• Issue front cover thumbnail

      Volume 33, Issue 5

      October 2010,   pages  519-645

    • Size variation of polyaniline nanoparticles dispersed in polyvinyl alcohol matrix

      J Bhadra D Sarkar

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      We report the preparation of polyaniline (PANI) nanoparticles dispersed in polyvinyl alcohol (PVA) matrix. From SEM picture it is seen that the particle sizes vary from 100–20 nm. Also with increase in PVA content the stability of dispersion is found to increase. Apart from SEM, spin cast films of PANI in PVA are also characterized through XRD and FTIR. XRD shows increase in crystallinity with PVA content and FTIR gives evidence of crosslinking between PANI and PVA molecules. In plane electrical conductivity (in the range of 102 Scm-1) and the exponent of nonlinear 𝐼–𝑉 are found to decrease with increase of PVA content. There is a good correlation between SEM, XRD, FTIR and electrical properties.

    • Effect of nanoparticles on tensile, impact and fatigue properties of fibre reinforced plastics

      R Nagalingam S Sundaram B Stanly Jones Retnam

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      Advanced composite, fibre-reinforced polymer (FRP), has been favoured for certain aerospace, military, marine and automotive applications. Polymer nanocomposites containing layered silicates have attracted much attention. These exhibit increased modulus, decreased thermal expansion coefficient, increased solvent resistance and enhanced ionic conductivity when compared to the polymer alone. Here we have developed eight different combinations of composites FRP with nanoclay (montmorillonite) by layered manufacturing techniques (LM) and measured the mechanical properties. The measurement showed that the tensile strength, impact strength and fatigue life are greatly increased. A plausible explanation for high increase of properties has also been discussed.

    • Dispersion effect and auto-reconditioning performance of nanometer WS2 particles in green lubricant

      Shi Chen Mao Daheng Zhou Ming

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      This paper reported on dispersion effect and dispersing techniques of nanometer WS2 particles in the green lubricant concocted by us. And it also researched on auto-reconditioning performance of nanometer WS2 particles to the abrasive surfaces of steel ball from four-ball tribology test and piston ring from engine lubrication test. The treated and untreated nanometer WS2 particles were analysed by infrared spectrum. And the elementary component and interior elementary distribution of abrasive surface repaired by nanometer WS2 particles were analysed by multifunction electron spectrometer. The results showed that the combinative method of ultrasonic dispersion, mechanical agitation and surface modification could improve the dispersion uniformity and stability of nanometer WS2 particles in the green lubricant effectively. And the optimal ratio of the mass between surface modifier and nanometer WS2 particles was 1 : 2.5, the optimal treating time was 5 h. And IR analysis indicated that surface modifier could react with hydroxide radicals on surfaces of WS2 particles and modify the surfaces, and the long lipophilic groups on surfaces of nanometer WS2 particles could stretch in oil adequately and form steric hindrance layers between particles which prevented particles from conglomerating and depositing. In addition, tribological tests and surface analysis indicated that there were WS2 adsorption film and reaction film on abrasive surfaces during the tribological tests, which could fill and level up the furrows on abrasive surfaces. As a result, the abrasive surfaces were repaired effectively by nanometer WS2 particles.

    • Effect of solvent-induced structural modifications on optical properties of CdS nanoparticles

      Puja Chawla Geeta Sharma S P Lochab Nafa Singh

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      We have investigated the effects of solvent used during synthesis on structural and optical properties of CdS quantum dots. Different methods of synthesis for the production of CdS quantum dots are presented. These are:

      1. wet chemical co-precipitation in non-aqueous medium (i.e. methanol);

      2. wet chemical co-precipitation in aqueous medium (deionized water) and

      3. solid state reaction.

      It is demonstrated that the use of methanol as solvent leads to a strong enhancement of PL intensity of CdS quantum dots for use in optoelectronic devices.These products were characterized by X-ray powder diffraction (XRD), high resolution transmission electron microscopy (HRTEM) and scanning electron microscopy (SEM). The change in bandgap with size-quantization was investigated by UV-VIS absorption spectroscopy. CdS nanocrystals prepared in non-aqueous medium have narrow size distribution than those prepared in aqueous medium and solid state reaction. Phase transformation of CdS nanocrystals from a cubic to hexagonal structure was observed in methanol solution. The formation of CdS/Cd(OH)2 nanostructure was also confirmed using X-ray diffraction pattern. This suggests that the strong enhancement of the PL intensity may have originated from the remarkable reduction of non-radiative recombination process, due to surface defects of quantum dots. The red shift of the Raman peaks compared to that for bulk CdS may be attributed to optical phonon confinement.

    • Rapid synthesis of CdSe nanocrystals in aqueous solution at room temperature

      Yilin Wang Jian Ping Lu Zhang Fa Tong

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      Water-soluble thioglycolic acid-capped CdSe nanocrystals (NCs) were prepared in aqueous solution at room temperature. We investigated the effects of pH values on the fluorescence intensity of the as-prepared CdSe NCs, and discussed the influence of the initial pH values on the fluorescence property. Their mean diameter was estimated to be 1.9 nm depending on the initial pH values in the preparation, the photoluminescence quantum yield could reach as high as 1.9%, almost comparable to the CdSe NCs prepared by an organometallic route. Finally, the products were characterized by Fourier transform infrared spectrometry (FTIR), atomic force microscope (AFM) and X-ray powder diffraction (XRD). AFM image showed that the NCs were ball-shaped with good dispersibility. XRD analysis disclosed that the CdSe NCs were of cubic zinc-blended structure.

    • Effects of reaction temperature on size and optical properties of CdSe nanocrystals

      Shutang Chen Xiaoling Zhang Yanbing Zhao Qiuhua Zhang

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      We report experimental results on the reaction temperature dependence of luminescence properties in size-controlled CdSe nanocrystals. Such reaction temperature dependent property is also sizedependent. The diameter of the CdSe nanocrystals is tuned from 4–11.0 nm by varying the reaction temperatures. The growth process and characterization of CdSe nanocrystals are determined by photoluminescence (PL) spectroscopy, ultraviolet-visible (UV–Vis) spectroscopy, X-ray photoelectron spectrometry (XPS), X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM). The influence of reaction conditions on the growth of CdSe nanocrystals demonstrates that low reaction temperature is favourable for the formation of high quality CdSe nanocrystals.

    • Fabrication of ultra thin and aligned carbon nanofibres from electrospun polyacrylonitrile nanofibres

      Javed Rafique Jie Yu Xiaoxiong Zha Khalid Rafique

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      Ultra thin and aligned carbon nanofibres (CNFs) have been fabricated by heat treatment from aligned polyacrylonitrile (PAN) nanofibre precursors prepared by electrospinning. The alignment of the precursor nanofibres was achieved by using a modified electrospinning set up developed recently, where a tip collector was used to collect and align the nanofibres. The average diameter of the aligned CNFs is about 80 nm. The stabilization and carbonization behaviour were studied mainly based on the randomly oriented PAN nanofibres. The effects of stabilization and carbonization temperatures, temperature-increasing rates, and with and without substrates on the morphology and structure of the CNFs were investigated. Fourier transform infrared spectroscopy, scanning electron microscopy, X-ray diffraction, transmission electron microscopy and Raman spectroscopy were used to characterize the structure of the CNFs and thermogravimetric/differential temperature analysis was used to evaluate the thermal behaviour of PAN nanofibres.

    • Effect of stress-induced grain growth during room temperature tensile deformation on ductility in nanocrystalline metals

      Weichang Xu Pinqiang Dai Xiaolei Wu

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      In the present study defect-free nanocrystalline (nc) Ni–Co alloys with the Co content ranging from 2.4–59.3% (wt.%) were prepared by pulse electrodeposition. X-ray diffraction analysis shows that only a single face-centred cubic solid solution is formed for each alloy and that the grain size reduces monotonically with increasing Co content, which is consistent with transmission electron microscopy (TEM) observations. In the nc Ni–Co alloys, both the ultimate tensile strength and the elongation to failure increase as the Co content increases. The TEM observations reveal that stress-induced grain growth during tensile deformation is significantly suppressed for the nc Ni–Co alloys rich in Co in sharp contrast to those poor in Co. We believe that sufficient solutes could effectively pin grain boundaries making grain boundary motions (e.g. grain boundary migration and/or grain rotation) during deformation more difficult. Thus, stress-induced grain growth is greatly suppressed. At the same time, shear banding plasticity instability is correspondingly delayed leading to the enhanced ductility.

    • Optical properties of d.c. magneto sputtered tantalum and titanium nanostructure thin film metal hydrides

      M Singh S Srivastava S Agarwal S Kumar Y K Vijay

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      Nanostructured thin films of tantalum and titanium were deposited on glass substrate using d.c. magnetron sputtering technique under the argon gas environment at a pressure of 0.1 mbar. Optical transmission and absorption studies were carried out for these samples with pressure of hydrogen. Large changes in both transmission and absorption on loading these films with hydrogen are accompanied by significant phase changes and electronic transformation. Optical photograph shows the colour variation after hydrogenation in case of tantalum film which may be used as decorative mirrors and hydrogen sensors. The hydrogen storage capability of thin films was confirmed by variation in optical properties.

    • Ethanol and LPG sensing characteristics of SnO2 activated Cr2O3 thick film sensor

      Ravi Chand Singh Nipin Kohli Manmeet Pal Singh Onkar Singh

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      The sensing response of pure and SnO2 activated Cr2O3 to ethanol vapours and liquefied petroleum gas (LPG) has been investigated. Fine particles of commercial chromium oxide powder were selected and deposited as thick film to act as a gas sensor. The sensor surface has been activated by tin dioxide, on surface oxidation of tin chloride. The concentration of tin chloride solution, used as activator, was varied from 0 to 5% and its effect on gas response, selectivity and operating temperature has been studied. It was found that response to ethanol vapours significantly improved, whereas response to LPG remained unaffected. Moreover, operating temperature remains unchanged both for LPG and ethanol vapours.

    • Effect of indium doping on zinc oxide films prepared by chemical spray pyrolysis technique

      Girjesh Singh S B Shrivastava Deepti Jain Swati Pandya T Shripathi V Ganesan

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      We report the conducting and transparent In doped ZnO films fabricated by a homemade chemical spray pyrolysis system (CSPT). The effect of In concentration on the structural, morphological, electrical and optical properties have been studied. These films are found to show (0 0 2) preferential growth at low indium concentrations. An increase in In concentration causes a decrease in crystalline quality of films as confirmed by X-ray diffraction technique which leads to the introduction of defects in ZnO. Indium doping also significantly increased the electron concentrations, making the films heavily 𝑛 type. However, the crystallinity and surface roughness of the films decreases with increase in indium doping content likely as a result of the formation of smaller grain size, which is clearly displayed in AFM images. Typical optical transmittance values in the order of (80%) were obtained for all films. The lowest resistivity value of 0.045 𝛺-m was obtained for film with 5% indium doping.

    • Effect of Ba(Ti(0.9)Sn0.1)O3 ceramic doping on optical, thermal and dielectric properties of polycarbonate host

      Ayman S Ayesh Rami Abdel-Rahem

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      Ba(Ti(0.9)Sn0.1)O3 (BTS) ceramic was prepared by a conventional ceramic processing. BTS–polycarbonate (PC) composites were prepared at different BTS concentrations by weight in order to study their optical and dielectric properties. The absorption coefficient (𝛼) was determined in the wavelength range from 250–600 nm at room temperature for all BTS–PC composites. The optical gap (𝐸opt) was also determined for BTS–PC composites. The variation of the absorption coefficient (𝛼) and optical gap (𝐸opt) with BTS content are reported. It was found that BTS ceramic highly enhances the UV absorption of PC host at 300 nm. The optical gap decreases up to the value of 3.93 eV as BTS content increases up to 35 wt% and this was attributed to the formation of localized states in the forbidden gap. The relative dielectric permittivity, dielectric loss and loss tangent were measured at temperature range from room temperature up to 150°C and at frequency values 1 kHz, 10 kHz and 50 kHz. Addition of BTS to PC host, however, will increase relative dielectric permittivity, dielectric loss and loss tangent. Besides, increasing of temperature will also increase relative dielectric permittivity, dielectric loss and loss tangent especially above the glass transition temperature of PC host and this behaviour was attributed to the segmental motion of polymer chains. On the other hand, this study shows that there is a good agreement between SEM, DSC and dielectric results and also between optical gap and a.c. conductivity results. Moreover, SEM and DSC results reveal that addition of BTS ceramic particles to PC host will reduce the physical bond between polymer chains or may be will increase the free volume in the polymer host and consequently will enhance the segmental motion of polymer chains and this behaviour is independent of ceramic phase.

    • Cure and mechanical properties of recycled NdFeB–natural rubber composites

      P Saramolee P Lertsuriwat A Hunyek C Sirisathitkul

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      Magnetic polymer composites containing recycled neodymium–iron–boron (NdFeB) powder and natural rubber (NR) were prepared by the two-roll mill technique. Their mechanical and cure properties were studied as a function of NdFeB loading from 0–120 phr. With increasing magnetic loading, the cure time of the NdFeB–NR composites were exponentially decreased because of the reduction of the polymer chain crosslink. The tensile strength of the NR compound, related to the cure characteristics, was reduced by 40% by the addition of 10 phr NdFeB fillers because of the inhibition of the stress-induced crystallization. However, the variation in loading from 30–90 phr has modest effects on the tensile strength as well as elongation at break and the hardness. Furthermore, recycled NdFeB–NR composites had higher modulus and lower percentage of swelling in this magnetic loading regime. Simple tests confirmed the distribution of magnetic stray field around pieces of NdFeB–NR composites.

    • Resolution of conflicting views on thermodynamics of glass transition: A unified model

      K T Jacob Sagar Prabhudev R M Mallya

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      Classical description of thermodynamic properties during glass transition has been questioned by the entropy-loss model. The uncompensated loss of entropy at the glass transition temperature and zero residual entropy is at the heart of the controversy. Both the models are critically reviewed. A unified model is presented which incorporates features of both entropy loss and residual entropy. It implies two different types of contributions to the entropy of the supercooled liquid, one of which vanishes at the transition and the other which contributes to residual entropy. Entropy gain during spontaneous relaxation of glass, and the nature of heat capacity ‘hysteresis’ during cooling and heating through the glass transition range support the proposed model. Experiments are outlined for differentiating between the models.

    • Solution combustion synthesis of (La, K) FeO3 orthoferrite ceramics: structural and magnetic property studies

      Manjunath B Bellakki V Manivannan

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      Polycrystalline La1–𝑥K𝑥FeO3 ceramic oxides were synthesized by a solution combustion process using glycine as a fuel. The synthesized ceramic powders were characterized for structural features applying characterization techniques such as powder X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and magnetic and optical property studies applying characterization techniques such as SQUID magnetometer and diffuse reflectance (DR). The changes in magnetic properties are correlated to changes in structural features resulting from Rietveld structural refinement.

    • Preparation and characterization of porous Si3N4 ceramics prepared by compression molding and slip casting methods

      Yu Fangli Wang Huanrui Bai Yu Yang Jianfeng

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      Porous silicon nitride (Si3N4) ceramics were fabricated by compression molding and slip casting methods using petroleum coke as pore forming agent, and Y2O3–Al2O3 as sintering additives. Microstructure, mechanical properties and gas permeability of porous Si3N4 ceramics were investigated. The mechanical properties and microstructure of porous Si3N4 ceramics prepared by compression molding were better than those which were prepared by slip casting method, whereas slip casting method is suitable for the preparation of porous Si3N4 ceramics with higher porosity and excellent gas permeability.

    • Effect of carbon on mechanical properties of powder-processed Fe–0.35%P alloys

      Shefali Trivedi Yashwant Mehta K Chandra P S Mishra

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      The present paper records the results of mechanical tests on iron-phosphorus powder alloys which were made using a hot powder forging technique. In this process mild steel encapsulated powders were hot forged into slabs, hot rolled and annealed to relieve the residual stresses. These alloys were characterized in terms of microstructure, porosity content/densification, hardness and tensile properties. Densification as high as 98.9% of theoretical density, has been realized. Microstructures of these alloys consist of single-phase ferrite only. Alloys containing 0.35 wt% P, such as Fe–0.35P–2Cu–2Ni–1Si–0.5Mo and Fe–0.35P–2Cu–2Ni–1Si–0.5Mo–0.15C show very high strength. It was observed in this present investigation that, the alloying additions, such as Si, Mo, Ni, and C to Fe–P based alloys caused increase in strength along with reduction in ductility. Cu reduces porosity of Fe–P alloys. Alloys developed in the present investigation were capable of hot working to very thin gauge of sheets and wires.

    • Electromagnetic properties of carbonyl iron and their microwave absorbing characterization as filler in silicone rubber

      Yuping Duan Guofang Li Lidong Liu Shunhua Liu

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      The complex permittivity, permeability and microwave-absorbing properties of rubber composites filled with carbonyl iron are measured at frequencies from 2–18 GHz. The results indicate that the reflection loss peak shifts towards low frequency region with increasing layer thickness or increasing weight concentration. The minimum reflection loss value of –23.06 dB was obtained at 3.3 GHz for the composites with 80% wt. These results show that the composites possess good microwave absorbing ability in both low- and highfrequency bands.

    • Preparation and crystal structure characterization of CuNiGaSe3 and CuNiInSe3 quaternary compounds

      G E Delgado A J Mora P Grima-Gallardo S Durán M Muñoz M Quintero

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      Samples of the quaternary chalcogenide compounds, CuNiGaSe3 and CuNiInSe3, prepared by direct fusion and annealing method, were characterized by X-ray powder diffraction. In each case, the crystal structure was refined using the Rietveld method. Both compounds were found to crystallize in the tetragonal system, space group 𝑃$\bar{4}$2𝑐 (N°112), with unit cell parameter values 𝑎 = 5.6213(1) Å, 𝑐 = 11.0282(3) Å, 𝑉 = 348.48(1) Å3 and 𝑎 = 5.7857(2) Å, 𝑐 = 11.6287(5) Å, 𝑉 = 389.26(3) Å3 for CuNiGaSe3 and CuNiInSe3, respectively. These compounds have a normal adamantane structures and are isostructural with CuFeInSe3.

    • Fabrication of micro-Ni arrays by electroless and electrochemical depositions with etched porous aluminum template

      Houfang Lu Kangping Yan Jixin Yan Jianzhong Wang

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      Nickel micro-arrays were fabricated by electroless and electrochemical deposition in an etched porous aluminum membrane. The aluminum membrane with metal characteristic could be fabricated from high-purity aluminium by electrochemical method. The aluminum reduced Ni2+ into Ni and the formed Ni nuclei served as the catalyst for further reduction of Ni2+ in electroless solution. With the help of the membrane, nickel micro-columns of about 1–2 𝜇m diameter were obtained. The surface-deposited nickel layer served as a substrate for the nickel micro-columns, and the resulting material possessed strong mechanical strength. Electrochemical deposition was operated without preparing a conductive layer on the template due to the conductivity of the aluminum membrane. Nickel micro-tubes with an outer diameter of about 1–2 𝜇m and a wall thickness in the order of tens of nm were obtained. The nickel micro-arrays were characterized by scanning electron microscope (SEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS).

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