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ISSN 1005-0302
CN 21-1315/TG
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      15 April 2014, Volume 30 Issue 4 Previous Issue    Next Issue
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    A Comparative in vitro Study on Biomedical Zre2.5X (X [ Nb, Sn) Alloys
    F.Y. Zhou, K.J. Qiu, D. Bian, Y.F. Zheng, J.P. Lin
    J. Mater. Sci. Technol., 2014, 30 (4): 299-306.  DOI: 10.1016/j.jmst.2013.12.006
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    Nb and Sn are major alloying elements in Zr alloys. In this study, the microstructure, mechanical properties, corrosion behavior, cytocompatibility and magnetic resonance imaging (MRI) compatibility of Zr–2.5X (X = Nb, Sn) alloys for biomedical application are comparatively investigated. It is found that Zr–2.5Nb alloy has a duplex structure of α and β phase and Zr–2.5Sn alloy is composed of α phase. Both separate addition of Nb and Sn can strengthen Zr but Nb is more effective in strengthening Zr than Sn. The studied Zr–2.5X (X = Nb, Sn) alloys show improved corrosion resistance compared to pure Zr as indicted by the decreased corrosion current density. The alloying addition of Nb enhances the pitting resistance of Zr, whereas the addition of Sn decreases the pitting resistance of Zr. The extracts of Zr–2.5X alloys produce no significant deleterious effect on fibroblast cells (L-929) and osteoblast-like cells (MG 63), indicating good in vitro cytocompatibility. The Zr–2.5X (X = Nb, Sn) alloys show decreased magnetic susceptibility compared to pure Zr and their magnetic susceptibility is far lower than that of pure Ti and Ti–6Al–4V alloy. Based on these facts, Zr–2.5Nb alloy is more suitable for implant material than Zr–2.5Sn alloy. Sn is not suitable as individual alloying addition for Zr because Sn addition decreases the pitting resistance in physiological solution.

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    Synthesis and Characterization of Nano-hydroxyapatite Powder Using Wet Chemical Precipitation Reaction
    Syed Sibte Asghar Abidi, Qasim Murtaza
    J. Mater. Sci. Technol., 2014, 30 (4): 307-310.  DOI: 10.1016/j.jmst.2013.10.011
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    Hydroxyapatite (HA) nano-powder was synthesized via wet chemical technique in a used precipitation reaction, in which Ca(OH)2 and H3PO4 were used as precursors. Deionised water was used as a diluting media for the reaction and ammonia was used to adjust the pH. The synthetic HA nano-powder has some medical applications such as a coating material in orthopaedic implants and in dental. HA powder has been studied at different temperatures from 100 to 800 °C to achieve the stoichiometric Ca/P ratio 1.667. The optimum temperature was found to be 600 °C. Above this temperature, the HA powder decomposed to CaO. The crystallite size of HA powder was found to be in the range of 8.47–24.47 nm. The crystallographic properties were evaluated by X-ray diffraction, Fourier transform infrared spectroscopy, energy dispersive X-ray spectroscopy and scanning electron microscopy. The results show that, high purity of nano-hydroxyapatite powders could be obtained at low temperatures, and the crystallinity, crystallite size and Ca/P ratio of the resulting nanoparticles were found to be dependent on the calcination temperature. When Ca/P ratio exceeded 1.75, formation of CaO phase was observed.

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    Dielectric Relaxation and Conductivity of Ba(Mg1/3Ta2/3)O3 and Ba(Zn1/3Ta2/3)O3
    Md. Monwar Hoque, Alo Dutta, Sanjay Kumar, Tripurari Prasad Sinha
    J. Mater. Sci. Technol., 2014, 30 (4): 311-320.  DOI: 10.1016/j.jmst.2013.10.021
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    The frequency dependent dielectric properties of barium magnesium tantalate (BMT), Ba(Mg1/3Ta2/3)O3 and barium zinc tantalate (BZT), Ba(Zn1/3Ta2/3)O3 synthesized by solid state reaction technique have been investigated at various temperatures by impedance spectroscopy. BMT and BZT possess cubic structure with lattice parameter a = 0.708 and 0.451 nm, respectively. The resonance peaks due to dielectric relaxation processes are observed in the loss tangent of these oxides. The relaxation in the samples is polydispersive in nature. The temperature dependence of dc conductivity, the most probable relaxation frequency (ωm) obtained from tanδ vs logω plots and ωm obtained from imaginary parts of the complex electrical modulus vs logω plots follow the Arrhenius behavior. According to these Arrhenius plots the activation energies of BMT and BZT are about 0.54 and 0.40 eV, respectively. Thus the results indicate that samples are semiconducting in nature. The frequency-dependent electrical data are analyzed in the framework of conductivity and electric modulus formalisms. Both these formalisms show qualitative similarities in relaxation time. Our study points that for complex perovskite oxides with general formula A(BB″)O3, the dielectric properties significantly depend on the atomic radii of both A and B type cations. BMT and BZT exhibit enhancement in dielectric property compared to their niobate counterparts. They may find several technological applications such as in capacitors, resonators and filters owing to their high dielectric constant and low loss tangent.

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    Effect of Graphene Oxide as a Dopant on the Electrochemical Performance of Graphene Oxide/Polyaniline Composite
    Fang Hu, Wenhai Li, Ji Zhang, Wei Meng
    J. Mater. Sci. Technol., 2014, 30 (4): 321-327.  DOI: 10.1016/j.jmst.2013.10.009
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    A method for preparing a graphene oxide/polyaniline (GO/PANI) composite electrode was developed to investigate the effect of GO doped in PANI. PANI was first prepared by the polymerisation of aniline and then dedoped by NH4OH to form emeraldine base (EB). The dedoped PANI and as-prepared GO were dissolved in N-methyl-2-pyrrolidone (NMP) to generate a homogeneous dispersion. The GO/PANI composites were redoped in HCl before use as electrode materials. These composites were characterised by Raman spectroscopy, X-ray diffraction, UV–vis adsorption spectroscopy, scanning electron microscopy, atomic force microscopy and electrochemical measurements. The GO/PANI composite electrode (containing 2.5% GO) has an initial gravimetric capacitance of 896 F g−1 at a scan rate of 5 mV s−1 and a retention life of 51% after 500 cycles, which is an improvement over that of pure PANI (23%). The results show that the synergy of GO and PANI attributes to the good electrochemical performance of the GO/PANI composite electrode.

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    CaCO3/TiO2 Nanoparticles Based Dye Sensitized Solar Cell
    Manveen Kaur, N.K. Verma
    J. Mater. Sci. Technol., 2014, 30 (4): 328-334.  DOI: 10.1016/j.jmst.2013.10.016
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    In this communication, the synthesis and structural, morphological, optical, and photo-electrochemical properties of TiO2 and CaCO3/TiO2 nanoparticles as well as their applications in dye sensitized solar cells (DSSCs), have been reported. In an X-ray diffraction pattern of CaCO3/TiO2 nanoparticles, the peak at 29.41° of CaCO3 has been detected, demonstrating its coating on the surface of TiO2, which is further verified using high resolution-transmission electron microscopy, energy dispersive X-ray spectroscopy and Fourier transform infrared spectroscopy. The strong quenching in photoluminescence emission, in the case of CaCO3/TiO2 nanoparticles, has been attributed to the decrease in recombination rate of photo-generated electron–hole pairs. In the case of UV–visible reflectance spectra, the absorption edge for CaCO3/TiO2 nanoparticles has slightly been found to be blue-shifted as compared to bare TiO2 nanoparticles, which corresponds to an increase in energy band gap of the former. The dye desorption studies reveal that CaCO3/TiO2 electrodes adsorbed more dye than the bare TiO2 electrode. CaCO3/TiO2 based DSSC show improved photo-electrochemical properties compared to the bare TiO2 based DSSC as CaCO3 coating on TiO2 forms an energy barrier, and, consequently suppressing the charge recombination, and, thus, improving the overall energy conversion efficiency (η) from 0.46% to 1.44% under the illumination of simulated light of 100 mW/cm2.

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    Ce-substituted Lithium Ferrite: Preparation and Electrical Relaxation Studies
    Viswarupa Mohanty, Rajesh Cheruku, Lakshmi Vijayan, G. Govindaraj
    J. Mater. Sci. Technol., 2014, 30 (4): 335-341.  DOI: 10.1016/j.jmst.2013.10.028
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    Ce-substituted lithium ferrite, Li0.5CexFe2.5−xO4 (x = 0, 0.05 and 0.1) compositions were synthesized from metal nitrates and citric acid by the solution combustion process by keeping the oxidizer to fuel ratio at unity. The thermal decomposition process was investigated by thermogravimetry–differential thermal analysis, which showed a stable phase formation above 600 °C. The phase composition and molecular bonding of Li0.5CexFe2.5−xO4 were characterized by X-ray powder diffraction analysis and Fourier transform infrared spectroscopy, respectively. An extensive study of electrical relaxation process has been represented with impedance and modulus as a function of frequency at different temperatures. The activation energy obtained from both the formalisms was found to be equal within the error. The dc conductivity and hopping frequency were thermally activated and their activation energies were found to be in the range of 0.69–0.64 eV for x = 0.05. The scaling of modulus and impedance were used to understand the electrical relaxation behaviour of the compositions and they suggest the time temperature superposition principle.

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    Hydrothermal Synthesis of CsxWO3 and the Effects of N2 Annealing on its Microstructure and Heat Shielding Properties
    Fei Shi, Jingxiao Liu, Xiaoli Dong, Qiang Xu, Jiayu Luo, Hongchao Ma
    J. Mater. Sci. Technol., 2014, 30 (4): 342-346.  DOI: 10.1016/j.jmst.2013.08.018
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    Cesium tungsten bronze (CsxWO3) powders were synthesized by hydrothermal reaction at 190 °C by using sodium tungstate and cesium carbonate as raw materials, and the effects of N2 annealing on the microstructure and near-infrared (NIR) shielding as well as heat insulation properties of CsxWO3 were investigated. The results indicated that the synthesized CsxWO3 powders exhibited hexagonal Cs0.32WO3 crystal structure, and subsequent N2 annealing could further improve the crystallinity of CsxWO3 particles. Moreover, the NIR shielding and heat insulation properties of CsxWO3 could be further improved after N2 annealing at appropriate temperature for a period of time. Particularly, the 500 °C-annealed CsxWO3 products in the N2 atmosphere showed the best NIR shielding and heat insulation properties. When the N2 annealing temperature was higher than 700 °C, the NIR shielding properties decreased again. The 800 °C-annealed samples in the N2 atmosphere showed higher visible light transmittance, however, the NIR shielding properties were lower than that of the non-annealed samples.

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    Thermal Stability of ALD Lanthanum Aluminate Thin Films on Si (100)
    Xiaofeng She, Hongtao Wang
    J. Mater. Sci. Technol., 2014, 30 (4): 347-352.  DOI: 10.1016/j.jmst.2013.12.009
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    The thermal stability of high-κ dielectrics on Si is critical in avoiding the malfunction of metal oxide field effect transistors (MOSFET) in devices. Series of annealing experiments have been performed to investigate the thermal stability of atomic layer deposited (ALD) lanthanum aluminate (LAO) thin films, a promising amorphous high-κ candidate. The abrupt interface between LAO and Si remains intact at temperatures below 600 °C. Above this temperature, a SiO2-rich interfacial layer begins to appear and thickens at higher temperatures. At 900 °C, the interface is roughened due to the formation of nano sized crystal nuclei above the interfacial layer, which indicates the interfacial reactions with the Si substrate. The thermal stability of ALD Al2O3 thin films on Si have also been studied under similar conditions. The Al2O3/Si interface retains its smoothness even after full crystallization. This comparison suggests that the rare earth element may catalyze the interfacial reactions. Further annealing experiments on LAO films with different thickness and with a capping layer show that the oxygen source of the interfacial layer mainly comes from the ALD oxide films.

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    Characterization of the Protective Surface Films Formed on Molten AZ91D Magnesium Alloy in SO2/Air Atmospheres in a Sealed Furnace
    Xianfei Wang, Shoumei Xiong
    J. Mater. Sci. Technol., 2014, 30 (4): 353-358.  DOI: 10.1016/j.jmst.2013.10.026
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    Surface films that formed on molten AZ91D magnesium alloy in SO2/air cover gases at 680 °C in a sealed furnace were characterized by scanning electron microscopy, energy dispersive spectroscopy, X-ray diffraction and Auger electron spectroscopy. It is revealed that the film formed on molten AZ91D alloy surface in cover gas with high air content can prevent the molten AZ91D alloy from oxidation and ignition. The surface film contained three elements, namely magnesium, oxygen and sulfur, and was mainly composed of MgO and MgS. The properties of the film depended on air content in the cover gas and holding time. Thermodynamic calculation showed that MgSO4 was the stable phase, and it was concluded that the formation of MgSO4 was important for the formation of the protective surface film in SO2/air atmospheres.

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    Characterization of Microstructural and Morphological Properties in As-deposited Ta/NiFe/IrMn/CoFe/Ta Multilayer System
    Xianfei Wang, Shoumei Xiong
    J. Mater. Sci. Technol., 2014, 30 (4): 359-364.  DOI: 10.1016/j.jmst.2013.10.024
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    Surface films that formed on molten AZ91D magnesium alloy in SO2/air cover gases at 680 °C in a sealed furnace were characterized by scanning electron microscopy, energy dispersive spectroscopy, X-ray diffraction and Auger electron spectroscopy. It is revealed that the film formed on molten AZ91D alloy surface in cover gas with high air content can prevent the molten AZ91D alloy from oxidation and ignition. The surface film contained three elements, namely magnesium, oxygen and sulfur, and was mainly composed of MgO and MgS. The properties of the film depended on air content in the cover gas and holding time. Thermodynamic calculation showed that MgSO4 was the stable phase, and it was concluded that the formation of MgSO4 was important for the formation of the protective surface film in SO2/air atmospheres.

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    Effect of Tb Doping on Structural and Electrical Properties of BiFeO3 Thin Films Prepared by Sol–Gel Technique
    Guohua Dong, Guoqiang Tan, Wenlong Liu, Ao Xia, Huijun Ren
    J. Mater. Sci. Technol., 2014, 30 (4): 365-370.  DOI: 10.1016/j.jmst.2013.09.015
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    Bi1−xTbxFeO3 thin films were prepared on SnO2 (fluorine doped tin oxide) substrates by a sol–gel method. The structural and electrical properties of the BiFeO3 thin films were characterized and tested. The results indicated that the diffraction peak of the Tb-doped BiFeO3 films was shifted towards right as the doping amounts were increased. The structure was transformed from the rhombohedral to tetragonal/orthorhombic phase. The Bi0.89Tb0.11FeO3 thin film showed the well-developed PE loops, which enhanced remnant polarization (Pr = 88.05 μC/cm2) at room temperature. The dielectric constant and dielectric loss of Bi0.89Tb0.11FeO3 thin film at 100 kHz were 185 and 0.018, respectively. Furthermore, the Bi0.89Tb0.11FeO3 thin film showed a relatively low leakage current density of 2.07 × 10−5 A/cm2 at an applied electric field of 150 kV/cm. The X-ray photoelectron spectroscopy (XPS) spectra indicated that the presence of Fe2+ ions in the Bi0.89Tb0.11FeO3 thin film was less than that in the pure BiFeO3.

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    Finite Element Simulation on Thermal Fatigue of a Turbine Blade with Thermal Barrier Coatings
    L. Yang, Q.X. Liu, Y.C. Zhou, W.G. Mao, C. Lu
    J. Mater. Sci. Technol., 2014, 30 (4): 371-380.  DOI: 10.1016/j.jmst.2013.11.005
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    In this paper, a finite element model was developed for a turbine blade with thermal barrier coatings to investigate its failure behavior under cyclic thermal loading. Based on temperature and stress fields obtained from finite element simulations, dangerous regions in ceramic coating were determined in terms of the maximum principal stress criterion. The results show that damage preferentially occurs in the chamfer and rabbet of a turbine blade with thermal barrier coatings and its thermal fatigue life decreases with the increase of thermal stress induced by high service temperature.

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    Substituent Influence of Yttria by Gadolinia on the Tetragonal Phase Stability for Y2O3–Ta2O5–ZrO2 Ceramics at 1300 °C
    Xiaoqing Niu, Min Xie, Fen Zhou, Rende Mu, Xiwen Song, Shengli An
    J. Mater. Sci. Technol., 2014, 30 (4): 381-386.  DOI: 10.1016/j.jmst.2013.12.008
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    The influences of equimolar substitution of yttria by gadolinia on the phase constituent and stability for Y2O3–Ta2O5–ZrO2 ceramics have been investigated. The ceramics with the Gd content lower than 8 mol% exhibit pure tetragonal phase as well as high tetragonal phase stability. However, the high Gd containing ceramics consist of t-ZrO2, m-ZrO2 and monoclinic GdTaO4 and show complicated phase evolution behaviors. The fractions of monoclinic ZrO2 and GdTaO4 increase with increasing Gd content, indicating that the excessive substitution of Gd for Y results in a reduction in the tetragonal phase stability. In addition, the lower Gd containing ceramics show an almost invariable tetragonality, while the higher Gd containing ceramics reveal a composition-dependent tetragonality. Accordingly, an association of the tetragonal phase stability and tetragonality with the Gd concentration is established, which provides us a clue to understand the phase stability of these ceramics.

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    Nanocrystalline Growth Activation Energy of Zirconia Polymorphs Synthesized by Mechanochemical Technique
    Taghi Dallali Isfahani, Jafar Javadpour, Alireza Khavandi, Massoud Goodarzi,Hamid Reza Rezaie
    J. Mater. Sci. Technol., 2014, 30 (4): 387-393.  DOI: 10.1016/j.jmst.2013.10.012
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    The synthesis of ZrO2 by mechanochemical reaction using ZrCl4 and CaO as raw materials and subsequent annealing of the products were investigated. The effect of thermal treatment on the structural evolution and morphological characteristics of the nanopowders was studied by X-ray diffractometry, Raman spectroscopy, transmission electron microscopy, scanning electron microscopy, differential thermal analysis and Rietveld refinement. The results showed that the average crystallite size of ZrO2 was less than 100 nm up to around 1100 °C. The activation energy for ZrO2 nanocrystallite growth during calcination was calculated to be about 13,715 and 27,333 J/mol for tetragonal (t-ZrO2) and monoclinic (m-ZrO2) polymorphs, respectively. Mechanism of the nanocrystallite growth of the ZrO2 polymorphs during annealing is primarily investigated.

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    Preparation and Structural Characterization of Rapidly Solidified Al–Cu Alloys
    Iuliana Lichioiu, Ildiko Peter, Bela Varga, Mario Rosso
    J. Mater. Sci. Technol., 2014, 30 (4): 394-400.  DOI: 10.1016/j.jmst.2013.12.001
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    Rapidly solidified Al100−x–Cux alloys (x = 5, 10, 15, 25, 35 wt%) were prepared and analyzed. High cooling rate increased the Cu solubility in α-Al matrix. The influence of the cooling rate on Cu solubility extension in Al was experimentally simulated. Thus the pouring was performed in metallic die and by melt spinning-low pressure (MS-LP) technique. Melt processing by liquid quenching was performed using a self-designed melt spinning set-up which combined the cooling technology of a melt jet on the spinning disc with the principle of the mold feeding from low pressure casting technology. The thickness of the melt-spun ribbons was in the range of 30–70 μm. The cooling rate provided by MS-LP was within 105–106 K/s after the device calibration. The obtained alloys were characterized from structural, thermal and mechanical point of view. Optical microscopy and scanning electron microscopy were employed for the microstructural characterization which was followed by X-ray analysis. The thermal properties were evaluated by dilatometric and differential scanning calorimetric measurements. Vickers microhardness measurements were performed in the study. In the case of the hypereutectic alloy with 35 wt% Cu obtained by MS-LP method, the microhardness value increased by 45% compared to the same alloy obtained by gravity casting method. This was due to the extended solubility of the alloying element in the α-Al solid solution.

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    Microstructural Morphologies and Experimental Growth Laws during Solidification of Monotectic and Hypermonotectic Al–Pb Alloys
    Adrina P. Silva, Amauri Garcia, José E. Spinelli
    J. Mater. Sci. Technol., 2014, 30 (4): 401-407.  DOI: 10.1016/j.jmst.2013.10.027
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    Al–Pb alloys with monotectic and hypermonotectic compositions were directionally solidified under unsteady-state heat flow conditions. The cooling curves recorded during solidification allowed solidification thermal parameters such as the cooling rate (View the MathML sourceT˙), growth rate (v) and thermal gradient (G) to be experimentally determined. Different microstructural patterns have been associated with the alloy solute content, i.e., Al–1.2 and 2.1 wt% Pb. A sequence of morphologies from the bottom to the top of the Al–1.2 wt% Pb alloy casting (monotectic) can be observed: Pb-rich droplets in the aluminum-rich matrix, followed by a region of microstructural transition formed by droplets and fibers and finally by a mixture of fibers and strings of pearls. A completely fibrous structure (without transition) has been observed along the entire Al–2.1 wt% Pb alloy casting (hypermonotectic). The interphase spacing (λ) was measured along the casting length, and experimental correlations between λ and experimental solidification thermal parameters have been established. Power laws with a −2.2 exponent expressing λ as a function of the growth rate, v, were found to better represent the fibrous growth of both Al–Pb alloys. Moreover, a single experimental law expressing λ as a function of both G and v was found to describe the fibrous growth of both the monotectic and the hypermonotectic alloys experimentally examined.

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    Influence of Shear Banding on the Formation of Brass-type Textures in Polycrystalline fcc Metals with Low Stacking Fault Energy
    Haile Yan, Xiang Zhao, Nan Jia, Yiran Zheng, Tong He
    J. Mater. Sci. Technol., 2014, 30 (4): 408-416.  DOI: 10.1016/j.jmst.2013.11.010
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    Texture evolution in nickel, copper and α-brass that are representative of face-centered-cubic (fcc) materials with different stacking fault energy (SFE) during cold rolling was systematically investigated. X-ray diffraction, scanning electron microscopy and electron backscatter diffraction techniques were employed to characterize microstructures and local orientation distributions of specimens at different thickness reductions. Besides, Taylor and Schmid factors of the {111} <110> slip systems and {111} <112> twin systems for some typical orientations were utilized to explore the relationship between texture evolution and deformation microstructures. It was found that in fcc metals with low SFE at large deformations, the copper-oriented grains rotated around the <110> crystallographic axis through the brass-R orientation to the Goss orientation, and finally toward the brass orientation. The initiation of shear banding was the dominant mechanism for the above-mentioned texture transition.

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    Mechanical Properties of a Low-thermal-expansion Aluminum/Silicon Composite Produced by Powder Metallurgy
    Y.Q. Liu, S.H. Wei, J.Z. Fan, Z.L. Ma, T. Zuo
    J. Mater. Sci. Technol., 2014, 30 (4): 417-422.  DOI: 10.1016/j.jmst.2013.11.003
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    Al matrix composite containing high volume fraction silicon has been promising candidate for lightweight and low-thermal-expansion components. Whereas, optimization of its mechanical properties still is an open challenge. In this article, a flexile powder metallurgy processing was used to produce a fully dense Al–4.0Cu (wt%) alloy composite reinforced with 65 vol.% Si particles. In this composite, Si particles were homogenously distributed, and the particle size was refined to the range of 3–15 μm. Tensile and flexural strength of the composite were 282 and 455 MPa, respectively, about 100% and 50% higher than the best properties reported in literature. The measured fracture toughness of the composite was 4.90 MPa m1/2. The improved strength of 65%Si/Al was attributed to the optimized particle characteristics and matrix properties. This investigation is expected to provide a primary understanding of the mechanical behaviors of Si/Al composites, and also promote the structural applications of this low-thermal-expansion material.

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    Thermoelectric Properties of Ca3Co4O9/Polyaniline Composites
    Bin Zheng, Yuanhua Lin, Jinle Lan, Xiaoping Yang
    J. Mater. Sci. Technol., 2014, 30 (4): 423-426.  DOI: 10.1016/j.jmst.2013.11.008
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    Ca3Co4O9/polyaniline bulk composites have been successfully fabricated by ball-milling and hot-pressing method. Our results indicate that the Seebeck coefficient can be increased nearly by 400% with adding 15 wt% Ca3Co4O9 to the polyaniline. The thermal conductivity changes slightly with increasing filler content. The highest figure of merit, ZT can reach 5 × 10−4 at 329 K for these bulk composites, which is almost 50 times larger than that of pure polyaniline, suggesting that the polymer-thermoelectric oxide composites are promising candidates for light-weight, low-cost and non-toxic thermoelectric applications.

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