Search results for: Scanning Electron Microscopy-Energy Dispersive Spectroscopy

Authors: Agnieszka Feliczak-Guzik, Paulina Szczyglewska, Izabela Nowak

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A catalyst-assisted oxidation reaction is one of the key reactions exploited by various industries. Their conductivity yields essential compounds and intermediates, such as alcohols, epoxides, aldehydes, ketones, and organic acids. Researchers are devoting more and more attention to developing active and selective materials that find application in many catalytic reactions, such as cyclohexene epoxidation. This reaction yields 1,2-epoxycyclohexane and 1,2-diols as the main products. These compounds are widely used as intermediates in the perfume industry and synthesizing drugs and lubricants. Hence, our research aimed to use hierarchical zeolites modified with transition metal ions, e.g., Nb, V, and Ta, in the epoxidation reaction of cyclohexene using microwaveheating. Hierarchical zeolites are materials with secondary porosity, mainly in the mesoporous range, compared to microporous zeolites. In the course of the research, materials based on two commercial zeolites, with Faujasite (FAU) and Zeolite Socony Mobil-5 (ZSM-5) structures, were synthesized and characterized by various techniques, such as X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and low-temperature nitrogen adsorption/desorption isotherms. The materials obtained were then used in a cyclohexene epoxidation reaction, which was carried out as follows: catalyst (0.02 g), cyclohexene (0.1 cm3), acetonitrile (5 cm3) and dihydrogen peroxide (0.085 cm3) were placed in a suitable glass reaction vessel with a magnetic stirrer inside in a microwave reactor. Reactions were carried out at 45° C for 6 h (samples were taken every 1 h). The reaction mixtures were filtered to separate the liquid products from the solid catalyst and then transferred to 1.5 cm3 vials for chromatographic analysis. The test techniques confirmed the acquisition of additional secondary porosity while preserving the structure of the commercial zeolite (XRD and low-temperature nitrogen adsorption/desorption isotherms). The results of the activity of the hierarchical catalyst modified with niobium in the cyclohexene epoxidation reaction indicate that the conversion of cyclohexene, after 6 h of running the process, is about 70%. As the main product of the reaction, 2-cyclohexanediol was obtained (selectivity > 80%). In addition to the mentioned product, adipic acid, cyclohexanol, cyclohex-2-en-1-one, and 1,2-epoxycyclohexane were also obtained. Furthermore, in a blank test, no cyclohexene conversion was obtained after 6 h of reaction. Acknowledgments The work was carried out within the project “Advanced biocomposites for tomorrow’s economy BIOG-NET,” funded by the Foundation for Polish Science from the European Regional Development Fund (POIR.04.04.00-00-1792/18-00.

Keywords: epoxidation, oxidation reactions, hierarchical zeolites, synthesis

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Authors: J. Ramos, V. Gil, A. F. Torres

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The nodular iron is a material that has shown great advantages respect to other materials (steel and gray iron) in the production of machine elements. The engineering industry, especially automobile, are potential users of this material. As it is known, the alloying elements modify the properties of steels and castings. Copper has been investigated as a structural modifier of nodular iron, but studies of its mechanical and tribological implications still need to be addressed for industrial use. With the aim of improving the mechanical properties of nodular iron, alloying elements (Mn, Si, and Cu) are added in order to increase their pearlite (or ferrite) structure according to the percentage of the alloying element. In this research (using induction furnace process) nodular iron with three different percentages of copper (residual, 0,5% and 1,2%) was obtained. Chemical analysis was performed by optical emission spectrometry and microstructures were characterized by Optical Microscopy (ASTM E3) and Scanning Electron Microscopy (SEM). The study of mechanical behavior was carried out in a mechanical test machine (ASTM E8) and a Pin on disk tribometer (ASTM G99) was used to assess wear resistance. It is observed that copper increases the pearlite structure improving the wear behavior; tension behavior. This improvement is observed in higher proportion with 0,5% due to the fact that too much increase of pearlite leads to ductility loss.

Keywords: copper, mechanical properties, nodular iron, pearlite structure, wear

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Authors: K. J. Sannapapamma, H. Malligawad Lokanath, Sakeena Naikwadi

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Eco-friendly textiles are gaining importance among the consumers and textile manufacturers in the healthcare sector due to increased environmental pollution which leads to several health and environmental hazards. Hence, the research was designed to cultivate and develop the organic cotton knit, to prepare and characterize the Vetiver oil microcapsules for textile finishing and to access the wash durability of finished knits. The cotton SAHANA variety grown under organic production systems was processed and spun into 30 single yarn dyed with four natural colorants (Arecanut slurry, Eucalyptus leaves, Pomegranate rind and Indigo) and eco dyed yarn was further used for development of single jersy knitted fabric. Vetiveria zizanioides is an aromatic grass which is being traditionally used in medicine and perfumery. Vetiver essential oil was used for preparation of microcapsules by interfacial polymerization technique subjected to Gas Chromatography Mass Spectrometry (GCMS), Fourier Transform Infrared Spectroscopy (FTIR), Thermo Gravimetric Analyzer (TGA) and Scanning Electron Microscope (SEM) for characterization of microcapsules. The knitted fabric was finished with vetiver oil microcapsules by exhaust and pad dry cure methods. The finished organic knit was assessed for laundering on antimicrobial efficiency and aroma intensity. GCMS spectral analysis showed that, diethyl phthalate (28%) was the major compound found in vetiver oil followed by isoaromadendrene epoxide (7.72%), beta-vetivenene (6.92%), solavetivone (5.58%), aromadenderene, azulene and khusimol. Bioassay explained that, the vetiver oil and diluted vetiver oil possessed greater zone of inhibition against S. aureus and E. coli than the coconut oil. FTRI spectra of vetiver oil and microcapsules possessed similar peaks viz., C-H, C=C & C꞊O stretching and additionally oil microcapsules possessed the peak of 3331.24 cm^-1 at 91.14 transmittance was attributed to N-H stretches. TGA of oil microcapsules revealed that, there was a minimum weight loss (5.835%) recorded at 467.09°C compared to vetiver oil i.e., -3.026% at the temperature of 396.24°C. The shape of the microcapsules was regular and round, some were spherical in shape and few were rounded by small aggregates. Irrespective of methods of application, organic cotton knits finished with microcapsules by pad dry cure method showed maximum zone of inhibition compared to knits finished by exhaust method against S. aureus and E. coli. The antimicrobial activity of the finished samples was subjected to multiple washing which indicated that knits finished with pad dry cure method showed a zone of inhibition even after 20^th wash and better aroma retention compared to knits finished with the exhaust method of application. Further, the group of respondents rated that the 5^th washed samples had the greater aroma intensity in both the methods than the other samples. Thus, the vetiver microencapsulated organic cotton knits are free from hazardous chemicals and have multi-functional properties that can be suitable for medical and healthcare textiles.

Keywords: exhaust and pad dry cure finishing, interfacial polymerization, organic cotton knits, vetiver oil microcapsules

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Authors: S. Lekhavat, U. Srimongkoluk, P. Ratanachamnong, G. Laungsopapun

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Quercetin was encapsulated with whey protein and high methoxyl pectin by spray drying technique. Feed solution, consisting of 0.1875 0.125 and 0.0625 % w/w quercetin, respectively, was prepared and then sprays at outlet temperature of 70, 80 and 90 °C. Quercetin contents either in feed solution or in spray dried powder were determined by HPLC technique. Physicochemical properties such as viscosity and total soluble solid of feed solution as well as moisture content and water activity of spray dried powder were examined. Particle morphology was imaged using scanning electron microscope. The results showed that feed solution has total soluble solid and viscosity in range of 1.73-5.60 ºBrix and 2.58-8.15 cP, in that order. After spray drying, the moisture content and water activity value of powder are in range of 0.58-2.72 % and 0.18-0.31, respectively. Quercetin content in dried sample increased along with outlet drying temperature but decreased when total soluble solid increased. It was shown that particles are likely to shrivel when spray drying at high temperature. The suggested conditions for encapsulation of quercetin are feed solution with 0.0625 % (w/w) quercetin and spray drying at drying outlet temperature of 90°C.

Keywords: drying temperature, particle morphology, spray drying, quercetin

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Authors: Surendra Kumar Gautam, Mahesh Dhungana

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Magnesium oxide nanoparticles (MgO NPs) are less toxic to humans and the environment as compared to other metal oxide nanoparticles. Various conventional chemical and physical methods are used for synthesis whose toxicity level is high and highly expensive. As the best alternative, phyto-assisted synthesis has emerged, which uses extracts from plant parts for the synthesis of nanoparticles. Here, we report the synthesis of MgO nanoparticles with the assistance of beetroot extract and leaf extract of P. guajava and A. adenophora. The synthesized MgO NPs were characterized by X-ray diffraction (XRD), Fourier transforms infrared spectroscopy (FTIR), and UV-visible spectroscopy. X-ray analysis for the broadening of peaks was used to evaluate the crystallite size and lattice strain using Debye-Scherer and Williamson–Hall method. The results of crystallite size obtained by both methods are in close proximity. The crystallite size obtained by the Williamson-Hall method seems more accurate, with values being 8.1 nm and 13.2 nm for beetroot MgO NPs and P. guajava MgO NPs, respectively. The FT-IR spectroscopy revealed the dominance of chemical bonds as well as functional groups on MgO NPs surfaces. The UV-visible absorption spectra of MgO NPs were found to be 310 nm, 315 nm, and 315 nm for beetroot, P. guajava, and A. adenophora leaf extract, respectively. Among the three samples, beetroot-mediated MgO NPs were effective antibacterial against both gram-positive and Gram-negative bacteria. In addition, synthesized MgO NPs also show significant antioxidant efficacy against 1,1-diphenyl-2-picrylhydrazyl radical. Further, beetroot MgO NPs showed the highest photocatalytic activity of about 91% in comparison with other samples.

Keywords: MgO NPs, XRD, FTIR, antibacterial, antioxidant and photocatalytic activity

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Authors: Dahmane Mohamed, Tab Asma, Trari Mohamed

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BaMnO₃ nanoparticles were synthesized by a nitrate route. Its structure and physical properties were characterized by means of X-ray powder diffraction, radio crystallographic analysis, ultraviolet-visible absorption spectroscopy in diffuse reflectance mode, infrared spectroscopy, and electrochemical measurements. The optical study showed that barium manganese oxide presents a direct transition with band energy 2.13 eV. The electrochemical study allowed us to identify the redox peaks and the corrosion parameters. Capacitance measurement clearly showed n-type conductivity. The photodegradation of paracetamol by BaMnO₃ was followed by UV-visible spectrophotometry; the results were then confirmed by HPLC. BaMnO₃ has shown its photocatalytic efficiency in the photodegradation of 10 mg/L paracetamol under solar irradiation, with a yield of ≈ 88%. The kinetic study has shown that paracetamol degrades with first-order kinetics.

Keywords: BaMnO₃, photodegradation, paracetamol, electrochemical measurements, solar light

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Authors: Kemal Efe Eseller, Göktuğ Yazici

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Laser-induced breakdown spectroscopy (LIBS) is a rapid optical atomic emission spectroscopy which is used for material identification and analysis with the advantages of in-situ analysis, elimination of intensive sample preparation, and micro-destructive properties for the material to be tested. LIBS delivers short pulses of laser beams onto the material in order to create plasma by excitation of the material to a certain threshold. The plasma characteristics, which consist of wavelength value and intensity amplitude, depends on the material and the experiment’s environment. In the present work, medicine samples’ spectrum profiles were obtained via LIBS. Medicine samples’ datasets include two different concentrations for both paracetamol based medicines, namely Aferin and Parafon. The spectrum data of the samples were preprocessed via filling outliers based on quartiles, smoothing spectra to eliminate noise and normalizing both wavelength and intensity axis. Statistical information was obtained and principal component analysis (PCA) was incorporated to both the preprocessed and raw datasets. The machine learning models were set based on two different train-test splits, which were 70% training – 30% test and 80% training – 20% test. Cross-validation was preferred to protect the models against overfitting; thus the sample amount is small. The machine learning results of preprocessed and raw datasets were subjected to comparison for both splits. This is the first time that all supervised machine learning classification algorithms; consisting of Decision Trees, Discriminant, naïve Bayes, Support Vector Machines (SVM), k-NN(k-Nearest Neighbor) Ensemble Learning and Neural Network algorithms; were incorporated to LIBS data of paracetamol based pharmaceutical samples, and their different concentrations on preprocessed and raw dataset in order to observe the effect of preprocessing.

Keywords: machine learning, laser-induced breakdown spectroscopy, medicines, principal component analysis, preprocessing

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Authors: Liseane Padilha Thives, Mayara S. S. Lima, João Victor Staub De Melo, Glicério Trichês

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Red mud is a waste resulting from the processing of bauxite to alumina, the raw material of the production of aluminum. The large quantity of red mud generated and inadequately disposed in the environment has motivated researchers to develop methods for reinsertion of this waste into the productive cycle. This work aims to evaluate the resistance to permanent deformation of dense asphalt mixtures with red mud filler. The red mud was characterized by tests of X-ray diffraction, fluorescence, specific mass, laser granulometry, pH and scanning electron microscopy. For the analysis of the influence of the quantity of red mud in the mechanical performance of asphalt mixtures, a total filler content of 7% was established. Asphalt mixtures with 3%, 5% and 7% red mud were produced. A conventional mixture with 7% stone powder filler was used as reference. The asphalt mixtures were evaluated for performance to permanent deformation in the French Rutting Tester (FRT) traffic simulator. The mixture with 5% red mud presented greater resistance to permanent deformation with rutting depth at 30,000 cycles of 3.50%. The asphalt mixtures with red mud presented better performance, with reduction of the rutting of 12.63 to 42.62% in relation to the reference mixture. This study confirmed the viability of reinserting the red mud in the production chain and possible usage in the construction industry. The red mud as filler in asphalt mixtures is a reuse option of this waste and mitigation of the disposal problems, as well as being an environmentally friendly alternative.

Keywords: asphalt mixtures, permanent deformation, red mud, pavements

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Authors: Yves Monette, Brad Loewen, Louise Pothier

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This study explores the first bog iron ore extraction activities which took place in colonial New France. Archaeological excavations carried on the founding site of Montreal in the last ten years have revealed the remains of Fort Ville-Marie erected in 1642. In a level related to the fort occupation between 1660 and 1680, kilos of scories, a dozen of half-finished iron artefacts and a light yellow clayey ore material have recovered that point to extractive metallurgy activities at the fort. Examples of scories, artefacts and of a possible bog iron ore were submitted to SEM-EDS analysis. The results clearly indicate that iron was extracted from local limonite ores in a bloomery. We discovered that the gangue material could be traced from the ore to the scories. However, some lime silicates and some accessory minerals found in the scories, like barite and celestine for example, were absent from the ore but present in dolomite fragments found in the same archaeological context. The tracing of accessory minerals suggests that the ironmaster introduced a lime flux in the bloomery charge to maximize the separation of the iron ore. Before the introduction of the blast furnace in Western Europe during the first half of the 18th Century, the use of fluxes in iron bloomery was not a common practice.

Keywords: bog iron ore, extractive metallurgy, French colonial America, Montreal, scanning electron microscopy (SEM)

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Authors: Mardiana Ahamad Zabidi, Akmalluddin Md. Yunus

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Soursop (Anona muricata) is one of the underutilized tropical fruits containing nutrients, particularly dietary fibre and antioxidant properties that are beneficial to human health. This objective of this study is to investigate the feasibility of matured soursop pulp flour (SPF) to be substituted with high-protein wheat flour in bread. Bread formulation was substituted with different levels of SPF (0%, 5%, 10% and 15%). The effect on physicochemical properties and sensory attributes were evaluated. Higher substitution level of SPF resulted in significantly higher (p<0.05) fibre, protein and ash content, while fat and carbohydrate content reduced significantly (p<0.05). FESEM showed that the bread crumb surface of control and 5% SPF appeared to distribute evenly and coalesced by thin gluten film. However, higher SPF substitution level in bread formulation exhibited a deleterious effect by formation of discontinuous gluten network. For texture profile analysis, 5% SPF bread resulted in the lowest value of hardness. The score of sensory evaluation showed that 5% SPF bread received good acceptability and is comparable with control bread.

Keywords: soursop pulp flour, bread, physicochemical properties, sensory attributes, scanning electron microscopy (SEM)

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Authors: Dehong Li, Yuchen Chen, Alireza Kaboorani, Denis Rodrigue, Xiaodong (Alice) Wang

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Utilizing solar energy for thermal energy storage has emerged as an appealing option for lowering the amount of energy that is consumed by buildings. Due to their high heat storage density, and non-corrosive and non-polluting properties, alcohols can be a good alternative to petroleum-derived paraffin phase change materials (PCMs). In this paper, ternary eutectic PCMs with suitable phase change temperatures were designed and prepared using lauryl alcohol (LA), cetyl alcohol (CA), stearyl alcohol (SA), and xylitol (X). The differential scanning calorimetry (DSC) results revealed that the phase change temperatures of LA-CA-SA, LA-CA-X, and LA-SA-X were 20.52°C, 20.37°C, and 22.18°C, respectively. The latent heat of phase change of the ternary eutectic PCMs was all stronger than that of the paraffinic PCMs at roughly the same temperature. The highest latent heat was 195 J/g. It had good thermal energy storage capacity. The preparation mechanism was investigated using Fourier-transform Infrared Spectroscopy (FTIR), and it was found that the ternary eutectic PCMs were only physically mixed among the components. Ternary eutectic PCMs had a simple preparation process, suitable phase change temperature, and high energy storage density. They are suitable for low-temperature architectural packaging applications.

Keywords: thermal energy storage, buildings, phase change materials, alcohols

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Authors: Jaroslaw Mizera, Pawel Wisniewski, Ryszard Sitek

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Selective Laser Melting (SLM) is an advanced additive manufacturing technique used for producing parts made of wide range of materials such as: austenitic steel, titanium, nickel etc. In the our experiment we produced a Ti-AlN composite from a mixture of titanium and aluminum nitride respectively 70% at. and 30% at. using SLM technique. In order to define the size of powder particles, laser diffraction tests were performed on HORIBA LA-950 device. The microstructure and chemical composition of the composite was examined by Scanning Electron Microscopy (SEM). The chemical composition in micro areas of the obtained samples was determined by of EDS. The phase composition was analyzed by X-ray phase analysis (XRD). Microhardness Vickers tests were performed using Zwick/Roell microhardness machine under the load of 0.2kG (HV0.2). Hardness measurements were made along the building (xy) and along the plane of the lateral side of the cuboid (xz). The powder used for manufacturing of the samples had a mean particle size of 41μm. It was homogenous with a spherical shape. The specimens were built chiefly from Ti, TiN and AlN. The dendritic microstructure was porous and fine-grained. Some of the aluminum nitride remained unmelted but no porosity was observed in the interface. The formed material was characterized by high hardness exceeding 700 HV0.2 over the entire cross-section.

Keywords: Selective Laser Melting, Composite, SEM, microhardness

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Authors: Tokuei Sako

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Laser-induced current in a quasi-one-dimensional nanostructure has been studied by a model of a few electrons confined in a 1D electrostatic potential coupled to electrodes at both ends and subjected to a pulsed laser field. The time-propagation of the one- and two-electron wave packets has been calculated by integrating the time-dependent Schrödinger equation directly by the symplectic integrator method with uniform Fourier grid. The temporal behavior of the resultant light-induced current in the studied systems has been discussed with respect to the lifetime of the quasi-bound states formed when the static bias voltage is applied.

Keywords: pulsed laser field, nanowire, electron wave packet, quantum dots, time-dependent Schrödinger equation

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Authors: M. A. Ahmadu, S. S. Rabia

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During the past few decades, energy dissipation in the ionosphere resulting from the geomagnetic activity has caused an increasing number of major disruptions of important power and communication services, malfunctions and loss of expensive facilities. Here, the electron precipitation energy, w(ep) and joule heating energy, w(jh) was used in the computation of this dissipation using Østgaard’s empirical relation from hourly geomagnetic indices of 2012, under the assumption that the magnetosphere does not store any energy, so that at the beginning of the activity t1=0 and end at t2=t, the statistical results obtained show that ionospheric dissipation varies month to month, day to day and hour to hour and estimated with a value ~3.6 w(ep), which is in agreement with experimental result.

Keywords: Ostgaard's, ionospheric dissipation, joule heating, electron precipitation, geomagnetic indices, empirical relation

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Authors: Sanam Pudasaini, A. T. K. Perera, Ahmed Syed Shaheer Uddin, Sum Huan Ng, Chun Yang

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Development of high-efficiency and environment friendly bacterial inactivation methods is of great importance for preventing waterborne diseases which are one of the leading causes of death in the world. Traditional bacterial inactivation methods (e.g., ultraviolet radiation and chlorination) have several limitations such as longer treatment time, formation of toxic byproducts, bacterial regrowth, etc. Recently, an electroporation-based inactivation method was introduced as a substitute. Here, an electroporation-based continuous flow microfluidic device equipped with an array of micropillars is developed, and the device achieved high bacterial inactivation performance ( > 99.9%) within a short exposure time ( < 1 s). More than 99.9% reduction of Escherichia coli bacteria was obtained for the flow rate of 1 mL/hr, and no regrowth of bacteria was observed. Images from scanning electron microscope confirmed the formation of electroporation-induced nano-pore within the cell membrane. Through numerical simulation, it has been shown that sufficiently large electric field strength (3 kV/cm), required for bacterial electroporation, were generated using PDMS micropillars for an applied voltage of 300 V. Further, in this method of inactivation, there is no involvement of chemicals and the formation of harmful by-products is also minimum.

Keywords: electroporation, high-efficiency, inactivation, microfluidics, micropillar

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Authors: Sukhleen Bindra Narang, Dalveer Kaur, Kunal Pubby

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Dielectric ceramic samples in the BaO-Re2O3-TiO2 ternary system were synthesized with structural formula Ba2-xRe4+2x/3Ti8O24 where Re= rare earth metal and Re= Sm and La where x varies from 0.0 to 0.6 with step size 0.1. Polycrystalline samples were prepared by the conventional solid state reaction technique. The dielectric, electrical and impedance analysis of all the samples in the frequency range 1KHz- 1MHz at room temperature (25°C) have been done to get the understanding of electrical conduction and dielectric relaxation and their correlation. Dielectric response of the samples at lower frequencies shows dielectric dispersion while at higher frequencies it shows dielectric relaxation. The ac conductivity is well fitted by the Jonscher law (σac = σdc+Aωn). The spectroscopic data in the impedance plane confirms the existence of grain contribution to the relaxation. All the properties are found out to be function of frequency as well as the amount of substitution.

Keywords: dielectric ceramics, dielectric constant, loss tangent, AC conductivity, impedance spectroscopy

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Authors: Asmaa M. Hussein, Amr Wassal, Ahmed Farouk Al-Sadek, A. F. Abd El-Rahman

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In this study, a multivariate analysis of potato spectroscopic data was presented to detect the presence of brown rot disease or not. Near-Infrared (NIR) spectroscopy (1,350-2,500 nm) combined with multivariate analysis was used as a rapid, non-destructive technique for the detection of brown rot disease in potatoes. Spectral measurements were performed in 565 samples, which were chosen randomly at the infection place in the potato slice. In this study, 254 infected and 311 uninfected (brown rot-free) samples were analyzed using different advanced statistical analysis techniques. The discrimination performance of different multivariate analysis techniques, including classification, pre-processing, and dimension reduction, were compared. Applying a random forest algorithm classifier with different pre-processing techniques to raw spectra had the best performance as the total classification accuracy of 98.7% was achieved in discriminating infected potatoes from control.

Keywords: Brown rot disease, NIR spectroscopy, potato, random forest

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Authors: Sena Su, Burak Ozbek, Yesim M. Sahin, Sevil Yucel, Dilek Kazan, Faik N. Oktar, Nazmi Ekren, Oguzhan Gunduz

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In recent years, protein, lipid or polysaccharide-based polymers have been used in order to develop biodegradable materials and their chemical nature determines the physical properties of the resulting films. Among these polymers, proteins from different sources have been extensively employed because of their relative abundance, film forming ability, and nutritional qualities. In this study, the biodegradable composite nanofiber films based on fish sarcoplasmic protein (FSP) were prepared via electrospinning technique. Biodegradable polycaprolactone (PCL) was blended with the FSP to obtain hybrid FSP/PCL nanofiber mats with desirable physical properties. Mixture solutions of FSP and PCL were produced at different concentrations and their density, viscosity, electrical conductivity and surface tension were measured. Mechanical properties of electrospun nanofibers were evaluated. Morphology of composite nanofibers was observed using scanning electron microscopy (SEM). Moreover, Fourier transform infrared spectrometer (FTIR) studies were used for analysis chemical composition of composite nanofibers. This study revealed that the FSP based nanofibers have the potential to be used for different applications such as biodegradable packaging, drug delivery, and wound dressing, etc.

Keywords: edible film, electrospinning, fish sarcoplasmic protein, nanofiber

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Authors: D. Berdous, H. Ferfera-Harrar

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Superabsorbent polymers (SAPs) or hydrogels with three-dimensional hydrophilic network structure are high-performance water absorbent and retention materials. The in situ synthesis of metal nanoparticles within polymeric network as antibacterial agents for bio-applications is an approach that takes advantage of the existing free-space into networks, which not only acts as a template for nucleation of nanoparticles, but also provides long term stability and reduces their toxicity by delaying their oxidation and release. In this work, SAP/nanosilver nanocomposites were successfully developed by a unique green process at room temperature, which involves in situ formation of silver nanoparticles (AgNPs) within hydrogels as a template. The aim of this study is to investigate whether these AgNPs-loaded hydrogels are potential candidates for antimicrobial applications. Firstly, the superabsorbents were prepared through radical copolymerization via grafting and crosslinking of acrylamide (AAm) onto chitosan backbone (Cs) using potassium persulfate as initiator and N,N’-methylenebisacrylamide as the crosslinker. Then, they were hydrolyzed to achieve superabsorbents with ampholytic properties and uppermost swelling capacity. Lastly, the AgNPs were biosynthesized and entrapped into hydrogels through a simple, eco-friendly and cost-effective method using aqueous silver nitrate as a silver precursor and curcuma longa tuber-powder extracts as both reducing and stabilizing agent. The formed superabsorbents nanocomposites (Cs-g-PAAm)/AgNPs were characterized by X-ray Diffraction (XRD), UV-visible Spectroscopy, Attenuated Total reflectance Fourier Transform Infrared Spectroscopy (ATR-FTIR), Inductively Coupled Plasma (ICP), and Thermogravimetric Analysis (TGA). Microscopic surface structure analyzed by Transmission Electron Microscopy (TEM) has showed spherical shapes of AgNPs with size in the range of 3-15 nm. The extent of nanosilver loading was decreased by increasing Cs content into network. The silver-loaded hydrogel was thermally more stable than the unloaded dry hydrogel counterpart. The swelling equilibrium degree (Q) and centrifuge retention capacity (CRC) in deionized water were affected by both contents of Cs and the entrapped AgNPs. The nanosilver-embedded hydrogels exhibited antibacterial activity against Escherichia coli and Staphylococcus aureus bacteria. These comprehensive results suggest that the elaborated AgNPs-loaded nanomaterials could be used to produce valuable wound dressing.

Keywords: antibacterial activity, nanocomposites, silver nanoparticles, superabsorbent Hydrogel

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Authors: Nadia Ezzat Al-Kirbasee, Ahlam Hussein Hassan, Shatha Raheem Helal Alhimidi, Doaa Ezzat Al-Kirbasee, Muhsen Abood Muhsen Al-Ibadi

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Through DFT/QTAIM calculations, we have provided new insights into the nature of the M-M, M-H, M-O, and M-C bonds of the (Cp*Ru)n(Cp*Os)3−n(μ3-O)2(μ-H)(Cp* = η5-C5Me5, n= 3,2,1,0). The topological analysis of the electron density reveals important details of the chemical bonding interactions in the clusters. Calculations confirm the absence of bond critical points (BCP) and the corresponding bond paths (BP) between Ru-Ru, Ru-Os, and Os-Os. The position of bridging hydrides and Oxo atoms coordinated to Ru-Ru, Ru-Os, and Os-Os determines the distribution of the electron densities and which strongly affects the formation of the bonds between these transition metal atoms. On the other hand, the results confirm that the four clusters contain a 6c–12e and 4c–2e bonding interaction delocalized over M3(μ-H)(μ-O)2 and M3(μ-H), respectively, as revealed by the non-negligible delocalization indexes calculations. The small values for electron density ρ(b) above zero, together with the small values, again above zero, for laplacian ∇2ρ(b) and the small negative values for total energy density H(b) are shown by the Ru-H, Os-H, Ru-O, and Os-O bonds in the four clusters are typical of open shell interactions. Also, the topological data for the bonds between Ru and Os atoms with the C atoms of the pentamethylcyclopentadienyl (Cp*) ring ligands are basically similar and show properties very consistent with open shell interactions in the QTAIM classification.

Keywords: metal-metal and metal-ligand interactions, organometallic complexes, topological analysis, DFT and QTAIM analyses

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Authors: Mehmet Fahri Sarac, Gokcen Akgun

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Ti–6Al–4V alloys are widely used in biomedical industries because of its attractive mechanical and physicochemical properties. However, they have poor wear resistance. High velocity oxygen fuel (HVOF) coatings were investigated as a way to improve the wear resistance of this alloy. In this paper, different mass ratio of Al₂O₃-TiO₂ powders (60/40, 87/13 and 97/3) was employed to enhance the tribological properties of Ti–6Al–4V. The tribological behavior was investigated by wear tests using ball-on-disc and pin-on-disc tribometer. The microstructures of the contact surfaces were determined by a scanning electron microscopy before and after the test to study the wear mechanism. Uncoated and coated surfaces after wear test are also subjected to micro-hardness tests. The tribological test results showed that the microhardness, friction and wear resistance of coated Ti-6Al-4V alloys increases by increasing TiO₂ content in the powder composite when other experimental conditions were constant. Finally, Al₂O₃-TiO₂ powder composites for the investigated conditions, both coating samples had satisfactory values of friction and wear resistance, and they could be suitable candidates for Ti–6Al–4V material.

Keywords: HVOF (High Velocity Oxygen Fuel), Al₂O₃-TiO₂, Ti-6Al-4V, tribology

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

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

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

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Authors: J. O. Ajayi, S. S. Oluyamo, D. B. Agunbiade

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In this work, tin oxide thin films (SnO2) were prepared using the spin coating technique. The effects of precursor concentration on the thin film properties were investigated. Tin oxide was synthesized from anhydrous Tin (II) Chloride (SnCl2) dispersed in Methanol and Acetic acid. The metallic oxide (SnO2) films deposited were characterized using the UV Spectrophotometer and the Scanning Electron Microscope (SEM). From the absorption spectra, absorption increases with decrease in precursor concentration. Absorbance in the VIS region is lower than 0 % at higher concentration. The optical transmission spectrum shows that transmission increases as the concentration of precursor decreases and the maximum transmission in visible region is about 90% for films prepared with 0.2 M. Also, there is increase in the reflectance of thin films as concentration of precursor increases. The films have high transparency (more than 85%) and low reflectance (less than 40%) in the VIS region. Investigation showed that the direct band gap value increased from 3.79eV, to 3.82eV as the precursor concentration decreased from 0.6 M to 0.2 M. Average direct bandgap energy for all the tin oxide films was estimated to be 3.80eV. The effect of precursor concentration was directly observed in crystal outgrowth and surface particle densification. They were found to increase proportionately with higher concentration.

Keywords: anhydrous TIN (II) chloride, densification, NIS- VIS region, spin coating technique

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Authors: Mahyar Maali, Merve Sagiroglu, Mahmut Kilic, Abdulkadir Cuneyt Aydin

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In order to evaluate the residual strength of S235 (St37) steel structures after the fire, an experimental program was undertaken to investigate the post-fire mechanical properties. Tensile coupons taken from S235 sheets were exposed to varying temperatures as 200°C, 400°C, 600°C, and 800 °C. The samples were then allowed to cool down to ambient temperature before they were tested to failure. To obtain the mechanical properties of steels; tensile tests are performed, and the post-fire stress-strain curves are evaluated. The microstructures of the heat-treated specimens were examined by Scanning Electron Microscope (SEM). It is seen that morphology and size of the precipitates in the specimens change, as the heat increases. The modulus of elasticity decreases, and deformation increases with temperature. Energy dissipation decreases due to lower stress according to the stress-strain curves of the specimens. Especially, the mechanical properties were decreased compared with the pre-fire ones. As a result of the post-fire and pre-fire behavior of S235, a set of equations is evaluated to predict the mechanical properties after the fire. These types of equations may allow the structural and/or fire engineers to predict accurately the post-fire behavior of the buildings constructed with S235 type steel.

Keywords: post-fire behavior, stress-strain curves, experimental study, S235 steel

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Authors: Blessing Atim Aderibigbe

Abstract:

A series of amine/ester-linked hybrid compounds containing pharmacophores, such as ursolic acid, oleanolic acid, ferrocene and bisphosphonates, were synthesized in an attempt to develop potent antibacterial and anticancer agents. Their structures were analyzed and confirmed using Nuclear Magnetic Resonance, Fourier Transform Infrared Spectroscopy, and mass spectroscopy. All the synthesized hybrid compounds were evaluated for their antibacterial activities against eleven selected bacterial strains using a serial dilution method. Some of the compounds displayed significant antibacterial activity against most of the bacterial and fungal strains. In addition, the in vitro cytotoxicity of these compounds was also performed against selected cancer cell lines. Some of the compounds were also found to be more active than their parent compounds, revealing the efficacy of designing hybrid molecules using plant-based bioactive agents.

Keywords: ursolic acid, hybrid drugs, oleanolic acid, bisphosphonates

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Authors: S. Said, Asmaa A. Abdulrahman

Abstract:

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

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

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Authors: Lorenza Fabiocchi, Marco Mariani, Andrea Lucchini Huspek, Matteo Pozzi, Massimiliano Bestetti, Serena Graziosi, Nora Lecis

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Additive manufacturing of stainless steels is rapidly developing thanks to the ability to achieve complex designs effortlessly. Stainless steel 17-4PH is valued for its high strength and corrosion resistance, however intricate geometries are challenging to obtain due to rapid tool wear when machined. Binder jetting additive manufacturing was used to produce 17–4PH samples and pulsed electron beam surface treatment was investigated to enhance surface properties of components. The aim is to improve the tribological performance compared to the as-sintered condition and the H900 aging process, which optimizes hardness and wear resistance. Printed samples were sintered in a reducing atmosphere and superficially treated with an electron beam by varying the voltage (20 - 25 - 30 kV) and pulse count (20 – 40 pulses). Then, the surface was characterized from a microstructural and mechanical standpoint. Scratch tests were performed, and a reciprocating linear pin-on-disk wear test was conducted at 2 N and 10 Hz. Results showed that the voltage affects the roughness and thickness of the treated layer, whilst the number of pulses influences the hardening of the microstructure and consequently the wear resistance. Treated samples exhibited lower coefficients of friction compared to as-printed surfaces, though the values approached those of aged samples after the abrasion of the melted layer, indicating a deeper heat-affected zone formation. Different amounts of residual stress in the heat effected zone were individuated through the scratch tests. Still, the friction remained lower than that of as-printed specimens. This study demonstrates that optimizing electron beam parameters is vital for achieving surface performance comparable to bulk aging treatments, with significant implications for long-term wear resistance.

Keywords: low energy high current pulsed electron beam, tribology, binder jetting 3D printing, 17-4PH stainless steel

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Authors: S. Kassou, R. El Mrabet, A. Belaaraj, P. Guionneau, N. Hadi, T. Lamcharfi

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The organic–inorganic hybrid perovskite-like [C₆H₅C₂H₄NH₃]₂ZnCl₄ (PEA-ZnCl₄) was synthesized by saturated solutions method. X-ray powder diffraction, Raman spectroscopy, UV-visible transmittance, and capacitance meter measurements have been used to characterize the structure, the functional groups, the optical parameters, and the dielectric constants of the material. The material has a layered structure. The optical transmittance (T %) was recorded and applied to deduce the absorption coefficient (α) and optical band gap (Eg). The hybrid shows an insulator character with a direct band gap about 4.46 eV, and presents high dielectric constants up to a frequency of about 10⁵ Hz, which suggests a ferroelectric behavior. The reported optical and dielectric properties can help to understand the fundamental properties of perovskite materials and also to be used for optimizing or designing new devices.

Keywords: dielectric constants, optical band gap (eg), optical parameters, Raman spectroscopy, self-assembly organic inorganic hybrid

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Authors: Kathleen Moyer, Nora Ait Boucherbil, Murtaza Zohair, Janna Eaves-Rathert, Cary Pint

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This study demonstrates the significance of interface engineering in the field of structural energy by being the first case where the performance of the system with the structural battery is greater than the performance of the same system with a battery separate from the system. The benefits of improving the interface in the structural battery were tested by creating carbon fiber composite batteries (and independent graphite electrodes and lithium iron phosphate electrodes) with and without an improved interface. Mechanical data on the structural batteries were collected using tensile tests and electrochemical data was collected using scanning electron microscopy equipment. The full-cell lithium-ion structural batteries had capacity retention of over 80% exceeding 100 cycles with an average energy density of 52 W h kg−1 and a maximum energy density of 58 W h kg−1. Most scientific developments in the field of structural energy have been done with supercapacitors. Most scientific developments with structural batteries have been done where batteries are simply incorporated into the structural element. That method has limited advantages and can create mechanical disadvantages. This study aims to show that a large improvement in structure energy research can be made by improving the interface between the structural device and the battery.

Keywords: composite materials, electrochemical performance, mechanical properties, polymer interface, structural batteries

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Authors: Marcin Stasiulewicz, Sebastian Filipkowski, Aneta Panuszko

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Background: The hallmark of neurodegenerative diseases, including Alzheimer's and Parkinson's diseases, is an aggregation of the abnormal forms of peptides and proteins. Water is essential to functioning biomolecules, and it is one of the key factors influencing protein folding and misfolding. However, the hydration studies of proteins are complicated due to the complexity of protein systems. The use of model compounds can facilitate the interpretation of results involving larger systems. Objectives: The goal of the research was to characterize the properties of the hydration water surrounding the two three-residue K peptide fragments INS (Isoleucine - Asparagine - Serine) and NSR (Asparagine - Serine - Arginine). Methods: Fourier-transform infrared spectra of aqueous solutions of the tripeptides were recorded on Nicolet 8700 spectrometer (Thermo Electron Co.) Measurements were carried out at 25°C for varying molality of solute. To remove oscillation couplings from water spectra and, consequently, obtain narrow O-D semi-heavy water bands (HDO), the isotopic dilution method of HDO in H₂O was used. The difference spectra method allowed us to isolate the tripeptide-affected HDO spectrum. Results: The structural and energetic properties of water affected by the tripeptides were compared to the properties of pure water. The shift of the values of the gravity center of bands (related to the mean energy of water hydrogen bonds) towards lower values with respect to the ones corresponding to pure water suggests that the energy of hydrogen bonds between water molecules surrounding tripeptides is higher than in pure water. A comparison of the values of the mean oxygen-oxygen distances in water affected by tripeptides and pure water indicates that water-water hydrogen bonds are shorter in the presence of these tripeptides. The analysis of differences in oxygen-oxygen distance distributions between the tripeptide-affected water and pure water indicates that around the tripeptides, the contribution of water molecules with the mean energy of hydrogen bonds decreases, and simultaneously the contribution of strong hydrogen bonds increases. Conclusions: It was found that hydrogen bonds between water molecules in the hydration sphere of tripeptides are shorter and stronger than in pure water. It means that in the presence of the tested tripeptides, the structure of water is strengthened compared to pure water. Moreover, it has been shown that in the vicinity of the Asparagine - Serine - Arginine, water forms stronger and shorter hydrogen bonds. Acknowledgments: This work was funded by the National Science Centre, Poland (grant 2017/26/D/NZ1/00497).

Keywords: amyloids, K-peptide, hydration, FTIR spectroscopy

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