Search results for: EDX

Authors: Atilla Evcin, Bahri Ersoy, Süleyman Akpınar, I. Sinan Atlı

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Ceramic, polymer and composite nanofibers are nowadays begun to be utilized in many fields of nanotechnology. By the means of dimensions, these fibers are as small as nano scale but because of having large surface area and microstructural characteristics, they provide unique mechanic, optical, magnetic, electronic and chemical properties. In terms of nanofiber production, electrospinning has been the most widely used technique in recent years. In this study, carbon nanofibers have been synthesized from solutions of Polyacrylonitrile (PAN)/ N,N-dimethylformamide (DMF) by electrospinning method. The carbon nanofibers have been stabilized by oxidation at 250 °C for 2 h in air and carbonized at 750 °C for 1 h in H2/N2. Images of carbon nanofibers have been taken with scanning electron microscopy (SEM). The images have been analyzed to study the fiber morphology and to determine the distribution of the fiber diameter using FibraQuant 1.3 software. Then polymer composites have been produced from mixture of carbon nanofibers and silicone polymer. The final polymer composites have been characterized by X-ray diffraction method and scanning electron microscopy (SEM) energy dispersive X-ray (EDX) measurements. These results have been reported and discussed. At result, homogeneous carbon nanofibers with 100-167 nm of diameter were obtained with optimized electrospinning conditions.

Keywords: Electrospinning, characterization, composites, nanofiber.

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Authors: M. Al Nur, M. S. Kaiser

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Corrosion behaviour of hypereutectic Al-19Si automotive alloy in different pH=1, 3, 5, 7, 9, 11, and 13 environments was carried out using conventional gravimetric measurements and was complemented by resistivity, optical micrograph, scanning electron microscopy (SEM) and X-ray analyzer (EDX) investigations. Gravimetric analysis confirmed that the highest corrosion rate is shown at pH 13 followed by pH 1. Minimum corrosion occurs in the pH range of 3.0 to 11 due to establishment of passive layer on the surface. The highest corrosion rate at pH 13 is due to the presence of sodium hydroxide in the solution which dissolves the surface oxide film at a steady rate. At pH 1, it can be attributed that the presence of aggressive chloride ions serves to pick up the damage of the passive films at localized regions. With varying exposure periods by both, the environment complies with the normal corrosion rate profile that is an initial steep rise followed by a nearly constant value of corrosion rate. Resistivity increases in case of pH 1 solution for the higher pit formation and decreases at pH 13 due to formation of thin film. The SEM image of corroded samples immersed in pH 1 solution clearly shows pores on the surface and in pH 13 solution, and the corrosion layer seems more compact and homogenous and not porous.

Keywords: Al-Si alloy, corrosion, pH, resistivity, SEM.

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Authors: Josef Fládr, Jiří Němeček, Veronika Koudelková, Petr Bílý

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Mechanical parameters of cementitious composites differ quite significantly based on the composition of cement matrix. They are also influenced by mixing times and procedure. The research presented in this paper was aimed at identification of differences in microstructure of normal strength (NSC) and differently mixed high strength (HSC) cementitious composites. Scanning electron microscopy (SEM) investigation together with energy dispersive X-ray spectroscopy (EDX) phase analysis of NSC and HSC samples was conducted. Evaluation of interfacial transition zone (ITZ) between the aggregate and cement matrix was performed. Volume share, thickness, porosity and composition of ITZ were studied. In case of HSC, samples obtained by several different mixing procedures were compared in order to find the most suitable procedure. In case of NSC, ITZ was identified around 40-50% of aggregate grains and its thickness typically ranged between 10 and 40 µm. Higher porosity and lower share of clinker was observed in this area as a result of increased water-to-cement ratio (w/c) and the lack of fine particles improving the grading curve of the aggregate. Typical ITZ with lower content of Ca was observed only in one HSC sample, where it was developed around less than 15% of aggregate grains. The typical thickness of ITZ in this sample was similar to ITZ in NSC (between 5 and 40 µm). In the remaining four HSC samples, no ITZ was observed. In general, the share of ITZ in HSC samples was found to be significantly smaller than in NSC samples. As ITZ is the weakest part of the material, this result explains to large extent the improved mechanical properties of HSC compared to NSC. Based on the comparison of characteristics of ITZ in HSC samples prepared by different mixing procedures, the most suitable mixing procedure from the point of view of properties of ITZ was identified.

Keywords: Energy dispersive X-ray spectroscopy, high strength concrete, interfacial transition zone, mixing procedure, normal strength concrete, scanning electron microscopy.

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Authors: N. Nowzari-Dalini, S. Sabbaghi

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Phenol is a hazardous material found in many industrial wastewaters. Photocatalytic degradation and furthermore catalyst doping are promising techniques in purpose of effective phenol removal, which have been studied comprehensively in this decade. In this study, Fe, Cr codoped TiO₂ were prepared by sol-gel method, and its photocatalytic activity was investigated through degradation of phenol under visible light. The catalyst was characterized by XRD, SEM, FT-IR, BET, and EDX. The results showed that nanoparticles possess anatase phase, and the average size of nanoparticles was about 21 nm. Also, photocatalyst has significant surface area. Effect of experimental parameters such as pH, irradiation time, pollutant concentration, and catalyst concentration were investigated by using Design-Expert^® software. 98% of phenol degradation was achieved after 6h of irradiation.

Keywords: Wastewater, doping, metals, sol-gel, titanium dioxide.

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Authors: Gopalu Karunakaran, Matheswaran Jagathambal, Nguyen Van Minh, Evgeny Kolesnikov, Denis Kuznetsov

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This work investigated the use of Beijerinckia indica extracellular extract for the synthesis of silver nanoparticles using AgNO₃. The formation of nanoparticles was confirmed by different methods, such as UV-Vis absorption spectroscopy, XRD, FTIR, EDX, and TEM analysis. The formation of silver nanoparticles (AgNPs) was confirmed by the change in color from light yellow to dark brown. The absorbance peak obtained at 430 nm confirmed the presence of silver nanoparticles. The XRD analysis showed the cubic crystalline phase of the synthesized nanoparticles. FTIR revealed the presence of groups that acts as stabilizing and reducing agents for silver nanoparticles formation. The synthesized silver nanoparticles were generally found to be spherical in shape with size ranging from 5 to 20 nm, as evident by TEM analysis. These nanoparticles were found to inhibit pathogenic bacterial strains. This work proved that the bacterial extract is a potential eco-friendly candidate for the synthesis of silver nanoparticles with promising antibacterial and antioxidant properties. 

Keywords: Antioxidant activity, antimicrobial activity, Beijerinckia indica, characterisation, extracellular extracts, silver nanoparticles.

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Authors: Merve Küçük, M. Lütfi Öveçoğlu

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Zinc oxide particles were synthesized using the sol-gel method and dip coated on polyester fabric. X-ray diffraction (XRD) analysis revealed a single crystal phase of ZnO particles. Chemical characteristics of the polyester fabric surface were investigated using attenuated total reflection-Fourier transform infrared (ATR-FTIR) measurements. Morphology of ZnO coated fabric was analyzed using field emission scanning electron microscopy (FESEM). After particle analysis, the aqueous ZnO solution resulted in a narrow size distribution at submicron levels. The deposit of ZnO on polyester fabrics yielded a homogeneous spread of spherical particles. Energy dispersive X-ray spectroscopy (EDX) results also affirmed the presence of ZnO particles on the polyester fabrics.

Keywords: Dip coating, polyester fabrics, sol-gel, zinc oxide.

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Authors: G. Çelik Gül, F. Kurtuluş

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Rare earths containing complex metal oxides have drawn much attention due to physical, chemical and optical properties which make them feasible in so many areas such as non-linear optical materials and ion exchanger. We have researched a systematic study to obtain rare earth containing zirconium molybdate compound, characterization, investigation of crystal system and calculation of unit cell parameters.  After a successful synthesis of Nd₂Zr₃(MoO₄)₉ which is a member of rare earth metal containing complex oxides family, X-ray diffraction (XRD), High Score Plus/Rietveld refinement analysis, and Fourier Transform Infrared Spectroscopy (FTIR) were completed to determine the crystal structure. Morphological properties and elemental composition were determined by scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) analysis. Thermal properties were observed via Thermogravimetric-differential thermal analysis (TG/DTA).

Keywords: Nd2Zr3(MoO4)9, solid state synthesis, powder x-ray diffraction, zirconium molybdates.

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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: Asma Perveen, M. P. Jahan

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Ni alloys have managed to cover wide range of applications such as automotive industries, oil gas industries, and aerospace industries. However, these alloys impose challenges while using conventional machining technologies. On the other hand, Micro-Electro-Discharge machining (micro-EDM) is a non-conventional machining method that uses controlled sparks energy to remove material irrespective of the materials hardness. There has been always a huge interest from the industries for developing optimum methodology and parameters in order to enhance the productivity of micro-EDM in terms of reducing machining time and tool wear for different alloys. Therefore, the aims of this study are to investigate the effects of the micro-EDM process parameters, in order to find their optimal values. The input process parameters include voltage, capacitance, and electrode rotational speed, whereas the output parameters considered are machining time, entrance diameter of hole, overcut, tool wear, and crater size. The surface morphology and element characterization are also investigated with the use of SEM and EDX analysis. The experimental result indicates the reduction of machining time with the increment of discharge energy. Discharge energy also contributes to the enlargement of entrance diameter as well as overcut. In addition, tool wears show reduction with the increase of discharge energy. Moreover, crater size is found to be increased in size along with the increment of discharge energy.

Keywords: Micro EDM, Ni alloy, discharge energy, micro-holes.

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Authors: Asım Egitmen, Aysen Demir, Burcu Darendeli, Fatma Ulusal, Bilgehan Güzel

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Synthesizing supercritical carbon dioxide (scCO₂) soluble precursors would be helpful for many processes of material syntheses based on scCO₂. Ligand (amphi-(1Z, 2Z)-N-(2-fluoro-3-(trifluoromethyl) phenyl)-N'-hydroxy-2-(hydroxyimino) were synthesized from chloro glyoxime and flourus aniline and Pd(II) complex (precursor) prepared. For scCO₂ deposition method, organometallic precursor was dissolved in scCO₂ and impregnated onto the SBA-15 at 90 °C and 3000 psi. Then the organometallic precursor was reduced with H₂ in the CO₂ mixture (150 psi H₂ + 2850 psi CO₂). Pd deposited support material was characterized by ICP-OES, XRD, FE-SEM, TEM and EDX analyses. The Pd loading of the prepared catalyst, measured by ICP-OES showed a value of about 1.64% mol/g Pd of catalyst. Average particle size was found 5.3 nm. The catalytic activity of prepared catalyst was investigated over Suzuki-Miyaura C-C coupling reaction in different solvent with K₂CO₃ at 50 ^oC. The conversion ratio was determined by gas chromatography.

Keywords: Nanoparticle, nanotube, oximes, precursor, supercritical CO2.

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Authors: P. Acosta-Santamaría, A. Ibatá-Soto, A. López-Vásquez

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Organic compounds in wastewaters coming from textile and pharmaceutical industry generated multiple harmful effects on the environment and the human health. One of them is the methyl orange (MeO), an azoic dye considered to be a recalcitrant compound. The heterogeneous photocatalysis emerges as an alternative for treating this type of hazardous compounds, through the generation of OH radicals using radiation and a semiconductor oxide. According to the author’s knowledge, catalysts such as TiO₂ doped with metals show high efficiency in degrading MeO; however, this presents economic limitations on industrial scale. Black sand can be considered as a naturally doped catalyst because in its structure is common to find compounds such as titanium, iron and aluminum oxides, also elements such as zircon, cadmium, manganese, etc. This study reports the photocatalytic activity of the mineral black sand used as semiconductor in the discoloration of MeO by oxidation and reduction photocatalytic techniques. For this, magnetic composites from the mineral were prepared (RM, M1, M2 and NM) and their activity were tested through MeO discoloration while TiO₂ was used as reference. For the fractions, chemical, morphological and structural characterizations were performed using Scanning Electron Microscopy with Energy Dispersive X-Ray (SEM-EDX), X-Ray Diffraction (XRD) and X-Ray Fluorescence (XRF) analysis. M2 fraction showed higher MeO discoloration (93%) in oxidation conditions at pH 2 and it could be due to the presence of ferric oxides. However, the best result to reduction process was using M1 fraction (20%) at pH 2, which contains a higher titanium percentage. In the first process, hydrogen peroxide (H₂O₂) was used as electron donor agent. According to the results, black sand mineral can be used as natural semiconductor in photocatalytic process. It could be considered as a photocatalyst precursor in such processes, due to its low cost and easy access.

Keywords: Black sand mineral, methyl orange, oxidation, photocatalysis, reduction.

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Authors: Chanchal Biswas, Anrin Bhattacharyya, Gopes Chandra Das, Mahua Ghosh Chaudhuri, Rajib Dey

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Boiler coals with low fixed carbon and higher ash content have always challenged the metallurgists to develop a suitable method for their utilization. In the present study, an attempt is made to establish an energy effective method for the reduction of iron ore fines in the form of nuggets by using ‘Syngas’. By devolatisation (expulsion of volatile matter by applying heat) of boiler coal, gaseous product (enriched with reducing agents like CO, CO2, H2, and CH4 gases) is generated. Iron ore nuggets are reduced by this syngas. For that reason, there is no direct contact between iron ore nuggets and coal ash. It helps to control the minimization of the sulphur intake of the reduced nuggets. A laboratory scale devolatisation furnace designed with reduction facility is evaluated after in-depth studies and exhaustive experimentations including thermo-gravimetric (TG-DTA) analysis to find out the volatile fraction present in boiler grade coal, gas chromatography (GC) to find out syngas composition in different temperature and furnace temperature gradient measurements to minimize the furnace cost by applying one heating coil. The nuggets are reduced in the devolatisation furnace at three different temperatures and three different times. The pre-reduced nuggets are subjected to analytical weight loss calculations to evaluate the extent of reduction. The phase and surface morphology analysis of pre-reduced samples are characterized using X-ray diffractometry (XRD), energy dispersive x-ray spectrometry (EDX), scanning electron microscopy (SEM), carbon sulphur analyzer and chemical analysis method. Degree of metallization of the reduced nuggets is 78.9% by using boiler grade coal. The pre-reduced nuggets with lesser sulphur content could be used in the blast furnace as raw materials or coolant which would reduce the high quality of coke rate of the furnace due to its pre-reduced character. These can be used in Basic Oxygen Furnace (BOF) as coolant also.

Keywords: Alternative ironmaking, coal devolatisation, extent of reduction, nugget making, syngas based DRI, solid state reduction.

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Authors: K. F. Khan, Samsuddin Khan

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The Paleoproterozoic phosphorite deposit of Sallopat block of Banswara district of Rajasthan belongs to kalinjara formation of lunavada group of Aravalli Super Group. The phosphorites are found to occur as massive, brecciated, laminated and stromatolitic associated with calcareous quartzite, interbedded dolomite and multi coloured chert. The phosphorites are showing alternate brown and grey coloured concentric rims which are composed of phosphate, calcite and quartz minerals. Petro-mineralogical studies of phosphorite samples using petrological microscope, XRD, FEG- SEM and EDX reveal that apatite-(CaF) and apatite-(CaOH) are phosphate minerals which are intermixed with minor amount of carbonate materials. Sporadic findings of the uniform tiny granules of partially anisotropic apatite-(CaF) along with dolomite, calcite, quartz, muscovite, zeolite and other gangue minerals have been observed with the replacement of phosphate material by quartz and carbonate. The presence of microbial filaments of organic matter and alternate concentric rims of stromatolitic structure may suggest that the deposition of the phosphate took place in shallow marine oxidizing environmental conditions leading to the formation of phosphorite layers as primary biogenic precipitates by bacterial or algal activities. Different forms and texture of phosphate minerals may be due to environmental vicissitudes at the time of deposition followed by some replacement processes and biogenic activities.

Keywords: Petro-mineralogy, phosphorites, sallopat, apatite.

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Authors: Adewale O. Adegbenjo, Elsie Nsiah-Baafi, Mxolisi B. Shongwe, Mercy Ramakokovhu, Peter A. Olubambi

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The sintering step in powder metallurgy (P/M) processes is very sensitive as it determines to a large extent the properties of the final component produced. Spark plasma sintering over the past decade has been extensively used in consolidating a wide range of materials including metallic alloy powders. This novel, non-conventional sintering method has proven to be advantageous offering full densification of materials, high heating rates, low sintering temperatures, and short sintering cycles over conventional sintering methods. Ti6Al4V has been adjudged the most widely used α+β alloy due to its impressive mechanical performance in service environments, especially in the aerospace and automobile industries being a light metal alloy with the capacity for fuel efficiency needed in these industries. The P/M route has been a promising method for the fabrication of parts made from Ti6Al4V alloy due to its cost and material loss reductions and the ability to produce near net and intricate shapes. However, the use of this alloy has been largely limited owing to its relatively poor hardness and wear properties. The effect of sintering temperature on the densification, hardness, and wear behaviors of spark plasma sintered Ti6Al4V powders was investigated in this present study. Sintering of the alloy powders was performed in the 650–850°C temperature range at a constant heating rate, applied pressure and holding time of 100°C/min, 50 MPa and 5 min, respectively. Density measurements were carried out according to Archimedes’ principle and microhardness tests were performed on sectioned as-polished surfaces at a load of 100gf and dwell time of 15 s. Dry sliding wear tests were performed at varied sliding loads of 5, 15, 25 and 35 N using the ball-on-disc tribometer configuration with WC as the counterface material. Microstructural characterization of the sintered samples and wear tracks were carried out using SEM and EDX techniques. The density and hardness characteristics of sintered samples increased with increasing sintering temperature. Near full densification (99.6% of the theoretical density) and Vickers’ micro-indentation hardness of 360 HV were attained at 850°C. The coefficient of friction (COF) and wear depth improved significantly with increased sintering temperature under all the loading conditions examined, except at 25 N indicating better mechanical properties at high sintering temperatures. Worn surface analyses showed the wear mechanism was a synergy of adhesive and abrasive wears, although the former was prevalent.

Keywords: Hardness, powder metallurgy, Spark plasma sintering, wear.

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Authors: G. Wagner, R. Herrmann

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Cytotoxic platinum compounds play a major role in the chemotherapy of a large number of human cancers. However, due to the severe side effects for the patient and other problems associated with their use, there is a need for the development of more efficient drugs and new methods for their selective delivery to the tumours. One way to achieve the latter could be in the use of nanoparticular substrates that can adsorb or chemically bind the drug. In the cell, the drug is supposed to be slowly released, either by physical desorption or by dissolution of the particle framework. Ideally, the cytotoxic properties of the platinum drug unfold only then, in the cancer cell and over a longer period of time due to the gradual release. In this paper, we report on our first steps in this direction. The binding properties of a series of cytotoxic Pt(II) oxadiazoline compounds to mesoporous silica particles has been studied by NMR and UV/vis spectroscopy. High loadings were achieved when the Pt(II) compound was relatively polar, and has been dissolved in a relatively nonpolar solvent before the silica was added. Typically, 6-10 hours were required for complete equilibration, suggesting the adsorption did not only occur to the outer surface but also to the interior of the pores. The untreated and Pt(II) loaded particles were characterised by C, H, N combustion analysis, BET/BJH nitrogen sorption, electron microscopy (REM and TEM) and EDX. With the latter methods we were able to demonstrate the homogenous distribution of the Pt(II) compound on and in the silica particles, and no Pt(II) bulk precipitate had formed. The in vitro cytotoxicity in a human cancer cell line (HeLa) has been determined for one of the new platinum compounds adsorbed to mesoporous silica particles of different size, and compared with the corresponding compound in solution. The IC50 data are similar in all cases, suggesting that the release of the Pt(II) compound was relatively fast and possibly occurred before the particles reached the cells. Overall, the platinum drug is chemically stable on silica and retained its activity upon prolonged storage.

Keywords: Cytotoxicity, mesoporous silica, nanoparticles platinum compounds.

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Authors: I. Siti Rabiatull Aisha, A. Ourdjini, O. Saliza Azlina

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The aim of this paper is to study the effectiveness of bismuth addition in the solder alloy to retard the intermetallic compound formation and growth. In this study, three categories of solders such as Sn-4Ag-xCu (x = 0.5, 0.7, 1.0) and Sn-4Ag-0.5Cu-xBi (x = 0.1, 0.2, 0.4) were used. Ni/Au surface finish substrates were dipped into the molten solder at a temperature of 180-190 ^oC and allowed to cool at room temperature. The intermetallic compound (IMCs) were subjected to the characterization in terms of composition and morphology. The IMC phases were identified by energy dispersive x-ray (EDX), whereas the optical microscope and scanning electron microscopy (SEM) were used to observe microstructure evolution of the solder joint. The results clearly showed that copper concentration dependency was high during the reflow stage. Besides, only Ni₃Sn₄ and Ni₃Sn₂ were detected for all copper concentrations. The addition of Bi was found to have no significant effect on the type of IMCs formed, but yet the grain became further refined.

Keywords: Bismuth addition, intermetallic compound, composition, morphology.

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Authors: Rana Th. A. Al-Rubaye

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A novel chromium-free protective coating films based on a zeolite coating was growing onto a FeCrAlloy metal using in – situ hydrothermal method. The zeolite film was obtained using in-situ crystallization process that is capable of coating large surfaces with complex shape and in confined spaces has been developed. The zeolite coating offers an advantage of a high mechanical stability and thermal stability. The physicochemical properties were investigated using X-ray diffraction (XRD), Electron Microscopy (SEM), Energy Dispersive X–ray Analysis (EDX) and Thermogravimetric Analysis (TGA). The transition from oxide-on-alloy wires to hydrothermally synthesised uniformly zeolite coated surfaces was followed using SEM and XRD. In addition, the robustness of the prepared coating was confirmed by subjecting these to thermal cycling (ambient to 550oC).

Keywords: FeCrAlloy, Zeolite ZSM-5. Zeolite coating.

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Authors: Savvas Varitis, Panagiotis Kavouras, George Vourlias, Eleni Pavlidou, Theodoros Karakostas, Philomela Komninou

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A chromium-loaded ash originating from incineration of tannery sludge under anoxic conditions was mixed with low grade soda-lime glass powder coming from commercial glass bottles. The relative weight proportions of ash over glass powder tested were 30/70, 40/60 and 50/50. The solid mixtures, formed in green state compacts, were sintered at the temperature range of 800o C up to 1200o C. The resulting products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (EDXS) and micro-indentation. The above methods were employed to characterize the various phases, microstructure and hardness of the produced materials. Thermal treatment at 800o C and 1000o C produced opaque ceramic products composed of a variety of chromium-containing and chromium-free crystalline phases. Thermal treatment at 1200o C gave rise to composite products, where only chromium-containing crystalline phases were detected. Hardness results suggest that specific products are serious candidates for structural applications.

Keywords: Chromium-rich tannery residues, glass-ceramic materials, mechanical properties, microstructure

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Authors: Lenka Hurtalová, Eva Tillová, Mária Chalupová, Juraj Belan, Milan Uhríčik

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The secondary alloy A226 is used for many automotive casting produced by mould casting and high pressure die casting. This alloy has excellent castability, good mechanical properties and cost-effectiveness. Production of primary aluminium alloys belong to heavy source fouling of life environs. The European Union calls for the emission reduction and reduction in energy consumption therefore increase production of recycled (secondary) aluminium cast alloys. The contribution is deal with influence of recycling on the quality of the casting made from A226 in automotive industry. The properties of the casting made from secondary aluminium alloys were compared with the required properties of primary aluminium alloys. The effect of recycling on microstructure was observed using combination different analytical techniques (light microscopy upon black-white etching, scanning electron microscopy - SEM upon deep etching and energy dispersive X-ray analysis - EDX). These techniques were used for the identification of the various structure parameters, which was used to compare secondary alloy microstructure with primary alloy microstructure.

Keywords: A226 secondary aluminium alloy, deep etching, mechanical properties, recycling foundry aluminium alloy.

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Authors: Amira Shakila Razali, Faridah Lisa Supian, Muhammad Mat Salleh, Suraini Abu Bakar

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Water contamination by toxic compound is one of the serious environmental problems today. These toxic compounds mostly originated from industrial effluents, agriculture, natural sources and human waste. These studies focus on modification of multiwalled carbon nanotube (MWCNTs) with nanoparticle of calixarene and explore the possibility of using this modification for the remediation of cadmium in water. The nanocomposites were prepared by dissolving calixarene in chloroform solution as solvent, followed by additional multiwalled carbon nanotube (MWCNTs) then sonication process for 3 hour and fabricated the nanocomposites on substrate by spin coating method. Finally, the nanocomposites were tested on cadmium ion (10 mg/ml). The morphology of nanocomposites was investigated by FESEM showing the formation of calixarene on the outer walls of carbon nanotube and cadmium ion also clearly seen from the micrograph. This formation was supported by using energy dispersive x-ray (EDX). The presence of cadmium ions in the films, leads to some changes in the surface potential and Fourier Transform Infrared spectroscopy (FTIR).The nanocomposites MWCNTs-calixarene have potential for development of sensor for pollutant monitoring and nanoelectronics devices applications.

Keywords: Calixarene, Multiwalled Carbon Nanotubes, Cadmium, Surface Potential.

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Authors: Andreea Cârâc, Elena Moroşan, Ana Corina Ioniță, Rica Boscencu, Geta Cârâc

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Although, lanthanum carbonate has not been approved by the FDA for treatment of hyperphosphatemia, we prospectively evaluated the efficacy of the combination of Calcium hydroxyapatite (CHAp) and Lanthanum Carbonate (LaC) for the treatment of hyperphosphatemia on mice. CHAp was prepared by co-precipitation method using Ca(OH)2, H3PO4, NH4OH with calcination at 1200ºC. Lanthanum carbonate was prepared by chemical method using NaHCO3 and LaCl3 at low pH environment, below 4.0. The structures were characterized by FTIR spectra and SEM -EDX analysis. The study group included 16 subjects-mice divided into four groups according to the administered substance: lanthanum carbonate (group A), CHAp (group B), lanthanum carbonate + CHAp (group C) and salt water (group D). The results indicate a phosphate decrease when subjects (mice) were treated with CHAp and lanthanum carbonate (0.5% CMC), in a single dose of 1500 mg/kg. Serum phosphate concentration decreased [(from 4.5 ± 0.8 mg/dL) to 4.05 ± 0.2 mg/dL), P < 0.01] in group A and in group C (to 3.6 ± 0.2 mg/dL) at 12 hours from the administration. The combination of CHAp and lanthanum carbonate is a suitable regimen for hyperphosphatemia treatment because it avoids both the hypercalcemia of CaCO3 and the adverse effects of CHAp.

Keywords: Calcium hydroxyapatite, hyperphosphatemia, lanthanum carbonate, phosphatebinder, structures.

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Authors: Phuong T. Dang, Hy G. Le, Giang T. Pham, Hong T. M. Vu, Kien T, Nguyen, Canh D. Dao, Giang H. Le, Hoa T. K. Tran, Quang K. Nguyen, Tuan A. Vu

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Nanostructured catalysts were successfully prepared by acidification of diatomite and regeneration of FCC spent catalysts. The obtained samples were characterized by IR, XRD, SEM, EDX, MAS-NMR (27Al and 29Si), NH3-TPD and tested in catalytic pyrolysis of biomass (rice straw). The results showed that the similar bio-oil yield of 41.4% can be obtained by pyrolysis with catalysts at 450oC as compared to that of the pyrolysis without catalyst at 550oC. The bio-oil yield reached a maximum of 42.55% at the pyrolysis temperature of 500oC with catalytic content of 20%. Moreover, by catalytic pyrolysis, bio-oil quality was better as reflected in higher ratio of H/C, lower ratio of O/C. This clearly indicated high application potential of these new nanostructured catalysts in the production of bio-oil with low oxygenated compounds.

Keywords: Acidified diatomite, biomass, catalytic pyrolysis, bio-oil, nanostructured catalysts, regenerated FCC catalyst.

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Authors: A. Alshebani, Y. Swesi, S. Mrayed, F. Altaher

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This paper present some preliminary work on the preparation and physicochemical caracterization of nanocomposite MFI-alumina structures based on alumina hollow fibres. The fibers are manufactured by a wet spinning process. α-alumina particles were dispersed in a solution of polysulfone in NMP. The resulting slurry is pressed through the annular gap of a spinneret into a precipitation bath. The resulting green fibres are sintered. The mechanical strength of the alumina hollow fibres is determined by a three-point-bending test while the pore size is characterized by bubble-point testing. The bending strength is in the range of 110 MPa while the average pore size is 450 nm for an internal diameter of 1 mm and external diameter of 1.7 mm. To characterize the MFI membranes various techniques were used for physicochemical characterization of MFI–ceramic hollow fibres membranes: The nitrogen adsorption, X-ray diffractometry, scanning electron microscopy combined with X emission microanalysis. Scanning Electron Microscopy (SEM) and Energy Dispersive Microanalysis by the X-ray were used to observe the morphology of the hollow fibre membranes (thickness, infiltration into the carrier, defects, homogeneity). No surface film, has been obtained, as observed by SEM and EDX analysis and confirmed by high temperature variation of N2 and CO2 gas permeances before cation exchange. Local analysis and characterise (SEM and EDX) and overall (by ICP elemental analysis) were conducted on two samples exchanged to determine the quantity and distribution of the cation of cesium on the cross section fibre of the zeolite between the cavities.

Keywords: Physicochemical characterization of MFI, Ceramic hollow fibre, CO2, Ion-exchange.

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Authors: M. S. Kaiser, Swagata Dutta

Abstract:

In the present work, the effect of load and sliding distance on the performance tribology of commercially used aluminium-silicon engine block and piston was evaluated at ambient conditions with humidity of 80% under dry sliding conditions using a pin-on-disc with two different loads of 5N and 20N yielding applied pressure of 0.30MPa and 1.4MPa, respectively, at sliding velocity of 0.29ms-1 and with varying sliding distance ranging from 260m- 4200m. Factors and conditions that had significant effect were identified. The results showed that the load and the sliding distance affect the wear rate of the alloys and the wear rate increased with increasing load for both the alloys. Wear rate also increases almost linearly at low loads and increase to a maximum then attain a plateau with increasing sliding distance. For both applied loads the piston alloy showed the better performance due to higher Ni and Mg content. The worn surface and wear debris was characterized by optical microscope, SEM and EDX analyzer. The worn surface was characterized by surface with shallow grooves at loads while the groove width and depth increased as the loads increases. Oxidative wear was found to be the predominant mechanisms in the dry sliding of Al-Si alloys at low loads.

Keywords: Wear, friction, gravimetric analysis, aluminiumsilicon alloys, SEM, EDX.

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Authors: Hong Seung Kim, Chang Hoi Kim, Lili Yue

Abstract:

Single-phase, high band gap energy Zn_0.5Mg_0.5O films were grown under oxygen pressure, using pulse laser deposition with a Zn_0.5Mg_0.5O target. Structural characterization studies revealed that the crystal structures of the Zn_X-1Mg_XO films could be controlled via changes in the oxygen pressure. TEM analysis showed that the thickness of the deposited Zn_1-xMg_xO thin films was 50–75 nm. As the oxygen pressure increased, we found that one axis of the crystals did not show a very significant increase in the crystallization compared with that observed at low oxygen pressure. The X-ray diffraction peak intensity for the hexagonal-ZnMgO (002) plane increased relative to that for the cubic-ZnMgO (111) plane. The corresponding c-axis of the h-ZnMgO lattice constant increased from 5.141 to 5.148 Å, and the a-axis of the c-ZnMgO lattice constant decreased from 4.255 to 4.250 Å. EDX analysis showed that the Mg content in the mixed-phase ZnMgO films decreased significantly, from 54.25 to 46.96 at.%. As the oxygen pressure was increased from 100 to 150 mTorr, the absorption edge red-shifted from 3.96 to 3.81 eV; however, a film grown at the highest oxygen pressure tested here (200 mTorr).

Keywords: MgO, UV LED, ZnMgO, ZnO.

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Authors: M. I. Aida Isma, Azni Idris, Rozita Omar, A. R. Putri Razreena

Abstract:

40L of hollow fiber membrane bioreactor with solids retention times (SRT) of 30, 15 and 4 days were setup for treating synthetic wastewater at hydraulic retention times (HRT) of 12, 8 and 4 hours. The objectives of the study were to investigate the effects of SRT and HRT on membrane fouling. A comparative analysis was carried out for physiochemical quality parameters (turbidity, suspended solids, COD, NH₃-N and PO₄^3-). Scanning electron microscopy (SEM), energy diffusive X-ray (EDX) analyzer and particle size distribution (PSD) were used to characterize the membrane fouling properties. The influence of SRT on the quality of effluent, activated sludge quality, and membrane fouling were also correlated. Lower membrane fouling and slower rise in trans-membrane pressure (TMP) were noticed at the longest SRT and HRT of 30d and 12h, respectively. Increasing SRT results in noticeable reduction of dissolved organic matters. The best removal efficiencies of COD, TSS, NH₃-N and PO₄^3- were 93%, 98%, 80% and 30% respectively. The high HRT with shorter SRT induced faster fouling rate. The main fouling resistance was cake layer. The most severe membrane fouling was observed at SRT and HRT of 4 and 12, respectively with thickness cake layer of 17mm as reflected by higher TMP, lower effluent removal and thick sludge cake layer.

 

Keywords: Membrane bioreactor, SRT, HRT, membrane fouling.

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Authors: Rana Th. A. Al-Rubaye, Arthur A. Garforth

Abstract:

This work details the generation of thin films of structured zeolite catalysts (ZSM–5 and Y) onto the surface of a metal substrate (FeCrAlloy) using in-situ hydrothermal synthesis. In addition, the zeolite Y is post-synthetically modified by acidified ammonium ion exchange to generate US-Y. Finally the catalytic activity of the structured ZSM-5 catalyst films (Si/Al = 11, thickness 146 0m) and structured US–Y catalyst film (Si/Al = 8, thickness 230m) were compared with the pelleted powder form of ZSM–5 and USY catalysts of similar Si/Al ratios. The structured catalyst films have been characterised using a range of techniques, including X-ray diffraction (XRD), Electron microscopy (SEM), Energy Dispersive X–ray analysis (EDX) and Thermogravimetric Analysis (TGA). The transition from oxide-onalloy wires to hydrothermally synthesised uniformly zeolite coated surfaces was followed using SEM and XRD. In addition, the robustness of the prepared coating was confirmed by subjecting these to thermal cycling (ambient to 550oC). The cracking of n–heptane over the pellets and structured catalysts for both ZSM–5 and Y zeolite showed very similar product selectivities for similar amounts of catalyst with an apparent activation energy of around 60 kJ mol-1. This paper demonstrates that structured catalysts can be manufactured with excellent zeolite adherence and when suitably activated/modified give comparable cracking results to the pelleted powder forms. These structured catalysts will improve temperature distribution in highly exothermic and endothermic catalysed processes.

Keywords: FeCrAlloy, Structured catalyst, and Zeolite Y, Zeolite ZSM-5.

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Authors: A. M. Metak, T. T. Ajaal

Abstract:

Commercial nanocomposite food packaging type nano-silver containers were characterised using scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX). The presence of nanoparticles consistent with the incorporation of 1% nano-silver (Ag) and 0.1% titanium dioxide (TiO₂) nanoparticle into polymeric materials formed into food containers was confirmed. Both nanomaterials used in this type of packaging appear to be embedded in a layered configuration within the bulk polymer. The dimensions of the incorporated nanoparticles were investigated using X-ray diffraction (XRD) and determined by calculation using the Scherrer Formula; these were consistent with Ag and TiO₂ nanoparticles in the size range 20-70nm both were spherical shape nanoparticles. Antimicrobial assessment of the nanocomposite container has also been performed and the results confirm the antimicrobial activity of Ag and TiO₂ nanoparticles in food packaging containers. Migration assessments were performed in a wide range of food matrices to determine the migration of nanoparticles from the packages. The analysis was based upon the relevant European safety Directives and involved the application of inductively coupled plasma mass spectrometry (ICP-MS) to identify the range of migration risk. The data pertain to insignificance levels of migration of Ag and TiO₂ nanoparticles into the selected food matrices.

Keywords: Nano-silver, antimicrobial food packaging, migration, titanium dioxide.

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Authors: B. A. Berns, V. Romanovicz, M. M. de Camargo Forte, D. E. O. S. Carpenter

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The Proton Exchange Membranes (PEM) are largely studied because they operate at low temperatures and they are suitable for mobile applications. However, there are some deficiencies in their operation, mainly those that use ethanol as a hydrogen source, that require a certain attention. Therefore, this research aimed to develop Nafion® composite membranes, mixing clay minerals, kaolin and halloysite to the polymer matrix in order to improve the ethanol molecule retentions and, at the same time, to keep the system’s protonic conductivity. The modified Nafion/Kaolin, Nafion/Halloysite composite membranes were prepared in weight proportion of 0.5, 1.0 and 1.5. The membranes obtained were characterized as to their ethanol permeability, protonic conductivity and water absorption. The composite morphology and structure are characterized by SEM and EDX and the thermal behavior is determined by TGA and DSC. The analysis of the results shows ethanol permeability reduction from 48% to 63%. However, the protonic conductivity results are lower in relation to pure Nafion®. As to the thermal behavior, the Nafion® composite membranes were stable up to a temperature of 325ºC.

Keywords: Polymer-matrix composites (PMCs), Thermal properties, Nanoclay, Differential scanning calorimetry.

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Authors: M. Areekijseree, M. Pumipaiboon, S. Nuamsukon, K. Kittiwattanawong, C. Thongchai, S. Sikiwat, T. Chuen-Im

Abstract:

There are few studies on eggshell of leatherback turtle which is endangered species in Thailand. This study was focusing on the ultrastructure and elemental composition of leatherback turtle eggshells collected from Andaman Sea Shore, Thailand during the nesting season using scanning electron microscope (SEM). Three eggshell layers of leatherback turtle; the outer cuticle layer or calcareous layer, the middle layer or middle multistrata layer and the inner fibrous layer were recognized. The outer calcareous layer was thick and porosity which consisted of loose nodular units of various crystal shapes and sizes. The loose attachment between these units resulted in numerous spaces and openings. The middle layer was compact thick with several multistrata and contained numerous openings connecting to both outer cuticle layer and inner fibrous layer. The inner fibrous layer was compact and thin, and composed of numerous reticular fibers. Energy dispersive X-ray microanalysis detector revealed energy spectrum of X-rays character emitted from all elements on each layer. The percentages of all elements were found in the following order: carbon (C) > oxygen (O) > calcium (Ca) > sulfur (S) > potassium (K) > aluminum (Al) > iodine (I) > silicon (Si) > chlorine (Cl) > sodium (Na) > fluorine (F) > phosphorus (P) > magnesium (Mg). Each layer consisted of high percentage of CaCO3 (approximately 98%) implying that it was essential for turtle embryonic development. A significant difference was found in the percentages of Ca and Mo in the 3layers. Moreover, transition metal, metal and toxic non-metal contaminations were found in leatherback turtle eggshell samples. These were palladium (Pd), molybdenum (Mo), copper (Cu), aluminum (Al), lead (Pb), and bromine (Br). The contamination elements were seen in the outer layers except for Mo. All elements were readily observed and mapped using Smiling program. X-ray images which mapped the location of all elements were showed. Calcium containing in the eggshell appeared in high contents and was widely distributing in clusters of the outer cuticle layer to form CaCO3 structure. Moreover, the accumulation of Na and Cl was observed to form NaCl which was widely distributing in 3 eggshell layers. The results from this study would be valuable on assessing the emergent success in this endangered species.

Keywords: Leatherback turtle (Dermochelys coriacea), SEM (SEI/EDX), turtle eggshell.

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