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      30 October 2013, Volume 29 Issue 10 Previous Issue    Next Issue
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    Rapid Synthesis of Piezoelectric ZnO-Nanostructures for Micro Power-Generators
    Nai-Feng Hsu, Tien-Kan Chung, Ming Chang, Hong-Jun Chen
    J. Mater. Sci. Technol., 2013, 29 (10): 893-897.  DOI: 10.1016/j.jmst.2013.07.005
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    In this paper, we report a rapid synthesis of piezoelectric ZnO-nanostructures and fabrication of the nanostructures-based power-generators demonstrating an energy conversion from an environmental mechanical/ultrasonic energy to an electrical energy. The ZnO nanostructures are grown on a silicon wafer by a modified chemical solution method (CSD, chemical-solution-deposition) with a two-step thermal-oxidation approach. The synthesis process can be completed within 1 h. By varying the mixture-ratio of Zn micro-particles in an oxalic acid solution with 0.75 mol/l concentration in the CSD process, the growth mechanism is well-controlled to synthesize three different types of ZnO-nanostructures (i.e., dandelion-like nanostructures, columnar nanostructures, and nanowires). Furthermore, through oxidizing at different temperatures in the thermal-oxidation process, the featured geometry of the nanostructures (e.g., the length and diameter of a nanowire) is modified. The geometry, size, morphology, crystallization, and material phase of the modified nanostructures are characterized by scanning electron microscopy and X-ray diffraction. Finally, the nanostructures are used to fabricate several micro power-generators. Through the piezoelectric effect, a maximum current density output of 0.28 μA cm−2 generated by a power-generator under an ultrasonic wave is observed.

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    Effect of Fuel to Oxidant Molar Ratio on Structural and DC Electrical Conductivity of ZnO Nanoparticles Prepared by Simple Solution Combustion Method
    C.S. Naveen, M.L. Dinesha, H.S. Jayanna
    J. Mater. Sci. Technol., 2013, 29 (10): 898-902.  DOI: 10.1016/j.jmst.2013.07.011
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    ZnO nanoparticles of different sizes were prepared by varying the molar ratio of glycine and zinc nitrate hexahydrate as fuel and oxidizer (0.1, 0.8, 1.11, 1.3, 1.5, 1.7, 2.0) by simple solution combustion method. UV–Visible spectrophotometry studies show that, the band gap of the prepared ZnO nanoparticles increases with increasing fuel to oxidant (F/O) molar ratio up to 1.7 revealing the formation of ZnO nanoparticles. The decrease in band gap for the sample of F/O molar ratio 2.0 is due to an increase in particle size. Powder X-ray diffraction patterns of the prepared samples show the formation of single phase ZnO nanoparticles and the particle size decreases with increasing F/O molar ratio up to 1.7. Surface morphology of the prepared samples was studied by scanning electron microscopy and it was observed that, the porosity increases with increasing F/O molar ratio. DC electrical conductivity at room temperature and in the temperature range of 303–563 K was studied for all the samples and the results revealed that, the sample of F/O molar ratio 1.7 has low electrical conductivity at room temperature and high EAH (high temperature activation energy) compared to other samples.

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    Magnetic Flux Alignment Studies on Entrapped Ferrofluid Nanoparticles in Poly Vinyl Alcohol Matrix
    K. Jeyasubramanian, N. Selvakumar, J. Ilakkiya, P. Santhoshkumar, Nikil Satish,Sumanta Kumar Sahoo
    J. Mater. Sci. Technol., 2013, 29 (10): 903-908.  DOI: 10.1016/j.jmst.2013.07.002
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    Highly surface active super paramagnetic colloidal suspensions of nano crystalline ferrofluid have been synthesized through wet-chemical route. Entrapment of magnetic domains presented in the nano ferrofluid in a polymer matrix like poly vinyl alcohol film was accomplished by developing polymer composite film in between two magnetic poles by solvent casting method. Similarly poly vinyl alcohol-ferrofluid composite films were also developed in the absence of magnetic field. Atomic force microscopy image of nano-composite film makes it clear that the film developed in the absence of magnetic field possesses randomly oriented domains, whereas film developed with magnetic field shows well aligned flux lines. The characteristics and nature of forces acting between magnetic domains along the magnetic flux lines were explored from magnetic force microscopy imaging. The number of flux lines developed in the polymer matrix was observed to be directly proportional to applied external magnetic field. Approximate number of magnetic lines passing through unit area of composite film was evaluated from line profile data analysis of atomic force microscopy image. The particle sizes of the nanoparticles encapsulated in the polymer matrix were found to be in the range of 10–20 nm. Scanning electron microscopy micrographs confirm aggregation of ferrofluid particles of ribbon like morphology along the magnetic flux lines. Magnetic properties of the entrapped nanoparticles in polymer matrix film were analyzed using vibrating sample magnetometer at room temperature. The super paramagnetic nature and other magnetic properties were evaluated from the hysteresis loop.

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    Flower-shaped CuO Nanostructures: Synthesis, Characterization and Antimicrobial Activity
    K. Mageshwari, R. Sathyamoorthy
    J. Mater. Sci. Technol., 2013, 29 (10): 909-914.  DOI: 10.1016/j.jmst.2013.04.020
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    In the present work, flower-like CuO nanostructures were synthesized by reflux condensation method without using any surfactants or templates. Structural analysis by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and Raman studies revealed the formation of highly crystalline single phase CuO, exhibiting monoclinic structure. Morphological analysis by field emission scanning electron microscopy (FESEM) showed flower-shaped CuO hierarchical architecture made up of interpenetrating self-assembled nanosheets. Optical analysis by UV–Vis diffused reflectance spectra (DRS) exhibited considerable blue-shift in the optical band gap due to quantum confinement effect. Photoluminescence (PL) spectrum showed both UV as well as visible emissions. The antibacterial activity of flower-shaped CuO nanostructures were tested against gram-positive (Bacillus subtilis, Bacillus thuringiensis) and gram-negative (Salmonella paratyphi, Salmonella paratyphi-a, Salmonella paratyphi-b, Escherichia coli and Pseudomonas aeruginosa) bacteria. Also, the antifungal activity of CuO was investigated against Aspergillus niger, Rhizopus oryzae, Aspergillus flavus, Cladosporium carrionii, Mucor, Penicillium notatum and Alternaria alternata. Results demonstrate that the flower-shaped CuO nanostructures act as an effective antimicrobial agent against pathogenic bacteria and fungi.

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    Facile Growth of Porous Hierarchical Structure of ZnO Nanosheets on Alumina Particles via Heterogeneous Precipitation
    Hamid Tajizadegan, Majid Jafari, Mehdi Rashidzadeh, Reza Ebrahimi-Kahrizsangi,Omid Torabi
    J. Mater. Sci. Technol., 2013, 29 (10): 915-918.  DOI: 10.1016/j.jmst.2013.06.008
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    ZnO nanosheets and nanoflakes were grown on alumina particles in the absence of surfactants via heterogeneous precipitation using urea, zinc acetate and bayerite as precursors. Thermo-gravimetric analysis (TGA), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) were used and the results indicated the formation of only two phases: wurtzite-type ZnO and γ-Al2O3. ZnO nanoflakes were grown on alumina particles in the samples with ZnO content of 40 and 60 wt%. By increasing the ZnO content to 80 wt%, a porous hierarchical structure of ZnO with nanosheet arrays appeared. Both of these nanoflakes and nanosheets were about 40–80 nm in thickness and about 1–2 μm in diameter. It was proposed that Zn5(CO3)2(OH)6 nuclei undergo higher growth rates in thin sheets at edges of bayerite particles with a higher surface energy. The Brunauer–Emmett–Teller (BET) measurements proved a reachable high surface area for hierarchical structures of ZnO nanosheets, which could mainly be attributed to their unique growth on alumina particles. Also, UV absorption results revealed that ZnO–Al2O3 compositions still show the UV characteristic absorption of ZnO, which can evidence the presence of photocatalytic properties in ZnO–Al2O3 compositions.

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    Modifying the Properties of Tungsten Based Plasma Facing Materials with Single-Wall Carbon Nanotubes
    Shuming Wang, Chongxiao Sun, Wenhao Guo, Changchun Ge, Qingzhi Yan, Qiang Zhou,Pengwan Chen, Zhibao Chen
    J. Mater. Sci. Technol., 2013, 29 (10): 919-922.  DOI: 10.1016/j.jmst.2013.07.013
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    Tungsten is one of the best candidates for plasma-facing components in fusion reactors owing to its unique properties. But disadvantages such as its brittleness and high ductile-to-brittle transition temperature have restricted its fusion energy application. Single-walled carbon nanotubes (SWCNTs) have the potential to be used as reinforcements due to their excellent mechanical properties. A new method of modifying the properties of tungsten by doping with SWCNTs was introduced. An efficient way of dispersing SWCNTs into the tungsten matrix with strong interfaces by heterocoagulation and ultrasonication was employed, and hot explosive compaction (HEC) technology was selected to compact and sinter the composite powders. The sintering properties, microstructure, densification effect, thermal conductivity, hardness and fracture toughness of the obtained SWCNTs/W bulk samples were tested, and compared with pure tungsten. The influences of SWCNTs on these properties and the main toughening mechanism of SWCNTs in a tungsten matrix were discussed.

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    Synthesis and Characterization of Indium Niobium Oxide Thin Films via Sol-Gel Spin Coating Method
    Saeed Mohammadi, Mohammad Reza Golobostanfard, Hossein Abdizadeh
    J. Mater. Sci. Technol., 2013, 29 (10): 923-928.  DOI: 10.1016/j.jmst.2013.06.012
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    In the present study, niobium-doped indium oxide thin films were prepared by sol–gel spin coating technique. The effects of different Nb-doping contents on structural, morphological, optical, and electrical properties of the films were characterized by means of X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), atomic force microscopy (AFM), UV–Vis spectroscopy, and four point probe methods. XRD analysis confirmed the formation of cubic bixbyite structure of In2O3 with a small shift in major peak position toward lower angles with addition of Nb. FESEM micrographs show that grain size decreased with increasing the Nb-doping content. Optical and electrical studies revealed that optimum opto-electronic properties, including minimum electrical resistivity of 119.4 × 10−3 Ω cm and an average optical transmittance of 85% in the visible region with a band gap of 3.37 eV were achieved for the films doped with Nb-doping content of 3 at.%. AFM studies show that addition of Nb at optimum content leads to the formation of compact films with smooth surface and less average roughness compared with the prepared In2O3 films.

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    Optical and Microstructural Characterisations of Pulsed rf Magnetron Sputtered Alumina Thin Film
    I. Neelakanta Reddy, V. Rajagopal Reddy, N. Sridhara, S. Basavaraja, A.K. Sharma,Arjun Dey
    J. Mater. Sci. Technol., 2013, 29 (10): 929-936.  DOI: 10.1016/j.jmst.2013.05.002
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    Alumina thin films were deposited on fused quartz and SS304 substrate by pulsed rf magnetron sputtering with both direct and reactive methods. The films were characterised by energy dispersive X-ray spectroscopy, X-ray diffraction, scanning electron microscopy, field emission scanning electron microscopy and atomic force microscopy to reveal the microstructure, surface morphology and topography of thin films. Transmittance and reflectance of alumina thin film were evaluated after deposition on the quartz substrate. Transmittance of the quartz remains almost un-altered when alumina was deposited by the reactive sputtering. A marginal decrease of ∼4% in the transmittance of quartz was, however, observed after deposition of alumina by direct sputtering. Infrared emittance of the substrate also remains almost constant after deposition of thin alumina film. Further, as-deposited alumina on SS304 obtained by both direct and reactive sputtering process was amorphous in nature. However, after annealing crystalline peaks were observed.

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    Solid State Reaction Preparation of LiFePO4/(C+Cu) Cathode Material and Its Electrochemical Performance
    Yanhong Yin, Xiangnan Li, Xinxin Mao, Xianliang Ding, Shuting Yang
    J. Mater. Sci. Technol., 2013, 29 (10): 937-942.  DOI: 10.1016/j.jmst.2013.06.004
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    Cu–C co-coated LiFePO4 (LiFePO4/(C + Cu)) cathode material was successfully prepared through solid state reduction reaction. The optimized additive amount of CuO was determined by electrochemical test of series content-dependent samples. Electrochemical performances of LiFePO4/(C + Cu) cathode material were investigated. Crystalline structure, morphology and electrochemical performance of the samples were characterized by X-ray diffraction, scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), charge–discharge tests and AC impedance techniques. Results showed that crystal structure of the bulk material was not destroyed after Cu particles distributed on the surface of LiFePO4/C. With 5 wt% CuO additive, the LiFePO4/(C + Cu) cathode material showed improved electrochemical performance especially at high rates and low temperature. At 25 °C and 0.1 C current rate, specific capacity of the Cu-coated sample reaches 161.3 mA h/g. The result was 47 mA h/g higher than that of the un-coated one. At −20 °C, the discharge capacity of Cu-coated materials was 113.4 mA h/g at 0.1 C rate and 83.8 mA h/g at 5 C rate, which reached about 70% of that at room temperature, respectively.

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    A Novel Aminoalkylsilane Compound with Oligo(ethylene oxide) Units as Effective Additive for Improving Cyclability of Lithium-ion Batteries
    Suqing Wang, Jinglun Wang, Hao Luo, Xinyue Zhao, Lingzhi Zhang
    J. Mater. Sci. Technol., 2013, 29 (10): 943-947.  DOI: 10.1016/j.jmst.2013.06.003
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    A new aminoalkylsilane compound, ((2-(2-(N,N-dimethylamino)ethoxy)ethoxy) methyl)trimethylsilane (TMSC1N2) based on the oligo(ethylene oxide) chain end-capped with organosilicon functional group and alkylamine group on each end, was introduced as an electrolyte additive for lithium-ion batteries. Electrochemical performances of different volume ratios of TMSC1N2 in the baseline electrolyte were conducted through cyclic voltammetry, electrochemical impedance spectroscopy and galvanostatic charge/discharge tests of lithium-ion batteries. With adding 5 vol.% TMSC1N2 to the baseline electrolyte (1 mol/L LiPF6 in ethylene carbonate and diethyl carbonate (EC:DEC = 1:1, in volume)), the capacity retention of LiFePO4/Li cells could be significantly improved from 74.7% to 90.8% after 130 cycles. Furthermore, TMSC1N2 showed good compatibility with graphite electrode and would not deteriorate the electrochemical performance of graphite/Li anode cells. These data suggested that TMSC1N2 could be utilized as an effective additive for lithium-ion batteries.

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    Al 1060/Pure Iron Clad Materials by Vacuum Roll Bonding and Their Solderability
    Qian Wang, Xuesong Leng, Jiuchun Yan, Weibing Guo, Yu Fu, Tianming Luan
    J. Mater. Sci. Technol., 2013, 29 (10): 948-954.  DOI: 10.1016/j.jmst.2013.07.001
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    Al 1060/pure iron clad materials were produced by vacuum roll bonding. The effects of preheating temperature, vacuum roll reduction and initial thickness of the Al 1060 sheet on the metal interface and bonding strength were investigated. The interfacial microstructure was investigated and the mechanical properties of the joint were evaluated by shear testing. The bonding strength of the clad materials was generally enhanced by increasing the total reduction or preheating temperature, which caused the metal interface to flatten. No obvious reaction or diffusion layer was observed at the interface between Al 1060 and pure iron. The bonding strength increased with decreasing the initial thickness of the Al 1060 sheets. The Al 1060/pure iron clad materials were soldered with Zn–Al alloy by using an ultrasonic-assisted method. Strong bonding of the Al 1060 layer and Al 7N01 was realized without obvious Al 1060 dissolution or effect on the initial interface of Al 1060/pure iron clad materials by soldering at relatively low temperature.

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    Effect of Temperature on Material Transfer Behavior at Different Stages of Friction Stir Welded 7075-T6 Aluminum Alloy
    S.D. Ji, Y.Y. Jin, Y.M. Yue, S.S. Gao, Y.X. Huang, L. Wang
    J. Mater. Sci. Technol., 2013, 29 (10): 955-960.  DOI: 10.1016/j.jmst.2013.05.018
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    In this work, the morphologies of weld of 7075-T6 aluminum alloy via friction stir welding (FSW) were analyzed by optical microscopy, the temperature field was attained by numerical simulation, and the effect of temperature on material transfer behavior in the thermal-mechanical affected zone (TMAZ) at different stages was mainly investigated. The FSW process consists of three stages. It is very interesting to find that the maximum transfer displacement of material appears at the final stage of welding process, then at the stable stage and at the initial stage, which results from the difference of peak temperatures at different stages. At any stage, the material in TMAZ near the surface of weld transfers downwards, the material in the middle of weld moves upwards and the material near the bottom of weld hardly moves. In any cross section of weld, the largest transfer displacement of material appears in the middle of weld. The increase of rotational velocity and the decrease of welding speed are both beneficial to the transfer displacement of material in the middle of weld.

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    Effect of Brazing Conditions on Microstructure and Mechanical Properties of Al2O3/Tie6Ale4V Alloy Joints Reinforced by TiB Whiskers
    Minxuan Yang, Peng He, Tiesong Lin
    J. Mater. Sci. Technol., 2013, 29 (10): 961-970.  DOI: 10.1016/j.jmst.2013.05.009
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    Al2O3 and Ti–6Al–4V alloy were brazed with Ag–Cu–Ti + B fillers in different brazing conditions. Effects of brazing temperature, holding time and additive Ti content on joints microstructure and shear strength were investigated by scanning electron microscopy, energy dispersive spectrometry, X-ray diffraction, transmission electron microscopy and shear testing. Results indicate that TiCu and Ti(Cu,Al) decrease, but Ti2Cu and Ti2(Cu,Al) increase in brazing seam with increasing brazing temperature, holding time and additive Ti content. Area consisting of Ti3(Cu,Al)3O and TiO near Al2O3 becomes gradually discontinuous from continuity when brazing temperature rises or holding time extends. As Ti additive content increases, TiO is absent near Al2O3; area consisting of only Ti3(Cu,Al)3O thickens. TiB whiskers are in situ synthesized by Ti and B atoms during brazing process. The brazing temperature, holding time and additive Ti content on joints microstructure influence the joints shear strength directly. The shear strength of joints, obtained at 850 °C holding for 10 min, reaches the maximum of 78 MPa. According to the experimental results, phase diagram and thermodynamics calculation, the interface evolution mechanism of the Al2O3/Ti–6Al–4V alloy joint was analyzed.

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    Microstructural Evolution during Partial Remelting of AleSi Alloys Containing Different Amounts of Magnesium
    A. Abedi, M. Shahmiri, B. Amir Esgandari, B. Nami
    J. Mater. Sci. Technol., 2013, 29 (10): 971-978.  DOI: 10.1016/j.jmst.2013.04.021
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    The effect of magnesium on the microstructures of A356 aluminum alloy in as-cast and semi-solid conditions was investigated. The result showed that magnesium refined the size of primary α(Al) phase and eutectic silicon. Magnesium also modified considerably the eutectic silicon and decreased the size of globular α(Al) solid phase in the semi-solid processed alloy. Coarsening rate of the solid α(Al) phase during partial remelting at semi-solid temperature decreased by adding magnesium, probably due to the decrease of both the solid–liquid interfacial energy and inter-diffusion coefficient of solute atoms.

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    Formation of Fine Spheroidal Microstructure of Semi-Solid AleZneMgeCu Alloy by Hyperthermally and Subsequent Isothermally Reheating
    Gang Chen, Jufu Jiang, Zhiming Du, Qi Cao, Hongwei Li, Xin Zhang
    J. Mater. Sci. Technol., 2013, 29 (10): 979-982.  DOI: 10.1016/j.jmst.2013.05.008
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    The high strength 7xxx series aluminium alloys are usually difficult to be prepared as semi-solid feedstock, because some dispersoid particles (soluble only in liquid) could pin at grain and subgrain boundary to make the alloy difficultly recrystallise. In this work, a novel multistep reheating regime is developed for recrystallisation and partial melting (RAP) route to prepare fine spheroidal microstructure of semi-solid Al–Zn–Mg–Cu alloy. After reheating to 665 °C, holding for 4 min and subsequent isothermally holding at 620 °C with total heating time of 15 min, fine spheroidal microstructures with grain size of ∼40 μm were prepared without remained unrecrystallised grains and directionality, which are much finer than the conventionally obtained microstructures (∼100 μm).

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    Influence of Composition on Self-toughening and Oxidation Properties of Y-α-Sialons
    Chunfeng Liu, Feng Ye, Rongsen Xia, Lei Zhang, Yu Zhou, Yudong Huang
    J. Mater. Sci. Technol., 2013, 29 (10): 983-988.  DOI: 10.1016/j.jmst.2013.05.014
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    Y-α-sialon ceramics with different compositions were hot-press sintered. Varying the m or n value in the α-Sialon general formula, both the α-sialon grain morphology and phase assemblages present diversification, therefore, affecting the toughness and hardness. Meanwhile, varying the compositional parameters also influenced the composition and structure of the intergranular glass phase, as well as its oxidation behavior at 1100–1200 °C. The oxidation of the intergranular phase M′ in the Y-α-sialon ceramics was significantly enhanced with further rising the oxidation temperature to 1300 °C.

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    Positive MR and Large Temperature-Field Sensitivity in Manganite Based Heterostructures
    Uma Khachar, P.S. Solanki, R.J. Choudhary, D.M. Phase, D.G. Kuberkar
    J. Mater. Sci. Technol., 2013, 29 (10): 989-994.  DOI: 10.1016/j.jmst.2013.05.011
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    Studies on the ZnO/La0.5Pr0.2Sr0.3MnO3 (LPSMO)/SrNb0.002Ti0.998O3 (SNTO) heterostructure having varying thickness of p-type LPSMO (100 nm – LP1) and (200 nm – LP2) manganite are carried out. ZnO/LPSMO (n–p) and LPSMO/SNTO (p–n) junctions of both the heterostructures exhibit good rectifying behavior in a wide range of temperature and applied field. Forward and reverse bias characteristics of both the junctions of heterostructures show opposite behavior. The observation of negative magnetoresistance (MR) at 5 K and positive MR at 300 K, in both the heterostructures, has been explained in the context of interface region effects and filling of energy bands of LPSMO manganite. Further, at high temperature, the heterostructures exhibit large temperature (46%K−1) and field (40%T−1) sensitivities. Dependence of transport, magnetotransport, IV and sensing properties of the heterostructures, on the temperature, field and film thicknesses have been discussed in this communication.

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    Rapidly Solidified Steel Droplets with B and P Addition
    Na Li, Junwei Zhang, Qian Xu, Lulu Zhai, Shengli Li, Jiguang Li
    J. Mater. Sci. Technol., 2013, 29 (10): 995-998.  DOI: 10.1016/j.jmst.2013.05.012
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    Low carbon steels with B and P additions were remelted by electromagnetic levitation and solidified in a vacuum drop tube. The droplet volumes were set to be 2 mm × 2 mm × 2 mm (TM) and 5 mm × 5 mm × 5 mm (FM), respectively. The microstructure of rapidly solidified steel droplets (cooled in silicon oil) with P and both B and P addition was observed. The microstructures of B-bearing droplet samples were more uniform than those of B-free ones, for both TM and FM samples. The distribution of C and P along the diameter of each sample was detected. The well-distribution of C and P was detected in B-bearing droplet samples. So it could be deduced that B was also well distributed in the steels. It was B atoms that promoted the well-distribution of C and P, which further improved the uniformity of microstructure under the condition of rapid solidification. The micro-hardness of B-bearing samples was higher than that of B-free samples, and the hardening mechanism was discussed in detail.

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    Phase-field Study for Texture Evolution in Polycrystalline Materials under Applied Stress
    Yanli Lu, Liuchao Zhang, Yingying Zhou, Zheng Chen, Jianguo Zhang
    J. Mater. Sci. Technol., 2013, 29 (10): 999-1004.  DOI: 10.1016/j.jmst.2013.08.011
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    The formation and evolution of deformation texture in polycrystalline materials are studied by phase-field dynamic model. In addition, the driving force of texture evolution is also discussed. In this model, grains with different orientation are defined by a set of continuous non-conserved order parameter fields. Simulation results show that grains with preferred orientation grow at the expense of those with unfavorable orientations. It is more important that, elastic potential rather than elastic energy plays a crucial role in the evolution of texture whether the polycrystalline system is subjected to uniaxial stress or shear stress.

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