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      Volume 33, Issue 6

      December 2010,   pages  647-767

    • XPS study of palladium sensitized nano porous silicon thin film

      J Kanungo L Selegård C Vahlberg K Uvdal H Saha S Basu

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      Nano porous silicon (PS) was formed on 𝑝-type monocrystalline silicon of 2–5 𝛺 cm resistivity and (100) orientation by electrochemical anodization method using HF and ethanol as the electrolytes. High density of surface states, arising due to its nano structure, is responsible for the uncontrolled oxidation in air and for the deterioration of the PS surface with time. To stabilize the material PS surface was modified by a simple and low cost chemical method using PdCl2 solution at room temperature. X-ray photoelectron spectroscopy (XPS) was performed to reveal the chemical composition and the relative concentration of palladium on the nanoporous silicon thin films. An increase of SiO2 formation was observed after PdCl2 treatment and presence of palladium was also detected on the modified surface. 𝐼–𝑉 characteristics of Al/PS junction were studied using two lateral Al contacts and a linear relationship was obtained for Pd modified PS surface. Stability of the contact was studied for a time period of around 30 days and no significant ageing effect could be observed.

    • Realizing NiO nanocrystals from a simple chemical method

      Neelabh Srivastava P C Srivastava

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      Nanocrystalline NiO has been prepared successfully by a simple chemical route using NiCl2.6H2O and NaOH aqueous solution at a temperature of 70°C. The prepared material has been characterized from XRD, SEM, and M–H characteristics. It has been found that NiO nanocrystals have been formed which shows a superparamagnetic/superantiferromagnetic behaviour.

    • Synthesis of nanosized barium titanate/epoxy resin composites and measurement of microwave absorption

      M Murugan V K Kokate M S Bapat A M Sapkal

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      Barium titanate/epoxy resin composites have been synthesized and tested for microwave absorption/transmission. Nanocrystalline barium titanate (BaTiO3 or BT) was synthesized by the hydrothermal method and the composites of BT/epoxy resin were fabricated as thin solid slabs of four different weight ratios. BT was obtained in the cubic phase with an average particle size of 21 nm, deduced from the X-ray diffraction data. The reflection loss (RL) and transmission loss (TL) of the composite materials were measured by the reflection/transmission method using a vector network analyser R&S: ZVA40, in the frequency range 8.0–18.5 GHz (X and Ku-bands). The RL was found to be better than −10 dB over wide frequency bands. The higher RL for lower concentration of BT could be due to increase in impedance matching effects. Low TL values indicate that the absorption by BT is quite low. This could be due to formation of BT in the cubic paraelectric phase.

    • Preparation and characterization of nanostructured copper bismuth diselenide thin films from a chemical route

      R H Bari L A Patil

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      Thin films of copper bismuth diselenide were prepared by chemical bath deposition technique onto glass substrate below 60°C. The deposition parameters such as time, temperature of deposition and pH of the solution, were optimized. The set of films having different elemental compositions was prepared by varying Cu/Bi ratio from 0.13–1.74. Studies on structure, composition, morphology, optical absorption and electrical conductivity of the films were carried out and discussed. Characterization includes X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), energy dispersive X-ray analysis (EDAX), absorption spectroscopy, and electrical conductivity. The results are discussed and interpreted.

    • Influence of high velocity oxy-fuel parameters on properties of nanostructured TiO2 coatings

      Maryamossadat Bozorgtabar Mehdi Salehi Mohammadreza Rahimipour Mohammadreza Jafarpour

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      A liquid fuel high velocity oxy-fuel (HVOF) thermal spray process has been used to deposit TiO2 nanostructured coatings utilizing a commercially available nanopowder as the feedstock. The coatings were characterized by means of X-ray diffraction analysis (XRD), scanning electron microscopy (SEM) and transmission electron microscope (TEM), respectively. Photocatalytic activity was evaluated as a rate constant of decomposition reaction of methylene blue (MB) determined from the changes of relative concentration of MB with UV irradiation time. The results indicate that the sprayed TiO2 coatings were composed of both TiO2 phases viz. anatase and rutile, with different phase contents and crystallite sizes. A high anatase content of 80% by volume was achieved at 0.00015, fuel-to-oxygen ratio with nanostructure coating by grain size smaller than feedstock powder. Photocatalytic activity evaluation results indicated that all the TiO2 coatings are effective to degradation MB under UV radiation and their activities differ in different spray conditions. It is found that fuel flow rate strongly influenced on phase transformation of anatase to rutile and by optimizing the rate which can promote structural transformation and grain coarsening in coating and improving photocatalytic activity.

    • Electrochemical and optical properties of a new donor–acceptor type conjugated polymer derived from 3,4–didodecyloxythiophene

      Pramod Kumar Hegde A Vasudeva Adhikari M G Manjunatha

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      In this communication, we report the synthesis and characterization of a new donor–acceptor type conjugated polymer carrying alternate 3,4-didodecyloxythiophene and (1,3,4-oxadiazol-yl)pyridine moieties and evaluation of its optical and electrochemical properties. The polymer was synthesized through precursor polyhydrazide route. It has well defined structure, stability and it shows good solubility in common organic solvents. Optical and electrochemical properties were studied by UV-visible, fluorescence spectroscopy and cyclic voltammetric studies, respectively. It displays bluish-green fluorescence both in solution and in film state. Cyclic voltammetric studies showed that the polymer P1 possesses a HOMO energy level of −6.01 and LUMO energy level of −3.34 eV. The preliminary studies clearly reveal that the new polymer can have potential application in the fabrication of light emitting diodes. The studies on its device application are in progress.

    • Dielectric and complex impedance studies of BaTi0.85W0.15O3+𝛿 ferroelectric ceramics

      Sheela Devi A K Jha

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      In the present work, tungsten substituted barium titanate have been synthesized and studied. The structural analysis indicates that the specimen is a single phase material with tetragonal crystal structure. The observed polarization–electric field hysteresis loop confirms the ferroelectric nature of the prepared compound. Variation of dielectric constant with temperature at different frequencies shows that the compound has a dielectric anomaly at 75 °C and exhibits diffuse type phase transition. Variation of dielectric loss with temperature at different frequencies shows a decrease in loss with increasing frequency. The Nyquist plots (Cole–Cole plots) have been measured at temperatures 325 °C, 345 °C and 365 °C. The plot at 365 °C shows a grain boundary effect. Relaxation time has been found to decrease with the rise in temperature and obey the Arrhenius relationship. The variations of d.c. conductivity as a function of temperature have also been studied.

    • Effect of paramagnetic manganese ions doping on frequency and high temperature dependence dielectric response of layered Na1.9Li0.1Ti3O7 ceramics

      Dharmendra Pal J L Pandey

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      The manganese doped layered ceramic samples (Na1.9Li0.1)Ti3O7 : XMn(0.01 ≤ X ≤ 0.1) have been prepared using high temperature solid state reaction. The room temperature electron paramagnetic resonance (EPR) investigations exhibit that at lower percentage of doping the substitution of manganese ions occur as Mn3+ at Ti4+ sites, whereas for higher percentage of doping Mn2+ ions occupy the two different interlayer sodium/lithium sites. In both cases, the charge compensation mechanism should operate to maintain the overall charge neutrality of the lattice. The manganese doped derivatives of layered Na1.9Li0.1Ti3O7 (SLT) ceramics have been investigated through frequency dependence dielectric spectroscopy in this work. The results indicate that the dielectric losses in these ceramics are the collective contribution of electric conduction, dipole orientation and space charge polarization. Smeared peaks in temperature dependence of permittivity plots suggest diffuse nature of high temperature ferroelectric phase transition. The light manganese doping in SLT enhances the dielectric constant. However, manganese doping decreases dielectric loss due to inhibition of domain wall motion, enhances electronhopping conduction, and impedes the interlayer ionic conduction as well. Manganese doping also gives rise to contraction of interlayer space.

    • Beneficiation of Iranian magnesite ores by reverse flotation process and its effects on shaped and unshaped refractories properties

      S Aslani H R Samim Bani Hashemi F Arianpour

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      The primary aim of this study is the beneficiation of magnesite ores from eastern part of Iran by reverse flotation process. For this purpose, the mineralogical and microstructural characteristics of the as-received and the processed ores from Iranian Afzal Abad mine were established. The liberation degree of ore was estimated at about 75 𝜇m. Then the as-received ore and the processed one were dead burnt to produce magnesia aggregates. These aggregates were used for production of shaped and unshaped refractories. Bricks and monolithic ramming mixes which were made from these aggregates were analysed and their mechanical and physical properties, studied. The results of this investigation showed that the application of reverse flotation process on the magnesite ore of eastern part of Iran causes an acceptable reduction on the amount of its siliceous inclusions, so that this type of the processed magnesia is suitable for utilization in the refractory industries. The magnesia produced from the original calcined ore was not suitable for this industry due to the presence of unacceptable amount of siliceous inclusions, which make its properties very poor.

    • Microstructure and fracture behaviour of Ti3Al/TC4 dissimilar materials joints welded by electron beam

      H T Zhang H Y Zhao W X He

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      Electron beam was used to join TC4 alloy to Ti3Al-based alloy. The composition of the weld was analysed by XRD and TEM and the results showed that the weld mainly composed of 𝛼' martensites. The change of heat input had little influence on the composition of the weld but can make the grain size increasing. The fracture path of the joints was mainly decided by the microstructure of the weld and started from coarse grain zone to HAZ and base metal of Ti3Al alloy.

    • Synthesis and properties of dental zirconia–leucite composites

      Ming Kang Xiaoming Liao Guangfu Yin Xun Sun Xing Yin Lu Xie Jun Liu

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      The dental zirconia–leucite composites were synthesized by high temperature solid-state method using potash feldspar, potassium carbonate and zirconia as raw materials. The mechanical properties and the coefficient of thermal expansion (CTE) of the prepared zirconia–leucite composites were tested. The results show that the bending strength, the fracture toughness and the metal–ceramic bonding strength of the prepared samples are about 110 MPa, 3.5 MPa/m1/2 and 45 MPa, respectively. The CTE was about 13.73×10$^{-6}\ ^\circ $C-1 and close to that of Ni–Cr dental alloy (14.0×10$^{-6}\ ^\circ $C-1). The results indicate that the introduction of zirconia is beneficial to the improvement in the mechanical properties and CTE adjustment of porcelain material. The clinical application of the zirconia–leucite composites with good metal–ceramic bonding strength in the dental restoration could be envisioned.

    • Study on durability of natural fibre concrete composites using mechanical strength and microstructural properties

      M Sivaraja Kandasamy N Velmani M Sudhakaran Pillai

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      Investigations to overcome the brittle response and limiting post-yield energy absorption of concrete led to the development of fibre reinforced concrete using discrete fibres within the concrete mass. Out of the commonly used fibres, easily available low cost natural fibres are renewable source materials. Though these fibres are ecologically advantageous, they have some limitations such as lower durability and lesser strength. But recent research provides several treatment processes to enhance the durability of natural fibres. In this paper, the durability of natural fibres such as coconut coir and sugarcane bagasse has been reported by conducting an experimental investigation. This investigation includes two parts. The first part focuses on the determination of mechanical strength properties such as compressive, tensile, modulus of rupture and flexural properties of natural fibre reinforced concrete specimens once every 3 months for a period for 2 years under alternate wetting and drying conditions. Gain or loss in strength of composite concrete at 9 intervals were computed and are reported here. The second part covers the microstructural properties of fresh natural fibres in as received condition and natural fibres reacted with concrete under accelerated curing conditions for two years. SEM and EDAC test results are discussed.

    • Electrical resistivity measurement to predict uniaxial compressive and tensile strength of igneous rocks

      Sair Kahraman Tekin Yeken

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      Electrical resistivity values of 12 different igneous rocks were measured on core samples using a resistivity meter in the laboratory. The resistivity tests were conducted on the samples fully saturated with brine (NaCl solution) and the uniaxial compressive strength (UCS), Brazilian tensile strength, density and porosity values of the samples were determined in the laboratory. The test results were evaluated using simple and multiple regression analysis. It was seen that the UCS and tensile strength values were linearly correlated with the electrical resistivity. The correlation coefficients are generally higher for the multiple regression models than that of the simple regression models. It was concluded that the UCS and tensile strength of igneous rocks can be estimated from electrical resistivity. However, the derived relations are purely empirical and they should be checked for other igneous rocks. The effect of rock types such as sedimentary and metamorphic rocks on the derived equations also needs to be investigated.

    • Microwave assisted hydrolysis of aluminium metal and preparation of high surface area 𝛾 Al2O3 powder

      A K Sivadasan I Packia Selvam Sankara Narayanan Potty

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      Phase pure boehmite particles were prepared by microwave assisted hydrolysis of aluminium sheets. These particles were calcined in air to produce 𝛾 Al2O3 particles with specific surface area of ∼210 m2/g. The alumina particles were characterized by studying X-ray diffraction, transmission electron microscopy and Fourier transform infrared spectroscopy. For comparison, the aluminium hydroxide particles were also prepared by normal hydrolysis of aluminium metal. Normal hydrolysis yielded a mixture of boehmite and bayerite particles whereas microwave assisted hydrolysis produced phase pure boehmite particles. The importance of using microwave radiation for the hydrolysis of aluminium metal is also manifested in a shorter reaction time.

    • Catalytic property of TiO2/PS complex nanoparticles prepared via a novel TSM

      Bitao Su Xiaohong Zhang Zhanying Ma Peng Fei Jiaxing Sun Ziqiang Lei

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      With an average size of 7 nm and good catalytic property under the natural light, TiO2/PS complex nanoparticles were successfully prepared through a novel two-step method (TSM) from TiCl4, used as both the catalyst for polymerization of styrene and Ti source, and styrene monomer and characterized by TG-DTA, XRD, IR, TEM and UV-Vis techniques. Its catalytic property was evaluated by the decolourization and degradation of dye MB solution under the natural light. From its TEM, the particles with an average size of 7 nm were observed without the separation of TiO2 and PS phases, i.e., TiO2/PS was hybrid material in nanosize scale. IR spectrum of TiO2/PS showed increase of unsaturated degree and growth of the group C=O on the chain of PS and Ti–O–C coordination bond between TiO2 and PS. The nanosize of the TiO2/PS complex particles and the conjugated structure and polar groups of PS were advantageous to good adsorptive property and strong interaction of PS and TiO2. And they brought multi-functions of inorganic and organic materials in the single material. Catalytic experiments indicated that the complex nanoparticles could catalytically degrade dye MB solution in 10 min under the natural light while P25 basically showed adsorptive property for MB molecules under the same conditions.

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