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      Volume 32, Issue 1

      February 2009,   pages  1-115

    • Prospects of microwave processing: An overview

      S Das A K Mukhopadhyay S Datta D Basu

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      Microwave processing has been emerging as an innovative sintering method for many traditional ceramics, advanced ceramics, specialty ceramics and ceramic composites as well as polymer and polymer composites. Development of functionally gradient materials: joining; melting; fibre drawing; reaction synthesis of ceramics; synthesis of ceramic powder, phosphor materials, whiskers, microtubes and nanotubes; sintering of zinc oxide varistors; glazing of coating surface and coating development have been performed using microwave heating. In addition, microwave energy is being explored for the sintering of metal powders also. Ceramic and metal nanopowders have been sintered in microwave. Furthermore, initiatives have been taken to process the amorphous materials (e.g. glass) by microwave heating. Besides this, attempt has been made to study the heating behaviour of materials in the electric and magnetic fields at microwave frequencies. The research is now focused on the use of microwave processing for industrial applications.

    • 2-Methoxycycloocta-1,5-dienyl platinum complexes as precursors for platinum nanoparticles

      Ninad Ghavale Sandip Dey Vimal K Jain R Tewari

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      Thermolysis of [Pt2 (𝜇-OR)2 (C8H12OMe)2] (R = Me or Ac) in hexadecylamine (HDA) at 210°C under argon atmosphere gave platinum nanoparticles which were characterized by XRD, EDAX and TEM analysis. Both spherical (∼ 10 nm) and rod-like (∼ 19 nm length with aspect ratio of 2.3) face centred cubic (fcc) platinum metal nanoparticles could be isolated. The thermogravimetric analyses of these complexes revealed that they undergo a single step decomposition leading to the formation of platinum metal powder.

    • Modeling nano-scale grain growth of intermetallics

      Mohsen Kazeminezhad

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      The Monte Carlo simulation is utilized to model the nano-scale grain growth of two nanocrystalline materials, Pd81Zr19 and RuAl. In this regard, the relationship between the real time and the time unit of simulation, i.e. Monte Carlo step (MCS), is determined. The results of modeling show that with increasing time of heating, the grain sizes of both nano-crystalline materials increased as in the case of conventional materials. Moreover, it is found that for both nano-crystalline materials the relationship between the real time and MCS is in power law form, which is linear for the conventional materials.

    • Preparation and characterization of nanostructured ZnO thin films for photoelectrochemical splitting of water

      Monika Gupta Vidhika Sharma Jaya Shrivastava Anjana Solanki A P Singh V R Satsangi S Dass Rohit Shrivastav

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      Nanostructured zinc oxide thin films (ZnO) were prepared on conducting glass support (SnO2: F overlayer) via sol–gel starting from colloidal solution of zinc acetate 2-hydrate in ethanol and 2-methoxy ethanol. Films were obtained by spin coating at 1500 rpm under room conditions (temperature, 28–35°C) and were subsequently sintered in air at three different temperatures (400, 500 and 600°C). The evolution of oxide coatings under thermal treatment was studied by glancing incidence X-ray diffraction and scanning electron microscopy. Average particle size, resistivity and bandgap energy were also determined. Photoelectrochemical properties of thin films and their suitability for splitting of water were investigated. Study suggests that thin films of ZnO, sintered at 600°C are better for photoconversion than the films sintered at 400 or 500°C. Plausible explanations have been provided.

    • Wavelength dependent laser-induced etching of Cr–O doped GaAs: Morphology studies by SEM and AFM

      B Joshi S S Islam H S Mavi Vinita Kumari T Islam A K Shukla Harsh

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      The laser induced etching of semi-insulating GaAs $\langle$100$\rangle$ is carried out to create porous structure under super- and sub-bandgap photon illumination (ℎν). The etching mechanism is different for these separate illuminations where defect states play the key role in making distinction between these two processes. Separate models are proposed for both the cases to explain the etching efficiency. It is observed that under sub-bandgap photon illumination the etching process starts vigorously through the mediation of intermediate defect states. The defect states initiate the pits formation and subsequently pore propagation occurs due to asymmetric electric field in the pore. Formation of GaAs nanostructures is observed using scanning electron (SEM) and atomic force microscopy (AFM).

    • Structural, optical and electrical properties of chemically deposited copper selenide films

      R H Bari V Ganesan S Potadar L A Patil

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      Stoichiometric and nonstoichiometric thin films of copper selenide have been prepared by chemical bath deposition technique at temperature below 60°C on glass substrate. The effect of nonstoichiometry on the optical, electrical and structural properties of the film was studied. The bandgap energy was observed to increase with the increase in at % of copper in composition. The grain size was also observed to increase with the decrease of at % of copper in composition. The films were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDS), absorption spectroscopy, and AFM. The results are discussed and interpreted.

    • Structural characterization of lead sulfide thin films by means of X-ray line profile analysis

      N Choudhury B K Sarma

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      X-ray diffraction patterns of chemically deposited lead sulphide thin films have been recorded and X-ray line profile analysis studies have been carried out. The lattice parameter, crystallite size, average internal stress and microstrain in the film are calculated and correlated with molarities of the solutions. Both size and strain are found to contribute towards the broadening of X-ray diffraction line. The values of the crystallite size are found to be within the range from 22–33 nm and the values of strain to be within the range from 1.0 × 10-3–2.5 × 10-3.

    • Fabrication and characterization of S. cilliare fibre reinforced polymer composites

      A S Singha Vijay Kumar Thakur

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      In the recent times, there has been an ever-increasing interest in green composite materials for its applications in the field of industries, aerospace, sports, household etc and in many other fields. In this paper, fabrication of Saccharum cilliare fibre reinforced green polymer composites using resorcinol formaldehyde (RF) as a novel matrix has been reported. A systematic approach for processing of polymer is presented. Effect of fibre loading on mechanical properties like flexural, tensile, compressive and wear resistances has also been determined. Reinforcing of the RF resin with Saccharum cilliare (SC) fibre was done in the form of particle size (200 micron). Present work reveals that mechanical properties of the RF resin have been found to increase up to 30% fibre loading and then decreases. Morphological and thermal studies of the resin, fibre and particle reinforced (P-Rnf) green composites have also been studied.

    • Effect of ellipse orientation on the thermoelastic behaviour of skew laminated composite plate with elliptical cutout

      M S R Niranjan Kumar M M M Sarcar V Bala Krishna Murthy K M Rao

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      An effort is made to study the thermoelastic behaviour of a cross-ply laminated composite skew plate with elliptical cutout subjected to pressure and non-linearly varying temperature loading in the present analysis. Orientation of the elliptical cut out is varied from 0° to 180° with respect to horizontal at an interval of 30° in the anti clockwise direction is considered for the present analysis. A three-dimensional heat conduction analysis in fibre reinforced composite laminates has been simulated by finite element method to get realistic temperature in the laminate under different thermal boundary conditions. A finite element method, which works on the basis of three-dimensional theory of elasticity, is employed to evaluate the stresses and deformations. The effect of orientation due to pressure loading on the stresses and transverse deflection is observed to be insignificant. The magnitudes of the in-plane normal stresses, 𝜎x and 𝜎y, for temperature loading are greatly affected by ellipse orientation and are observed to be minimum at the ellipse orientation of 0° and 90°, respectively. The in-plane and inter-laminar shear stresses are observed to be minimum at the ellipse orientation of 90°.

    • Influence of fibre-surface treatment on structural, thermal and mechanical properties of jute fibre and its composite

      E Sinha S K Rout

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      Jute fibres (Corchorus olitorious), an environmentally and ecologically friendly product, were chemically modified and treated with 5% NaOH solution at room temperature for 2 h, 4 h and 8 h. The above samples were characterized and morphologically analysed by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT–IR), differential scanning calorimetry (DSC), scanning electron microscopy (SEM) and Instron 1185. Alkali treatment affects the supramolecular structure of the fibre as shown by XRD by improving the degree of crystallinity of the fibre. Surface chemistry of the fibre also altered as depicted by FT–IR studies. This chemical treatment was also found to alter the characteristic of the fibre surface topography as seen by the SEM. From the mechanical single fibre test it was found that the tenacity and modulus of the fibre improved after alkali treatment. This might be due to the improvement in the crystallinity. DSC data demonstrated that the thermal degradation temperature for the cellulose get lowered from 365.26°C to 360.62°C after alkali treatment led to the reduction in fibre thermal stability. Jute fibre reinforced composite were prepared with treated and untreated jute fibre (15 wt%) reinforced unsaturated polyester (UPE). Effectiveness of these composites was experimentally investigated through the study of the composites by DSC, Instron 1195 for mechanical property of composites, volume fraction of the porosity and hydrophobic finishing of the composite. From the DSC analysis it was found that thermal stability enhanced for treated fibre reinforced composite. This could be due to the resistance offered by the closely packed cellulose chain in combination with the resin. Flexural strength of the composite prepared with 2 h and 4 h alkali treated fibre were found to increase by 3.16% and 9.5%, respectively. Although 8 h treated fibre exhibited maximum strength properties, but the composite prepared with them showed lower strength value. Alkali treatment helped in the development of hydrophobicity and reduction in volume fraction of the porosity. This may be due to the better fibre matrix interface adhesion caused due to the fibre surface treatment by alkali.

    • Effects of fibre content on mechanical properties and fracture behaviour of short carbon fibre reinforced geopolymer matrix composites

      Tiesong Lin Dechang Jia Meirong Wang Peigang He Defu Liang

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      Geopolymer matrix composites reinforced with different volume fractions of short carbon fibres (Cf/geopolymer composites) were prepared and the mechanical properties, fracture behaviour and microstructure of as-prepared composites were studied and correlated with fibre content. The results show that short carbon fibres have a great strengthening and toughening effect at low volume percentages of fibres (3.5 and 4.5 vol.%). With the increase of fibre content, the strengthening and toughening effect of short carbon fibres reduce, possibly due to fibre damage, formation of high shear stresses at intersect between fibres and strong interface cohesion of fibre/matrix under higher forming pressure. The property improvements are primarily based on the network structure of short carbon fibre preform and the predominant strengthening and toughening mechanisms are attributed to the apparent fibre bridging and pulling-out effect.

    • Enhancement in electrical conductivity of Li2O : B2O3 : V2O5 glasses

      R S Gedam V K Deshpande

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      The study of electrical conductivity of 30Li2O : (70 – 𝑥) B2O3 : 𝑥V2O5 glass samples has been carried out. The results have been explained by dividing the temperature range into two regions. In region I, conductivity shows Arrhenius behaviour for all the samples. The conductivity increases with addition of V2O5. The results have been explained in the light of Anderson and Stuart Model. In region II, an anomalous enhancement in the conductivity is observed for all the samples up to certain temperature beyond which the conductivity decreases. The enhancement in the conductivity in the annealed glass sample has been attributed to nanocrystallization.

    • Study of variation of thermal diffusivity of advanced composite materials of E-glass fibre reinforced plastic (GFRP) in temperature range 5–300 K

      Kalobaran Das S M Kamaruzzaman Tapas Ranjan Middya Siddhartha Datta

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      Modified Angstrom method is applied to study the variation of thermal diffusivity of plain woven fabric composite in closed cycle cryo-refrigerator (CCR) based set up in the temperature range 5–300 K. The set up used is plug in type and its small size offers portability. The set up works without use of any liquid cryogen. The temperature versus thermal diffusivity curve shows three distinct regions viz. 5–30 K, 30–120 K and 120–300 K. In the first region thermal diffusivity varies exponentially and rapidly. In the second region thermal diffusivity changes exponentially but relatively slowly than that in the first region. In the last region the change in thermal diffusivity with temperature is exponential in nature but very slow.

    • Influence of seeding on crystallization behaviour of BaNaB9O15 glasses

      Rahul Vaish K B R Varma

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      Transparent BaNaB9O15 (BNBO) glasses were fabricated via the conventional melt-quenching technique. X-ray powder diffraction (XRD) followed by differential scanning calorimetric (DSC) studies confirmed the amorphous and glassy nature of the as-quenched samples, respectively. The effect of seeding on the crystallization of BNBO glasses was studied by non-isothermal DSC method and was modeled using the Johnson–Mehl–Avrami and Ozawa equations. The activation energy for seeded glasses decreased with the increase in fraction of crystallization. The values for the onset of crystallization and Avrami exponent were found to be lower for seeded samples which were associated with the heterogeneous nucleation and epitaxial processes.

    • Effect of substitution of titanium by magnesium and niobium on structure and piezoelectric properties in (Bi1/2Na1/2)TiO3 ceramics

      Zhou Chang-Rong Liu Xin-Yu Li Wei-Zhou Yuan Chang-Lai

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      To develop new (Bi1/2Na1/2)TiO3-based ceramics with excellent piezoelectric properties, the similarities and the differences between PZT and (Bi1/2Na1/2)TiO3 ceramics were analysed. Based on the analysis, a new (Bi1/2Na1/2)TiO3-based piezoelectric ceramic of B-site substitution of complex ions (Mg1/3Nb2/3)4+ for Ti4+ was prepared by a conventional ceramic technique, and effect of complex ions (Mg1/3Nb2/3)4+ addition on the microstructure, dielectric and piezoelectric properties was investigated. The results show that all compositions are mono-perovskite phase and the grain size increases with increasing content of (Mg1/3Nb2/3)4+. The piezoelectric constant, 𝑑33, first increases and then decreases, and electromechanical coupling factor, 𝑘p, varies insignificantly with increasing content of (Mg1/3Nb2/3)4+.

    • X-ray absorption spectroscopy of PbMoO4 single crystals

      D Bhattacharyya A K Poswal S N Jha Sangeeta S C Sabharwal

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      X-ray absorption spectra of PbMoO4 (LMO) crystals have been investigated for the first time in literature. The measurements have been carried out at Mo absorption edge at the dispersive EXAFS beamline (BL-8) of INDUS-2 Synchrotron facility at Indore, India. The optics of the beamline was set to obtain a band of 2000 eV at 20,000 eV and the channels of the CCD detector were calibrated by recording the absorption edges of standard Mo and Nb foils in the same setting. The absorption spectra have been measured for three LMO samples prepared under different conditions viz.

      1. grown in air from stoichiometric starting charge,

      2. grown in argon from stoichiometric starting charge and

      3. grown in air from PbO-rich starting charge.

      The results have been explained on the basis of the defect structure analysed in LMO crystals prepared under different conditions. The Mo absorption edge is significantly influenced by the deviations in crystal stoichiometry.

    • Growth, characterization and transport properties of Pb𝑥Zn1–𝑥S mixed crystals

      M Nagabhushanam E Nagabushan D Jaya Prakash B Rajam K Yadaiah

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      The polycrystalline Pb𝑥Zn1–𝑥S semiconductor powder with (0 ≤ 𝑥 ≤ 0.5) has been prepared by controlled co-precipitation method from an alkaline medium using thiourea as a sulphide ion source. Pellets are made with these powders applying 10 ton/sq.cm. pressure and sintered at 800°C for 2 h in nitrogen atmosphere. X-ray studies of these samples have indicated that the compounds are polycrystalline in nature with mixed hexagonal and cubic structure of ZnS and cubic structure of PbS. Lattice parameters (𝑎 and 𝑐) of all the compounds are determined from the X-ray data and are found to decrease nonlinearly with increase in Pb concentration (𝑥). It is also observed that the grain size of the crystallites increases in samples with 𝑥 = 0–0.5. Scanning electron micrographs have shown that both cubic and hexagonal crystallites are present in the mixed crystals. The electrical conductivity in Pb𝑥Zn1–𝑥S is found to decrease with increase in composition (𝑥 = 0–0.5), whereas it increases at all temperatures in all samples. Mobility of charge carrier concentration is found to increase with increasing temperature. The increase in carrier mobility in Pb𝑥Zn1–𝑥S samples may be due to reduced grain boundary potential. In Pb𝑥Zn1–𝑥S samples with 𝑥 = 0–0.3, the sum of the activation energy due to charge carriers and grain boundary potential is equal to the activation energy due to conductivity.

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