitride (TiN) nanoparticles have sparked interest over the past decade due to their characteristics such as thermal stability, extreme hardness, low production cost, and similar optical properties to gold. In this study, TiN nanoparticles were synthesized via a thermal benzene route to obtain a black powder of nanoparticles. The final product was drop cast onto conductive carbon tape and sputter coated with gold/palladium at a thickness of 4 nm for characterization by field emission scanning electron microscopy (FE-SEM) with energy dispersive X-Ray spectroscopy (EDX) that revealed they were spherical. ImageJ software determined the average size of the TiN nanoparticles was 79 nm in diameter. EDX revealed the elements present in the sample and showed no impurities. Further characterization by X-ray diffraction (XRD) revealed characteristic peaks of cubic phase titanium nitride, and crystallite size was calculated to be 14 nm using the Debye-Scherrer method. Dynamic light scattering (DLS) analysis revealed the size and size distribution of the TiN nanoparticles, with average size being 154 nm. Zeta potential concluded the surface of the TiN nanoparticles is negatively charged. Biocompatibility studies using MTT(3-(4,5-Dimethylthiazol-2-yl)-2,5-Diphenyltetrazolium Bromide) assay showed TiN nanoparticles are not cytotoxic at low concentrations (2, 5, 10, 25, 50, 75 mcg/well), and cell viability began to decrease at a concentration of 100 mcg/well.

Keywords: biocompatibility, characterization, cytotoxicity, nanoparticles, synthesis, titanium nitride

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Authors: A. González-Caro, A. M. Merino-Lechuga, D. Suescum-Morales, E. Fernández-Ledesma, J. R. Jiménez, J. M. Fernández-Rodríguez

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Climate change is one of the most significant issues today. Since the 19th century, the rise in temperature has not only been due to natural change, but also to human activities, which have been the main cause of climate change, mainly due to the burning of fossil fuels such as coal, oil and gas. The boom in the construction sector in recent years is also one of the main contributors to CO₂ emissions into the atmosphere; for example, for every tonne of cement produced, 1 tonne of CO₂ is emitted into the atmosphere. Most of the research being carried out in this sector is focused on reducing the large environmental impact generated during the manufacturing process of building materials. In detail, this research focuses on the recovery of waste from olive oil mills. Spain is the world's largest producer of olive oil, and this sector generates a large amount of waste and by-products such as olive pits, “alpechín” or “alpeorujo”. This olive stone by means of a pyrosilisis process gives rise to the production of active carbon. The process causes the carbon to develop many internal spaces. This study is based on the manufacture of porous mortars with Portland cement and natural limestone sand, with an addition of 5% and 10% of activated carbon. Two curing environments were used: i) dry chamber, with a humidity of 65 ± 10% and temperature of 21 ± 2 ºC and an atmospheric CO₂ concentration (approximately 0.04%); ii) accelerated carbonation chamber, with a humidity of 65 ± 10% and temperature of 21 ± 2 ºC and an atmospheric CO₂ concentration of 5%. In addition to eliminating waste from an industry, the aim of this study is to reduce atmospheric CO₂. For this purpose, first, a physicochemical and mineralogical characterisation of all raw materials was carried out, using techniques such as fluorescence and X-ray diffraction. The particle size and specific surface area of the activated carbon were determined. Subsequently, tests were carried out on the hardened mortar, such as thermogravimetric analysis (to determine the percentage of CO₂ capture), as well as mechanical properties, density, porosity, and water absorption. It was concluded that the activated carbon acts as a sink for CO₂, causing it to be trapped inside the voids. This increases CO₂ capture by 300% with the addition of 10% activated carbon at 7 days of curing. There was an increase in compressive strength of 17.5% with the CO₂ chamber after 7 days of curing using 10% activated carbon compared to the dry chamber.

Keywords: olive stone, activated carbon, porous mortar, CO₂ capture, economy circular

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Authors: Mohammadjavad Yaghoubi, Arul Arulrajah, Mahdi M. Disfani, Suksun Horpibulsuk, Myint W. Bo, Stephen P. Darmawan

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This paper investigates the changes in the strength development of a high water content soft soil stabilised with alkaline activation of fly ash (FA) to use in deep soil mixing (DSM) technology. The content of FA was 20% by dry mass of soil, and the alkaline activator was sodium silicate (Na2SiO3). Samples were cured for 3, 7, 14, 28 and 56 days to evaluate the effect of curing time on strength development. To study the effect of adding slag (S) to the mixture on the strength development, 5% S was replaced with FA. In addition, the effect of the initial unit weight of samples on strength development was studied by preparing specimens with two different static compaction stresses. This was to replicate the field conditions where during implementing the DSM technique, the pressure on the soil while being mixed, increases with depth. Unconfined compression strength (UCS), scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS) tests were conducted on the specimens. The results show that adding S to the FA based geopolymer activated by Na2SiO3 decreases the strength. Furthermore, samples prepared at a higher unit weight demonstrate greater strengths. Moreover, samples prepared at lower unit weight reached their final strength at about 14 days of curing, whereas the strength development continues to 56 days for specimens prepared at a higher unit weight.

Keywords: alkaline activation, curing time, fly ash, geopolymer, slag

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Authors: Hubert Beisch, Janik Marx, Svenja Garlof, Roman Shvets, Ivan Grygorchak, Andriy Kityk, Bodo Fiedler

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Three-dimensional carbon materials can be used as electrode materials for energy storage systems such as batteries and supercapacitors. Fast charging and discharging times are realizable without reducing the performance due to aging processes. Furthermore high specific surface area (SSA) of three-dimensional carbon structures leads to high specific capacities. One newly developed carbon foam is Globugraphite. This interconnected globular carbon morphology with statistically distributed hierarchical pores is manufactured by a chemical vapor deposition (CVD) process from ceramic templates resulting from a sintering process. Via scanning electron (SEM) and transmission electron microscopy (TEM), the morphology is characterized. Moreover, the SSA was measured by the Brunauer–Emmett–Teller (BET) theory. Measurements of Globugraphite in an organic and inorganic electrolyte show high energy densities and power densities resulting from ion absorption by forming an electrochemical double layer. A comparison of the specific values is summarized in a Ragone diagram. Energy densities up to 48 Wh/kg and power densities to 833 W/kg could be achieved for an SSA from 376 m²/g to 859 m²/g. For organic electrolyte, a specific capacity of 100 F/g at a density of 20 mg/cm³ was achieved.

Keywords: BET, carbon foam, CVD process, electrochemical cell, Ragone diagram, SEM, TEM

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Authors: Z. N. Ali, O. A. Babatunde, S. Garba, H. M. S. Haruna

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The potency of modified and unmodified activated carbons prepared from shells of Cocos nucifera (coconut shell), straws of Pennisetum glaucum (millet) and Sorghum bicolor (sorghum) for adsorption of hydrogen sulphide gas were investigated using an adsorption apparatus (stainless steel cylinder) at constant temperature (ambient temperature). The adsorption equilibria states were obtained when the pressure indicated on the pressure gauge remained constant. After modification with nitric acid, results of the scanning electron microscopy of the unmodified and modified activated carbons showed that HNO3 greatly improved the formation of micropores and mesopores on the activated carbon surface. The adsorption of H2S gas was found to be highest in modified Cocos nucifera activated carbon with maximum monolayer coverage of 28.17 mg/g, and the adsorption processes were both physical and chemical with the physical process being predominant. The adsorption data were well fitted into the Langmuir isotherm model with the adsorption capacities of the activated carbons in the order modified Cocos nucifera > modified Pennisetum glaucum > modified Sorghum bicolor > unmodified Cocos nucifera > unmodified Pennisetum glaucum > unmodified Sorghum bicolour.

Keywords: activated carbon adsorption, hydrogen sulphide, nitric acid, modification, stainless steel cylinder

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Authors: Z. Ž. Lazarević, D. L. Sekulić, V. N. Ivanovski, N. Ž. Romčević

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NiFe2O4 (nickel ferrite), ZnFe2O4 (zinc ferrite) and Ni0.5Zn0.5Fe2O4 (nickel-zinc ferrite) were prepared by mechanochemical route in a planetary ball mill starting from mixture of the appropriate quantities of the Ni(OH)2/Fe(OH)3, Zn(OH)2/Fe(OH)3 and Ni(OH)2/Zn(OH)2/Fe(OH)3 hydroxide powders. In order to monitor the progress of chemical reaction and confirm phase formation, powder samples obtained after 25 h, 18 h and 10 h of milling were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), IR, Raman and Mössbauer spectroscopy. It is shown that the soft mechanochemical method, i.e. mechanochemical activation of hydroxides, produces high quality single phase ferrite samples in much more efficient way. From the IR spectroscopy of single phase samples it is obvious that energy of modes depends on the ratio of cations. It is obvious that all samples have more than 5 Raman active modes predicted by group theory in the normal spinel structure. Deconvolution of measured spectra allows one to conclude that all complex bands in the spectra are made of individual peaks with the intensities that vary from spectrum to spectrum. The deconvolution of Raman spectra allows to separate contributions of different cations to a particular type of vibration and to estimate the degree of inversion.

Keywords: ferrites, Raman spectroscopy, IR spectroscopy, Mössbauer measurements

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Authors: Woei-Shyan Lee, Yu-Liang Chuang

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The nano-mechanical properties of as-deposited Cu/Si thin films indented to a depth of 2000 nm are investigated using a nanoindentation technique. The nanoindented specimens are annealed at a temperature of either 160 °C or 210°C, respectively. The microstructures of the as-deposited and annealed samples are then examined via transmission electron microscopy (TEM). The results show that both the loading and the unloading regions of the load-displacement curve are smooth and continuous, which suggests that no debonding or cracking occurs during nanoindentation. In addition, the hardness and Young’s modulus of the Cu/Si thin films are found to vary with the nanoindentation depth, and have maximum values of 2.8 GPa and 143 GPa, respectively, at the maximum indentation depth of 2000 nm. The TEM observations show that the region of the Cu/Si film beneath the indenter undergoes a phase transformation during the indentation process. In the case of the as-deposited specimens, the indentation pressure induces a completely amorphous phase within the indentation zone. For the specimens annealed at a temperature of 160°C, the amorphous nature of the microstructure within the indented zone is maintained. However, for the specimens annealed at a higher temperature of 210°C, the indentation affected zone consists of a mixture of amorphous phase and nanocrystalline phase. Copper silicide (η-Cu3Si) precipitates are observed in all of the annealed specimens. The density of the η-Cu3Si precipitates is found to increase with an increasing annealing temperature.

Keywords: nanoindentation, Cu/Si thin films, microstructural evolution, annealing temperature

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Authors: Khushboo Bhavsar, Nisha K. Shah, Neha Parekh

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The status of wastewater treatment needs a novel and quick method for treating the wastewater containing ammoniacal nitrogen. Adsorption behavior of ammoniacal nitrogen from wastewater using the nanoparticles loaded coconut coir was investigated in the present work. Manganese Oxide (MnO2) and Zinc Oxide (ZnO) nanoparticles were prepared and used for the further adsorption study. Manganese nanoparticles loaded coconut coir (MNLCC) and Zinc nanoparticles loaded coconut coir (ZNLCC) were prepared via a simple method and was fully characterized. The properties of both MNLCC and ZNLCC were characterized by Scanning electron microscopy, Fourier Transform Infrared Spectroscopy and X-ray diffraction. Adsorption characteristics were studied using batch technique considering various parameters like pH, adsorbent dosage, time, temperature and agitation time. The NH3-N adsorption process for MNLCC and ZNLCC was thoroughly studied from both kinetic and equilibrium isotherm view-points. The results indicated that the adsorption efficiency of ZNLCC was better when compared to MNLCC. The adsorption kinetics at different experimental conditions showed that second order kinetic model best fits ensuring the monovalent binding sites existing in the present experimental system. The outcome of the entire study suggests that the ZNLCC can be a smart option for the treatment of the ammoniacal nitrogen containing wastewater.

Keywords: ammoniacal nitrogen, MnO2, Nanoparticles, ZnO

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Authors: M. Masłowski, M. Zaborski

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Magnetorheological elastomer composites based on micro- and nano-sized Fe3O4 magnetoactive fillers in silicone rubber are reported and studied. To improve the dispersion of applied fillers in polymer matrix, ionic liquids such as 1-ethyl-3-methylimidazolium diethylphosphate, 1-butyl-3-methylimidazolium hexafluorophosphate, 1-hexyl-3-methylimidazolium chloride, 1-butyl-3-methylimidazolium trifluoromethanesulfonate,1-butyl-3-methylimidazolium tetrafluoroborate, trihexyltetradecylphosphonium chloride were added during the process of composites preparation. The method of preparation process influenced the specific properties of MREs (isotropy/anisotropy), similarly to ferromagnetic particles content and theirs quantity. Micro and non-sized magnetites were active fillers improving the mechanical properties of elastomers. They also changed magnetic properties and reinforced the magnetorheological effect of composites. Application of ionic liquids as dispersing agents influenced the dispersion of magnetic fillers in the elastomer matrix. Scanning electron microscopy images used to observe magnetorheological elastomer microstructures proved that the dispersion improvement had a significant effect on the composites properties. Moreover, the particles orientation and their arrangement in the elastomer investigated by vibration sample magnetometer showed the correlation between MRE microstructure and their magnetic properties.

Keywords: magnetorheological elastomers, iron oxides, ionic liquids, dispersion

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Authors: H. Mokaddem, D. Miroud, N. Azouaou, F. Si-Ahmed, Z. Sadaoui

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The synthesis and characterization of activated carbon from local lignocellulosic precursor (Algerian alfa) was carried out for the removal of cationic dyes from aqueous solutions. The effect of the production variables such as impregnation chemical agents, impregnation ratio, activation temperature and activation time were investigated. Carbon obtained using the optimum conditions (CaCl2/ 1:1/ 500°C/2H) was characterized by various analytical techniques scanning electron microscopy (SEM), infrared spectroscopic analysis (FTIR) and zero-point-of-charge (pHpzc). Adsorption tests of methylene blue on the optimal activated carbon were conducted. The effects of contact time, amount of adsorbent, initial dye concentration and pH were studied. The adsorption equilibrium examined using Langmuir, Freundlich, Temkin and Redlich–Peterson models reveals that the Langmuir model is most appropriate to describe the adsorption process. The kinetics of MB sorption onto activated carbon follows the pseudo-second order rate expression. The examination of the thermodynamic analysis indicates that the adsorption process is spontaneous (ΔG ° < 0) and endothermic (ΔH ° > 0), the positive value of the standard entropy shows the affinity between the activated carbon and the dye. The present study showed that the produced optimal activated carbon prepared from Algerian alfa is an effective low-cost adsorbent and can be employed as alternative to commercial activated carbon for removal of MB dye from aqueous solution.

Keywords: activated carbon, adsorption, cationic dyes, Algerian alfa

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Authors: S. Mezghani, E. Perrin, J. L. Bodnar, J. Marthe, B. Cauwe, V. Vrabie

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Non contact evaluation of the thickness of paint coatings can be attempted by different destructive and nondestructive methods such as cross-section microscopy, gravimetric mass measurement, magnetic gauges, Eddy current, ultrasound or terahertz. Infrared thermography is a nondestructive and non-invasive method that can be envisaged as a useful tool to measure the surface thickness variations by analyzing the temperature response. In this paper, the thermal quadrupole method for two layered samples heated up with a pulsed excitation is firstly used. By analyzing the thermal responses as a function of thermal properties and thicknesses of both layers, optimal parameters for the excitation source can be identified. Simulations show that a pulsed excitation with duration of ten milliseconds allows to obtain a substrate-independent thermal response. Based on this result, an experimental setup consisting of a near-infrared laser diode and an Infrared camera was next used to evaluate the variation of paint coating thickness between 60 µm and 130 µm on two samples. Results show that the parameters extracted for thermal images are correlated with the estimated thicknesses by the Eddy current methods. The laser pulsed thermography is thus an interesting alternative nondestructive method that can be moreover used for non conductive substrates.

Keywords: non destructive, paint coating, thickness, infrared thermography, laser, heterogeneity

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Authors: Umran Kurtan, Hamide Aydin, Sevim Unugur Celik, Ayhan Bozkurt

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In the present work, novel hBN/polyacrylonitrile composite nanofibers were produced via electrospinning approach and loaded with the electrolyte for rechargeable lithium-ion battery applications. The electrospun nanofibers comprising various hBN contents were characterized by using Fourier transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques. The influence of hBN/PAN ratios onto the properties of the porous composite system, such as fiber diameter, porosity, and the liquid electrolyte uptake capability were systematically studied. Ionic conductivities and electrochemical characterizations were evaluated after loading electrospun hBN/PAN composite nanofiber with liquid electrolyte, i.e., 1 M lithium hexafluorophosphate (LiPF6) in ethylene carbonate (EC)/ethyl methyl carbonate (EMC) (1:1 vol). The electrolyte loaded nanofiber has a highest ionic conductivity of 10−3 S cm⁻¹ at room temperature. According to cyclic voltammetry (CV) results it exhibited a high electrochemical stability window up to 4.7 V versus Li+/Li. Li//10 wt% hBN/PAN//LiCO₂ cell was produced which delivered high discharge capacity of 144 mAhg⁻¹ and capacity retention of 92.4%. Considering high safety and low cost properties of the resulting hBN/PAN fiber electrolytes, these materials can be suggested as potential separator materials for lithium-ion batteries.

Keywords: hexagonal boron nitride, polyacrylonitrile, electrospinning, lithium ion battery

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Authors: S. Kerakra, S. Bouhelal, M. Poncot

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The aim of this study is to give a comprehensive overview of the effect of short hollow and solid recycled polyethylene terephthalate (PET) fibers in different breaking tenacities reinforced isotactic polypropylene (iPP) composites on the mechanical and morphological properties. Composites of iPP/3, 7and 10 wt% of solid and hollow recycled PET fibers were prepared by batched melt mixing in a Brabender. The incorporation of solid recycled-PET fibers in isotactic polypropylene increase Young’s modulus of iPP relatively, meanwhile it increased proportionally with hollow fibers content. An improvement of the storage modulus, and a shift up in glass transition temperatures of hollow fibers/iPP composites was determined by DMA results. The morphology of composites was determined by scanning electron microscope (SEM) and optical polarized microscopy (OM) showing a good dispersion of the hollow fibers. Also, their flexible aspect (folding, bending) was observed. But, one weak interaction between the polymer/fibers phases was shown. Polymers can be effectively reinforced with short hollow recycled PET fibers due to their characteristics like recyclability, lightweight and the flexible aspect, which allows the absorbance of the energy of a striker with a minimum damage of the matrix. Aiming to improve the affinity matrix–recycled hollow PET fibers, it is suggested the addition of compatibilizers, as maleic anhydride.

Keywords: isotactic polypropylene, hollow recycled PET fibers, solid recycled-PET fibers, composites, short fiber, scanning electron microscope

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Authors: G. Nyongombe, Guy L. Kabongo, B. M. Mothudi, M. S. Dhlamini

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A series of Transition Metals Oxides (TMOs) doped graphene were synthesized and successfully used as supercapacitor electrode materials. The as-synthesized materials exhibited exceptional electrochemical properties owing to the combined properties of its constituents; high surface area and good conductivity were achieved. Several analytical characterization techniques were employed to investigate the morphology, crystal structure atomic arrangement and elemental chemical state in the materials for which scanning electron microscopy (SEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) were conducted, respectively. Moreover, the electrochemical properties of the as-synthesized materials were examined by performing cyclic voltammetry (CV), galvanostatic charge-discharge (GCD) and electrochemical impedance spectroscopy (EIS) measurements. Furthermore, the effect of doping concentration on the interlayer distance of the graphene materials and the charge transfer resistance are investigated and correlated to the exceptional current density which was multiplied by a factor of ~80 after TMOs doping in graphene. Finally, the resulting high capacitance obtained confirms the contribution of grapheme exceptional electronic conductivity and large surface area on the electrode materials. Such good-performing electrode materials are highly promising for supercapacitors and other energy storage devices.

Keywords: energy density, graphene, supercapacitors, TMOs

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Authors: Adinarayana Gorajana, Venkata Srikanth Meka, Sanjay Garg, Lim Sue May

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This study was designed to evaluate and enhance the solubility of poorly soluble drug, docetaxel through solid dispersion (SD) technique prepared using freeze drying method. Docetaxel solid dispersions were formulated with Soluplus in different weight ratios. Freeze drying method was used to prepare the solid dispersions. Solubility of the solid dispersions were evaluated respectively and the optimized of drug-solubilizers ratio systems were characterized with different analytical methods like Differential scanning calorimeter (DSC), Scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR) to confirm the formation of complexes between drug and solubilizers. The solubility data revealed an overall improvement in solubility for all SD formulations. The ternary combination 1:5:2 gave the highest increase in solubility that is approximately 3 folds from the pure drug, suggesting the optimum drug-solubilizers ratio system. This data corresponds with the DSC and SEM analyses, which demonstrates presence of drug in amorphous state and the dispersion in the solubilizers in molecular level. The solubility of the poorly soluble drug, docetaxel was enhanced through preparation of solid dispersion formulations employing freeze drying method. Solid dispersion with multiple carrier system shows better solubility compared to single carrier system.

Keywords: docetaxel, freeze drying, soluplus, solid dispersion technique

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Authors: Bharat Kumar, Deepak Kumar, Vijay Chaudhry

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Zirconium alloys are used as core components of nuclear reactors due to their high wear resistance, good corrosion properties, and good mechanical stability at high temperatures. Water flows inside the pressure tube through fuel claddings, which produces vibration of these core components and results in the wear of some components. Some components are subjected to the environment of coolant water containing LiOH which results in the corrosion of these components. The present work simulates some of these conditions to determine the failure mechanisms under these conditions and the effect of various parameters on them. Friction and wear experiments were performed varying the surrounding environment (room temperature, high temperature, and water submerged), duration, frequency, and displacement amplitude. Electrochemical corrosion experiments were performed by varying the concentration of LiOH in water. The worn and corroded surfaces were analyzed using scanning electron microscopy (SEM) to analyze the wear and corrosion mechanism and energy dispersive x-ray spectroscopy (EDS) and Raman spectroscopy to analyze the tribo-oxide layer formed during the wear and oxide layer formed during the corrosion. Wear increases with frequency and amplitude, and corrosion increases with LiOH concentration in water.

Keywords: zirconium alloys, wear, oxide layer, corrosion, EIS, linear polarization

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Authors: Zohreh Derikvand, Hadis Cheraghi, Azadeh Azadbakht, Vaclav Eigner, Michal Dusek

Abstract:

Two new one and two dimensional metal organic coordination polymers of Cu(II), [Cu(3-nph)2(H2O)2pz]n (1) and Ag(I), {[Ag(3-nph)pz].H2O}n (2) with pyrazine (pz) and 3- nitrophthalic acid (3-nph) have been synthesized and characterized by elemental analysis, spectral (IR, UV-Vis), thermal (TG/DTG) analysis and single crystal X-ray diffraction. We used these compounds to preparation modified electrode with Au/Pt nanosparticles in order to investigation electrochemistry and electrocatalysis activities. The surface structure and composition of the sensor were characterized by scanning electron microscopy (SEM). The Ag(I) coordination polymer shows a 2D layer structure constructed from dinuclear silver (I) building blocks in which two crystallographically Ag+ ions are connected to each other by a covalent bond. The pyrazine ligands adopt μ2 bridging modes, linking the metal centers into a one and two -dimensional coordination framework in 1 and 2. The two AgI cations are surrounded by pyrazine and 3-nitrophthalate mono anions and indicate distorted tetrahedral geometry. In the crystal structures of Ag(I) complex there are non-classical hydrogen bonding arrangements, C–O•••π and π–π stacking interactions. In Cu(II) coordination polymer, the coordination geometry around Cu(II) atom is a distorted octahedron. Interestingly, the structural analysis illustrates that the strong and weak hydrogen bond accompanied with C–H•••π and C–O•••π stacking interactions assemble the crystal structure of 1 and 2 into fascinating 3D supramolecular architecture.

Keywords: 3-nithrophethalic acid, crystal structure, coordination polymer, electrocatalysis

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Authors: Abdelmajid Timoumi, Salah Alamri, Hatem Alamri

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TiO₂ Graphene Oxide (TiO₂-GO) nanocomposite was prepared using the spin coating technique of suspension of Graphene Oxide (GO) nanosheets and Titanium Tetra Isopropoxide (TIP). The prepared nanocomposites samples were characterized by X-ray diffractometer, Scanning Electron Microscope and Atomic Force Microscope to examine their structures and morphologies. UV-vis transmittance and reflectance spectroscopy was employed to estimate band gap energies. From the TiO₂-GO samples, a 0.25 μm thin layer on a piece of glass 2x2 cm was created. The X-ray diffraction analysis revealed that the as-deposited layers are amorphous in nature. The surface morphology images demonstrate that the layers grew in distributed with some spherical/rod-like and partially agglomerated TiGO on the surface of the composite. The Atomic Force Microscopy indicated that the films are smooth with slightly larger surface roughness. The analysis of optical absorption data of the layers showed that the values of band gap energy decreased from 3.46 eV to 1.40 eV, depending on the grams of GO doping. This reduction might be attributed to electron and/or hole trapping at the donor and acceptor levels in the TiO₂ band structure. Observed results have shown that the inclusion of GO in the TiO₂ matrix have exhibited significant and excellent properties, which would be promising for application in the photovoltaic application.

Keywords: titanium dioxide, graphene oxide, thin films, solar cells

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