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      Volume 31, Issue 1

      February 2008,   pages  1-100

    • Influence of minor elements additions on microstructure and properties of 93W–4.9Ni–2.1Fe alloys

      Liu Wensheng Ma Yunzhu Huang Baiyun

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      Effects of elements rhenium and chromium additions on properties and microstructure of 93W–4.9Ni–2.1Fe alloys were investigated. Optical microscope (OM), scanning electron microscope (SEM) and EDAX energy spectrometer were used to characterize the microstructure and compositions of the alloys, respectively. The tensile strength and elongation of alloys were evaluated using the quasi-static tensile testing machine, and the relative densities of the alloys were evaluated using the Archimedes water immersion method. The experimental results indicated that when elements Re and Cr were in the range of 0–1.0 wt.%, relative density, elongation, tensile strength of 93W–4.9Ni–2.1Fe alloys varied from 99.4%, 26.4%, 997.2 MPa without Re additions to 99.5%, 8.6%, 1161.2 MPa with 1.0 wt.% Re addition, respectively. Rhenium generated solid-solution strengthening, grain refinement, reducing ductile tearing and increasing transcrystalline fracture, which resulted in the ductility reduction and the strength increase of the heavy alloys. With the increase of Cr content from 0–1.0 wt.%, the tensile strength, relative density and elongation of 93W–Ni–Fe alloy reduced from 997.2 MPa, 99.3%, 15% to 844.4 MPa, 95.2%, 5.7%, respectively. Element Cr formed interphases with elements W, Ni, Fe and O and gathered along the interface of the alloys, which induced interfacial cohesion and resulted in lower mechanical properties of 93W–Ni–Fe alloys.

    • Pressure induced graft-co-polymerization of acrylonitrile onto Saccharum cilliare fibre and evaluation of some properties of grafted fibre

      A S Singha Anjali Shama Vijay Kumar Thakur

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      In the present work, graft co-polymerization of acrylonitrile (AN) onto Saccharum cilliare fibre has been carried out in the presence of potassium persulphate and ferrous ammonium sulphate (FAS–KPS) as redox initiator. The reactions were carried out under pressure in an autoclave. Various reaction parameters such as pressure, time, pH, concentrations of initiator and monomer were optimized to get maximum graft yield (35.59%). Grafted and ungrafted Saccharum cilliare fibres were then subjected to evaluation of some of their properties like swelling behaviour in different solvents, moisture absorbance under different humidity levels, water uptake and resistance towards chemicals such as hydrochloric acid and sodium hydroxide. The characterization of the graft copolymers were carried out by FTIR spectrophotometer, X-ray diffraction (XRD) and scanning electron microscopic (SEM) studies.

    • Comparison of performance parameters of poly(3,4 ethylenedioxythiophene) (PEDOT) based electrochromic device on glass with and without counter electrode

      S Sindhu K Narasimha Rao E S R Gopal

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      Conjugated polymers are promising materials for electrochromic device technology. Aqueous dispersions of poly(3,4-ethylenedioxythiophene)-(PEDOT) were spin coated onto transparent conducting oxide (TCO) coated glass substrates. A seven-layer electrochromic device was fabricated with the following configuration: glass/transparent conducting oxide (TCO)/PEDOT (main electrochromic layer)/gel electrolyte/prussian blue (counter electrode)/TCO/glass. The device fabricated with counter electrode (Prussian blue) showed a contrast of 18% and without counter electrode showed visible contrast of 5% at 632 nm at a voltage of 1.9 V. The comparison of the device is done in terms of the colouration efficiency of the devices with and without counter electrode.

    • Asbestos free friction composition for brake linings

      Arnab Ganguly Raji George

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      An asbestos free friction material composite for brake linings is synthesized containing fibrous reinforcing constituents, friction imparting and controlling additives, elastomeric additives, fire retarding components and a thermosetting resin. The composite shows exemplary friction characteristics and has great resistance to wear and shows good temperature stability.

    • Polypropylene–clay composite prepared from Indian bentonite

      Madhuchhanda Sarkar Kausik Dana Sankar Ghatak Amarnath Banerjee

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      In the present work, a set of experimental polypropylene (PP) clay composites containing pristine bentonite clay of Indian origin has been prepared and then characterized. The polymer clay composites are processed by solution mixing of polypropylene with bentonite clay using a solvent xylene and high speed electric stirrer at a temperature around 130°C and then by compression molding at 170°C. The mechanical properties of PP–clay composites like tensile strength, hardness and impact resistance have been investigated. Microstructural studies were carried out using scanning electron microscope and transmission electron microscope and the thermal properties were studied using differential scanning calorimeter. Mechanical properties of the prepared composites showed highest reinforcing and toughening effects of the clay filler at a loading of only 5 mass % in PP matrix. Tensile strength was observed to be highest in case of 5 mass % of clay loading and it was more than 14% of that of the neat PP, while toughness increased by more than 80%. Bentonite clay–PP composite (5 mass %) also showed 60% increase in impact energy value. However, no significant change was observed in case of hardness and tensile modulus. Higher percentages of bentonite clay did not further improve the properties with respect to pristine polypropylene. The study of the microstructure of the prepared polymer layered silicate clay composites showed a mixed morphology with multiple stacks of clay layers and tactoids of different thicknesses.

    • Thermal degradation kinetics and solid state, temperature dependent, electrical conductivity of charge–transfer complex of phenothiazine with chloranil and picric acid

      M A Ashok B N Achar

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      Temperature dependent electrical conductivity and thermal degradation kinetics of charge–transfer (C–T) complexes of phenothiazine (PTZ) with 𝑝-chloranil (CHL) and picric acid (PA), are reported. These C–T complexes exhibited semiconducting behaviour. The activation energies for PTZ–CHL and PTZ–PA complexes are calculated based on their electrical conductivities measured over the temperature ranges 30–110°C and 30–90°C, respectively. And these energies for PTZ–CHL and PTZ–PA are 0.54 eV and 0.75 eV, respectively. The complexes are analysed for the kinetic parameters like the activation energy for decomposition and the Arrhenius pre-exponential factors in their pyrolysis region using Broido’s, Coats–Redfern as well as Horowitz–Metzger methods. Using standard equations, thermodynamic parameters such as enthalpy, entropy and free energies, are calculated.

    • Chemical treatment of zinc surface and its corrosion inhibition studies

      S K Rajappa T V Venkatesha B M Praveen

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      The surface treatment of zinc and its corrosion inhibition was studied using a product (BTSC) formed in the reaction between benzaldehyde and thiosemicarbozide. The corrosion behaviour of chemically treated zinc surface was investigated in aqueous chloride–sulphate medium using galvanostatic polarization technique. Zinc samples treated in BTSC solution exhibited good corrosion resistance. The measured electrochemical data indicated a basic modification of the cathode reaction during corrosion of treated zinc. The corrosion protection may be explained on the basis of adsorption and formation of BTSC film on zinc surface. The film was binding strongly to the metal surface through nitrogen and sulphur atoms of the product. The formation of film on the zinc surface was established by surface analysis techniques such as scanning electron microscopy (SEM–EDS) and Fourier transform infrared spectroscopy (FTIR).

    • Synthesis of nanocrystalline TiO2 thin films by liquid phase deposition technique and its application for photocatalytic degradation studies

      Noor Shahina Begum H M Farveez Ahmed

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      A transparent, high purity titanium dioxide thin film composed of densely packed nanometer sized grains has been successfully deposited on a glass substrate at 30°C from an aqueous solution of TiO2–HF with the addition of boric acid as a scavenger by liquid phase deposition technique. From X-ray diffraction measurement, the deposited film was found to be amorphous and turns crystalline at 500°C. The deposited film showed excellent adherence to the substrate and was characterized by homogeneous flat surface. TiO2 thin films can be used as a photocatalyst to clean up organohalides, a class of compound in pesticides that pollute the ground water. Photocatalytic degradation experiments show that indanthrene golden orange dye undergoes degradation efficiently in presence of TiO2 thin films by exposing its aqueous solution to ultraviolet light. The suitable surface structure and porosity increases the photocatalytic activity. It was also observed that hemin doped TiO2 thin films break up organohalides at a surprisingly high rate under visible light.

    • Effect of oxygen intercalation on properties of sputtered CuYO2 for potential use as 𝑝-type transparent conducting films

      R Manoj M Nisha K A Vanaja M K Jayaraj

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      Transparent films of copper yttrium oxide doped with 2% calcium have been prepared by rf magnetron sputtering. The films show a conductivity of 8 Scm-1 on intercalation of oxygen at high pressure, which reduced the transparency in the visible region. The Ca-doped CuYO2 films before oxygen intercalation show an average transmission of about 60% which reduces to about 45% upon oxygen intercalation. The temperature dependence of the conductivity indicates semiconductor behaviour with low activation energy of 0.59 eV at room temperature. The positive sign of Seebeck coefficient (+274 𝜇VK-1) confirms the 𝑝-type conductivity of the films. The optical bandgap of CuYO2 was found to be 3.15 eV.

    • Preparation of high dielectric constant thin films of CaCu3Ti4O12 by sol–gel

      Deepam Maurya Devendra P Singh D C Agrawal Y N Mohapatra

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      Preparation of sol–gel derived CaCu3Ti4O12 (CCTO) thin films using two different sols and their characterization including their dielectric response are reported. The properties of CCTO films depend heavily on solvents used to prepare the sols. Dielectric constant as high as ∼900 at 100 kHz could be obtained when acetic acid was used to prepare the sol; in contrast, use of hexanoic acid in the sol yielded films with a much lower dielectric constant. The variation in grain and grain boundary conductivities with temperature has been measured. Activation energies of 0.08 eV and 0.68 eV have been found for grain and grain boundary conduction, respectively.

    • Preparation and antibacterial activity of Ag–TiO2 composite film by liquid phase deposition (LPD) method

      S-Q Sun B Sun Wenqin Zhang D Wang

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      A liquid phase deposition (LPD) method has been devised for the deposition of Ag–TiO2 thin films on ceramic tiles with glazed surface at a low temperature. The Ag–TiO2 thin films obtained were welladhered, homogenous and coloured by interference of reflected light. The films were characterized by X-ray diffraction and scanning electron microscopy. From these analyses, it was found that silver ions were trapped in TiO2 matrix and their reduction could be achieved at 600°C annealing temperature. The antibacterial activity against S. aureus and 𝐸. coli has been studied applying the so called antibacterial-drop test. The Ag–TiO2 thin films exhibited a high antibacterial activity. AAS was used for the quantitave determination of silver ion concentration releasing from the Ag–TiO2 thin film. The releasing rate of silver ions from the Ag–TiO2 film was 0.118 𝜇g/ml during 192 h. The antibacterial effect of Ag–TiO2 thin film before and after aging in a weathering chamber for 48 h was compared and the results show that the antibacterial activity is not compromised after weathering.

    • MOCVD of ZrO2 films from $bis(t$-butyl-3-oxo-butanoato)zirconium(IV): some theoretical (thermodynamic) and experimental aspects

      Sukanya Dhar M S Dharmaprakash S A Shivashankar

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      The equilibrium concentrations of various condensed and gaseous phases were calculated from thermodynamic modeling of MOCVD of ZrO2 films using a 𝛽-ketoesterate complex of zirconium as precursor. This leads to the construction of the `CVD phase stability diagram’ for the formation of solid phases. In the reactive ambient of oxygen, the calculations predict carbon-free ZrO2 film over a wide range of process conditions. The thermodynamic yields are in reasonable agreement with experimental observations, though the removal of carbon from the MOCVD grown films is not as complete as the thermodynamic calculations predict.

    • Electrical and optical properties of silicon-doped gallium nitride polycrystalline films

      S R Bhattacharyya A K Pal

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      Si-doped GaN films in polycrystalline form were deposited on quartz substrates at deposition temperatures ranging from 300–623 K using r.f. sputtering technique. Electrical, optical and microstructural properties were studied for these films. It was observed that films deposited at room temperature contained mainly hexagonal gallium nitride (ℎ-GaN) while films deposited at 623 K were predominantly cubic (𝑐-GaN) in nature. The films deposited at intermediate temperatures were found to contain both the hexagonal and cubic phases of GaN. Studies on the variation of conductivity with temperature indicated Mott’s hopping for films containing 𝑐-GaN while Efros and Shklovskii (E–S) hopping within the Coulomb gap was found to dominate the carrier transport mechanism in the films containing ℎ-GaN. A crossover from Mott’s hopping to E–S hopping in the `soft’ Coulomb gap was noticed with lowering of temperature for films containing mixed phases of GaN. The relative intensity of the PL peak at ∼ 2.73 eV to that for peak at ∼ 3.11 eV appearing due to transitions from deep donor to valence band or shallow acceptors decreased significantly at higher temperature. Variation of band gap showed a bowing behaviour with the amount of cubic phase present in the films.

    • Effects of electron beam irradiation on tin dioxide gas sensors

      Zheng Jiao Xiaojuan Wan Bing Zhao Huijiao Guo Tiebing Liu Minghong Wu

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      In this paper, the effects of electron beam irradiation on the gas sensing performance of tin dioxide thin films toward H2 are studied. The tin dioxide thin films were prepared by ultrasonic spray pyrolysis. The results show that the sensitivity increased after electron beam irradiation. The electron beam irradiation effects on tin dioxide thin films were simulated and the mechanism was discussed.

    • Synthesis and characterization of metal oxide nanorod brushes

      Kalyan Raidongia M Eswaramoorthy

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      Nanorod brushes of 𝛼-Al2O3, MoO3 and ZnO have been synthesized using amorphous carbon nanotube (𝑎-CNT) brushes as the starting material. The brushes of 𝛼-Al2O3 and MoO3 are made up of single crystalline nanorods. In the case of ZnO brushes, the nanorod bristles are made by the fusion of 15–25 nm size nanoparticles and are porous in nature. Metal oxide nanorod brushes thus obtained have been characterized by XRD, FESEM, TEM and Raman spectroscopy. Single crystalline ruby nanorods were obtained by introducing chromium ions during the synthesis of alumina rods.

    • Synthesis of iron oxide nanoparticles of narrow size distribution on polysaccharide templates

      M Nidhin R Indumathy K J Sreeram Balachandran Unni Nair

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      We report here the preparation of nanoparticles of iron oxide in the presence of polysaccharide templates. Interaction between iron (II) sulfate and template has been carried out in aqueous phase, followed by the selective and controlled removal of the template to achieve narrow distribution of particle size. Particles of iron oxide obtained have been characterized for their stability in solvent media, size, size distribution and crystallinity and found that when the negative value of the zeta potential increases, particle size decreases. A narrow particle size distribution with 𝐷100 = 275 nm was obtained with chitosan and starch templates. SEM measurements further confirm the particle size measurement. Diffuse reflectance UV–vis spectra values show that the template is completely removed from the final iron oxide particles and powder XRD measurements show that the peaks of the diffractogram are in agreement with the theoretical data of hematite. The salient observations of our study shows that there occurs a direct correlation between zeta potential, polydispersity index, bandgap energy and particle size. The crystallite size of the particles was found to be 30–35 nm. A large negative zeta potential was found to be advantageous for achieving lower particle sizes, owing to the particles remaining discrete without agglomeration.

    • Large scale synthesis and characterization of Ni nanoparticles by solution reduction method

      Huazhi Wang Xinli Kou Jie Zhang Jiangong Li

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      Ni nanoparticles were mass synthesized by solution reduction process successfully. The influence of the parameters on the particle size of Ni nanoparticles were studied and the referential process parameters were obtained. The morphology and structure of the synthesized Ni nanoparticles were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET) surface area analysis and infrared spectroscopy (IR). The results show that Ni nanoparticles are of high purity and are covered by hydroxyethyl carboxymethyl cellulose (HECMC) layer and the mean size being about 31 nm. The magnetic measurement revealed that Ni nanoparticles are ferromagnetic.

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