Search results for: electron backscatter diffraction

Authors: Louis Denis Kevin Catherine, Raja Aziz Raja Ma’arof, Azrina Arshad, Sangeeth Suresh

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Machining parameters are very important in determining the surface quality of any material. In the past decade, some new engineering materials were developed for the manufacturing industry which created a need to conduct an investigation on the impact of the said parameters on their surface roughness. The polyurethane (PU) block is widely used in the automotive industry to manufacture parts such as checking fixtures that are used to verify the dimensional accuracy of automotive parts. In this paper, the design of experiment (DOE) was used to investigate the effect of the milling parameters on the PU block. Furthermore, an analysis of the machined surface chemical composition was done using scanning electron microscope (SEM). It was found that the surface roughness of the PU block is severely affected when PU undergoes a flood machining process instead of a dry condition. In addition, the step over and the silicon content were found to be the most significant parameters that influence the surface quality of the PU block.

Keywords: polyurethane (PU), design of experiment (DOE), scanning electron microscope (SEM), surface roughness

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Authors: Keivan Jamshidi

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Distal swelling and eventual degeneration of axon in the CNS and PNS have been considered to be the characteristic neuropathological effects of acrylamide (ACR) neuropathy. This study was conducted to determine the neurotoxic effects of different doses of ACR (0.5, 5, 50, 100, and 500 mg/kg per day × 11days i. p.) on hypothalamus of rat using the de Olmos amino cupric-silver stain and electron microscopy. For this purpose 60 adult male rats (Wistar, approximately 250 g) were randomly assigned in 5 treatment groups as A, B, C, D, E) exposed to 0.5, 5, 50, 100, and 500 mg/kg per dayx11days i. p. and one control group as F received daily i. p. injections of 0.9% saline (3ml/kg). As indices of developing neurotoxicity, weight gain, gait scores and landing hindlimb foot splay were determined. After 11 days, two rats for silver stain, and two rats for EM were randomly selected; dissected and proper samples were collected from hypothalamus. Results did show no neurological behavior in groups A, B and F were observed in group C. Rats in groups D and E died within 1-2 hours due to sever toxemia. In histopathological studies based on de Olmos technique no argyrophilic neurons or processes were observed in stained sections obtained from hypothalamus of rats belong to groups A, B, and F while moderate to severe argyrophilic changes were observed in different nuclei and regions of stained sections obtained from hypothalamus of rats belong to group C. In ultra-structural studies some variations in the myelin sheet of injured axons including decompactation, interlaminar space formation, disruption of the laminar sheet, accumulation of neurofilaments, vacculation, and clumping inside the axolem, and finally complete disappearance of laminar sheet were observed.

Keywords: acrylamide, hypothalamus, rat, de Olmos amino cupric, silver stain, electron microscopy

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Authors: Andrey V. Malyshev, Anna B. Petrova, Anatoly P. Surzhikov

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The article presents the results of the influence of diamagnetic additives on the defects level of ferrite ceramics. For this purpose, we use a previously developed method based on the mathematical analysis of experimental temperature dependences of the initial permeability. A phenomenological expression for the description of such dependence was suggested and an interpretation of its main parameters was given. It was shown, that the main criterion of the integral defects level of ferrite ceramics is the relation of two parameters correlating with elastic stress value in a material. Model samples containing a controlled number of intergranular phase inclusions served to prove the validity of the proposed method, as well as to assess its sensitivity in comparison with the traditional XRD (X-ray diffraction) analysis. The broadening data of diffraction reflexes of model samples have served for such comparison. The defects level data obtained by the proposed method are in good agreement with the X-ray data. The method showed high sensitivity. Therefore, the legitimacy of the selection relationship β/α parameters of phenomenological expression as a characteristic of the elastic state of the ferrite ceramics confirmed. In addition, the obtained data can be used in the detection of non-magnetic phases and testing the optimal sintering production technology of soft magnetic ferrites.

Keywords: cure point, initial permeability, integral defects level, homogeneity

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Authors: Paula Salazar, Rodrigo Henríquez, Pablo Zerega

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The textile, food and pharmaceutical industries are expanding daily worldwide, and they are located within the most polluting industries due to the fact that wastewater is discharged into watercourses with high concentrations of dyes and traces of drugs. Many of these compounds are stable to light and biodegradation, being considered as emerging organic contaminants. Advanced oxidation processes (AOPs) emerge as an effective alternative for the removal and elimination of this type of contaminants. Heterogeneous photocatalysis has been extensively studied as it is an efficient, low-cost and durable method. As the main photocatalyst, TiO₂ has been used for the degradation of a large number of dyes and drugs. The disadvantage of TiO₂ is its absorption in the UV region of the solar spectrum. On the other hand, quaternary chalcogenides based on Cu₂SnZnX₄ (X = S, Se) are a possible alternative due to their narrow bandgap (ca. between 0.8 to 1.5 eV depending on the phase considered), low cost, an abundance of its constituent elements in the earth's crust and its low toxicity. The objective of this research was to synthesize Cu₂SnZnS₄ (CZTS) through of a low-cost hydrothermal method and evaluate it as a potential photo-catalyst in the photo-degradation process of Congo Red. The synthesis of the nanoparticle in suspension and film onto fluorine-doped tin oxide coated glass (FTO) was carried out using a mixture of: 2 mmol CuCl₂, 1 mmol ZnCl₂, 1 mmol SnCl₂ and 4 mmol CH4N₂S in a Teflon reactor at 180⁰C for 72 h. Characterization was performed through scanning electron microscopy (SEM), X-ray diffraction (XRD) and UV VIS spectroscopy. Photo-degradation monitoring was carried out employing a UV VIS spectrophotometer. The results show that photodegradation of 55% of the dye can be obtained after 4h of exposure to polychromatic light, it should be noted that the Congo Red dye is being studied for the first time.

Keywords: CZTS, hydrothermal, photocatalysis, dye

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Authors: A. Elain, M. Le Fellic, A. Le Pemp, N. Hachet

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Iodinated Compounds (IC) are widely detected contaminants in most aquatic environments including sewage treatment plant, surface water, ground water and even drinking water, up to the µg.L-1 range. As IC contribute in the adsorbable organic halides (AOX) level, their removal or dehalogenation is expected. We report here on the biodegradability of a mixture of IC from an industrial effluent using a microbial consortium adapted to grow on IC as well as the native microorganisms. Both aerobic and anaerobic treatments were studied during batch experiments in 500-mL flasks. The degree of mineralization and recovery of iodide were monitored by HPLC-UV, TOC analysis and potentiometric titration. Providing ethanol as an electron acceptor was found to stimulate anaerobic reductive deiodination of IC while sodium chloride even at high concentration (22 g.l-1) had no influence on the degradation rates nor on the microbial viability. Phylogenetic analysis of 16S RNA gene sequence (MicroSeq®) was applied to provide a better understanding of the degradative microbial community.

Keywords: iodinated compounds, biodegradability, deiodination, electron-accepting conditions, microbial consortium

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Authors: Lucky Malise, Hilary Rutto, Tumisang Seodigeng

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The use of tires in automobiles is very important in the automobile industry. However, there is a serious environmental problem concerning the disposal of these rubber tires once they become worn out. The main aim of this study was to prepare activated carbon from waste tire pyrolysis char by impregnating KOH on pyrolytic char. Adsorption studies on lead onto chemically activated carbon was carried out using response surface methodology. The effect of process parameters such as temperature (°C), adsorbent dosage (g/1000ml), pH, contact time (minutes) and initial lead concentration (mg/l) on the adsorption capacity were investigated. It was found that the adsorption capacity increases with an increase in contact time, pH, temperature and decreases with an increase in lead concentration. Optimization of the process variables was done using a numerical optimization method. Fourier Transform Infrared Spectra (FTIR) analysis, XRay diffraction (XRD), Thermogravimetric analysis (TGA) and scanning electron microscope was used to characterize the pyrolytic carbon char before and after activation. The optimum points 1g/ 100 ml for adsorbent dosage, 7 for pH value of the solution, 115.2 min for contact time, 100 mg/l for initial metal concentration, and 25°C for temperature were obtained to achieve the highest adsorption capacity of 93.176 mg/g with a desirability of 0.994. Fourier Transform Infrared Spectra (FTIR) analysis and Thermogravimetric analysis (TGA) show the presence of oxygen-containing functional groups on the surface of the activated carbon produced and that the weight loss taking place during the activation step is small.

Keywords: waste tire pyrolysis char, chemical activation, central composite design (CCD), adsorption capacity, numerical optimization

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Authors: O. I. H. Dimitry, N. A. Mansour, A. L. G. Saad

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Natural sodium montmorillonite (NaMMT), Cloisite Na⁺ and two organophilic montmorillonites (OMMTs), Cloisites 20A and 15A were used. Polycaprolactone (PCL)/MMT composites containing 1, 3, 5, and 10 wt% of Cloisite Na⁺ and PCL/OMMT nanocomposites containing 5 and 10 wt% of Cloisites 20A and 15A were prepared via solution intercalation technique to study the influence of organic modifier loading on particle dispersion of PCL/ NaMMT composites. Thermal stabilities of the obtained composites were characterized by thermal analysis using the thermogravimetric analyzer (TGA) which showed that in the presence of nitrogen flow the incorporation of 5 and 10 wt% of filler brings some decrease in PCL thermal stability in the sequence: Cloisite Na+>Cloisite 15A > Cloisite 20A, while in the presence of air flow these fillers scarcely influenced the thermoxidative stability of PCL by slightly accelerating the process. The interaction between PCL and silicate layers was studied by Fourier transform infrared (FTIR) spectroscopy which confirmed moderate interactions between nanometric silicate layers and PCL segments. The electrical conductivity (σ) which describes the ionic mobility of the systems was studied as a function of temperature and showed that σ of PCL was enhanced on increasing the modifier loading at filler content of 5 wt%, especially at higher temperatures in the sequence: Cloisite Na⁺<Cloisite 20A<Cloisite 15A, and was then decreased to some extent with a further increase to 10 wt%. The activation energy E_σ obtained from the dependency of σ on temperature using Arrhenius equation was found to be lowest for the nanocomposite containing 5 wt% of Cloisite 15A. The dispersed behavior of clay in PCL matrix was evaluated by X-ray diffraction (XRD) and scanning electron microscopy (SEM) analyses which revealed partial intercalated structures in PCL/NaMMT composites and semi-intercalated/semi-exfoliated structures in PCL/OMMT nanocomposites containing 5 wt% of Cloisite 20A or Cloisite 15A.

Keywords: electrical conductivity, montmorillonite, nanocomposite, organoclay, polycaprolactone

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Authors: Monu Verma, Hyunook Kim

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Heavy metals and organic dyes are the major sources of water pollution. Herein, a trifunctional β−cyclodextrin−ethylenediaminetetraacetic acid−chitosan (β−CD−EDTA−CS) polymer was synthesized using an easy and simple chemical route by the reaction of activated β−CD with CS through EDTA as a cross-linker (amidation reaction) for the removal of inorganic and organic pollutants from aqueous solution under different parameters such as pH, time effect, initial concentration, reusability, etc. The synthesized adsorbent was characterized using powder X-ray diffraction, Fourier transform infrared spectroscopy, field scanning electron microscopy, energy dispersive spectroscopy, Brunauer-Emmett-Teller (BET), thermogravimetric analyzer techniques to investigate their structural, functional, morphological, elemental compositions, surface area, and thermal properties, respectively. Two types of heavy metals, i.e., mercury (Hg²⁺) and cadmium (Cd²⁺), and three organic dyes, i.e., methylene blue (MB), crystal violet (CV), and safranin O (SO), were chosen as inorganic and organic pollutants, respectively, to study the adsorption capacity of β-CD-EDTA-CS in aqueous solution. The β-CD-EDTA-CS shows a monolayer adsorption capacity of 346.30 ± 14.0 and 202.90 ± 13.90 mg g−¹ for Hg²⁺ and Cd²⁺, respectively, and a heterogeneous adsorption capacity of 107.20 ± 5.70, 77.40 ± 5.30 and 55.30 ± 3.60 mg g−¹ for MB, CV and SO, respectively. Kinetics results followed pseudo-second order (PSO) kinetics behavior for both metal ions and dyes, and higher rate constants values (0.00161–0.00368 g mg−¹ min−¹) for dyes confirmed the cavitation of organic dyes (physisorption). In addition, we have also demonstrated the performance of β-CD-EDTA-CS for the four heavy metals, Hg²⁺, Cd²⁺, Ni²⁺, and Cu²⁺, and three dyes MB, CV, and SO in secondary treated wastewater. The findings of this study indicate that β-CD-EDTA-CS is simple and easy to synthesize and can be used in wastewater treatment.

Keywords: adsorption isotherms, adsorption mechanism, amino-β-cyclodextrin, heavy metal ions, organic dyes

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Authors: Alireza Abdikian

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By assuming a quantum relativistic degenerate electron-positron (e-p) plasma media, the nonlinear acoustic solitary propagation in the presence of the stationary ions for neutralizing the plasma background of bounded cylindrical geometry was investigated. By using the standard reductive perturbation technique with cooperation the quantum hydrodynamics model for the e-p fluid, the spherical Kadomtsev-Petviashvili equation was derived for small but finite amplitude waves and was given the solitary wave solution for the parameters relevant for dense astrophysical objects such as white dwarf stars. By using a suitable coordinate transformation and using improved F-expansion technique, the SKP equation can be solved analytically. The numerical results reveal that the relativistic effects lead to propagate the electrostatic bell shape structures and by increasing the relativistic effects, the amplitude and the width of the e-p acoustic solitary wave will decrease.

Keywords: Electron-positron plasma, Acoustic solitary wave, Relativistic plasmas, the spherical Kadomtsev-Petviashvili equation

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Authors: Mohieldin Elmashad, Salwa Yassin

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Expansive soils regarded as one of the most problematic unsaturated formations in the Egyptian arid zones and present a great challenge in civil engineering, in general, and geotechnical engineering, in particular. Severe geotechnical complications and consequent structural damages have been arising due to an excessive and differential volumetric change upon wetting and change in water content. Different studies have been carried out concerning the swelling performance of the expansive soils using different additives including phospho-gypsum as an industrial waste product. However, this paper describes the results of a comprehensive testing programme that was carried out to investigate the effect of phospho-gypsum (PG) and sodium chloride (NaCl), as an additive mixture, on the swelling performance of constituent samples of swelling soils. The constituent samples comprise commercial bentonite collected from a natural site, mixed with different percentages of PG-NaCl mixture. The testing programme had been scoped to cover the physical and chemical properties of the constituent samples. In addition, a mineralogical study using x-ray diffraction (XRD) was performed on the collected bentonite and the mixed bentonite with PG-NaCl mixture samples. The obtained results of this study showed significant improvement in the swelling performance of the tested samples with the increase of the proposed PG-NaCl mixture content.

Keywords: expansive soils, industrial waste, mineralogical study, swelling performance, X-ray diffraction

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Authors: Evrim Colak, Andriy E. Serebryannikov, Thore Magath, Ekmel Ozbay

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Single beam deflection and unidirectional transmission are examined for oblique incidence in a Photonic Crystal (PC) structure which employs defect layer instead of surface corrugations at the interfaces. In all of the studied cases, the defect layer is placed such that the symmetry is broken. Two types of deflection are observed depending on whether the zeroth order is coupled or not. These two scenarios can be distinguished from each other by considering the simulated field distribution in PC. In the first deflection type, Floquet-Bloch mode enables zeroth order coupling. The energy of the zeroth order is redistributed between the diffraction orders at the defect layer, providing deflection. In the second type, when zeroth order is not coupled, strong diffractions cause blazing and the evanescent waves deliver energy to higher order diffraction modes. Simulated isofrequency contours can be utilized to estimate the coupling behavior. The defect layer is placed at varying rows, preserving the asymmetry of PC while evancescent waves can still couple to higher order modes. Even for deeply buried defect layer, asymmetric transmission and beam deflection are still encountered when the zeroth order is not coupled. We assume ε=11.4 (refractive index close to that of GaAs and Si) for the PC rods. A possible operation wavelength can be within microwave and infrared range. Since the suggested material is low loss, the structure can be scaled down to operate higher frequencies. Thus, a sample operation wavelength is selected as 1.5μm. Although the structure employs no surface corrugations transmission value T≈0.97 can be achieved by means of diffraction order m=-1. Moreover, utilizing an extra line defect, T value can be increased upto 0.99, under oblique incidence even if the line defect layer is deeply embedded in the photonic crystal. The latter configuration can be used to obtain deflection in one frequency range and can also be utilized for the realization of another functionality like defect-mode wave guiding in another frequency range but still using the same structure.

Keywords: asymmetric transmission, beam deflection, blazing, bi-directional splitting, defect layer, dual beam splitting, Floquet-Bloch modes, isofrequency contours, line defect, oblique incidence, photonic crystal, unidirectionality

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Authors: Ifeoma Maryjane Iloamaeke, Kelvin Obazie, Mmesoma Offornze, Chiamaka Marysilvia Ifeaghalu, Cecilia Aduaka, Ugomma Chibuzo Onyeije, Claudine Ifunanaya Ogu, Ngozi Anastesia Okonkwo

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This work investigated the effects of pH, settling time, and coagulant dosages on the removal of color, turbidity, and heavy metals from paint industrial wastewater using the seed of Artocarpus heterophyllus (AH) by the coagulation-flocculation process. The paint effluent was physicochemically characterized, while AH coagulant was instrumentally characterized by Scanning Electron Microscope (SEM), Fourier Transform Infrared (FTIR), and X-ray diffraction (XRD). A Jar test experiment was used for the coagulation-flocculation process. The result showed that paint effluent was polluted with color, turbidity (36000 NTU), mercury (1.392 mg/L), lead (0.252 mg/L), arsenic (1.236 mg/L), TSS (63.40mg/L), and COD (121.70 mg/L). The maximum color removal efficiency was 94.33% at the dosage of 0.2 g/L, pH 2 at a constant time of 50 mins, and 74.67% at constant pH 2, coagulant dosage of 0.2 g/L and 50 mins. The highest turbidity removal efficiency was 99.94% at 0.2 g/L and 50 mins at constant pH 2 and 96.66% at pH 2 and 0.2 g/L at constant time of 50 mins. The mercury removal efficiency of 99.29% was achieved at the optimal condition of 0.8 g/L coagulant dosage, pH 8, and constant time of 50 mins and 99.57% at coagulant dosage of 0.8 g/L, time of 50 mins constant pH 8. The highest lead removal efficiency was 99.76% at a coagulant dosage of 10 g/L, time of 40 mins at constant pH 10, and 96.53% at pH 10, coagulant dosage of 10 g/L and constant time of 40 mins. For arsenic, the removal efficiency is 75.24 % at 0.8 g/L coagulant dosage, time of 40 mins, and constant pH of 8. XRD imaging before treatment showed that Artocarpus heterophyllus coagulant was crystalline and changed to amorphous after treatment. The SEM and FTIR results of the AH coagulant and sludge suggested there were changes in the surface morphology and functional groups before and after treatment. The reaction kinetics were modeled best in the second order.

Keywords: Artocarpus heterophyllus, coagulation-flocculation, coagulant dosages, setting time, paint effluent

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Authors: Sylwia Gieraltowska, Lukasz Wachnicki, Bartlomiej S. Witkowski, Marek Godlewski

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Oxide layers doped with rare-earth (RE) ions in optimized way can absorb short (ultraviolet light), which will be converted to visible light by so-called down-conversion. Down-conversion mechanisms are usually exploited to modify the incident solar spectrum. In down conversion, multiple low-energy photons are generated to exploit the energy of one incident high-energy photon. These RE-doped oxide materials have attracted a great deal of attention from researchers because of their potential for optical manipulation in optical devices (detectors, temperature sensors, and compact solid-state lasers, light-emitting diodes), bio-analysis, medical therapy, display technologies, and light harvesting (such as in photovoltaic cells). The zirconium dioxide (ZrO2) doped RE ions (Eu, Tb, Ce) multilayer structures were tested as active layers, which can convert short wave emission to light in the visible range (the down-conversion mechanism). For these applications original approach of deposition ZrO2 layers using the Atomic Layer Deposition (ALD) method and doping these layers with RE ions using the spin-coating technique was used. ALD films are deposited at relatively low temperature (well below 250°C). This can be an effective method to achieve the white-light emission and to improve on this way light conversion efficiency, by an extension of absorbed spectral range by a solar cell material. Photoluminescence (PL), X-ray diffraction (XRD), scanning electron microscope (SEM) and atomic force microscope (AFM) measurement are analyzed. The research was financially supported by the National Science Centre (decision No. DEC-2012/06/A/ST7/00398 and DEC- 2013/09/N/ST5/00901).

Keywords: ALD, oxide layers, photovoltaics, thin films

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Authors: Angelo Lanzilotto, Martin Kuss-Petermann, Catherine E. Housecroft, Edwin C. Constable, Oliver S. Wenger

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We recently described the synthesis of a new tetraphenylporphyrinatozinc(II)-conjugated 2,2':6',6"-terpyridine (1) in which the tpy domain enables the molecule to act as a metalloligand. The synthetic route to 1 has been optimized, the importance of selecting a particular sequence of synthetic steps will be discussed. Three homoleptic complexes have been prepared, [Zn(1)₂]²⁺, [Fe(1)₂]²⁺ and [Ru(1)₂]²⁺, and have been isolated as the hexafluoridophosphate salts. Spectroelectrochemical measurements have been performed and the spectral changes ascribed to redox processes are partitioned on either the porphyrin or the terpyridine units. Compound 1 undergoes a reversible one-electron oxidation/reduction. The removal/gain of a second electron leads to a further irreversible chemical transformation. For the homoleptic [M(1)₂]²⁺ complexes, a suitable potential can be chosen at which both the oxidation and the reduction of the {ZnTPP} core are reversible. When the homoleptic complex contains a redox active metal such as Fe or Ru, spectroelectrochemistry has been used to investigate the metal to ligand charge transfer (MLCT) transition. The latter is sensitive to the oxidation state of the metal, and electrochemical oxidation of the metal center suppresses it. Detailed spectroelectrochemical studies will be presented.

Keywords: homoleptic complexes, spectroelectrochemistry, tetraphenylporphyrinatozinc(II), 2, 2':6', 6"-terpyridine

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Authors: Deepa T., Inchara S. R., Venkatesh S. V., Seema Tharannum

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Concrete is the most widely used structural material. It is usually made using locally available materials. However, concrete has low tensile strength and may crack in the early days with exothermic hydration, for which water is essential. To address the increased construction water demand, treated greywater may be used. Bacillus subtilis bacteria that form endospores is the biological agent considered in this study for biomineralization or Microbially Induced Calcite Precipitation (MICP) technique to heal cracks. Treated grey water which is obtained from STP of PES University, opted in place of Potable water, which had qualities within the standard range as per codal provisions. In this work, M30 grade conventional concrete is designed using OPC 53-grade cement, manufactured sand, natural coarse aggregates, and potable water. Conventional concrete (CC), bacterial concrete with potable water (BS), and treated grey water concrete (TGWBS) are the three different concrete specimens cast. Experimental studies such as the strength test and the surface hardness test are performed on conventional and bacterial concrete samples after 7, 28, and 56 days of curing. Concrete cubes are subjected to a temperature of 50° C to investigate the effect of higher temperature. Cracked cube specimens are observed for self-healing -as well as microstructure analysis with Scanning Electron Microscope (SEM), Energy Dispersive X-Ray Analysis (EDAX), and X-Ray Diffraction Analysis (XRD). Noticeable calcium salt deposition is observed on the surface of the BS and TGWBS cracked specimen. Surface hardness and the EDAX test gave promising results on the advantage of using spore-forming bacteria in concrete. This is followed by the strength gained in compression and flexure. Results also indicate that treated grey water can be a substitute for potable water in concrete.

Keywords: Bacillus subtilis concrete, microstructure, temperature, treated greywater

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Authors: A. Bentabet, A. Aydin, N. Fenineche

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The mean penetration depth has a most important in the absorption transport phenomena. Analytical model of light ion backscattering coefficients from solid targets have been made by Vicanek and Urbassek. In the present work, we showed a mathematical expression (deterministic model) for Z1/2. In advantage, in the best of our knowledge, relatively only one analytical model exit for electron or positron mean penetration depth in solid targets. In this work, we have presented a simple geometric spherical model of absorbed particles based on CSDA scheme. In advantage, we have showed an analytical expression of the mean penetration depth by combination between our model and the Vicanek and Urbassek theory. For this, we have used the Relativistic Partial Wave Expansion Method (RPWEM) and the optical dielectric model to calculate the elastic cross sections and the ranges respectively. Good agreement was found with the experimental and theoretical data.

Keywords: Bentabet spherical geometric model, continuous slowing down approximation, stopping powers, ranges, mean penetration depth

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Authors: Galiya Zhanzakovna Alzhanova, Yelaman Kanatovich Aibuldinov, Zhanar Baktybaevna Iskakova, Gaziz Galymovich Abdiyussupov, Madi Toktasynuly Omirzak, Aizhan Doldashevna Gazizova

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The sustainable use of industrial waste has recently increased due to increased environmental problems in landfills. One of the best ways to utilise waste is as a road base material. Industrial waste is a less costly and more efficient way to strengthen local soils than by introducing new additive materials. This study explored the feasibility of utilising red mud, blast furnace slag, and lime production waste to develop environmentally friendly construction materials for stabilising natural loam. Four different ratios of red mud (20, 30, and 40%), blast furnace slag (25, 30, and 35%), lime production waste (4, 6, and 8%), and varied amounts of natural loam were combined to produce nine different mixtures. The results showed that the sample with 40% red mud, 35% blast furnace slag, and 8% lime production waste had the highest strength. The sample's measured compressive strength for 90 days was 7.38 MPa, its water resistance for the same period was 7.12 MPa, and its frost resistance for the same period was 7.35 MP; low linear expansion met the requirements of the Kazakh regulations for first-class building materials. The study of mineral composition showed that there was no contamination with heavy metals or dangerous substances. Road base materials made of red mud, blast furnace slag, lime production waste, and natural loam mix can be employed because of their durability and environmental performance. The chemical and mineral composition of raw materials was determined using X-ray diffraction, X-ray fluorescence, scanning electron microscopy, energy dispersive spectroscopy, atomic absorption spectroscopy, and axial compressive strength were examined.

Keywords: blast furnace slag, lime production waste, natural loam stabilizing, red mud, road base material

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Authors: G. Singh, H.Schuster, U. Füssel

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The stability of electric arc and durability of electrode tip used in Tungsten Inert Gas (TIG) welding demand a metallurgical study about the chemical transport mechanism of emitter oxide particles in tungsten electrode during its real welding conditions. The tungsten electrodes doped with emitter oxides of rare earth oxides such as La₂O₃, Th₂O₃, Y₂O₃, CeO₂ and ZrO₂ feature a comparatively lower work function than tungsten and thus have superior emission characteristics due to lesser surface temperature of the cathode. The local change in concentration of these emitter particles in tungsten electrode due to high temperature diffusion (chemical transport) can change its functional properties like electrode temperature, work function, electron emission, and stability of the electrode tip shape. The resulting increment in tip surface temperature results in the electrode material loss. It was also observed that the tungsten recrystallizes to large grains at high temperature. When the shape of grain boundaries are granular in shape, the intergranular diffusion of oxide emitter particles takes more time to reach the electrode surface. In the experimental work, the microstructure of the used electrode's tip surface will be studied by scanning electron microscope and reflective X-ray technique in order to gauge the extent of the diffusion and chemical reaction of emitter particles. Besides, a simulated model is proposed to explain the effect of oxide particles diffusion on the electrode’s microstructure, electron emission characteristics, and electrode tip erosion. This model suggests metallurgical modifications in tungsten electrode to enhance its erosion resistance.

Keywords: rare-earth emitter particles, temperature-dependent diffusion, TIG welding, Tungsten electrode

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Authors: Shashank Bahri, Divyanshu Arya, Rajni Jain, Sreedevi Upadhyayula

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Petroleum products can be obtained from syngas catalytic conversion using Fischer Tropsch Reaction. The liquid fuels obtained from FTS are sulphur and nitrogen free and thus may easily meet the increasing stringent environment regulations. In the present work we have synthesized Meso porous ZSM-5 supported catalyst. Meso structure were created in H-ZSM-5 crystallites by demetalation via subsequent base and acid treatment. Desilication through base treatment provides H-ZSM-5 with pore size and volumes similar to amorphous SiO2 (Conventional Carrier). Modifying the zeolite texture and surface chemistry by Desilication and acid washing alters its accessibility and interactions with metal phase and consequently the CO adsorption behavior and hydrocarbon product distribution. Increasing the mesoporosity via desilication provides the micro porous zeolite with essential surface area to support optimally sized metal crystallites. This improves the metal dispersion and hence improve the activity of the catalyst. Transition metal (Co) was loaded using wet impregnation method. Synthesized catalysts were characterized by Infrared Spectroscopy, Powdered X-Ray Diffraction, Scanning Electron Microscopy (SEM), BET Method analytical techniques. Acidity of the catalyst which plays an important role in FTS reaction was measured by DRIFT setup pyridine adsorption instead of NH3 Temperature Programmed Desorption. The major difference is that, Pyridine Adsorption can distinguish between Lewis acidity and Bronsted Acidity, thus giving their relative strengths in the catalyst sample, whereas TPD gives total acidity including Lewis and Bronsted ones.

Keywords: mesopourus, fischer tropsch reaction, pyridine adsorrption, drift study

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Authors: Srutirekha Giri, Manoranjan Sahoo, Anuradha Das, Pravanjan Mallick, Biswajit Mallick

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Ion Beam (IB) technique is a very powerful experimental technique for both material synthesis and material modifications. In this work, 3MeV proton beam was generated using the 3MV Tandem machine of the Institute of Physics, Bhubaneswar and extracted into air for the irradiation-induced modification purpose[1]. The polymeric material can be modeled for a three-phase system viz. crystalline(I), amorphous(II) and mesomorphic(III). So far, our knowledge is concerned. There are only few techniques reported for the synthesis of this third-phase(III) of polymer. The IB induced technique is one of them and has been reported very recently [2-4]. It was observed that by irradiating polyethylene terephthalate (PET) fiber at very low proton fluence, 10¹⁰ - 10¹² p/s, possess 2D mesophase structure. This was confirmed using X-ray diffraction technique. A low-intensity broad peak was observed at small angle of about 2θ =6º, when the fiber axis was mounted parallel to the X-ray direction. Such peak vanished in the diffraction spectrum when the fiber axis was mounted perpendicular to the beam direction. The appearance of this extra peak in a particular orientation confirms that the phase is 2-dimensionally oriented (mesophase). It is well known that the mesophase is a 2-dimensionally ordered structure but 3-dimensionally disordered. Again, the crystallite of the mesophase peak particle was measured about 3nm. The MeV proton-induced 2D mesophase patterning of nanocrystallites (3nm) of PET due to irradiation was observed within the above low fluence range and failed in high proton fluence. This is mainly due to the breaking of crystallites, radiation-induced thermal degradation, etc.

Keywords: Ion irradiation, mesophase, nanocrystallites, polymer

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Authors: Teguh Endah Saraswati, Kusumandari Kusumandari, Candra Purnawan, Annisa Dinan Ghaisani, Aufara Mahayum

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The present study aims to investigate the degradation of methylene blue (MB) using TiO₂-carbon (TiO₂-C) photocatalyst combined with dielectric discharge (DBD) plasma. The carbon materials used in the photocatalyst were activated carbon and graphite. The thin layer of TiO₂-C photocatalyst was prepared by ball milling method which was then deposited on the plastic sheet. The characteristic of TiO₂-C thin layer was analyzed using X-ray diffraction (XRD), scanning electron microscopy (SEM) with energy dispersive X-ray (EDX) spectroscopy, and UV-Vis diffuse reflectance spectrophotometer. The XRD diffractogram patterns of TiO₂-G thin layer in various weight compositions of 50:1, 50:3, and 50:5 show the 2θ peaks found around 25° and 27° are the main characteristic of TiO₂ and carbon. SEM analysis shows spherical and regular morphology of the photocatalyst. Analysis using UV-Vis diffuse reflectance shows TiO₂-C has narrower band gap energy. The DBD plasma reactor was generated using two electrodes of Cu tape connected with stainless steel mesh and Fe wire separated by a glass dielectric insulator, supplied by a high voltage 5 kV with an air flow rate of 1 L/min. The optimization of the weight composition of TiO₂-C thin layer was studied based on the highest reduction of the MB concentration achieved, examined by UV-Vis spectrophotometer. The changes in pH values and color of MB indicated the success of MB degradation. Moreover, the degradation efficiency of MB was also studied in various higher concentrations of 50, 100, 200, 300 ppm treated for 0, 2, 4, 6, 8, 10 min. The degradation efficiency of MB treated in combination system of photocatalysis and DBD plasma reached more than 99% in 6 min, in which the greater concentration of methylene blue dye, the lower degradation rate of methylene blue dye would be achieved.

Keywords: activated carbon, DBD plasma, graphite, methylene blue, photocatalysis

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Authors: Muhammad Habib, Lin Tang, Guoliang Xue, Attaur Rahman, Myong-Ho Kim, Soonil Lee, Xuefan Zhou, Yan Zhang, Dou Zhang

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Designing a high-performance, lead-free ceramic has become a cutting-edge research topic due to growing concerns about the toxic nature of lead-based materials. In this work, a convenient strategy of compositional design and domain engineering is applied to the lead-fee BiFeO₃-BaTiO₃ ceramics, which provides a flexible polarization-free-energy profile for domain switching. Here, simultaneously enhanced dynamic piezoelectric constant (d33* = 772 pm/V) and a good thermal-stability (d33* = 26% over the temperature of 20-180 ᵒC) are achieved with a high Curie temperature (TC) of 432 ᵒC. This high piezoelectric strain performance is collectively attributed to multiple effects such as thermal quenching, suppression of defect charges by donor doping, chemically induced local structure heterogeneity, and electric field-induced phase transition. Furthermore, the addition of BT content decreased octahedral tilting, reduced anisotropy for domain switching and increased tetragonality (cₜ/aₜ), providing a wider polar length for B-site cation displacement, leading to high piezoelectric strain performance. Atomic-resolution transmission electron microscopy and piezoelectric force microscopy combined with X-ray diffraction results strongly support the origin of high piezoelectricity. The high and temperature-stable piezoelectric strain response of this work is superior to those of other lead-free ceramics. The synergistic approach of composition design and the concept present here for the origin of high strain response provides a paradigm for the development of materials for high-temperature piezoelectric actuator applications.

Keywords: Piezoelectric, BiFeO3-BaTiO3, Quenching, Temperature-insensitive

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Authors: Diana Serbezeanu, Ionela-Daniela Carja, Tachita Vlad-Bubulac, Sergiu Sova

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New phosphorus-containing monomers having methoxy end functional groups were prepared from methyl 4-hydroxybenzoate and two different dichlorides with phosphorus, namely phenyl phosphonic dichloride and phenyl dichlorophosphate. The structures of the monomers were confirmed by FTIR and NMR spectroscopy. The assignments for the 1H, 13C and 31P chemical shifts are based on 1D and 2D NMR homo- and heteronuclear correlations (H,H-COSY (Correlation Spectroscopy), H,C-HMQC (Heteronuclear Multiple Quantum Correlation and H,C-HMBC (Heteronuclear Multiple Bond Correlation)) and 31P-13C couplings. The monomers exhibited good solubility in common organic solvents. Dimethyl sulfoxide was to be a good solvent to grow crystals of considerable size which were investigated by X-ray analysis. One of these two new monomers presented thermotropic liquid crystalline behaviour, as revealed by differential scanning calorimetry (DSC), polarized light microscopy (PLM) and X-ray diffraction (XRD). The transition temperature from crystal to liquid crystalline state (K→LC) was 143°C and from the LC to isotropic state (LC→I) was 167°C. Upon heating, bis(4-(methoxycarbonyl)phenyl formed fine textures, difficult to be ascribed to smectic or nematic phases. Upon cooling from the isotropic state, bis(4-(methoxycarbonyl)phenyl exhibited a mosaic-type texture. X-ray diffraction measurements at small angles (SAXS) of bis(4-(methoxycarbonyl)phenyl showed two peaks at 1.8 Å and 3.5 Å, respectively suggesting organization at supramolecular level.

Keywords: phosphorus-containing monomers, polarized light microscopy, structure investigation, thermotropic liquid crystalline properties

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Authors: Esraa Mohamed El-Fawal

Abstract:

A facile solvothermal procedure was applied to fabricate zinc ferrite nanoparticles (ZnFe₂O₄ NPs). Activated carbon (AC) derived from peanut shells is synthesized using a microwave through the chemical activation method. The ZnFe₂O₄-AC composite is then mixed with a cerium-based metal-organic framework (CeMOF) by solid-state adding to formulate ZnFe₂O₄-AC/CeMOF composite. The synthesized photo materials were tested by scanning/transmission electron microscope (SEM/TEM), Photoluminescence (PL), (XRD) X-Ray diffraction, (FTIR) Fourier transform infrared, (UV-Vis/DRS) ultraviolet-visible/diffuse reflectance spectroscopy. The prepared ZnFe₂O₄-AC/CeMOFphotomaterial shows significantly boosted efficiency for photodegradation of methyl orange /methylene blue (MO/MB) compared with the pristine ZnFe₂O₄ and ZnFe₂O₄-AC composite under the irradiation of visible-light. The favorable ZnFe₂O₄-AC/CeMOFphotocatalyst displays the highest photocatalytic degradation efficiency of MB/MO (R: 91.5-88.6%, consecutively) compared with the other as-prepared materials after 30 min of visible-light irradiation. The apparent reaction rate K: 1.94-1.31 min-1 is also calculated. The boosted photocatalytic proficiency is ascribed to the heterojunction at the interface of prepared photo material that assists the separation of the charge carriers. To reach optimization, statistical analysis using response surface methodology was applied. The effect of independent parameters (such as A (pH), B (irradiation time), and (c) initial pollutants concentration on the response function (%)photodegradation of MB/MO dyes (as examples of azodyes) was investigated via using central composite design. At the optimum condition, the photodegradation efficiency (%) of the MB/MO is 99.8-97.8%, respectively. ZnFe2O₄-AC/CeMOF hybrid reveals good stability over four consecutive cycles.

Keywords: azo-dyes, photo-catalysis, zinc ferrite, response surface methodology

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Authors: Khadijat Olabisi Abdulwahab, Mohammad Azad Malik, Paul O'Brien, Grigore Timco, Floriana Tuna

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The synthesis of spinel ferrite nanoparticles with a narrow size distribution is very crucial in their numerous applications including information storage, hyperthermia treatment, drug delivery, contrast agent in magnetic resonance imaging, catalysis, sensors, and environmental remediation. Ferrites have the general formula MFe₂O₄ (M = Fe, Co, Mn, Ni, Zn e.t.c) and possess remarkable electrical and magnetic properties which depend on the cations, method of preparation, size and their site occupancies. To the best of our knowledge, there are no reports on the use of a single source precursor to synthesise quaternary ferrite nanoparticles. Here in, we demonstrated the use of trimetallic iron pivalate cluster [CrCoFeO(O₂CᵗBu)₆(HO₂CᵗBu)₃] as a single source precursor to synthesise monodisperse cobalt chromium ferrite (FeCoCrO₄) nanoparticles by the hot injection thermolysis method. The precursor was thermolysed in oleylamine, oleic acid, with diphenyl ether as solvent at 260 °C. The effect of reaction time on the stoichiometry, phases or morphology of the nanoparticles was studied. The p-XRD patterns of the nanoparticles obtained after one hour was pure phase of cubic iron cobalt chromium ferrite (FeCoCrO₄). TEM showed that a more monodispersed spherical ferrite nanoparticles were obtained after one hour. Magnetic measurements revealed that the ferrite particles are superparamagnetic at room temperature. The nanoparticles were characterised by Powder X-ray Diffraction (p-XRD), Transmission Electron Microscopy (TEM), Energy Dispersive Spectroscopy (EDS) and Super Conducting Quantum Interference Device (SQUID).

Keywords: cobalt chromium ferrite, colloidal, hot injection thermolysis, monodisperse, reaction time, single source precursor, quaternary ferrite nanoparticles

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Authors: Débora N. Zambrano, Marina O. Gosatti, Leandro M. Dufou, Daniel A. Serrano, M. Mónica Guraya, Soledad Perez-Catán

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Nanoporous g-Al₂O₃ samples were synthesized via a sol-gel technique, introducing changes in the Yoldas´ method. The aim of the work was to achieve an effective control of the nanostructure properties and morphology of the final g-Al₂O₃. The influence of the reagent temperature during the hydrolysis was evaluated in case of water at 5 ºC and 98 ºC, and alkoxide at -18 ºC and room temperature. Sol-gel transitions were performed at 120 ºC and room temperature. All g-Al₂O₃ samples were characterized by X-ray diffraction, nitrogen adsorption and thermal analysis. Our results showed that temperature of both water and alkoxide has not much influence on the nanostructure of the final g-Al₂O₃, thus giving a structure very similar to that of samples obtained by the reference method as long as the reaction temperature above 75 ºC is reached soon enough. XRD characterization showed diffraction patterns corresponding to g-Al₂O₃ for all samples. Also BET specific area values (253-280 m²/g) were similar to those obtained by Yoldas’s original method. The temperature of the sol-gel transition does not affect the resulting sample structure, and crystalline boehmite particles were identified in all dried gels. We analyzed the reproducibility of the samples’ structure by preparing different samples under identical conditions; we found that performing the sol-gel transition at 120 ºC favors the production of more reproducible samples and also reduces significantly the time of the sol-gel reaction.

Keywords: nanostructure alumina, boehmite, sol-gel technique, N2 adsorption/desorption isotherm, pore size distribution, BET area.

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Authors: Stephen Rathinaraj Benjamin, Flavio Colmati Junior, Maria Izabel Florindo Guedes, Rosa Amalia Fireman Dutra

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A new enzymatic electrochemical biosensor based on multiwall carbon nanotubes and cerium oxide nanoparticles for the detection of rutin has been developed. The cerium oxide nanoparticles /HRP/ multiwall carbon nanotubes/ carbon paste electrode (HRP/ CeO2/MWCNTs/CPE) was prepared by ensuing addition of MWCNTs and HRP on the CPE, followed by the mixing with cerium oxide nanoparticles. Surface physical characteristics of the modified electrode and the electrochemical properties of the composite were investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM), cylic voltammetry (CV), differential pulse voltammetry (DPV) and square wave voltammetry (SWV). The HRP/ CeO2/MWCNTs/CPE showed good selectivity, stability and reproducibility, which was further applied to detect rutin tablet and capsule samples with satisfactory results.

Keywords: cerium dioxide nanoparticles, horseradish peroxidase, multiwall carbon nanotubes, rutin

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Authors: Ben Yahia Nouha, Harris Chris, Sebei Abdelaziz, Boussen Slim, Chaabani Fredj

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The present work has set itself the objective of studying non-detritic siliceous rocks of the extreme northwest Tunisia. It aims to examine the origin and their sedimentary depositional environment based on mineralogical and geochemical characteristics. The different sections were located in the area of Babouch and the area of Tabarka. The collected samples were subjected to mineralogical and geochemical characterization using different analytical methods: X-ray diffraction (XRD), geochemical analysis (ICP- AES), isotopic geochemistry (δ18O), to assess their suitability for industrial use. X-ray powder diffraction of the pure siliceous rock indicates quartz as the major mineral, with the total lack of amorphous silica. Trace impurities, such as carbonate and clay minerals, are concealed in the analytical results. The petrographic examination revealed allowed us to deduce that this rock was deriving from tests of siliceous organisms (the radiolarians). The chemical composition shows that SiO2, Al2O3, and Fe2O3 represent the most abundant oxides. The other oxides are present in negligible quantities. Geochemical data support a biogenic and non-hydrothermal origin of babouchite silica. Oxygen isotopic has shown that babouchites were formed in an environment with a high temperature ranging from 56 °C to 73 °C.

Keywords: biogenic silica, babouchite formation, XRD, chemical analysis, oxygen isotopic, northwest tunisia

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Authors: H. Djaaboube, I. Loucif, Y. Bouachiba, R. Aouati, A. Maameri, A. Taabouche, A. Bouabellou

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Thin films of pure and barium-doped zinc oxide (ZnO) were prepared using a spray pyrolysis process. The films were deposited on glass substrates at 450°C. The different samples are characterized by X-ray diffraction (XRD) and UV-Vis spectroscopy. X-ray diffraction patterns reveal the formation of a single ZnO Wurtzite structure and the good crystallinity of the films. The substitution of Ba ions influences the texture of the layers and makes the (002) plane a preferential growth plane. At concentrations below 6% Ba, the hexagonal structure of ZnO undergoes compressive stresses due to barium ions which have a radius twice of the Zn ions. This result leads to the decrees of a and c parameters and, therefore, the volume of the unit cell. This result is confirmed by the decrease in the number of crystallites and the increase in the size of the crystallites. At concentrations above 6%, barium substitutes the zinc atom and modifies the structural parameters of the thin layers. The bandgap of ZnO films decreased with increasing doping; this decrease is probably due to the 4d orbitals of the Ba atom due to the sp-d spin-exchange interactions between the band electrons and the localized d-electrons of the substituted Ba ion. Although, the Urbache energy undergoes an increase which implies the creation of energy levels below the conduction band and decreases the band gap width. The photocatalytic activity of ZnO doped 9% Ba was evaluated by the photodegradation of methylene blue under UV irradiation.

Keywords: barium, doping, photodegradation, spray pyrolysis, ZnO

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Authors: Hina Verma, Karine Le Guen, Renaud Dalaunay, Iyas Ismail, Vita Ilakovac, Jean Pascal Rueff, Yunlin Jacques Zheng, Philippe Jonnard

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To the extent of our knowledge, X-ray emission spectroscopy (XES) has been applied in the soft x-ray region (photon energy ≤ 2 keV) to study the buried layers and interfaces of stacks of nanometer-thin films. Now we extend the methodology to study the buried interfaces in the hard X-ray region (i.e., ≥ five keV). The emission spectra allow us to study the interactions between elements in the buried layers from the analysis of their valence states, thereby providing sensitive information about the physical-chemical environment of the emitting element in multilayers. We exploit the chemical sensitivity of XES to study the interfaces between Fe and Si layers in the Fe/Si multilayer from the Fe Kβ₂,₅ emission spectra (7108 eV). The Fe Kβ₅ emission line results from the electronic transition from occupied 3d to 1s levels (i.e., valence to core transition) and is hence sensitive to the chemical state of emitting Fe atoms. The comparison of emission spectra recorded for Fe/Si multilayer with Fe and FeSi₂ references reveal the formation of FeSi₂ at the Fe-Si interfaces inside the multilayer stack. The interfacial thickness was calculated to be 1.4 ± 0.2 nm by taking into consideration the intensity of Fe atoms emitted from the interface and the Fe layer. The formation of FeSi₂ at the interface was further confirmed by the X-ray diffraction and X-ray photoelectron spectroscopy done on the Fe/Si multilayer. Hence, we can conclude that the XES in the hard X-ray range could be used to study multilayers and their interfaces and obtain information both qualitatively and quantitatively.

Keywords: buried interfaces, hard X-ray emission spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy

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