Search results for: 4D scanning ultrafast microscopy

Authors: Ala Abobakr Abdulhafidh Al-Dubai

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Biomaterials, specifically metals and ceramics, are indispensable components in the realm of medical science, shaping the landscape of implantology and prosthetics. This study delves into the intricate interplay between these materials and biological systems, aiming to scrutinize their suitability, performance, and biocompatibility. Employing a multi-faceted approach, a range of methodologies were meticulously employed to comprehensively characterize these biomaterials. Advanced material characterization techniques were paramount in this research, with scanning electron microscopy providing intricate insights into surface morphology, and X-ray diffraction unraveling the crystalline structures. These analyses were complemented by in vitro assessments, which gauged the biological response of cells to metals and ceramics, shedding light on their potential applications within the human body. A key facet of our investigation involved a comparative study, evaluating the corrosion resistance and osseointegration potential of both metals and ceramics. Through a series of experiments, we sought to understand how these biomaterials interacted with physiological environments, paving the way for informed decisions in medical applications

Keywords: metals, ceramics, biomaterials, biocompatibility, osseointegration

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

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

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

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Authors: Mahmoud H. Abu Elella, Riham R. Mohamed, Magdy W. Sabaa

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Introduction: Microbial pollution is global problem threatening the human health. It is resulted by pathogenic microorganisms such as Escherichia coli (E. coli), Staphylococcus aureus (S. aureus) and other pathogenic strains. They cause a dangerous effect on human health, so great efforts have been exerted to produce new and effective antimicrobial agents. Nowadays, natural polysaccharides, such as chitosan and its derivatives are used as antimicrobial agents. The aim of our work is to synthesize of a biodegradable polymer such as N-quaternized chitosan (NQC) then Characterization of NQC by using different analysis techniques such as Fourier transform infrared (FTIR) and Scanning electron microscopy (SEM) and using it as an antibacterial agent against different pathogenic bacteria. Methods: Synthesis of NQC using dimethylsulphate. Results: FTIR technique exhibited absorption peaks of NQC, SEM images illustrated that surface of NQC was smooth and antibacterial results showed that NQC had a high antibacterial effect. Discussion: NQC was prepared and it was proved by FTIR technique and SEM images antibacterial results exhibited that NQC was an antibacterial agent.

Keywords: antimicrobial agent, N-quaternized chitosan chloride, silver nanocomposites, sodium polyacrylate

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Authors: P. Slepicka, N. Slepickova Kasalkova, I. Michaljanicova, O. Nedela, Z. Kolska, V. Svorcik

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Polymers exposed to laser or plasma treatment or modified with different wet methods which enable the introduction of nanoparticles or biologically active species, such as amino-acids, may find many applications both as biocompatible or anti-bacterial materials or on the contrary, can be applied for a decrease in the number of cells on the treated surface which opens application in single cell units. For the experiments, two types of materials were chosen, a representative of non-biodegradable polymers, polyethersulphone (PES) and polyhydroxybutyrate (PHB) as biodegradable material. Exposure of solid substrate to laser well below the ablation threshold can lead to formation of various surface structures. The ripples have a period roughly comparable to the wavelength of the incident laser radiation, and their dimensions depend on many factors, such as chemical composition of the polymer substrate, laser wavelength and the angle of incidence. On the contrary, biopolymers may significantly change their surface roughness and thus influence cell compatibility. The focus was on the surface treatment of PES and PHB by pulse excimer KrF laser with wavelength of 248 nm. The changes of physicochemical properties, surface morphology, surface chemistry and ablation of exposed polymers were studied both for PES and PHB. Several analytical methods involving atomic force microscopy, gravimetry, scanning electron microscopy and others were used for the analysis of the treated surface. It was found that the combination of certain input parameters leads not only to the formation of optimal narrow pattern, but to the combination of a ripple and a wrinkle-like structure, which could be an optimal candidate for cell attachment. The interaction of different types of cells and their interactions with the laser exposed surface were studied. It was found that laser treatment contributes as a major factor for wettability/contact angle change. The combination of optimal laser energy and pulse number was used for the construction of a surface with an anti-cellular response. Due to the simple laser treatment, we were able to prepare a biopolymer surface with higher roughness and thus significantly influence the area of growth of different types of cells (U-2 OS cells).

Keywords: cell response, excimer laser, polymer treatment, periodic pattern, surface morphology

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Authors: Evdokia K. Oikonomou, Nikolay Christov, Galder Cristobal, Graziana Messina, Giovani Marletta, Laurent Heux, Jean-Francois Berret

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Fabric softeners are aqueous formulations that contain ~10 wt. % double tailed cationic surfactants. Here, a formulation in which 50% surfactant was replaced with low quantities of natural guar polymers was developed. Thanks to the reduced surfactant quantity this product has less environmental impact while the guars presence was found to maintain the product’s performance. The objective of this work is to elucidate the effect of the guar polymers on the softener deposition and the adsorption mechanism on the cotton surface. The surfactants in these formulations are assembled into large distributed (0.1 – 1 µm) vesicles that are stable in the presence of guars and upon dilution. The effect of guars on the vesicles adsorption on cotton was first estimated by using cellulose nanocrystals (CNC) as a stand-in for cotton. The dispersion of CNC in water permits to follow the interaction between the vesicles, guars, and CNC in the bulk. It was found that guars enhance the deposition on CNC and that the vesicles are deposited intactly on the fibers driven by electrostatics. The mechanism of the vesicles/guars adsorption on cellulose fibers was identified by quartz crystal microbalance with dissipation monitoring. It was found that the guars increase the surfactant deposited quantity, in agreement with the results in the bulk. Also, the structure of the adsorbed surfactant on the fibers' surfaces (vesicle or bilayer) was influenced by the guars presence. Deposition studies on cotton fabrics were also conducted. Attenuated total reflection and scanning electron microscopy were used to study the effect of the polymers on this deposition. Finally, fluorescent microscopy was used to follow the adsorption of surfactant vesicles, labeled with a fluorescent dye, on cotton fabrics in water. It was found that, in the presence or not of polymers, the surfactant vesicles are adsorbed on fiber maintaining their vesicular structure in water (supported vesicular bilayer structure). The guars influence this process. However, upon drying the vesicles are transformed into bilayers and eventually wrap the fibers (supported lipid bilayer structure). This mechanism is proposed for the adsorption of vesicular conditioner on cotton fiber and can be affected by the presence of polymers.

Keywords: cellulose nanocrystals, cotton fibers, fabric softeners, guar polymers, surfactant vesicles

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Authors: L. Chetibi, D. Hamana, T. O. Busko, M. P. Kulish, S. Achour

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TiO2 nanostructures have attracted much attention due to their optical, dielectric and photocatalytic properties as well as applications including optical coating, photocatalysis and photoelectrochemical solar cells. This work aims to prepare TiO2 nanofibers (NFs) on titanium substrate (Ti) by in situ oxidation of Ti foils in a mixture solution of concentrated H2O2 and NaOH followed by proton exchange and calcinations. Scanning Electron microscopy (SEM) revealed an obvious network of TiO2 nanofibers. The photoluminescence (PL) spectra of these nanostructures revealed a broad intense band in the visible light range with a reduced near edge band emission. The PL bands in the visible region, mainly, results from surface oxygen vacancies and others defects. After irradiation with Ti+ ions (the irradiation energy was E = 140 keV with doses of 1013 ions/cm2), the intensity of the PL spectrum decreased as a consequence of the radiation treatment. The irradiation with Ti+ leads to a reduction of defects and generation of non irradiative defects near to the level of the conduction band as evidenced by the PL results. On the other hand, reducing the surface defects on TiO2 nanostructures may improve photocatalytic and optoelectronic properties of this nanostructure.

Keywords: TiO2, nanofibers, photoluminescence, irradiation

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Authors: Miroslava Hujová, Patricia Rabello Monich, Jozef Kraxner, Dusan Galusek, Enrico Bernardo

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Inorganic waste upcycling offers a solution how to avoid landfilling and how to save raw materials at the same time. However, its practical implementations in Slovakia and elsewhere in Europe, are rather limited despite the potential smaller countries like Slovakia have their advantage in closely-knitted inorganic materials industry. One part of discussion should include an overview of wastes that can be possibly used for upcycling, i.e. fly ashes, red mud, glass cullets, vitrified bottom ashes etc. These wastes can be processed by a variety of strategies, the one of our choice, alkali activation, opens the possibility for the formation of novel materials at almost negligible energetic expense. In the research, these materials are characterized by comprehensive means (X-Ray Fluorescece, Diffraction methods, Thermal Analysis, Scanning Electron Microscopy, Mechanical tests and Chemical stability), which time and time again demonstrate their competitive properties against traditional materials available at the market. It is just a question for discussion why these materials do not receive more significant attention from industry and there is pressing interest for the solution of standing situation.

Keywords: upcycling, inorganic wastes, glass ceramics, alkali-activation

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Authors: Andualem Workie

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In this study, we examined the sinterability and bioactivity of MgO-SiO₂-P₂O₅-CaO-CaF₂ glass compositions created through spray pyrolysis. We evaluated the bioactivity of the materials by immersing them for varying periods of time in simulated bodily fluid (SBF) and found that bioactivity was related to the sintering temperature and soaking time. The material's pH value during immersion in SBF was within the range of 7.4-8.2, which is below 8.5 and improves compatibility and reduces toxicity in biological applications. We used X-ray diffraction and scanning electron microscopy to determine the phase compositions and morphologies of the samples and found that the 1100°C sintered A-W GC sample exhibited the highest bioactivity after soaking in SBF. This sample was dominated by fluorapatite, wollastonite, and whitlockite crystals scattered throughout the glass matrix. The crystallinity (%) of the A-W GC increased as its bioactivity improved, making it more suitable for use in pharmaceutical applications. We also conducted a cytotoxicity test on A-W GC samples sintered at different temperatures and found that the glass-ceramics were non-toxic to MC3T3-E1 cells at all extraction concentrations, except for those sintered at 700°C at concentrations of 250, 200, and 150 mg/ml where cell viability (%) was below the threshold of 70%.

Keywords: apatite wollastonite glass ceramics, bioactivity, calcination, cell viability

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Authors: Niru Chowdhury, Subhankar Bedanta, Alexander Weber, Thomas Brueckel

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We show the effect of interlayer coupling on magnetization reversal in purely dipolar coupled magnetic multilayers. Longitudinal magneto-optic Kerr microscopy (LMOKE) has been performed on [Co(10nm)/Al2O3(t)/Co(10nm)] for various thicknesses of Al2O3(t). We will show that inter-layer coupling interactions lead to layer-by-layer reversal in the magnetic multilayers. Also transverse component of magnetization was observed for higher thickness of the spacer layer.

Keywords: Interlayer coupling, Magnetic domains, Magneto – Optic Kerr effect microscopy, Magnetization reversal, Magnetic thin film

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Authors: A. Kaibi, A. Guittoum, M. Hemmous, D. Martínez-Blanco, P. Gorria, J. A. Blanco, M. Kechouane

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The present work deals with the effect of Si content on the physical properties of nanostructured (Ni75Fe25)100-x Six (x=0, 3.5, 6.5, 9, 12, and 15 at %) powders elaborated by mechanical alloying for a milling time of 96 h. The microstructure, hyperfine, and magnetic properties of the powders were investigated as a function of Si content by means of X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), Mössbauer Spectroscopy, and Vibrating Sample magnetometry (VSM). From XRD spectra, the formation of FCC disordered Ni (Fe,Si) solid solution was evidenced after 96 h. As Si content increases, the lattice parameter and the grain size decrease (from ~28 to 15 nm), while the microstrain level decreases from 0.98% to 0.65%. From SEM micrographs, we showed that powder particles become round in shape and decrease in size with increasing Si content. For all Si content, the adjustment of Mössbauer spectra confirmed the formation of a disordered ferromagnetic NiFeSi phase. From hysteresis curves, we have extracted the values of saturation magnetization and coercive field for all powders. The evolution of Ms and Hc as a function of Si content will be discussed.

Keywords: nanostructured powders, (Ni75Fe25)100-xSix alloy, microstructure, magnetic properties

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Authors: Ashish Kumar Singh, Preeti Tiwari, Shubham Srivastava, Rajiv Prakash, Herman Terryn, Gopal Ji

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Corrosion inhibition potential of azo dyes namely Allura red (AR), Sunset Yellow (SY) and Amaranth (AN) have been investigated in 0.5 M H2SO4 solutions by electrochemical impedance spectroscopy (EIS), Tafel polarization curves, linear polarization curves, open circuit potential (ocp) curves, UV-Visible spectroscopy, Fourier Transform Infrared spectroscopy (FTIR) and scanning electron microscopy (SEM) techniques. Amaranth dye is found to provide highest corrosion inhibition (90 %) against mild steel corrosion in sulfuric acid solutions among all the tested dyes; while SY and AR dye shows 80% and 78% corrosion inhibition efficiency respectively. The electrochemical measurements and surface morphology analysis reveal that molecular adsorption of dyes at metal acid interface is accountable for inhibition of mild steel corrosion in H2SO4 solutions. The adsorption behavior of dyes has been investigated by various isotherms models, which verifies that it is in accordance with Langmuir isotherm.

Keywords: mild steel, Azo dye, EIS, Langmuir isotherm

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

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

Keywords: codoped TiO₂, dendrimer, photodegradation, wastewater

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Authors: S. Wisutmethangoon, S. Pannaray, T. Plookphol, J. Wannasin

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2024 Aluminium alloy was squeezed cast by the Gas Induced Semi Solid (GISS) process. Effect of artificial aging on microstructure and mechanical properties of this alloy was studied in the present work. The solutionized specimens were aged hardened at temperatures of 175°C, 200°C, and 225°C under various time durations. The highest hardness of about 77.7 HRE was attained from specimen aged at the temperature of 175 °C for 36 h. Upon investigation the microstructure by using Transmission Electron Microscopy (TEM), the phase was mainly attributed to the strengthening effect in the aged alloy. The apparent activation energy for precipitation hardening of the alloy was calculated as 133,805 J/mol.

Keywords: 2024 aluminium alloy, gas induced semi solid, T6 heat treatment, aged hardening, transmission electron microscopy

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Authors: Farid Amidi Fazli

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Replacement of plastics used in the food industry seems to be a serious issue to overcome mainly the environmental problems in recent years. This study investigates the hydrophilicity and permeability properties of starch biopolymer which ethylene vinyl alcohol (EVOH) (0-10%) and nanocrystalline cellulose (NCC) (1 -15%) were used to enhance its properties. Starch -EVOH nanocomposites were prepared by casting method in different formulations. NCC production by acid hydrolysis was confirmed by scanning electron microscopy. Solubility, water vapor permeability, water vapor transmission rate and moisture absorbance were measured on each of the nanocomposites. The results were analyzed by SAS software. The lowest moisture absorbance was measured in pure starch nanocomposite containing 8% NCC. The lowest permeability to water vapor belongs to starch nanocomposite containing 8% NCC and the sample containing 7.8% EVOH and 13% NCC. Also, the lowest solubility was observed in the composite contains the highest amount of EVOH. Applied Process resulted in production of bio films which have good resistance to water vapor permeability and solubility in water. The use of NCC and EVOH leads to reduced moisture absorbance property of the biofilms.

Keywords: starch, EVOH, nanocrystalline cellulose, hydrophilicity

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Authors: Ahmad N. Abu-Baker

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This study investigated the corrosion of a group of heritage silver-copper alloy coins and their conservation treatment by potentiostatic methods. The corrosion products of the coins were characterized by a combination of scanning electron microscopy/ energy-dispersive X-ray spectroscopy (SEM/EDX) and X-ray diffraction (XRD) analyses. Cathodic polarization curves, measured by linear sweep voltammetry (LSV), also identified the corrosion products and the working conditions to treat the coins using a potentiostatic reduction method, which was monitored by chronoamperometry. The corrosion products showed that the decay mechanisms were dominated by selective attack on the copper-rich phases of the silver-copper alloys, which is consistent with an internal galvanic corrosion phenomenon, which leads to the deposition of copper corrosion products on the surface of the coins. Silver chloride was also detected on the coins, which reflects selective corrosion of the silver-rich phases under different chemical environments. The potentiostatic treatment showed excellent effectiveness in determining treatment parameters and monitoring the reduction process of the corrosion products on the coins, which helped to preserve surface details in the cleaning process and to prevent over-treatment.

Keywords: silver alloys, corrosion, conservation, heritage

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Authors: Erdinç Vural, Bülent Özdalyan, Serkan Özel

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The four-stroke single cylinder diesel engine has been used in this study, the pistons and valves of the engine have been stabilized, the aluminum oxide (Al₂O₃) in different ratios has been added in the power of zirconium (ZrO₂) magnesium oxide (MgO), and has been coated with the plasma spray method. The pistons and valves of the combustion chamber of the engine are coated with 5 different (ZrO₂ + MgO), (ZrO₂ + MgO + 25% Al₂O₃), (ZrO₂ + MgO + 50% Al₂O₃), (ZrO₂ + MgO + 75% Al₂O₃), (Al₂O₃) sample. The material tests have been made for each of the coated engine parts with the scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD) using Cu Kα radiation surface analysis methods. The engine tests have been repeated for each sample in any electric dynamometer in full power 1600 rpm, 2000 rpm, 2400 rpm and 2800 rpm engine speeds. The material analysis and engine tests have shown that the best performance has been performed with (ZrO₂ + MgO + 50% Al₂O₃). Thus, there is no significant change in HC and Smoke emissions, but NOx emission is increased, as the engine improves power, torque, specific fuel consumption and CO emissions in the tests made with sample A3.

Keywords: ceramic coating, material characterization, engine performance, exhaust emissions

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Authors: Salim Ahmed

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Electrocoagulation has proven its effectiveness in industrial effluent treatment by eliminating pollutants, particularly metallic ones. The electrochemical processes that occur at aluminium electrodes give excellent performance. In this work, electrocoagulation tests were carried out on an industrial effluent from an electroplating bath located in Casablanca (Morocco). The aim was to remove chromium and reuse the purified water for other purposes within the company. To this end, we have optimised the operating parameters that affect the efficiency of electrocoagulation, such as electrical voltage, electrode material, stirring speed and distance between electrodes. We also evaluated these parameters. The effect on pH, conductivity, turbidity and chromium concentration. The tests were carried out in a perfectly stirred reactor on an industrial solution rich in chromium. The effluent concentration was 1000 mg/L of Cr6+. Chromium removal efficiency was determined for the following operating conditions: aluminium electrodes, regulated voltage of 6 volts and 12 volts, optimum stirring speed of 600 rpm and distance between electrodes of 2 cm. The sludge produced by electrocoagulation was characterised by X-ray diffractometry, infrared spectroscopy (IR) and scanning electron microscopy (SEM).

Keywords: wastewater, chromium, electrocoagulation, aluminium, aluminium hydroxide

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Authors: Parvathy Anitha, Nilesh J. Vasa, M. S. Ramachandra Rao

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ZnO is a semiconducting material with a direct wide band gap of 3.37 eV and a large exciton binding energy of 60 meV at room temperature. Microspheres with high sphericity and symmetry exhibit unique functionalities which makes them excellent omnidirectional optical resonators. Hence there is an advent interest in fabrication of single crystalline semiconductor microspheres especially magnetic ZnO microspheres, as ZnO is a promising material for semiconductor device applications. Also, ZnO is non-toxic and biocompatible, implying it is a potential material for biomedical applications. Room temperature Photoluminescence (PL) spectra of the fabricated ZnO microspheres were measured, at an excitation wavelength of 325 nm. The ultraviolet (UV) luminescence observed is attributed to the room-temperature free exciton related near-band-edge (NBE) emission in ZnO. Besides the NBE luminescence, weak and broad visible luminescence (~560nm) was also observed. This broad emission band in the visible range is associated with oxygen vacancies related to structural defects. In transition metal (TM) ion-doped ZnO, 3d levels emissions of TM ions will modify the inherent characteristic emissions of ZnO. A micron-sized ZnO crystal has generally a wurtzite structure with a natural hexagonal cross section, which will serve as a WGM (whispering gallery mode) lasing micro cavity due to its high refractive index (~2.2). But hexagonal cavities suffers more optical loss at their corners in comparison to spherical structures; hence spheres may be a better candidate to achieve effective light confinement. In our study, highly smooth spherical shaped micro particles with different diameters ranging from ~4 to 6 μm were grown on different substrates. SEM (Scanning Electron Microscopy) and AFM (Atomic Force Microscopy) images show the presence of uniform smooth surfaced spheres. Raman scattering measurements from the fabricated samples at 488 nm light excitation provide convincing supports for the wurtzite structure of the prepared ZnO microspheres. WGM lasing studies from TM-doped ZnO microparticles are in progress.

Keywords: laser ablation, microcavity, photoluminescence, ZnO microsphere

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Authors: Karima Bourenane, Aissa Keffous

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In this paper, we present an experimental method on the etching reaction of p-type 6H-SiC, etching that was carried out in HF/K₂Cr₂O₇ solutions. The morphology of the etched surface was examined with varying K₂Cr₂O₇ concentrations, etching time and temperature solution. The surfaces of the etched samples were analyzed using Scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR) and Photoluminescence. The surface morphology of samples etched in HF/K₂Cr₂O₇ is shown to depend on the solution composition and bath temperature. The investigation of the HF/K₂Cr₂O₇ solutions on 6H-SiC surface shows that as K₂Cr₂O₇ concentration increases, the etch rate increases to reach a maximum value at about 0.75 M and then decreases. Similar behavior has been observed when the temperature of the solution is increased. The maximum etch rate is found for 80 °C. Taking into account the result, a polishing etching solution of 6H-SiC has been developed. In addition, the result is very interesting when, to date, no chemical polishing solution has been developed on silicon carbide (SiC). Finally, we have proposed a dissolution mechanism of the silicon carbide in HF/K₂Cr₂O₇ solutions.

Keywords: silicon carbide, dissolution, Chemical etching, mechanism

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Authors: Yen-Ping Peng, Ku-Fan Chen, Ken-Lin Chang, Jian Sun

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In this study, palladium loaded titanium dioxide nanotube arrays (Pd/TNAs) was successfully synthesized by anodic oxidation etching method combined with microwave hydrothermal method, using tea or coffee as a green reductant. Pd/TNAs was employed as an electrode in a photoelectrochemcial (PEC) system to simultaneously remove azo-dye and to generate hydrogen in the anodic and cathodic chamber, respectively. The chemical and physical properties of as-synthesized Pd/TNAs were characterized by scanning electron microscopy (SEM), ultraviolet–visible spectroscopy (UV-vis), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). SEM image indicates the diameter and the length of Pd/TNAs were approximately 300 nm and 2.5 μm, respectively. XPS analyses indicate that 1.13% (atomic %) of Pd was loaded onto the surface of TNAs. UV-vis results show that the band gap of TNAs was reduced from 3.2 eV to 2.37 eV after Pd loading. In addition, the electrochemical performances of Pd/TNAs were investigated by photocurrent density test and electrochemical impedance spectroscopy (EIS). The photocurrent (4.0 mA/cm²) of Pd /TNAs was higher than that of the uncoated TNAs (1.4 mA/cm²) at a bias potential of 1 V (vs. Ag/AgCl), indicating that Pd/TNAs-C can effectively separate photogenerated electrons and holes. The mechanism of our PEC system was proposed and discussed in detail in this study.

Keywords: Pd/TNAs, photoelectrochemical, azo-dye degradation, hydrogen generation

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Authors: Vivek Kumar, Alexander M. Zaitsev

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A study on chemical sensing properties of carbon nanofilms on diamond for developing all-carbon chemical sensors is presented. The films were obtained by high temperature graphitization of diamond followed by successive plasma etchings. Characterization of the films was done by Raman spectroscopy, atomic force microscopy, and electrical measurements. Fast and selective response to common organic vapors as seen as sensitivity of electrical conductance was observed. The phenomenological description of the chemical sensitivity is proposed as a function of the surface and bulk material properties of the films.

Keywords: chemical sensor, carbon nanofilm, graphitization of diamond, plasma etching, Raman spectroscopy, atomic force microscopy

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Authors: Hussein M. Etmimi, Peter E. Mallon

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

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

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Authors: E. G. Zaki, M. A. Migahed, A. M. Al-Sabagh, E. A. Khamis

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Inhibition effect of four novel nonionic surfactants based on sulphonamide, of linear alkyl benzene sulphonic acid (LABS), was reacted with 1 mole triethylenetetramine, tetraethylenepentamine then Ethoxylation of amide X 65 type carbon steel in oil wells formation water under H2S environment was investigated by electrochemical measurements. Scanning electron microscopy (SEM) and energy dispersion X-ray (EDX) were used to characterize the steel surface. The results showed that these surfactants act as a corrosion inhibitor in and their inhibition efficiencies depend on the ethylene oxide content in the system. The obtained results showed that the percentage inhibition efficiency (η%) was increased by increasing the inhibitor concentration until the critical micelle concentration (CMC) reached The quantum chemistry calculations were carried out to study the molecular geometry and electronic structure of obtained derivatives. The energy gap between the highest occupied molecular orbital and lowest unoccupied molecular orbital has been calculated using the theoretical computations to reflect the chemical reactivity and kinetic stability of compounds.

Keywords: corrosion, surfactants, steel surface, quantum

Procedia PDF Downloads 377

Authors: M. A. Ferhat, M. N. Boukhatem, F. Chemat

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Microwave Clevenger or microwave accelerated distillation (MAD) is a combination of microwave heating and distillation, performed at atmospheric pressure without added any solvent or water. Isolation and concentration of volatile compounds are performed by a single stage. MAD extraction of orange essential oil was studied using fresh orange peel from Valencia late cultivar oranges as the raw material. MAD has been compared with a conventional technique, which used a Clevenger apparatus with hydro-distillation (HD). MAD and HD were compared in term of extraction time, yields, chemical composition and quality of the essential oil, efficiency and costs of the process. Extraction of essential oils from orange peels with MAD was better in terms of energy saving, extraction time (30 min versus 3 h), oxygenated fraction (11.7% versus 7.9%), product yield (0.42% versus 0.39%) and product quality. Orange peels treated by MAD and HD were observed by scanning electronic microscopy (SEM). Micrographs provide evidence of more rapid opening of essential oil glands treated by MAD, in contrast to conventional hydro-distillation.

Keywords: clevenger, microwave, extraction; hydro-distillation, essential oil, orange peel

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Authors: M. Masłowski, M. Zaborski

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Magnetorheological elastomer composites based on micro- and nano-sized magnetite, gamma iron oxide and carbonyl iron powder in ethylene-octene rubber are reported and studied. The method of preparation process influenced the specific properties of MREs (isotropy/anisotropy). The use of extrusion method instead of traditional preparation processes (two-roll mill, mixer) of composites is presented. Micro and nan-sized magnetites as well as gamma iron oxide and carbonyl iron powder were found to be an active fillers improving the mechanical properties of elastomers. They also changed magnetic properties of composites. Application of extrusion process also influenced the mechanical properties of composites and the dispersion of magnetic fillers. Dynamic-mechanical analysis (DMA) indicates the presence of strongly developed secondary structure in vulcanizates. Scanning electron microscopy images (SEM) show that the dispersion improvement had significant effect on the composites properties. Studies investigated by vibration sample magnetometer (VSM) proved that all composites exhibit good magnetic properties.

Keywords: extrusion, magnetic fillers, magnetorheological elastomers, mechanical properties

Procedia PDF Downloads 320

Authors: Katia Ayouz-Chebout, Fatima Boudeffar, Maha Ayat, Malika Berouaken, Chafiaa Yaddaden, Saloua Merazga, Nouredine Gabouze

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Transition metal oxide composites have been widely reported in energy storage and conversion systems. In this regard, an attempt has been made to synthesize NiO@V₂O₅ nanocomposite. The structures and morphology of synthesized powder are investigated by X-ray diffraction, scanning electron microscope (SEM), and Attenuated Total Reflection (ATR). The electrochemical properties and performances as cathode electrodes based on active material NiO@V₂O₅ were studied by cyclic voltammetry (CV), between potential bias [0.01V to 3V], with scanning speed of 0,1mVs⁻¹, the galvanostatic charge/discharge (CDG) for 100 cycles was also measured.

Keywords: composite nanobelts, vanadium pentoxide, nickel oxide, Li-ion batteries

Procedia PDF Downloads 26

Authors: Faezeh Shalchy

Abstract:

Concrete is the most used materials in the world. It is also one of the most versatile while complex materials which human have used for construction. However, concrete is weak in tension, over the past thirty years many studies were accomplished to improve the tensile properties of concrete (cement-based materials) using a variety of methods. One of the most successful attempts is to use polymeric fibers in the structure of concrete to obtain a composite with high tensile strength and ductility. Understanding the mechanical behavior of fiber reinforced concrete requires the knowledge of the fiber/matrix interfaces at the small scale. In this study, a combination of numerical simulations and experimental techniques have been used to study the nano structure of fiber/matrix interfaces. A new model for calcium-silicate-hydrate (C-S-H)/fiber interfaces is proposed based on Scanning Electron Microscopy (SEM) and Energy-dispersive X-ray spectroscopy (EDX) analysis. The adhesion energy between the C-S-H gel and 2 different polymeric fibers (polyvinyl alcohol and polypropylene) was numerically studied at the atomistic level since adhesion is one of the key factors in the design of fiber reinforced composites. The mechanisms of adhesion as a function of the nano structure of fiber/matrix interfaces are also studied and discussed.

Keywords: fiber-reinforced concrete, adhesion, molecular modeling

Procedia PDF Downloads 328

Authors: Emmanuel Flores Huicochea, Guadalupe Borja Mendiola, Jacqueline Flores Lopez, Rodolfo Rendon Villalobos

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The usual procedure to investigate the properties of biodegradable films has been to prepare the film, measure the mechanical or transport properties and then decide whether the mixture has better properties than the individual components, instead of investigating whether the mixture has biopolymer-biopolymer interaction, then prepare the film and finally measure the properties of the film. The work investigates the presence of interaction biopolymer-biopolymer in a mixture of chia biopolymer and gelatin using Laser Confocal Microscopy (LCM). Previously, the chia biopolymer was obtained from chia seed. CML analysis of mixtures of chia biopolymer-gelatin without Na⁺ ions exhibited aggregates of different size, in the range of 100-400 μm, of defined color, for the two colors, but no mixing of color was observed. The increased of gelatin in the mixture decreases the size and number of aggregates. The tridimensional microstructure reveled that there are two layers of biopolymers, chia and gelatin well defined. The mixture chia biopolymer-gelatin with 10 mM Na⁺ and with a ratio 75:25 (chia-gelatin) showed lower aggregated size than others mixture with and without ions. This result could be explained because the chia biopolymer is a polyelectrolyte and the added sodium ions reduce the molecular rigidity by neutralizing the negative charges that the chia biopolymer possesses and therefore a better biopolymer-biopolymer interaction is allowed between the biopolymer of chia and gelatin.

Keywords: biopolymer-biopolymer interaction, confocal laser microscopy, CLM, microstructure, mixture chia-gelatin

Procedia PDF Downloads 209

Authors: Oyugi Ngure Robert, Kallen Mulilo Nalyanya, Tabitha A. Amollo

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Nanomaterials have attracted significant attention in research because of their exemplary properties, making them suitable for diverse applications. This paper reports the successful synthesis as well as the structural properties of silver sulfide/reduced graphene oxide (Ag_2 S-rGO) nanocomposite. The nanocomposite was synthesized by the chemical reduction method. Scanning electron microscopy (SEM) showed that the reduced graphene oxide (rGO) sheets were intercalated within the Ag_2 S nanoparticles during the chemical reduction process. The SEM images also showed that Ag_2 S had the shape of nanowires. Further, SEM energy dispersive X-ray (SEM EDX) showed that Ag_2 S-rGO is mainly composed of C, Ag, O, and S. X-ray diffraction analysis manifested a high crystallinity for the nanowire-shaped Ag2S nanoparticles with a d-spacing ranging between 1.0 Å and 5.2 Å. Thermal gravimetric analysis (TGA) showed that rGO enhances the thermal stability of the nanocomposite. Ag_2 S-rGO nanocomposite exhibited strong optical absorption in the UV region. The formed nanocomposite is dispersible in polar and non-polar solvents, qualifying it for solution-based device processing.

Keywords: silver sulfide, reduced graphene oxide, nanocomposite, structural properties, optical properties

Procedia PDF Downloads 101

Authors: Tsung-Yen Tsai, Naveen Bunekar, Ming Hsuan Chang, Wen-Kuang Wang, Satoshi Onda

Abstract:

The structure-property relationship and initiator effect on bulk polymerized poly(methyl methacrylate) (PMMA)–oragnomodified layered silicate nanocomposites was investigated. In this study, we used 2, 2'-azobis (4-methoxy-2,4-dimethyl valeronitrile and benzoyl peroxide initiators for bulk polymerization. The bulk polymerized nanocomposites’ morphology was investigated by X-ray diffraction and transmission electron microscopy. The type of initiator strongly influences the physiochemical properties of the polymer nanocomposite. The thermal degradation of PMMA in the presence of nanofiller was studied. 5 wt% weight loss temperature (T5d) increased as compared to pure PMMA. The peak degradation temperature increased for the nanocomposites. Differential scanning calorimetry and dynamic mechanical analysis were performed to investigate the glass transition temperature and the nature of the constrained region as the reinforcement mechanism respectively. Furthermore, the optical properties such as UV-Vis and Total Luminous Transmission of nanocomposites are examined.

Keywords: initiator, bulk polymerization, layered silicates, methyl methacrylate

Procedia PDF Downloads 292