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      Volume 26, Issue 7

      December 2003,   pages  655-773

    • Synthesis and characterization of biocompatible hydroxyapatite coated ferrite

      S Deb J Giri S Dasgupta D Datta D Bahadur

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      Ferrite particles coated with biocompatible phases can be used for hyperthermia treatment of cancer. We have synthesized substituted calcium hexaferrite, which is not stable on its own but is stabilized with small substitution of La. Hexaferrite of chemical composition (CaO)0.75(La2O3)0.20(Fe2O3)6 was prepared using citrate gel method. Hydroxyapatite was prepared by precipitating it from aqueous solution of Ca(NO3)2 and (NH4)2HPO4 maintaining pH above 11. Four different methods were used for coating of hydroxyapatite on ferrite particles. SEM with EDX and X-ray diffraction analysis shows clear evidence of coating of hydroxy-apatite on ferrite particles. These coated ferrite particles exhibited coercive field up to 2 kOe, which could be made useful for hysteresis heating in hyperthermia. Studies by culturing BHK-21 cells and WBC over the samples show evidence of biocompatibility. SEM micrographs and cell counts give clear indication of cell growth on the surface of the sample. Finally coated ferrite particle was implanted in Kasaulli mouse to test its biocompatibility. The magnetic properties and biocompatibility studies show that these hydroxyapatite coated ferrites could be useful for hyperthermia.

    • Aging of trivalent metal hydroxide/oxide gels in divalent metal salt solutions: Mechanism of formation of layered double hydroxides (LDHs)

      A V Radha P Vishnu Kamath

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    • A simple red-ox titrimetric method for the evaluation of photo-catalytic activity of titania based catalysts

      Y S Satpute S A Borkar S R Dharwadkar

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      A simple red-ox titrimetry method has been developed for rapid evaluation of the photo catalytic activity of TiO2 based photo-catalysts. The analytical procedure employs monitoring the kinetics of a simple one electron transfer reduction reaction of conversion of Ce4+ to Ce3+ in dilute aqueous solution in presence of sunlight. The photo-catalytic activity of TiO2 synthesized by two different routes was evaluated by the above technique. The effect of surface area, crystallite size and polymorphic contents on the photo-catalytic activity of TiO2 was also studied employing this method.

    • Electrochemical properties of tungsten oxysulphide thin films as positive electrodes for lithium microbatteries

      I Martin-Litas P Vinatier A Levasseur J C Dupin D Gonbeau

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      Several WO𝑦S𝑧 tungsten oxysulphide thin films were tested as positive electrodes for lithium microbatteries. The amorphous WO1.05S2 thin film was found very promising. A capacity decrease occurred during the first few cycles, after which the films were able to intercalate reversibly up to 1.1 lithium ion per formula unit under high regime (75 𝜇A/cm2). They were tested for 250 charge–discharge cycles, between 3.0 V and 1.2 V. X-ray photoelectron spectroscopy measurements were performed on different compounds in both intercalated (Li1WO1.05S2, Li2.7WO1.05S2 and Li3.8WO1.05S2) and partially de-intercalated (Li1WO1.05S2) states in order to understand the redox processes occurring during the first discharge–charge cycle. The analysis of both the W4𝑓 and the S2𝑝 peaks has shown that the redox processes involve not only the tungsten atoms but also sulphur atoms. At the beginning of the intercalation, W6+ was first partially reduced into W5+, and then into W4+, but the important stage was the reduction of W4+ into W0. In W0, the electron binding energy was very close to that of metallic tungsten. At the same time, S$^{2-}_2$ ions were partially reduced into S2- ions. But only the reduction process of tungsten atoms appeared to be totally reversible.

    • Optical band gap of Sn0.2Bi1.8Te3 thin films

      P H Soni M V Hathi C F Desai

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      Sn0.2Bi1.8Te3 thin films were grown using the thermal evaporation technique on a (001) face of NaCl crystal as a substrate at room temperature. The optical absorption was measured in the wave number range 500–4000 cm-1. From the optical absorption data the band gap was evaluated and studied as a function of film thickness and deposition temperature. The data indicate absorption through direct interband transition with a band gap of around 0.216 eV. The detailed results are reported here.

    • Influence of growth parameters on the surface morphology and crystallinity of InSb epilayers grown by liquid phase epitaxy

      N K Udayashankar H L Bhat

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      Unintentionally doped homoepitaxial InSb films have been grown by liquid phase epitaxy employing ramp cooling and step cooling growth modes. The effect of growth temperature, degree of supercooling and growth duration on the surface morphology and crystallinity were investigated. The major surface features of the grown film like terracing, inclusions, meniscus lines, etc are presented step-by-step and a variety of methods devised to overcome such undesirable features are described in sufficient detail. The optimization of growth parameters have led to the growth of smooth and continuous films. From the detailed morphological, X-ray diffraction, scanning electron microscopic and Raman studies, a correlation between the surface morphology and crystallinity has been established.

    • Electrical characterization of low temperature deposited oxide films on ZnO/𝑛-Si substrate

      S K Nandi S Chatterjee S K Samanta P K Bose C K Maiti

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      Thin films of silicon dioxide are deposited on ZnO/𝑛-Si substrate at a low temperature using tetraethylorthosilicate (TEOS). The ZnO/𝑛-Si films have been characterized by atomic force microscopy (AFM) and scanning electron microscopy (SEM). The border trap density (𝑄bt) and fixed oxide charge density (𝑄f/𝑞) of the SiO2/ZnO/𝑛-Si films are found to be 3.9 × 1010 cm-2 and 1.048 × 1011 cm-2, respectively. The trapping characteristics and stress induced leakage current (SILC) have also been studied under Fowler–Nordheim (F–N) constant current stressing.

    • Leaching of 60Co and 137Cs from spent ion exchange resins in cement–bentonite clay matrix

      I B Plecas R S Pavlovic S D Pavlovic

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      The leaching rate of 60Co and 137Cs from the spent cation exchange resins in cement–bentonite matrix has been studied. The solidification matrix was a standard Portland cement mixed with 290–350 (kg/m3) spent cation exchange resins, with or without 2–5% of bentonite clay. The leaching rates from the cement–bentonite matrix for 60Co: (4,2–7,0) × 10-5 (cm/d) and 137Cs: (3,2–6,6) × 10-4 (cm/d), after 125 days were measured. From the leaching data the apparent diffusivity of cobalt and cesium in cement–bentonite clay matrix with a waste load of 290–350 (kg/m3) spent cation exchange resins, was measured for 60Co: (1,1–4,0) × 10-6 (cm2/d) and 137Cs: (0,5–2,6) × 10-4 (cm2/d), after 125 days. The results presented in this paper are part of the results obtained in a 20-year mortar and concrete testing project which will influence the design of radioactive waste management for a future Serbian radioactive waste disposal centre.

    • Solid state sintering of lime in presence of La2O3 and CeO2

      T K Bhattacharya A Ghosh H S Tripathi S K Das

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      The sintering of lime by double calcination process from natural limestone has been conducted with La2O3 and CeO2 additive up to 4 wt.% in the temperature range 1500–1650°C. The results show that the additives enhanced the densification and hydration resistance of sintered lime. Densification is achieved up to 98.5% of the theoretical value with La2O3 and CeO2 addition in lime. Grain growth is substantial when additives are incorporated in lime. The grain size of sintered CaO (1600°C) with 4 wt.% La2O3 addition is 82 𝜇m and that for CeO2 addition is 50 𝜇m. The grains of sintered CaO in presence of additive are angular with pores distributed throughout the matrix. EDX analysis shows that the solid solubility of La2O3 and CeO2 in CaO grain is 2.9 and 1.7 weight %, respectively. The cell dimension of CaO lattice is 4.803 Å. This value decreases with incorporation of La2O3 and CeO2. The better hydration resistance of La2O3 added sintered lime compared to that of CeO2 added one, is related to the bigger grain size of the lime in former case.

    • Morphology and conductivity studies of a new solid polymer electrolyte: (PEG)𝑥LiClO4

      Th Joykumar Singh S V Bhat

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      A new solid polymer electrolyte, (PEG)𝑥LiClO4, consisting of poly(ethylene)glycol of molecular weight 2000 and LiClO4 was prepared and characterized using XRD, IR, SEM, DSC, NMR and impedance spectroscopy techniques. XRD and IR results show the formation of the polymer–salt complex. The samples with higher salt concentration are softer, less opaque and less smooth compared to the low salt concentration samples. DSC studies show an increase in the glass transition temperature and a decrease in the degree of crystallinity with increase in the salt concentration. Melting temperature of SPEs is lower than the pure PEG 2000. Room temperature 1H and 7Li NMR studies were also carried out for the (PEG)𝑥iClO4 system. The 1H linewidth decreases as salt concentration increases in a similar way to the decrease in the crystalline fraction and reaches a minimum at around 𝑥 = 46 and then increases. 7Li linewidth was found to decrease first and then to slightly increase after reaching a minimum at 𝑥 = 46 signifying the highest mobility of Li ions for this composition. Room temperature conductivity first increases with salt concentration and reaches a maximum value (𝜎 = 7.3 × 10-7 S/cm) at 𝑥 = 46 and subsequently decreases. The temperature dependence of the conductivity can be fitted to the Arrhenius and the VTF equations in different temperature ranges. The ionic conductivity reaches a high value of ∼ 10-4 S/cm close to the melting temperature.

    • Preparation and studies of some thermal, mechanical and optical properties of 𝑥Al2O3(1 – 𝑥)NaPO3 glass system

      K V Shah V Sudarsan M Goswami A Sarkar S Manikandan Rakesh Kumar B I Sharma V K Shrikhande G P Kothiyal

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      Sodium aluminophosphate glasses having compositions of 𝑥Al2O3(1 – 𝑥)NaPO3 (𝑥 = 0.05–0.2) were prepared using conventional melt-quench technique. Density, glass transition temperature, microhardness (MH), thermal expansion coefficient (TEC) and transmission characteristics were measured as a function of alumina content for different samples. They were found to depend on O/P ratio with pronounced changes taking place for O/P ratio ≥ 3.5. Density, glass transition temperature and microhardness were found to increase up to 15 mol% of alumina and then they showed a decreasing trend. Thermal expansion coefficient decreased continuously with alumina content. Optical gaps for different glass samples as measured from transmission characteristics were found to be in the range 3.13–3.51 eV. It initially decreased with alumina content up to 15 mol% and then increased. The behaviour was explained on the basis of change in the average aluminum coordination number from six Al(6) to four Al(4) (i.e. Al(OP)6/Al(OP)4 ratio) along with the changes in polyhedra linkages in the glass network due to change in O/P ratio.

    • Carbonization and demineralization of coals: A study by means of FT–IR spectroscopy

      V Gómez-Serrano M C Fernández-González M L Rojas-Cervantes M F Alexandre-Franco A Macías-García

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      Coal basically consists of two parts-a crystalline, inorganic part, and an amorphous, organic part. Based on this, we intended to study the changes that occurred on the composition and on the chemical structure of coals after carbonization at 1000 or 900°C and demineralization treatments with hydrochloric and hydrofluoric acids. For this, four coals of different categories (or levels) were chosen: semianthracite (A–O) and high volatile bituminous coal (B–O), which are high level coals, and lignite (Li–O) and leonardite (Le–O), these being low level coals. The coals were first analysed in terms of their proximate and elemental compositions and then carbonized and demineralized. Also, the starting coals and the prepared samples were examined by infrared spectroscopy. In addition, a study of the optimization of the application of this technique for only A–O was carried out. For A–O and B–O, the spectra recorded intense absorption bands that are ascribable to vibration modes in mineral components as quartz and aluminosilicates, such as kaolinite. For Li–O and Le–O, the spectra displayed some other bands as well, also quite intense, which have been assigned to bond vibrations in functional groups and structures of their organic part. The carbonization of the coals resulted in significant changes in their inorganic part as the content of quartz increased and the content of aluminosilicates decreased. In addition, the thermal decomposition of mineral carbonates occurred. The carbonization greatly affects the organic part of the coals, especially in Li–O and Le–O, as most functional groups and structures are not thermally stable under heating conditions. With regard to demineralization, HF is a more effective agent than HCl, achieving products with higher organic content. The mass losses are higher in Li–O and Le–O than in A–O and B–O. So, the infrared spectroscopy allows the analysis of both inorganic and organic parts of the coals and of their carbonization and demineralization products. These processes facilitate subsequent analysis of the inorganic and organic parts of coals by infrared spectroscopy. In the application of this technique, both the coal:KBr ratio and the thickness for the disks should be controlled, owing to the influence on the infrared absorption.

    • Synthesis, characterization and low frequency a.c. conduction of polyaniline/fly ash composites

      S C Raghavendra Syed Khasim M Revanasiddappa M V N Ambika Prasad A B Kulkarni

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      in situ polymerization of aniline was carried out in the presence of fly ash (FA) to synthesize polyaniline/fly ash (PANI/FA) composites. The PANI/FA composites have been synthesized with various compositions (15, 20, 30 and 40 wt%) of FA in PANI. The composites, thus synthesized have been characterized by infrared spectroscopy and X-ray diffraction. The morphology of these samples was studied by scanning electron microscopy. Further the a.c. conductivity of these composites have been investigated in the frequency range 102–106 Hz. The presence of polarons and bipolarons are made responsible for frequency dependence of a.c. conductivity in these composites. The Cole–Cole plots indicate clear shift in the distribution of relaxation times as the wt% of FA in PANI changes. These composites show almost symmetric semicircles of Cole–Cole plots indicating the Debye-type relaxation in their polarization response.

    • Comparative study of dielectric properties of MgNb2O6 prepared by molten salt and ceramic method

      Vishnu Shanker Ashok K Ganguli

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      Magnesium niobate (MgNb2O6) powder was synthesized by the conventional ceramic route as well as by the molten salt route using a eutectic mixture of NaCl–KCl as the salt and Mg(NO3)$_2\cdot$6H2O and TiO2 as the starting materials. Pure phase of MgNb2O6 could be obtained by the molten salt method at 1100°C. However, in ceramic method the pure phase of MgNb2O6 was obtained by heating at 1025°C for 20 h. On sintering at 1100°C the dielectric constant and dielectric loss of MgNb2O6 obtained by the molten salt method was found to be 19.5 and 0.004 at 100 kHz at room temperature. Lower values were obtained for these oxides prepared by the ceramic route, 16.6 and 0.000518, respectively. In both cases the dielectric constant was quite stable with frequency.

    • Dielectric properties of piezoelectric 3–0 composites of lithium ferrite/barium titanate

      P Sarah S V Suryanarayana

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      Piezoelectric 3–0 composite ceramics are prepared from a mixture of barium titanate and lithium ferrite phase constituents. Dielectric properties of composites are affected by a number of parameters that include electrical properties, size, shape and amount of constituent phases. The frequency dependent measurements can provide additional insight into mechanisms controlling electrical response. Frequency dependence of dielectric constant plots of lithium ferrite/barium titanate composites will be given and the relevance of trends seen in them will be discussed. Connectivity in composites developed is studied.

    • Influence of fretting on the fatigue strength at the vise clamp–specimen interface

      Abdulhaqq A Hamid Rafi K Yahya

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      Fretting fatigue is one of the most important phenomena for inducing a significant reduction of fatigue strength and consequently, leading to unexpected failure accidents of the engineering structures even at very low stresses. In the present study, both plain and fretting fatigue tests with zero mean stress were carried out on two different types of steel, low-carbon steel and martensitic stainless steel, by means of a reversed bending fatigue testing machine. The drop in the fatigue strengths through fretting at vise clamp–specimen interface were significant for both tested steels. The fretting processes produced a reduction in fatigue strength of about 27% for low-carbon steel and 16% for martensitic stainless steel.

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