Search results for: Diffraction grating

Authors: S. Guettala, B. Mezghiche

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In this paper, the effect of addition the dune sand powder (DSP) on development of compressive strength and hydration of cement pastes was investigated as a function of water/binder ratio, was varied, on the one hand, the percentage of DSP and on the other, the fineness of DSP. In order to understand better the pozzolanic effect of dune sand powder in cement pastes, we followed the mixtures hydration (50% Pure Lime + 50% DSP) by X-ray diffraction. These mixtures the pastes present a hydraulic setting which is due to the formation of a C-S-H phase (calcium silicate hydrate). The latter is semi-crystallized. This study is a simplified approach to that of the mixtures (80% ordinary Portland cement + 20% DSP), in which the main reaction is the fixing of the lime coming from the cement hydration in the presence of DSP, to form calcium silicate hydrate semi-crystallized of second generation. The results proved that up to (20% DSP) as Portland cement replacement could be used with a fineness of 4000 cm²/g without affecting adversely the compressive strength. After 28 days, the compressive strength at 5, 10 and 15% DSP is superior to Portland cement, with an optimum effect for a percentage of the order of 5% to 10% irrespective of the w/b ratio and fineness of DSP.

Keywords: Ordinary Portland Cement, Pure Lime, Dune Sand Powder, Compressive Strength, Hydration.

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Authors: Z. Abdolldhi, A. A. Ziaee M., A. Afshar

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In this paper the combination of thermal oxidation and electrochemical anodizing processes is used to produce titanium oxide layers. The response of titanium alloy Ti6Al4V to oxidation processes at various temperatures and electrochemical anodizing in various voltages are investigated. Scanning electron microscopy (SEM); X-Ray Diffraction (XRD) and porosity determination have been used to characterize the oxide layer thickness, surface morphology, oxide layer-substrate adhesion and porosity. In the first experiment, samples modified by thermal oxidation process then followed by electrochemical anodizing. Second experiment consists of surfaces modified by electrochemical anodizing process and then followed by thermal oxidation. The first method shows better properties than other one. In second experiment, Surfaces modified were achieved by thicker and more adherent thick oxide layers on titanium surface. The existence of an electrochemical anodized oxide layer did not improve the adhesion of thermal oxide layer. The high temperature, thermal formation of an oxide layer leads to a coarse oxide grain morphology and a complete oxidative particle. In addition, in high temperature oxidation porosity content is increased. The oxide layer of thermal oxidation and electrochemical anodizing processes; on Ti–6Al–4V substrate was covered with different colored oxide layers.

Keywords: Electrochemically anodizing, Porosity, Thermaloxidation, Ti6Al4 alloy.

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Authors: D.N Awang Sh'ri, E. Hamzah

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The deposition of diamond films on a Si3N4 substrate is an attractive technique for industrial applications because of the excellent properties of diamond. Pretreatment of substrate is very important prior to diamond deposition to promote nucleation and adhesion between coating and substrate. Deposition of nanocrystalline diamonds films on silicon nitride substrate have been carried out by HF-CVD technique using mixture of methane and hydrogen gases. Different pretreatment of substrate including chemical etching consists of hot acid etching and basic etching and mechanical etching were used to study the quality of diamond formed on the substrate. The structure and morphology of diamond coating have been studied using X-ray Diffraction (XRD) and Scanning Electron Microscope (SEM) while diamond film quality has been characterized using Raman spectroscopy. AFM was used to investigate the effect of chemical etching and mechanical pretreatment on the surface roughness of the substrates and the resultant morphology of nanocrystalline diamond. It was found that diamond film deposited on as-received, basic etched and grinded substrate shows the morphology of cauliflower while blasted and acidic etched substrates produce smooth, continuous diamond film. However, the Raman investigation did not show any deviation in quality of diamond film for any pretreatment.

Keywords: Nanocrystalline diamond, Chemical VaporDeposition, Pretreatment, Silicon Nitride

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Authors: Martin Klaumünzer, Jakob Hübner, Denis Spitzer

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Within this paper, latest results on processing of energetic nanomaterials by means of the Spray Flash Evaporation technique are presented. This technology constitutes a highly effective and continuous way to prepare fascinating materials on the nano- and micro-scale. Within the process, a solution is set under high pressure and sprayed into an evacuated atomization chamber. Subsequent ultrafast evaporation of the solvent leads to an aerosol stream, which is separated by cyclones or filters. No drying gas is required, so the present technique should not be confused with spray dying. Resulting nanothermites, insensitive explosives or propellants and compositions are foreseen to replace toxic (according to REACH) and very sensitive matter in military and civil applications. Diverse examples are given in detail: nano-RDX (n-Cyclotrimethylentrinitramin) and nano-aluminum based systems, mixtures (n-RDX/n-TNT - trinitrotoluene) or even cocrystalline matter like n-CL-20/HMX (Hexanitrohexaazaisowurtzitane/ Cyclotetra-methylentetranitramin). These nanomaterials show reduced sensitivity by trend without losing effectiveness and performance. An analytical study for material characterization was performed by using Atomic Force Microscopy, X-Ray Diffraction, and combined techniques as well as spectroscopic methods. As a matter of course, sensitivity tests regarding electrostatic discharge, impact, and friction are provided.

Keywords: Continuous synthesis, energetic material, nanoscale, nanothermite, nanoexplosive.

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Authors: Seyed Mohammad Hosseini, Amirhossein Moghanian

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The main purpose of this research was to design a biomimetic system by freeze-drying method for evaluating the effect of adding 5 and 10 mol. % of zinc (Zn) in 58S bioactive glass and gelatin (5ZnBG/G and 10ZnBG/G) in terms of structural and biological changes. The structural analyses of samples were performed by X-Ray Diffraction (XRD), scanning electron microscopy (SEM) and Fourier-transform infrared (FTIR) spectroscopy. Also, 3-(4,5dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) and alkaline phosphatase (ALP) activity tests were carried out for investigation of MC3T3-E1 cell behaviors. The SEM results demonstrated the spherical shape of the formed hydroxyapatite (HA) phases and also HA characteristic peaks were detected by XRD spectroscopy after 3 days of immersion in the simulated body fluid (SBF) solution. Meanwhile, FTIR spectra proved that the intensity of P–O peaks for 5ZnBG/G was more than 10ZnBG/G and control samples. Moreover, the results of ALP activity test illustrated that the optimal amount of Zn (5ZnBG/G) caused a considerable enhancement in bone cell growth. Taken together, the scaffold with 5 mol.% Zn was introduced as an optimal sample because of its higher biocompatibility, in vitro bioactivity and growth of MC3T3-E1 cells in comparison with other samples in bone tissue engineering.

Keywords: Scaffold, gelatin, modified bioactive glass, ALP, bone tissue engineering.

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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: Chun-Ying Lee, Kuan-Hui Cheng, Mei-Wen Wu

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The nickel-manganese (Ni-Mn) alloy coating prepared from DC electrodeposition process in sulphamate bath was studied. The effects of process parameters, such as current density and electrolyte composition, on the cathodic current efficiency, microstructure, internal stress and mechanical properties were investigated. Because of its crucial effect on the application to the electroforming of microelectronic components, the development of low internal stress coating with high leveling power was emphasized. It was found that both the coating’s manganese content and the cathodic current efficiency increased with the raise in current density. In addition, the internal stress of the deposited coating showed compressive nature at low current densities while changed to tensile one at higher current densities. Moreover, the metallographic observation, X-ray diffraction measurement, and polarization curve measurement were conducted. It was found that the Ni-Mn coating consisted of nano-sized columnar grains and the maximum hardness of the coating was associated with (111) preferred orientation in the microstructure. The grain size was refined along with the increase in the manganese content of the coating, which accordingly, raised its hardness and resistance to annealing softening. In summary, the Ni-Mn coating prepared at lower current density of 1-2 A/dm2 had low internal stress, high leveling power, and better corrosion resistance.

Keywords: DC plating, internal stress, leveling power, Ni-Mn coating.

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Authors: Hoda Aleali, Nastaran Mansour, Maryam Mirzaie

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In this paper, we study the optical nonlinearities of Silver sulfide (Ag2S) nanostructures dispersed in the Dimethyl sulfoxide (DMSO) under exposure to 532 nm, 15 nanosecond (ns) pulsed laser irradiation. Ultraviolet–visible absorption spectrometry (UV-Vis), X-ray diffraction (XRD), and transmission electron microscopy (TEM) are used to characterize the obtained nanocrystal samples. The band gap energy of colloid is determined by analyzing the UV–Vis absorption spectra of the Ag2S NPs using the band theory of semiconductors. Z-scan technique is used to characterize the optical nonlinear properties of the Ag2S nanoparticles (NPs). Large enhancement of two photon absorption effect is observed with increase in concentration of the Ag2S nanoparticles using open Zscan measurements in the ns laser regime. The values of the nonlinear absorption coefficients are determined based on the local nonlinear responses including two photon absorption. The observed aperture dependence of the Ag2S NP limiting performance indicates that the nonlinear scattering plays an important role in the limiting action of the sample. The concentration dependence of the optical liming is also investigated. Our results demonstrate that the optical limiting threshold decreases with increasing the silver sulfide NPs in DMSO.

Keywords: Nanoscale materials, Silver sulfide nanoparticles, Nonlinear absorption, Nonlinear scattering, Optical limiting.

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Authors: Gul Afreen, Sreedevi Upadhyayula, Mahendra K. Sunkara

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One-dimensional (1D) nanostructures like nanowires, nanotubes, and nanorods find variety of practical application owing to their unique physico-chemical properties. In this work, TiO₂ nanowires were synthesized by direct oxidation of titanium particles in a unique microwave plasma jet reactor. The prepared TiO₂ nanowires manifested the flexible features, and were characterized by using X-ray diffraction, Brunauer-Emmett-Teller (BET) surface area analyzer, UV-Visible and FTIR spectrophotometers, Scanning electron microscope, and Transmission electron microscope. Further, the photodegradation efficiency of these nanowires were tested against toxic organic dye like methylene blue (MB) and the results were compared with the commercial TiO₂. It was found that TiO₂ nanowires exhibited superior photocatalytic performance (89%) as compared to commercial TiO₂ (75%) after 60 min of reaction. This is attributed to the lower recombination rate and increased interfacial charge transfer in TiO₂ nanowire. Pseudo-first order kinetic modelling performed with the experimental results revealed that the rate constant of photodegradation in case of TiO₂ nanowire was 1.3 times higher than that of commercial TiO₂. Superoxide radical (O₂˙⁻) was found to be the major contributor in the photodegradation mechanism. Based on the trapping experiments, a plausible mechanism of the photocatalytic reaction is discussed.

Keywords: Heterogeneous catalysis, photodegradation, reactive oxygen species, TiO2 nanowires.

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Authors: Christian C. Vaso, Rinlee Butch M. Cervera

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One of the most promising anode materials for solid oxide electrolysis cell (SOEC) application is the Sr-doped LaMnO₃ (LSM) which is known to have a high electronic conductivity but low ionic conductivity. To increase the ionic conductivity or diffusion of ions through the anode, Yttria-stabilized Zirconia (YSZ), which has good ionic conductivity, is proposed to be combined with LSM to create a composite electrode and to obtain a high mixed ionic and electronic conducting anode. In this study, composite of lanthanum strontium manganite and YSZ oxide, La_0.8Sr_0.2MnO₃/Zr_0.92Y_0.08O₂ (LSM/YSZ), with different wt.% compositions of LSM and YSZ were synthesized using solid-state reaction. The obtained prepared composite samples of 60, 50, and 40 wt.% LSM with remaining wt.% of 40, 50, and 60, respectively for YSZ were fully characterized for its microstructure by using powder X-ray diffraction (XRD), Thermogravimetric analysis (TGA), Fourier transform infrared (FTIR), and Scanning electron microscope/Energy dispersive spectroscopy (SEM/EDS) analyses. Surface morphology of the samples via SEM analysis revealed a well-sintered and densified pure LSM, while a more porous composite sample of LSM/YSZ was obtained. Electrochemical impedance measurements at intermediate temperature range (500-700 °C) of the synthesized samples were also performed which revealed that the 50 wt.% LSM with 50 wt.% YSZ (L50Y50) sample showed the highest total conductivity of 8.27x10^-1 S/cm at 600 ^oC with 0.22 eV activation energy.

Keywords: Ceramics, microstructure, fuel cells, electrochemical impedance spectroscopy.

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Authors: Xingwen Lu, Kaimin Shih

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This study investigated a strategy of blending lead-laden sludge and Al-rich precursors to reduce the release of metals from the stabilized products. Using PbO as the simulated lead-laden sludge to sinter with γ-Al2O3 by Pb:Al molar ratios of 1:2 and 1:12, PbAl2O4 and PbAl12O19 were formed as final products during the sintering process, respectively. By firing the PbO + γ-Al2O3 mixtures with different Pb/Al molar ratios at 600 to 1000 °C, the lead transformation was determined through X-ray diffraction (XRD) data. In Pb/Al molar ratio of 1/2 system, the formation of PbAl2O4 is initiated at 700 °C, but an effective formation was observed above 750 °C. An intermediate phase, Pb9Al8O21, was detected in the temperature range of 800-900 °C. However, different incorporation behavior for sintering PbO with Al-rich precursors at a Pb/Al molar ratio of 1/12 was observed during the formation of PbAl12O19 in this system. In the sintering process, both temperature and time effect on the formation of PbAl2O4 and PbAl12O19 phases were estimated. Finally, a prolonged leaching test modified from the U.S. Environmental Protection Agency-s toxicity characteristic leaching procedure (TCLP) was used to evaluate the durability of PbO, Pb9Al8O21, PbAl2O4 and PbAl12O19 phases. Comparison for the leaching results of the four phases demonstrated the higher intrinsic resistance of PbAl12O19 against acid attack.

Keywords: Sludge, Lead, Stabilization, Leaching behavior

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Authors: G.Vinitha, A.Ramalingam

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TiO2 nanoparticles were synthesized by hydrothermal method at 180°C from TiOSO4 aqueous solution with1m/l concentration. The obtained products were coated with silica by means of a seeded polymerization technique for a coating time of 1440 minutes to obtain well defined TiO2@SiO2 core-shell structure. The uncoated and coated nanoparticles were characterized by using X-Ray diffraction technique (XRD), Fourier Transform Infrared Spectroscopy (FT-IR) to study their physico-chemical properties. Evidence from XRD and FTIR results show that SiO2 is homogenously coated on the surface of titania particles. FTIR spectra show that there exists an interaction between TiO2 and SiO2 and results in the formation of Ti-O-Si chemical bonds at the interface of TiO2 particles and SiO2 coating layer. The non linear optical limiting properties of TiO2 and TiO2@SiO2 nanoparticles dispersed in ethylene glycol were studied at 532nm using 5ns Nd:YAG laser pulses. Three-photon absorption is responsible for optical limiting characteristics in these nanoparticles and it is seen that the optical nonlinearity is enhanced in core-shell structures when compared with single counterparts. This effective three-photon type absorption at this wavelength, is of potential application in fabricating optical limiting devices.

Keywords: hydrothermal method, optical limiting devicesseeded polymerization technique, three-photon type absorption

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Authors: Chen-Fu Wang, Lin-Ya Kung

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For traditional painting materials, the artisan used to combine the pigments with different binders to create colors. As time goes by, the materials used for painting evolved from natural to chemical materials. The vast variety of ingredients used in chemical materials has complicated restoration work; it makes conservation work more difficult. Conservation work also becomes harder when the materials cannot be easily identified; therefore, it is essential that we take a more scientific approach to assist in conservation work. Paintings materials are high molecular weight polymer, and their analysis is very complicated as well other contamination such as smoke and dirt can also interfere with the analysis of the material. The current methods of composition analysis of painting materials include Fourier transform infrared spectroscopy (FT-IR), mass spectrometer, Raman spectroscopy, X-ray diffraction spectroscopy (XRD), each of which has its own limitation. In this study, FT-IR was used to analyze the components of the paint coating. We have taken the most commonly seen materials as samples and deteriorated it. The aged information was then used for the database to exam the temple painting materials. By observing the FT-IR changes over time, we can tell all of the painting materials will be deteriorated by the UV light, but only the speed of its degradation had some difference. From the deterioration experiment, the acrylic resin resists better than the others. After collecting the painting materials aging information on FT-IR, we performed some test on the paintings on the temples. It was found that most of the artisan used tune-oil for painting materials, and some other paintings used chemical materials. This method is now working successfully on identifying the painting materials. However, the method is destructive and high cost. In the future, we will work on the how to know the painting materials more efficiently.

Keywords: Temple painting, painting material, conservation, FT-IR.

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Authors: Z. Ž. Lazarević, D. L. Sekulić, V. N. Ivanovski, N. Ž. Romčević

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NiFe2O4 (nickel ferrite), ZnFe2O4 (zinc ferrite) and Ni0.5Zn0.5Fe2O4 (nickel-zinc ferrite) were prepared by mechanochemical route in a planetary ball mill starting from mixture of the appropriate quantities of the Ni(OH)2/Fe(OH)3, Zn(OH)2/Fe(OH)3 and Ni(OH)2/Zn(OH)2/Fe(OH)3 hydroxide powders. In order to monitor the progress of chemical reaction and confirm phase formation, powder samples obtained after 25 h, 18 h and 10 h of milling were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), IR, Raman and Mössbauer spectroscopy. It is shown that the soft mechanochemical method, i.e. mechanochemical activation of hydroxides, produces high quality single phase ferrite samples in much more efficient way. From the IR spectroscopy of single phase samples it is obvious that energy of modes depends on the ratio of cations. It is obvious that all samples have more than 5 Raman active modes predicted by group theory in the normal spinel structure. Deconvolution of measured spectra allows one to conclude that all complex bands in the spectra are made of individual peaks with the intensities that vary from spectrum to spectrum. The deconvolution of Raman spectra allows to separate contributions of different cations to a particular type of vibration and to estimate the degree of inversion.

Keywords: Ferrites, Raman spectroscopy, IR spectroscopy, Mössbauer measurements.

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Authors: Erfan Asghari Fesaghandis, Reza Ghaffari Adli, Abbas Kianvash, Hossein Aghajani, Homa Homaie

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NiTi alloys possess magnificent superelastic, shape memory, high strength and biocompatible properties. For improving mechanical properties, foremost, superelasticity behavior, heat treatment process is carried out. In this paper, two different heat treatment methods were undertaken: (1) solid solution, and (2) aging. The effect of each treatment in a constant time is investigated. Five samples were prepared to study the structure and optimize mechanical properties under different time and temperature. For measuring the upper plateau stress, lower plateau stress and residual strain, tensile test is carried out. The samples were aged at two different temperatures to see difference between aging temperatures. The sample aged at 500 °C has a bigger crystallite size and lower amount of Ni which causes the mentioned sample to possess poor pseudo elasticity behaviour than the other aged sample. The sample aged at 460 °C has shown remarkable superelastic properties. The mentioned sample’s higher plateau is 580 MPa with the lowest residual strain (0.17%) while other samples have possessed higher residual strains. X-ray diffraction was used to investigate the produced phases.

Keywords: Heat treatment, phase transformation, superelasticity, NiTi alloy.

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Authors: N. H. Abd Raof, H. Abu Hassan, S.K. Mohd Bakhori, S. S. Ng, Z. Hassan

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Quaternary InxAlyGa1-x-yN semiconductors have attracted much research interest because the use of this quaternary offer the great flexibility in tailoring their band gap profile while maintaining their lattice-matching and structural integrity. The structural and optical properties of InxAlyGa1-x-yN alloys grown by molecular beam epitaxy (MBE) is presented. The structural quality of InxAlyGa1-x-yN layers was characterized using high-resolution X-ray diffraction (HRXRD). The results confirm that the InxAlyGa1-x-yN films had wurtzite structure and without phase separation. As the In composition increases, the Bragg angle of the (0002) InxAlyGa1-x-yN peak gradually decreases, indicating the increase in the lattice constant c of the alloys. FWHM of (0002) InxAlyGa1-x-yN decreases with increasing In composition from 0 to 0.04, that could indicate the decrease of quality of the samples due to point defects leading to non-uniformity of the epilayers. UV-VIS spectroscopy have been used to study the energy band gap of InxAlyGa1-x-yN. As the indium (In) compositions increases, the energy band gap decreases. However, for InxAlyGa1-x-yN with In composition of 0.1, the band gap shows a sudden increase in energy. This is probably due to local alloy compositional fluctuations in the epilayer. The bowing parameter which appears also to be very sensitive on In content is investigated and obtained b = 50.08 for quaternary InxAlyGa1-x-yN alloys. From photoluminescence (PL) measurement, green luminescence (GL) appears at PL spectrum of InxAlyGa1-x-yN, emitted for all x at ~530 nm and it become more pronounced as the In composition (x) increased, which is believed cause by gallium vacancies and related to isolated native defects.

Keywords: HRXRD, nitrides, PL, quaternary, UV-VIS.

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Authors: Waranya Pongpaiboon, Warangkana Srichamnong, Supat Chaiyakul

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Enzymatic modification of rice flour can produce highly functional derivatives use in food industries. This study aimed to evaluate the physical properties and resistant starch content of rice flour residues hydrolyzed by α-amylase. Rice flour hydrolyzed by α-amylase (60 and 300 u/g) for 1, 24 and 48 hours were investigated. Increasing enzyme concentration and hydrolysis time resulted in decreased rice flour residue’s lightness (L*) but increased redness (a*) and yellowness (b*) of rice flour residues. The resistant starch content and peak viscosity increased when hydrolysis time increased. Pasting temperature, trough viscosity, breakdown, final viscosity, setback and peak time of the hydrolyzed flours were not significantly different (p>0.05). The morphology of native flour was smooth without observable pores and polygonal with sharp angles and edges. However, after hydrolysis, granules with a slightly rough and porous surface were observed and a rough and porous surface was increased with increasing hydrolyzed time. The X-ray diffraction patterns of native flour showed A-type configuration, which hydrolyzed flour showed almost 0% crystallinity indicated that both amorphous and crystalline structures of starch were simultaneously hydrolyzed by α-amylase.

Keywords: α-Amylase, Enzymatic hydrolysis, Pasting properties, Resistant starch

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

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

Keywords: Silver sulfide, reduced graphene oxide, nanocomposite, structural properties, optical properties.

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Authors: Keiji Komatsu, Tetsuo Sekiya, Ayumu Toyama, Atsushi Nakamura, Ikumi Toda, Shigeo Ohshio, Hiroyuki Muramatsu, Hidetoshi Saitoh, Atsushi Nakamura, Ariyuki Kato

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Yttrium oxide (Y2O3) films have been successfully deposited with yttrium-ethylenediamine tetraacetic acid (EDTA·Y·H) complexes prepared by various milling techniques. The effects of the properties of the EDTA·Y·H complex on the properties of the deposited Y2O3 films have been analyzed. Seven different types of the raw EDTA·Y·H complexes were prepared by various commercial milling techniques such as ball milling, hammer milling, commercial milling, and mortar milling. The milled EDTA·Y·H complexes exhibited various particle sizes and distributions, depending on the milling method. Furthermore, we analyzed the crystal structure, morphology and elemental distribution profile of the metal oxide films deposited on stainless steel substrate with the milled EDTA·Y·H complexes. Depending on the milling technique, the flow properties of the raw powders differed. The X-ray diffraction pattern of all the samples revealed the formation of Y2O3 crystalline phase, irrespective of the milling technique. Of all the different milling techniques, the hammer milling technique is considered suitable for fabricating dense Y2O3 films.

Keywords: Powder sizes and distributions, Flame spray coating techniques, Yttrium oxide.

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Authors: S. Palaniyappan, P. K. Chennam, M. Trautmann, H. Ahmad, T. Mehner, T. Lampke, G. Wagner

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In structural-health monitoring of fiber reinforced plastics (FRPs), every single inorganic fiber sensor that are integrated into the bulk material requires an electrical insulation around itself, when the surrounding reinforcing fibers are electrically conductive. This results in a more accurate data acquisition only from the sensor fiber without any electrical interventions. For this purpose, thin nano-films of aluminium oxide (Al₂O₃)-based electrical-insulation coatings have been fabricated around the Silicon Carbide (SiC) single fiber sensors through reactive DC magnetron sputtering technique. The sputtered coatings were amorphous in nature and the thickness of the coatings increased with an increase in the sputter time. Microstructural characterization of the coated fibers performed using scanning electron microscopy (SEM) confirmed a homogeneous circumferential coating with no detectable defects or cracks on the surface. X-ray diffraction (XRD) analyses of the as-sputtered and 2 hours annealed coatings (825 & 1125 ˚C) revealed the amorphous and crystalline phases of Al₂O₃ respectively. Raman spectroscopic analyses produced no characteristic bands of Al₂O₃, as the thickness of the films was in the nanometer (nm) range, which is too small to overcome the actual penetration depth of the laser used. In addition, the influence of the insulation coatings on the mechanical properties of the SiC sensor fibers has been analyzed.

Keywords: Al2O3 insulation coating, reactive sputtering, SiC single fiber sensor, single fiber tensile test.

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Authors: S. Sharma, U. Batra, S. Kapoor, A. Dua

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In this study, the effects and interactions of reaction time and capping agent assistance during sol-gel synthesis of magnesium substituted hydroxyapatite nanopowder (MgHA) on hydroxyapatite (HA) to β-tricalcium phosphate (β-TCP) ratio, Ca/P ratio and mean crystallite size was examined experimentally as well as through statistical analysis. MgHA nanopowders were synthesized by sol-gel technique at room temperature using aqueous solution of calcium nitrate tetrahydrate, magnesium nitrate hexahydrate and potassium dihydrogen phosphate as starting materials. The reaction time for sol-gel synthesis was varied between 15 to 60 minutes. Two process routes were followed with and without addition of triethanolamine (TEA) in the solutions. The elemental compositions of as-synthesized powders were determined using X-ray fluorescence (XRF) spectroscopy. The functional groups present in the assynthesized MgHA nanopowders were established through Fourier Transform Infrared Spectroscopy (FTIR). The amounts of phases present, Ca/P ratio and mean crystallite sizes of MgHA nanopowders were determined using X-ray diffraction (XRD). The HA content in biphasic mixture of HA and β-TCP and Ca/P ratio in as-synthesized MgHA nanopowders increased effectively with reaction time of sols (p<0.0001, two way ANOVA), however, these were independent of TEA addition (p>0.15, two way ANOVA). The MgHA nanopowders synthesized with TEA assistance exhibited 14 nm lower crystallite size (p<0.018, 2 sample t-test) compared to the powder synthesized without TEA assistance.

Keywords: Capping agent, hydroxyapatite, regression analysis, sol-gel, 2- sample t-test, two-way ANOVA.

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

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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: Teuku Rihayat, Suryani

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Polyurethanes (PURs) are very versatile polymeric materials with a wide range of physical and chemical properties. PURs have desirable properties such as high abrasion resistance, tear strength, shock absorption, flexibility and elasticity. Although they have relatively poor thermal stability, this can be improved by using treated clay. Polyurethane/clay nanocomposites have been synthesized from renewable sources. A polyol for the production of polyurethane by reaction with an isocyanate was obtained by the synthesis of palm oil-based oleic acid with glycerol. Dodecylbenzene sulfonic acid (DBSA) was used as catalyst and emulsifier. The unmodified clay (kunipia-F) was treated with cetyltrimethyl ammonium bromide (CTAB-mont) and octadodecylamine (ODAmont). The d-spacing in CTAB-mont and ODA-mont were 1.571 nm and 1.798 nm respectively and larger than that of the pure-mont (1.142 nm). The organoclay was completely intercalated in the polyurethane, as confirmed by a wide angle x-ray diffraction (WAXD) pattern. The results showed that adding clay demonstrated better thermal stability in comparison with the virgin polyurethane. Onset degradation of pure PU is at 200oC, and is lower than that of the CTAB-mont PU and ODA-mont PU which takes place at about 318oC and 330oC, respectively. The mechanical properties (including the dynamic mechanical properties) of pure polyurethane (PU) and PU/clay nanocomposites, were measured. The modified organoclay had a remarkably beneficial effect on the strength and elongation at break of the nanocomposites, which both increased with increasing clay content with the increase of the tensile strength of more than 214% and 267% by the addition of only 5 wt% of the montmorillonite CTAB-mont PU and ODA-mont PU, respectively.

Keywords: Polyurethane, Clay nanocomposites, Biobase

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Authors: Carolin Lutz, Jörg Matthes, Patrick Waibel, Ulrich Precht, Krassimir Garbev, Günter Beuchle, Uwe Schweike, Peter Stemmermann, Hubert B. Keller

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Online measurement of the product quality is a challenging task in cement production, especially in the production of Celitement, a novel environmentally friendly hydraulic binder. The mineralogy and chemical composition of clinker in ordinary Portland cement production is measured by X-ray diffraction (XRD) and X-ray fluorescence (XRF), where only crystalline constituents can be detected. But only a small part of the Celitement components can be measured via XRD, because most constituents have an amorphous structure. This paper describes the development of algorithms suitable for an on-line monitoring of the final processing step of Celitement based on NIR-data. For calibration intermediate products were dried at different temperatures and ground for variable durations. The products were analyzed using XRD and thermogravimetric analyses together with NIR-spectroscopy to investigate the dependency between the drying and the milling processes on one and the NIR-signal on the other side. As a result, different characteristic parameters have been defined. A short overview of the Celitement process and the challenging tasks of the online measurement and evaluation of the product quality will be presented. Subsequently, methods for systematic development of near-infrared calibration models and the determination of the final calibration model will be introduced. The application of the model on experimental data illustrates that NIR-spectroscopy allows for a quick and sufficiently exact determination of crucial process parameters.

Keywords: Calibration model, celitement, cementitious material, NIR spectroscopy.

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Authors: Eraricar Salleh, Ida Idayu Muhamad, Nozieanna Khairuddin

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Antimicrobial (AM) starch-based films were developed by incorporating chitosan and lauric acid as antimicrobial agent into starch-based film. Chitosan has wide range of applications as a biomaterial, but barriers still exist to its broader use due to its physical and chemical limitations. In this work, a series of starch/chitosan (SC) blend films containing 8% of lauric acid was prepared by casting method. The structure of the film was characterized by Fourier transform infrared spectroscopy (FTIR), Xray diffraction (XRD), and scanning electron microscopy (SEM). The results indicated that there were strong interactions were present between the hydroxyl groups of starch and the amino groups of chitosan resulting in a good miscibility between starch and chitosan in the blend films. Physical properties and optical properties of the AM starch-based film were evaluated. The AM starch-based films incorporated with chitosan and lauric acid showed an improvement in water vapour transmission rate (WVTR) and addition of starch content provided more transparent films while the yellowness of the film attributed to the higher chitosan content. The improvement in water barrier properties was mainly attributed to the hydrophobicity of lauric acid and optimum chitosan or starch content. AM starch based film also showed excellent oxygen barrier. Obtaining films with good oxygen permeability would be an indication of the potential use of these antimicrobial packaging as a natural packaging and an alternative packaging to the synthetic polymer to protect food from oxidation reactions

Keywords: Antimicrobial starch-based films, chitosan, lauric acid, starch.

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Authors: M. M. Morgham, A. A. Hameda, N. A. Zriba, H. A. Jawan

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This paper aims to study the effect of cold work condition on the microstructure of Cu-1.5wt%Ti, and Cu-3.5wt%Ti and hence mechanical properties. The samples under investigation were machined, and solution heat treated. X-ray diffraction technique is used to identify the different phases present after cold deformation by compression and also different heat treatment and also measuring the relative quantities of phases present. The metallographic examination is used to study the microstructure of the samples. The hardness measurements were used to indicate the change in mechanical properties. The results are compared with the mechanical properties obtained by previous workers. Experiments on cold compression followed by aging of Cu-Ti alloys have indicated that the most efficient hardening of the material results from continuous precipitation of very fine particles within the matrix. These particles were reported to be β`-type, Cu4Ti phase. The β`-β transformation and particles coarsening within the matrix as well as long grain boundaries were responsible for the overaging of Cu-1.5wt%Ti and Cu-3.5wt%Ti alloys. It is well known that plate-like particles are β – type, Cu3Ti phase. Discontinuous precipitation was found to start at the grain boundaries and expand into grain interior. At the higher aging temperature, a classic Widmanstätten morphology forms giving rise to a coarse microstructure comprised of α and the equilibrium phase β. Those results were confirmed by X-ray analysis, which found that a few percent of Cu3Ti, β precipitates are formed during aging at high temperature for long time for both Cu- Ti alloys (i.e. Cu-1.5wt%Ti and Cu-3.5wt%Ti).

Keywords: Metallographic, hardness, precipitation, aging.

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Authors: Murtaza Adil, Sen Yang, Zhou Chao, Song Xiaoping

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The morphotropic phase boundary (MPB) recently has attracted constant interest in ferromagnetic systems for obtaining enhanced large magnetoelastic response. In the present study, structural and magnetoelastic properties of MPB involved ferromagnetic Tb_1-xGd_xFe₂ (0≤x≤1) system has been investigated. The change of easy magnetic direction from <111> to <100> with increasing x up MPB composition of x=0.9 is detected by step-scanned [440] synchrotron X-ray diffraction reflections. The Gd substitution for Tb changes the composition for the anisotropy compensation near MPB composition of x=0.9, which was confirmed by the analysis of detailed scanned XRD, magnetization curves and the calculation of the first anisotropy constant K₁. The spin configuration diagram accompanied with different crystal structures for Tb_1-xGd_xFe₂ was designed. The calculated first anisotropy constant K₁ shows a minimum value at MPB composition of x=0.9. In addition, the large ratio between magnetostriction, and the absolute values of the first anisotropy constant │λ_S∕K₁│ appears at MPB composition, which makes it a potential material for magnetostrictive application. Based on experimental results, a theoretically approach was also proposed to signify that the facilitated magnetization rotation and enhanced magnetoelastic effect near MPB composition are a consequence of the anisotropic flattening of free energy of ferromagnetic crystal. Our work specifies the universal existence of MPB in ferromagnetic materials which is important for substantial improvement of magnetic and magnetostrictive properties and may provide a new route to develop advanced functional materials.

Keywords: Free energy, lattice distortion, magnetic anisotropy, magnetostriction, morphotropic phase boundary.

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Authors: H. K. G. K. D. K. Hapuhinna, R. D. Gunaratne, H. M. J. C. Pitawala

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Hydroxyapatite is a bioceramic which can be used for applications in orthopedics and dentistry due to its structural similarity with the mineral phase of mammalian bones and teeth. In this study, it was synthesized, chemically changing natural Eppawala chloroapatite mineral as a value-added product. Sol-gel approach and solid state sintering were used to synthesize products using diluted nitric acid, ethanol and calcium hydroxide under different conditions. Synthesized Eppawala hydroxyapatite powder was characterized using X-ray Fluorescence (XRF), X-ray Powder Diffraction (XRD), Fourier-transform Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM), Thermogravimetric Analysis (TGA) and Differential Scanning Calorimetry (DSC) in order to find out its composition, crystallinity, presence of functional groups, bonding type, surface morphology, microstructural features, and thermal dependence and stability, respectively. The XRD results reflected the formation of a hexagonal crystal structure of hydroxyapatite. Elementary composition and microstructural features of products were discussed based on the XRF and SEM results of the synthesized hydroxyapatite powder. TGA and DSC results of synthesized products showed high thermal stability and good material stability in nature. Also, FTIR spectroscopy results confirmed the formation of hydroxyapatite from apatite via the presence of hydroxyl groups. Those results coincided with the FTIR results of mammalian bones including human bones. The study concludes that there is a possibility of producing hydroxyapatite using commercially available Eppawala chloroapatite in Sri Lanka.

Keywords: Dentistry, eppawala chloroapatite, hydroxyapatite, orthopedics.

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Authors: Seok Hong Min, Woo Young Jung, Tae Kwon Ha

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Superplastic deformation and high temperature load relaxation behavior of coarse-grained iron aluminides with the composition of Fe-28 at.% Al have been investigated. A series of load relaxation and tensile tests were conducted at temperatures ranging from 600 to 850oC. The flow curves obtained from load relaxation tests were found to have a sigmoidal shape and to exhibit stress vs. strain rate data in a very wide strain rate range from 10-7/s to 10-2/s. Tensile tests have been conducted at various initial strain rates ranging from 3×10-5/s to 1×10-2/s. Maximum elongation of ~500 % was obtained at the initial strain rate of 3×10-5/s and the maximum strain rate sensitivity was found to be 0.68 at 850oC in binary Fe-28Al alloy. Microstructure observation through the optical microscopy (OM) and the electron back-scattered diffraction (EBSD) technique has been carried out on the deformed specimens and it has revealed the evidences for grain boundary migration and grain refinement to occur during superplastic deformation, suggesting the dynamic recrystallization mechanism. The addition of Cr by the amount of 5 at.% appeared to deteriorate the superplasticity of the binary iron aluminide. By applying the internal variable theory of structural superplasticity, the addition of Cr has been revealed to lower the contribution of the frictional resistance to dislocation glide during high temperature deformation of the Fe3Al alloy.

Keywords: Iron aluminide (Fe3Al), large grain size, structural superplasticity, dynamic recrystallization, chromium (Cr).

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Authors: Chongtham Jiten, Radhapiyari Laishram, K. Chandramani Singh

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Alkaline niobate (Na_0.5K_0.5)NbO₃ ceramic system has attracted major attention in view of its potential for replacing the highly toxic but superior lead zirconate titanate (PZT) system for piezoelectric applications. Recently, a more detailed study of this system reveals that the ferroelectric and piezoelectric properties are optimized in the Li- and V-modified system having the composition (K_0.485Na_0.5Li_0.015)(Nb_0.98V_0.02)O₃. In the present work, we further study the pyroelectric behaviour of this composition along with another doped with Mn⁴⁺. So, (K_0.485Na_0.5Li_0.015)(Nb_0.98V_0.02)O₃ + x MnO₂ (x = 0, and 0.01 wt. %) ceramic compositions were synthesized by conventional ceramic processing route. X-ray diffraction study reveals that both the undoped and Mn⁴⁺-doped ceramic samples prepared crystallize into a perovskite structure having orthorhombic symmetry. Dielectric study indicates that Mn⁴⁺ doping has little effect on both the Curie temperature (T_c) and tetragonal-orthorhombic phase transition temperature (T_ot). The bulk density, room-temperature dielectric constant (ε_RT), and room-c The room-temperature coercive field (E_c) is observed to be lower in Mn⁴⁺ doped sample. The detailed analysis of the P-E hysteresis loops over the range of temperature from about room temperature to T_ot points out that enhanced ferroelectric properties exist in this temperature range with better thermal stability for the Mn⁴⁺ doped ceramic. The study reveals that small traces of Mn⁴⁺ can modify (K_0.485Na_0.5Li_0.015)(Nb_0.98V_0.02)O₃ system so as to improve its ferroelectric properties with good thermal stability over a wide range of temperature.

Keywords: Ceramics, dielectric properties, ferroelectric properties, lead-free, sintering, thermal stability.

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