Search results for: confocal microscopy

Authors: S. Alrekabi, A. Cundy, A. Lampropoulos, I. Savina

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Due to their remarkable mechanical properties, multi-wall carbon nanotubes (MWCNTs) are considered by many researchers to be a highly promising filler and reinforcement agent for enhanced performance cementitious materials. Currently, however, achieving an effective dispersion of MWCNTs remains a major challenge in developing high performance nano-cementitious composites, since carbon nanotubes tend to form large agglomerates and bundles as a consequence of Van der Waals forces. In this study, effective dispersion of low concentrations of MWCNTs at 0.01%, 0.025%, and 0.05% by weight of cement in the composite was achieved by applying different sonication conditions in combination with the use of polycarboxylate ether as a surfactant. UV-Visible spectroscopy and Transmission electron microscopy (TEM) were used to assess the dispersion of MWCNTs in water, while the dispersion states of MWCNTs within the cement composites and their surface interactions were examined by scanning electron microscopy (SEM). A high sonication intensity applied over a short time period significantly enhanced the dispersion of MWCNTs at initial mixing stages, and 0.025% of MWCNTs wt. of cement, caused 86% and 27% improvement in tensile strength and compressive strength respectively, compared with a plain cement mortar.

Keywords: dispersion, mechanical performance, multi wall carbon nanotubes, sonication conditions

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Authors: Mehdi Rahimi-Nasrabadi, Seied Mahdi Pourmortazavi

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

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

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Authors: Ana Paula Gomes Nogueira, Pietro Tonolini, Andrea Bonfanti

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Automotive braking systems must convert kinetic into thermal energy by friction. Nowadays, the disc brake system is the most widespread configuration on the automotive market, which its specific configuration provides a very efficient heat dissipation. At the same time, both discs and pads wear out. Different wear mechanisms can act during the braking, which makes the understanding of the phenomenon essential for the strategies to be applied when an increased lifetime of the components is required. In this study, a specific characterization approach was conducted to analyze the worn surfaces of commercial pad friction materials and its conterface cast iron disc after dynobench tests. Scanning electronic microscope (SEM), confocal microscope, and focus ion beam microscope (FIB) were used as the main tools of the analysis, and they allowed imaging of the footprint of the different wear mechanisms presenting on the worn surfaces. Aspects such as the temperature and specific ingredients of the pad friction materials are discussed since they play an important role in the wear mechanisms.

Keywords: wear mechanism, surface characterization, brake tests, friction materials, disc brake

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Authors: Abdel Ghany F. Shoair, Mai M. A. H. Shanab

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The basic aqueous systems NiSO4.6H₂O / K₂S₂O₈ (PH= 14) or NiSO₄.6H₂O / KBrO₃ (PH = 11.5) were ‎investigated ‎for the ‎catalytic conversion benzyl alcohol and ‎some para-substituted benzyl ‎alcohols to their ‎corresponding ‎acids in 75-97 % yield at room ‎temperature. The active species ‎was isolated and characterized by scanning ‎electron ‎microscopy (SEM), ‎‎transmission electron microscopy (TEM), X-ray ‎powder diffraction, EDX and ‎‎FT-IR ‎techniques and identified as NiO₂ nanoparticles (NPNPs). The SEM and ‎TEM images of nickel peroxide samples show a fine spherical-like ‎aggregation of ‎NiO₂ molecules with a nearly homogeneous partial size and confirm the ‎aggregation's size ‎to ‎be in the range of 2-3 nm. The yields, turnover (TO) and turn ‎over frequencies (TOF) were calculated. ‎It was noticed ‎that the aromatic alcohols ‎containing para-substituted electron donation groups gave better ‎‎yields than ‎those having electron-withdrawing groups. The optimum conditions for this ‎‎catalytic reaction ‎were studied using benzyl alcohol as a model. The mechanism ‎of the ‎catalytic conversion reaction was ‎suggested, in which the produced ‎(NPNPs) convert alcohols ‎to acids in two steps through the formation of the ‎‎corresponding aldehyde. The produced ‎NiO, because of this conversion, is ‎converted again to (NPNPs) by ‎an excess of K₂S₂O₈ or KBrO₃. This ‎catalytic cycle continues ‎until all the substrate is oxidized.

Keywords: Nickel, oxidation, catalysts, benzyl alcohol

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Authors: Carla Caiazza, Valentina Preziosi, Giovanna Tomaiuolo, Denis O'Sullivan, Vincenzo Guida, Stefano Guido

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In the last decades, wormlike micellar solutions have been extensively used to tune the rheological behavior of home care and personal care products. This and other successful applications underlie the growing attention that both basic and applied research are devoting to these systems, and to their unique rheological and flow properties. One of the key research topics is the occurrence of flow instabilities at high shear rates (such as shear banding), with the possibility of appearance of flow induced structures. In this scenario, microfluidics is a powerful tool to get a deeper insight into the flow behavior of a wormlike micellar solution, as the high confinement of a microfluidic device facilitates the onset of the flow instabilities; furthermore, thanks to its small dimensions, it can be coupled with optical microscopy, allowing a direct visualization of flow structuring phenomena. Here, the flow of a widely used wormlike micellar solution through a glass capillary has been studied, by coupling the microfluidic device with μPIV techniques. The direct visualization of flow-induced structures and the flow visualization analysis highlight a relationship between solution structuring and the onset of discontinuities in the velocity profile.

Keywords: flow instabilities, flow-induced structures, μPIV, wormlike micelles

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Authors: Raees Khan, Sheikh Z. Ul Abidin, Abdul S. Mumtaz, Jie Liu

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The present study is intended to assess gymnosperms pollen flora of Pakistan using Light Microscope (LM) and Scanning Electron Microscopy (SEM) for its taxonomic significance in identification of gymnosperms. Pollens of 35 gymnosperm species (12 genera and five families) were collected from its various distributional sites of gymnosperms in Pakistan. LM and SEM were used to investigate different palyno-morphological characteristics. Five pollen types (i.e., Inaperturate, Monolete, Monoporate, Vesiculate-bisaccate, and Polyplicate) were observed. In equatorial view seven types of pollens were observed, in which ten species were sub-angular, nine species were triangular, six species were perprolate, three species were rhomboidal, three species were semi-angular, two species were rectangular and two species were prolate. While five types of pollen were observed in polar view, in which ten species were spheroidal, nine species were angular, eight were interlobate, six species were circular, and two species were elliptic. Eighteen species have rugulate and 17 species has faveolate ornamentation. Eighteen species have verrucate and 17 have gemmate type sculpturing. The data was analysed through cluster analysis. The study showed that these palyno-morphological features have significance value in classification and identification of gymnosperms. Based on these different palyno-morphological features, a taxonomic key was proposed for the accurate and fast identifications of gymnosperms from Pakistan.

Keywords: gymnosperms, palynology, Pakistan, taxonomy

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Authors: Rym Taktak, Achwek Elghazel, Jamel Bouaziz

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In the present work, we explored the potential of tribological behavior of tricalcium phosphate-Fluorapatite (β Tcp-Fap) bioceramic which has attracted considerable attention for orthopedics and dental applications. The approximate representatives Fap-βTcp were respectively [{13.26 wt%, 86.74 wt%} {19.9 wt%, 80.1 wt%},{ 26.52 wt%, 73.48 wt%}, {33.16 wt%, 66.84 wt%} and {40 wt%, 60 wt%}. The effects of Fluorapatite additives on friction and wear behavior were studied and discussed. The wear test was conducted using pion-disk tribometer at room temperature under dry condition using a constant sliding speed of 0,063 m/s, and three loads 3, 5 and 8 N. The wear rate and friction coefficient of β Tcp with different additive amounts were compared. An Alumina ball specimens were used as the pin and flat surface β Tcp-Fap specimens as the antagonist counterface. The results show a huge difference between the wear rate of β TCP samples and the other β TCP-Fap composites for all normal forces applied. This result shows the beneficial effect of fluorapatite on the tribological behavior of the β TCP. Moreover, we note that β Tcp-26% Fap specimens exhibit, under dry condition, the lower friction coefficient and the smaller wear rate than other biocomposites. Thereby, the friction and wear behavior is influenced by the addition of fluorapatite, the applied normal force, and the sliding velocity. To extend the understanding of the wear process, the surface topography of β Tcp-26% Fap specimens and the wear track obtained during the wear tests were studied using a surface profilometer, optical microscopy, and scanning electron microscopy.

Keywords: alumina, bioceramic, friction and wear test, tricalcium phosphate

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Authors: Eva Slaninova, Diana Cernayova, Zuzana Sedrlova, Katerina Mrazova, Petr Sedlacek, Jana Nebesarova, Stanislav Obruca

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Cyanobacteria are gram-negative prokaryotes belonging to a group of photosynthetic bacteria. In comparison with heterotrophic microorganisms, cyanobacteria utilize atmospheric nitrogen and carbon dioxide without any additional substrates. This ability of these microorganisms could be employed in biotechnology for the production of bioplastics, concretely polyhydroxyalkanoates (PHAs) which are primarily accumulated as a storage material in cells in the form of intracellular granules. In this study, there two cyanobacterial cultures from genera Synechocystis were used, namely Synechocystic sp. PCC 6803 and Synechocystis salina CCALA 192. There were optimized and used several various approaches, including microscopic techniques such as cryo-scanning electron microscopy (Cryo-SEM) and transmission electron microscopy (TEM), and fluorescence lifetime imaging microscopy using Nile red as a fluorescent probe (FLIM). Due to these instrumental techniques, the morphology of intracellular space and surface of cells were characterized. The next group of methods which were employed was spectroscopic techniques such as UV-Vis spectroscopy measured in two modes (turbidimetry and integration sphere) and Fourier transform infrared spectroscopy (FTIR). All these diverse techniques were used for the detection and characterization of pigments (chlorophylls, carotenoids, phycocyanin, etc.) and PHAs, in our case poly (3-hydroxybutyrate) (P3HB). To verify results, gas chromatography (GC) was employed concretely for the determination of the amount of P3HB in biomass. Cyanobacteria were also characterized as polyhydroxybutyrate producers by flow cytometer, which could count cells and at the same time distinguish cells including P3HB and without due to fluorescent probe called BODIPY and live/dead fluorescent probe SYTO Blue. Based on results, P3HB content in cyanobacteria cells was determined, as also the overall fitness of the cells. Acknowledgment: Funding: This study was partly funded by the projectGA19-29651L of the Czech Science Foundation (GACR) and partly funded by the Austrian Science Fund (FWF), project I 4082-B25.

Keywords: cyanobacteria, fluorescent probe, microscopic techniques, poly(3hydroxybutyrate), spectroscopy, chromatography

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Authors: Marcelle Muriel Domkam Tchunkam, Rolin Feudjio

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This work investigates the ultrastructure, physicochemical and thermal properties evaluation of Palm Kernel Shells (PKS). PKS Tenera waste samples were obtained from a palm oil mill in Dizangué Sub-Division, Littoral region of Cameroon, while PKS Dura waste samples were collected from the Institute of Agricultural Research for Development (IRAD) of Mbongo. A sodium hydroxide solution was used to wash the shells. They were then rinsed by demineralised water and dried in an oven at 70 °C during 72 hours. They were then grounded and sieved to obtained powders from 0.04 mm to 0.45 mm in size. Transmission Electron Microscopy (TEM) and Surface Electron Microscopy (SEM) were used to characterized powder samples. Chemical compounds and elemental constituents, as well as thermal performance were evaluated by Van Soest Method, TEM/EDXA and SEM/EDS techniques. Thermal characterization was also performed using Differential Scanning Calorimetry (DSC) and Thermogravimetric Analysis (TGA). Our results from microstructural analysis revealed that most of the PKS material is made of particles with irregular morphology, mainly amorphous phases of carbon/oxygen with small amounts of Ca, K, and Mg. The DSC data enabled the derivation of the materials’ thermal transition phases and the relevant characteristic temperatures and physical properties. Overall, our data show that PKS have nanopores and show potential in 3D printing and membrane filtration applications.

Keywords: DSC, EDXA, palm kernel shells, SEM, TEM

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Authors: Amine Harrane, Mahmoud Belalia

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During the last decade, polymer layered silicate nanocomposites have received increasing attention from scientists and industrial researchers because they generally exhibit greatly improved mechanical, thermal, barrier and flame-retardant properties at low clay content in comparison with unfilled polymers or more conventional micro composites. Poly(ε-caprolactone) (PCL)-layered silicate nanocomposites have the advantage of adding biocompatibility and biodegradability to the traditional properties of nanocomposites. They can be prepared by in situ ring-opening polymerization of ε-caprolactone using a conventional initiator to induce polymerization in the presence of an organophilic clay, such as organomodified montmorillonite. Messersmith and Giannelis used montmorillonite exchanged with protonated 12-amino dodecanoic acid and Cr3+ exchanged fluorohectorite, a synthetic mica type of silicate. Sn-based catalysts such as tin (II) octoate and dibutyltin (IV) dimethoxide have been reported to efficiently promote the polymerization of ε-caprolactone in the presence of organomodified clays. In this work, we have used an alternative method to prepare PCL/montmorillonite nanocomposites. The cationic polymerization of ε-caprolactone was initiated directly by Maghnite-TOA, organomodified montmorillonite clay, to produce nanocomposites (Scheme 1). Resulted from nanocomposites were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), force atomic microscopy (AFM) and thermogravimetry.

Keywords: polycaprolactone, polycaprolactone/clay nanocomposites, biodegradables nanocomposites, Maghnite, Insitu polymeriation

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Authors: Bunty Tomar, Shiva S.

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Fabrication of steel and copper-based functionally graded material (FGM) through cold metal transfer-based wire arc additive manufacturing is a novel exploration. Components combining Cu and steel show significant usage in many industrial applications as they combine high corrosion resistance, ductility, thermal conductivity, and wear resistance to excellent mechanical properties. Joining steel and copper is challenging due to the mismatch in their thermo-mechanical properties. In this experiment, a functionally graded material (FGM) structure of pure copper (Cu) and 316L stainless steel (SS) was successfully developed using cold metal transfer-based wire arc additive manufacturing (CMT-WAAM). The interface of the fabricated samples was characterized under optical microscopy, field emission scanning electron microscopy, and X-ray diffraction techniques. Detailed EBSD and TEM analysis was performed to analyze the grain orientation, strain distribution, grain boundary misorientations, and formation of metastable and intermetallic phases. Mechanical characteristics of deposits was also analyzed using tensile and wear testing. This works paves the way to use CMT-WAAM to fabricate steel/copper FGMs.

Keywords: wire arc additive manufacturing (waam), cold metal transfer (cmt), metals and alloys, mechanical properties, characterization

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Authors: Azeez O. Idris, Benjamin O. Orimolade, Potlako J. Mafa, Alex T. Kuvarega, Usisipho Feleni, Bhekie B. Mamba

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We report a simple and cheaper method for the electrochemical detection of Se(IV) using carbon nanodots (CNDTs) prepared from oat. The carbon nanodots were synthesised by green and facile approach and characterised using scanning electron microscopy, high-resolution transmission electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction, and Raman spectroscopy. The CNDT was used to fabricate an electrochemical sensor for the quantification of Se(IV) in water. The modification of glassy carbon electrode (GCE) with carbon nanodots led to an increase in the electroactive surface area of the electrode, which enhances the redox current peak of [Fe(CN)₆]₃₋/₄‒ in comparison to the bare GCE. Using the square wave voltammetry, the detection limit and quantification limit of 0.05 and 0.167 ppb were obtained under the optimised parameters using deposition potential of -200 mV, 0.1 M HNO₃ electrolyte, electrodeposition time of 60 s, and pH 1. The results further revealed that the GCE-CNDT was not susceptible to many interfering cations except Cu(II) and Pb(II), and Fe(II). The sensor fabrication involves a one-step electrode modification and was used to detect Se(IV) in a real water sample, and the result obtained is in agreement with the inductively coupled plasma technique. Overall, the electrode offers a cheap, fast, and sensitive way of detecting selenium in environmental matrices.

Keywords: carbon nanodots, square wave voltammetry, nanomaterials, selenium, sensor

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Authors: H. Beisch, J. Marx, S. Garlof, R. Shvets, I. I. Grygorchak, A. Kityk, B. Fiedler

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Carbon materials, especially three-dimensional carbon foams, show very high potential in the application as electrode material for energy storage systems such as batteries and supercapacitors with unique fast charging and discharging times. Regarding their high specific surface areas (SSA) high specific capacities can be reached. Globugraphite is a newly developed carbon foam with an interconnected globular carbon morphology. Especially, this foam has a statistically distributed hierarchical pore structure resulting from the manufacturing process based on sintered ceramic templates which are synthetized during a final chemical vapor deposition (CVD) process. For morphology characterization scanning electron (SEM) and transmission electron microscopy (TEM) is used. In addition, the SSA is carried out by nitrogen adsorption combined with the Brunauer–Emmett–Teller (BET) theory. Electrochemical measurements in organic and inorganic electrolyte provide high energy densities and power densities resulting from ion absorption by forming an electrochemical double layer. All values are summarized in a Ragone Diagram. Finally, power densities up to 833 W/kg and energy densities up to 48 Wh/kg could be achieved. The corresponding SSA is between 376 m²/g and 859 m²/g. For organic electrolyte a specific capacity of 71 F/g at a density of 20 mg/cm³ was achieved.

Keywords: BET, CVD process, electron microscopy, Ragone diagram

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Authors: Suresh Vidyasagar Chevuri, D. B. Karunakar Chevuri

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The main advantages of 'Metal Matrix Nano Composites (MMNCs)' include excellent mechanical performance, good wear resistance, low creep rate, etc. The method of fabrication of MMNCs is quite a challenge, which includes processing techniques like Spark Plasma Sintering (SPS), etc. The objective of the present work is to fabricate aluminum based MMNCs with the addition of small amounts of yttrium using Spark Plasma Sintering and to evaluate their mechanical and microstructure properties. Samples of 2024 AA with yttrium ranging from 0.1% to 0.5 wt% keeping 1 wt% TiB2 constant are fabricated by Spark Plasma Sintering (SPS). The mechanical property like hardness is determined using Vickers hardness testing machine. The metallurgical characterization of the samples is evaluated by Optical Microscopy (OM), Field Emission Scanning Electron Microscopy (FE-SEM) and X-Ray Diffraction (XRD). Unreinforced 2024 AA sample is also fabricated as a benchmark to compare its properties with that of the composite developed. It is found that the yttrium addition increases the above-mentioned properties to some extent and then decreases gradually when yttrium wt% increases beyond a point between 0.3 and 0.4 wt%. High density is achieved in the samples fabricated by spark plasma sintering when compared to any other fabrication route, and uniform distribution of yttrium is observed.

Keywords: spark plasma sintering, 2024 AA, yttrium addition, microstructure characterization, mechanical properties

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Authors: Shrestha Sharma, Jasjeet K. Sahni, Javed Ali, Sanjula Baboota

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Introduction: Rutin is a naturally occurring strong antioxidant molecule belonging to bioflavonoid category. Due to its free radical scavenging properties, it has been found to be beneficial in the treatment of various diseases including inflammation, cancer, diabetes, allergy, cardiovascular disorders and various types of microbial infections. Despite its beneficial effects, it suffers from the problem of low aqueous solubility which is responsible for low oral bioavailability. The aim of our study was to optimize and characterize self-nanoemulsifying drug delivery system (SNEDDS) of rutin using Box-Behnken design (BBD) combined with a desirability function. Further various antioxidant, pharmacokinetic and pharmacodynamic studies were performed for the optimized rutin SNEDDS formulation. Methodologies: Selection of oil, surfactant and co-surfactant was done on the basis of solubility/miscibility studies. Sefsol+ Vitamin E, Solutol HS 15 and Transcutol P were selected as oil phase, surfactant and co-surfactant respectively. Optimization of SNEDDS formulations was done by a three-factor, three-level (33)BBD. The independent factors were Sefsol+ Vitamin E, Solutol HS15, and Transcutol P. The dependent variables were globule size, self emulsification time (SEF), % transmittance and cumulative percentage drug released. Various response surface graphs and contour plots were constructed to understand the effect of different factor, their levels and combinations on the responses. The optimized Rutin SNEDDS formulation was characterized for various parameters such as globule size, zeta potential, viscosity, refractive index , % Transmittance and in vitro drug release. Ex vivo permeation studies and pharmacokinetic studies were performed for optimized formulation. Antioxidant activity was determined by DPPH and reducing power assays. Anti-inflammatory activity was determined by using carrageenan induced rat paw oedema method. Permeation of rutin across small intestine was assessed using confocal laser scanning microscopy (CLSM). Major findings:The optimized SNEDDS formulation consisting of Sefsol+ Vitamin E - Solutol HS15 -Transcutol HP at proportions of 25:35:17.5 (w/w) was prepared and a comparison of the predicted values and experimental values were found to be in close agreement. The globule size and PDI of optimized SNEDDS formulation was found to be 16.08 ± 0.02 nm and 0.124±0.01 respectively. Significant (p˂0.05) increase in percentage drug release was achieved in the case of optimized SNEDDS formulation (98.8 %) as compared to rutin suspension. Furthermore, pharmacokinetic study showed a 2.3-fold increase in relative oral bioavailability compared with that of the suspension. Antioxidant assay results indicated better efficacy of the developed formulation than the pure drug and it was found to be comparable with ascorbic acid. The results of anti-inflammatory studies showed 72.93 % inhibition for the SNEDDS formulation which was significantly higher than the drug suspension 46.56%. The results of CLSM indicated that the absorption of SNEDDS formulation was considerably higher than that from rutin suspension. Conclusion: Rutin SNEDDS have been successfully prepared and they can serve as an effective tool in enhancing oral bioavailability and efficacy of Rutin.

Keywords: rutin, oral bioavilability, pharamacokinetics, pharmacodynamics

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Authors: Patcharee Pripdeevech, Sarunpron Khruengsai

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Thirty fungi were tested for their degradation ability on low-density polyethylene (LDPE) plastic film. Biodegradation of all fungi was screened in mineral salt medium broth containing LDPE film as the sole carbon source for 30 days. Diaporthe italiana, Thyrostroma jaczewskii, Colletotrichum fructicola, and Stagonosporopsis citrulli were able to colonize and cover the surface of LDPE film in media. The degradation test result was compared to those obtained from Aspergillus niger. LDPE films cocultured with D. italiana, T. jaczewskii, C. fructicola, S. citrulli, A. niger, and control showed weight loss of 43.90%, 46.34%, 48.78%, 45.12%, 28.78%, and 10.85%, respectively. The tensile strength of degraded LDPE films cocultured with D. italiana, T. jaczewskii, C. fructicola, S. citrulli, A. niger, and control also reduced significantly by 1.56 MPa, 1.78 MPa, 0.43 MPa, 1.86 MPa, 3.34 MPa, and 9.98 MPa, respectively. Analysis of LDPE films by Fourier transform infrared spectroscopy and scanning electron microscopy confirmed the biodegradation by the presence of morphological changes such as cracks, scions, and holes on the surface of the film. These fungi have the ability to break down and consume the LDPE film, especially C. fructicola. These findings showed the potential of fungi in Thailand that play an important role in LDPE film degradation.

Keywords: plastic biodegradation, LDPE film, fungi, Fourier transform infrared, scanning electron microscopy

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Authors: Juiwen Liang, Choliang Chung

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In this study, the silicon-base oxide nanofibers with hollow structure were prepared using single-nozzle electrospinning and heat treatment. Firstly, precursor solution was prepared: the Polyvinylpyrrolidone (PVP) and Tetraethyl orthosilicate (TEOS) dissolved in ethanol and to make sure the concentration of solution in appropriate using single-nozzle electrospinning to produce the nanofibers. Secondly, control morphology of the electrostatic spinning nanofibers was conducted, and design the temperature profile to created hollow nanofibers, exploring the morphology and properties of nanofibers. The characterized of nanofibers, following instruments were used: Atomic force microscopy (AFM), Field Emission Scanning Electron Microscope (FE-SEM), Transmission electron microscopy (TEM), Photoluminescence (PL), X-ray Diffraction (XRD). The AFM was used to scan the nanofibers, and 3D Graphics were applied to explore the surface morphology of fibers. FE-SEM and TEM were used to explore the morphology and diameter of nanofibers and hollow nanofiber. The excitation and emission spectra explored by PL. Finally, XRD was used for identified crystallization of ceramic nanofibers. Using electrospinning technique followed by subsequent heat treatment, we have successfully prepared silicon-base oxide nanofibers with hollow structure. Thus, the microstructure and morphology of electrostatic spinning silicon-base oxide hollow nanofibers were explored. Major characteristics of the nanofiber in terms of crystalline, optical properties and crystal structure were identified.

Keywords: electrospinning, single-nozzle, hollow, nanofibers

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Authors: Shweta Maheshwari, Anish Dua

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Hematological changes reflect the adverse effects of heavy metals on fish. Hematology is a valuable tool to evaluate pathological condition of the fish. It helps in diagnosing the structural and functional status of fish exposed to toxicants. Morphological alteration in erythrocytes due to environmental stress can be studied through ultra-structural analysis. The aim of the present study was to assess the toxicity of mercuric chloride on red blood cells of an air breathing fish, Channa punctatus. Fish were subjected to chronic experiments using three sublethal concentration of mercuric chloride (0.020mg/L, 0.027mg/L, 0.040mg/L) for a period of 15, 30 and 60 days. Exposed fish of all the three concentrations were subjected to a recovery period of 30 days. A control was maintained in tap water simultaneously. For SEM analysis, blood from caudal vein of fish was taken and examined at an accelerating voltage of 20kV. Scanning electron micrographs revealed elliptical shaped erythrocytes of control fish. Alterations in the erythrocyte morphology such as presence of spherocytes, membrane internalization, crenation of membrane and development of lobopodial projections were observed in the exposed fish. The study revealed that ultra-structural analysis appears to be a sensitive method to evaluate the toxicity of various toxicants to fish.

Keywords: Channa punctatus, erythrocytes, mercuric chloride, scanning electron microscopy

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Authors: Manel Bouloudenine, Karima Djeddou, Hadjer Ben Manser, Hana Soualah Alila, Mohmed Bououdina

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This survey research involves the elaboration and characterization of silver nanoparticles for therapeutic and environmental applications. The silver nanoparticles "Ag NPs" were synthesized by reducing AgNO3 with microwaves. The characterization of nanoparticles was done by using Transmission Electron Microscopy " TEM ", Energy Dispersive Spectroscopy "EDS", Selected Area Electron Diffraction "SEAD", UV-Visible Spectroscopy and Dynamic Light Scattering "DLS". Transmission Electron Microscopy and Electron Diffraction have confirmed the nanoscale, the shape, and the crystalline quality of as synthesized silver nanoparticles. Elementary analysis has proved the purity of Ag NPs and the presence of the Surface Plasmon Resonance phenomenon "SPR". A strong absorption shift was observed in the visible range of the UV-visible spectrum of as synthesized Ag NPs, which indicates the presence of metallic silver. When the strong absorption in the ultraviolet range of the spectrum has revealed the presence of ionic Ag NPs ionic Ag aggregates species. The autocorrelation function measured by the Dynamic Light Scattering has shown a strong monodispersed character of Ag NPs, which is indicated by the presence of a single size population, with a minima and a maxima laying between 40 and 111 nm. Related to other research, our results confirm the performance properties of as synthesized Ag NPs, which allows them to be performing in many technological applications, including therapeutic and environmental ones.

Keywords: silvers nanoparticles, microwaves, EDS, TEM

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Authors: Anna V. Zaporozhchenko, Dmytro Kutnyakhov, Katherina Medjanik, Christian Tusche, Hans-Joachim Elmers, Olena Fedchenko, Sergey Chernov, Martin Ellguth, Sergej A. Nepijko, Gerd Schoenhense

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Graphene reveals a unique electronic structure that predetermines many intriguing properties such as massless charge carriers, optical transparency and high velocity of fermions at the Fermi level, opening a wide horizon of future applications. Hence, a detailed investigation of the electronic structure of graphene is crucial. The method of choice is angular resolved photoelectron spectroscopy ARPES. Here we present experiments using time-of-flight (ToF) momentum microscopy, being an alternative way of ARPES using full-field imaging of the whole Brillouin zone (BZ) and simultaneous acquisition of up to several 100 energy slices. Unlike conventional ARPES, k-microscopy is not limited in simultaneous k-space access. We have recorded the whole first BZ of graphene on Ir(111) including all six Dirac cones. As excitation source we used synchrotron radiation from BESSY II (Berlin) at the U125-2 NIM, providing linearly polarized (both polarizations p- and s-) VUV radiation. The instrument uses a delay-line detector for single-particle detection up the 5 Mcps range and parallel energy detection via ToF recording. In this way, we gather a 3D data stack I(E,kx,ky) of the full valence electronic structure in approx. 20 mins. Band dispersion stacks were measured in the energy range of 14 eV up to 23 eV with steps of 1 eV. The linearly-dispersing graphene bands for all six K and K’ points were simultaneously recorded. We find clear features of hybridization with the substrate, in particular in the linear dichroism in the angular distribution (LDAD). Recording of the whole Brillouin zone of graphene/Ir(111) revealed new features. First, the intensity differences (i.e. the LDAD) are very sensitive to the interaction of graphene bands with substrate bands. Second, the dark corridors are investigated in detail for both, p- and s- polarized radiation. They appear as local distortions of photoelectron current distribution and are induced by quantum mechanical interference of graphene sublattices. The dark corridors are located in different areas of the 6 Dirac cones and show chirality behaviour with a mirror plane along vertical axis. Moreover, two out of six show an oval shape while the rest are more circular. It clearly indicates orientation dependence with respect to E vector of incident light. Third, a pattern of faint but very sharp lines is visible at energies around 22eV that strongly remind on Kikuchi lines in diffraction. In conclusion, the simultaneous study of all six Dirac cones is crucial for a complete understanding of dichroism phenomena and the dark corridor.

Keywords: band structure, graphene, momentum microscopy, LDAD

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

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

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

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Authors: Adeyemi Isaac Sanusi, Gueguim E. B. Kana

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Nanoparticles have received attention of the scientific community due to their biotechnological potentials. They exhibit advantageous size, shape and concentration-dependent catalytic, stabilizing, immunoassays and immobilization properties. This study investigates the impact of metallic oxide nanoparticles (NPs) on ethanol production by Saccharomyces cerevisiae BY4743. Nine different nanoparticles were synthesized using precipitation method and microwave treatment. The nanoparticles synthesized were characterized by Fourier Transform Infra-Red spectroscopy (FTIR), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Fermentation processes were carried out at varied NPs concentrations (0 – 0.08 wt%). Highest ethanol concentrations were achieved after 24 h using Cobalt NPs (5.07 g/l), Copper NPs (4.86 g/l) and Manganese NPs (4.74 g/l) at 0.01 wt% NPs concentrations, which represent 13%, 8.7% and 5.4% increase respectively over the control (4.47 g/l). The lowest ethanol concentration (0.17 g/l) was obtained when 0.08 wt% of Silver NPs was used. And lower ethanol concentrations were observed at higher NPs concentration. Ethanol concentration decrease after 24 h for all the processes. In all set up with NPs, the pH was observed to be stable and the stability was directly proportional to nanoparticles concentrations. These findings suggest that the presence of some of the NPs in the bioprocesses has catalytic and pH stabilizing potential. Ethanol production by Saccharomyces cerevisiae BY4743 was enhanced in the presence of Cobalt NPs, Copper NPs and Manganese NPs. Optimization study using response surface methodology (RSM) will further elucidate the impact of these nanoparticles on bioethanol production.

Keywords: agitation, bioethanol, nanoparticles concentration, optimization, pH value

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Authors: Urszula Stachewicz

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Surface properties of materials are the key parameter in many applications, especially in the biomedical field, to control cell-material interactions. In our work, we want to achieve the controllability of surface properties of polymer fibers via a single-step electrospinning process by alternating voltage polarities. Voltage polarity defines the charge accumulated on the surface of the liquid jet and the surface of the fibers. Positive polarity attracts negatively charged groups to fibers’ surface, whereas negative polarity moves the negatively charged functional groups away from the surface. This way, we can control the surface chemistry, wettability, and additionally surface potential of electrospun fibers. Within our research, we characterized surface chemistry using X-ray photoelectron microscopy (XPS) and surface potential with Kelvin probe force microscopy (KPFM) on electrospun fibers of commonly used polymers such as PCL, PVDF, and PMMA, often used as biomaterials. We proved the significant effect of fibers' surface potential on cell integration with the scaffolds and further cells development for the regeneration processes based on the osteoblast and fibroblast culture studies. Acknowledgments: The study was conducted within ‘Nanofiber-based sponges for atopic skin treatment’ project, which is carried out within the First TEAM programme of the Foundation for Polish Science co-financed by the European Union under the European Regional Development Fund, project no POIR.04.04.00-00- 4571/18-00.

Keywords: cell attachment, fibers, fibroblasts, osteoblast, proliferation, surface potential

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Authors: Emie A. Salamangkit-Mirasol, Rinlee Butch M. Cervera

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Rice hull or rice husk (RH) is an agricultural waste obtained from milling rice grains. Since RH has no commercial value and is difficult to use in agriculture, its volume is often reduced through open field burning which is an environmental hazard. In this study, amorphous nanosilica from Philippine waste RH was prepared via acid precipitation method. The synthesized samples were fully characterized for its microstructural properties. X-ray diffraction pattern reveals that the structure of the prepared sample is amorphous in nature while Fourier transform infrared spectrum showed the different vibration bands of the synthesized sample. Scanning electron microscopy (SEM) and particle size analysis (PSA) confirmed the presence of agglomerated silica particles. On the other hand, transmission electron microscopy (TEM) revealed an amorphous sample with grain sizes of about 5 to 20 nanometer range and has about 95 % purity according to EDS analyses. The elemental mapping also suggests that leaching of rice hull ash effectively removed the metallic impurity such as potassium element in the material. Hence, amorphous nanosilica was successfully prepared via a low-cost acid precipitation method from Philippine waste rice hull. In addition, initial electrode performance of the synthesized samples as an anode material in Lithium Battery have been investigated.

Keywords: agricultural waste, anode material, nanosilica, rice hull

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Authors: F. Kashanian, M. M. Masoudi, A. Akbari, A. Shamloo, M. R. Zand, S. S. Salehi

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Nano-sized materials present new opportunities in biology and medicine and they are used as biomedical tools for investigation, separation of molecules and cells. To achieve more effective cancer therapy, it is essential to select cancer cells exactly. This research suggests that using the antibody-functionalized nontoxic Arginine-doped magnetic nanoparticles (A-MNPs), has been prosperous in detection, capture, and magnetic separation of circulating tumor cells (CTCs) in tumor tissue. In this study, A-MNPs were synthesized via a simple precipitation reaction and directly immobilized Ep-CAM EBA-1 antibodies over superparamagnetic A-MNPs for Mucin BCA-225 in breast cancer cell. The samples were characterized by vibrating sample magnetometer (VSM), FT-IR spectroscopy, Tunneling Electron Microscopy (TEM) and Scanning Electron Microscopy (SEM). These antibody-functionalized nontoxic A-MNPs were used to capture breast cancer cell. Through employing a strong permanent magnet, the magnetic separation was achieved within a few seconds. Antibody-Conjugated nontoxic Arginine-doped Fe₃O₄ nanoparticles have the potential for the future study to capture CTCs which are released from tumor tissue and for drug delivery, and these results demonstrate that the antibody-conjugated A-MNPs can be used in magnetic hyperthermia techniques for cancer treatment.

Keywords: tumor tissue, antibody, magnetic nanoparticle, CTCs capturing

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Authors: Yik Ling Chew, Adlina Maisarah Mahadi, Joo Kheng Goh

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Bauhinia kockiana originates from Peninsular Malaysia, and it is grown as a garden ornamental plant. However, it is used as medicinal plant by Malaysia ‘Kelabit’ ethic group in treating various diseases and illnesses. This study focused on the assessment of the antibacterial activity of B. kockiana towards MRSA, to purify and identify the antibacterial compounds, and to determine the mechanism of antibacterial activity. Antibacterial activity of B. kockiana flower is evaluated qualitatively and quantitatively using disc diffusion assay and microbroth dilution method to determine the minimum inhibitory concentration (MIC) and minimum bactericidal concentration (MBC) of extracts. Phytochemical analysis is performed to determine the classes of phytochemicals in the extracts. Bioactivity-guided isolation is performed to purify the antibacterial agents and identified the chemical structures via various spectroscopy methods. Scanning electron microscopy (SEM) technique is adopted to evaluate the antibacterial mechanism of extract and compounds isolated. B. kockiana flower is found to exhibit fairly strong antibacterial activity towards both strains of MRSA bacteria. Gallic acid and its ester derivatives are purified from ethyl acetate extract and the antibacterial activity is evaluated. SEM has revealed the mechanism of the extracts and compounds isolated.

Keywords: alkyl gallates, Bauhinia kockiana, MRSA, scanning electron microscopy

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Authors: Seyfullah Madakbaş, Ferhat Şen, Memet Vezir Kahraman

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The aim of this study was to improve thermal stability, mechanical and surface properties of thermoplastic polyurethane (TPU) with the addition of BaTiO3. The TPU/ BaTiO3 composites having various ratios of TPU and BaTiO3 were prepared. The chemical structure of the prepared composites was investigated by FT-IR. FT-IR spectra of TPU/ barium titanate composites show that they successfully were prepared. Thermal stability of the samples was evaluated by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The prepared composites showed high thermal stability, and the char yield increased as barium titanate content increased. The glass transition temperatures of the composites rise with the addition of barium titanate. Mechanical properties of the samples were characterized with stress-strain test. The mechanical properties of the TPU were increased with the contribution of the contribution of the barium titanate it increased. Hydrophobicity of the samples was determined by the contact angle measurements. The contact angles have the tendency to increase the hydrophobic behavior on the surface, when barium titanate was added into TPU. Moreover, the surface morphology of the samples was investigated by a scanning electron microscopy (SEM). SEM-EDS mapping images showed that barium titanate particles were dispersed homogeneously. Finally, the obtained results prove that the prepared composites have good thermal, mechanical and surface properties and that they can be used in many applications such as the electronic devices, materials engineering and other emergent.

Keywords: barium titanate, composites, thermoplastic polyurethane, scanning electron microscopy

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Authors: Moustafa Shawkey, Ahmed G. El-Deen, H. M. Mahmoud, M. M. Rashad

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Piezoelectric based cement nanocomposite is a promising technology for generating an electric charge upon mechanical stress of concrete structure. Moreover, piezoelectric nanomaterials play a vital role for providing accurate system of structural health monitoring (SHM) of the concrete structure. In light of increasing awareness of environmental protection and energy crises, generating renewable and green energy form cement based on piezoelectric nanomaterials attracts the attention of the researchers. Herein, we introduce a facial synthesis for bismuth ferrite nanoparticles (BiFeO3 NPs) as piezoelectric nanomaterial via sol gel strategy. The fabricated piezoelectric nanoparticles are uniformly distributed to cement-based nanomaterials with different ratios. The morphological shape was characterized by field emission scanning electron microscopy (FESEM) and high-resolution transmission electron microscopy (HR-TEM) as well as the crystal structure has been confirmed using X-ray diffraction (XRD). The ferroelectric and magnetic behaviours of BiFeO3 NPs have been investigated. Then, dielectric constant for the prepared cement samples nanocomposites (εr) is calculated. Intercalating BiFeO3 NPs into cement materials achieved remarkable results as piezoelectric cement materials, distinct enhancement in ferroelectric and magnetic properties. Overall, this present study introduces an effective approach to improve the electrical properties based cement applications.

Keywords: piezoelectric nanomaterials, cement technology, bismuth ferrite nanoparticles, dielectric

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

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Nickel spinel ferrite NiFe2O4 nanoparticles with different particle size at different annealing temperature were synthesized using the starch-assisted sol-gel auto-combustion method. The synthesized nanoparticles were characterized by conventional powder X-ray diffraction (XRD) spectroscopy, Raman Spectroscopy, Fourier Transform Infrared Spectroscopy, Field-Emission Scanning Electron Microscopy, X-ray Photoelectron Spectroscopy and Vibrating Sample Magnetometer. The XRD patterns confirmed the formation of NiFe2O4 spinel ferrite nanoparticles. Field-Emission Scanning Electron Microscopy revealed that particles are of spherical morphology with particle size 5-20 nm at lower annealing temperature. An infrared spectroscopy study showed the presence of two principal absorption bands in the frequency range around 525 cm-1 (ν1) and around 340 cm-1 (ν2); which indicate the presence of tetrahedral and octahedral group complexes, respectively, within the spinel ferrite nanoparticles. Raman spectroscopy study also indicated the change in octahedral and tetrahedral site related Raman modes in nickel ferrite nanoparticles with change of particle size. This change in magnetic behavior with change of particle size of NiFe2O4 nanoparticles was observed.

Keywords: nickel ferrite, nanoparticles, magnetic property, NiFe2O4

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Authors: Abdelghani May

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This paper reports on experimental investigations concerning the underlying reasons for the anisotropic behavior observed during the cyclic loading of AA2017 aluminum alloy. Initially, we quantified the evolution of fatigue damage resulting from controlled proportional cyclic loadings along the axial and shear directions. Our primary objective at this stage was to verify the anisotropic mechanical behavior recently observed. To accomplish this, we utilized various models of fatigue damage quantification and conducted a comparative study of the obtained results. Our analysis confirmed the anisotropic nature of the material under investigation. In the subsequent step, we performed microstructural investigations aimed at understanding the origins of the anisotropic mechanical behavior. To this end, we utilized scanning electron microscopy to examine the phases and precipitates in both the transversal and longitudinal sections. Our findings indicate that the structure and morphology of these entities are responsible for the anisotropic behavior observed in the aluminum alloy. Furthermore, results obtained from Kikuchi diagrams, pole figures, and inverse pole figures have corroborated these conclusions. These findings demonstrate significant differences in the crystallographic texture of the material.

Keywords: microstructural investigation, fatigue damage quantification, anisotropic behavior, AA2017 aluminum alloy, cyclic loading, crystallographic texture, scanning electron microscopy

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