Synchrotron X-ray diffraction evidences of the amorphization/dissolution of the second phase particles (SPPs) in neutron irradiated Zircaloy-4

X-ray diffraction diagrams of neutron irradiated Zircaloy-4 were obtained at the Brazilian Synchrotron Laboratory (LNLS) with the aim to obtain bulk information about the amorphization process in which the Zircaloy-4 second phase particles (SPPs) undergoes due to neutron irradiation. Owing to the low concentration of the SPPs in the alloy (∼ 0.4 V%), no data regarding to the bulk were obtained until now. The synchrotron experiences allowed to detect five of the more intense lines of the phase C14 (SPPs structure) in unirradited Zircaloy-4: <110>_θ, <103>_θ, <112>_θ, <201>_θ and <004>_θ in the 34° < 2θ < 45° Bragg angle range and others of minor intensity. The diagrams of the samples irradiated at moderate doses (10²⁰ n/cm²) show these lines even in the as received samples. In contrast, none of these lines are observed for high fluency samples (∼ 10²² neutrons/cm²), confirming in the bulk what is known by TEM in thin films. In addition, in similar high fluency samples annealed 24 h or 72 h at 600 °C the intensity rises just at the 2θ range where the C14 lines were observed, showing a wide peak. That peak is interpreted as a result of the superposition of unresolved diffraction lines corresponding to the Zircaloy SPPs which are in a reconstitution process of crystallization.     

An anisotropic Gurson type model to represent the ductile rupture of hydrided Zircaloy-4 sheets

The aim of this work is to model the ductile fracture of Zircaloy-4 sheets containing various amount of embrittling hydride precipitates. The proposed model is based on the Gurson–Tvergaard–Needleman model which is extended to take into account plastic anisotropy and viscoplasticity. The mechanical behavior is identified by conducting tensile tests and the damage nucleation rate (hydride cracking) is measured using quantitative metallography. The model is then used in a Finite Element software to represent crack propagation in Center Crack Panel specimens. Results are strongly mesh size dependent. The mesh size has to be identified by comparison with experimental results. Finally the model is validated by simulating crack initiation and growth in moderately complex structures (sheets containing holes).     

Facile synthesis and electrochemical properties of Mn3O4 nanoparticles with a large surface area

Mn₃O₄ nanoparticles were prepared by a novel oxidation-precipitation method at a low temperature. The crystal phase, microstructure, surface area and electrochemical properties of the products were characterized by X-ray diffraction (XRD), high-resolution transmission electron microscopy (HRTEM), N₂ adsorption-desorption isotherms and cyclic voltammetry (CV). The results indicate that the addition of citric acid and tartaric acid remarkably reduced the particle size and increased the specific surface area of Mn₃O₄ nanoparticles. The samples prepared by the addition of citric acid and tartaric acid have a narrow particle size distribution of 5-10 nm, a surface area of 119 and 122 m²/g, and a capacitance of 171 and 172 F g⁻¹, respectively.     

Microstructure and mechanical properties of laser welded wrought ZK21 magnesium alloy

The as-rolled ZK21 magnesium alloy sheets of 2 mm in thickness were successfully joined by laser welding. The effects of the welding parameters including the laser power and the welding speed on the microstructure and mechanical properties of the joints were investigated. A sound bead, with the ultimate tensile strength (UTS) of 289 MPa and up to 94% of the base metal, was obtained with the optimized welding parameters. The fusion zone (FZ) was characteristic of equiaxed dendritic grains of about 15 μm in size and fine Mg₂Zn₃ precipitates dispersed among the dendritic arms. Besides, a few columnar grains grew from the fusion boundary epitaxially. The fine grains in the heat-affected zone (HAZ) were ascribed to recrystallization.     

Enhanced electrochemical oxidation of methanol on copper electrodes modified by electrocorrosion and electrodeposition

In this paper, we report a study of electrocatalytic oxidation of methanol on copper electrodes subjected to different surface treatments, either electrocorrosion or electrodeposition in the absence of strong hydrogen co-deposition. The surface morphology of treated electrodes was examined by Field Emission Scanning Electron Microscopy (FE-SEM). The effect of different treatment conditions and the methanol concentration dependence were evaluated by cyclic voltammetric technique. The results indicate that the oxidation of methanol can be enhanced by a suitable micro and nano structure generated by these treatments. This enhanced electrode activity is related to an increase of the effective surface area and/or to an increase of the surface concentration of electroactive molecules or intermediates.     

Effect of ion irradiation in an Al90Fe2Ce8 metallic glass

Here the irradiation effect of an AlFeCe metallic glass under nitrogen ions was investigated. Ion irradiation induced crystallization can be observed in the studied metallic glass. The surface morphologies have been also examined by atomic force microscopy prior to and after ion irradiation. It is found that the surfaces have been smoothened after ion irradiation. The nanohardness and Young’s modulus of metallic glass increase after ion irradiation, which can be attributed to the formation of crystalline phases. The results obtained here clearly suggest that ion irradiation can be a useful method to tailor the microstructure and mechanical properties of metallic glasses.     

Effect of hydrogen charging on microstructural evolution and corrosion behavior of Ti-4Al-2V-1Mo-1Fe alloy

The effect of hydro gen charging on microstructural evolution and corrosion behavior of a Ti-4Al-2V-1Mo-1Fe alloy in a 3.5 wt.% NaCl solution was investigated.The results showed that the hydrogen charging induced the formation and growth of γ-TiH and δ-TiH₂ phases,leading to the initiation and propagation of hydrogen-induced cracks.It was also found that hydrogen charging can change the passivity of this alloy and increase its pitting corrosion susceptibility.The main reason for these was attributed to the fo rmation of hydrides in α phase in the Ti-4Al-2V-1Mo-1Fe alloy,leading to the preferential dissolution of the α phase and thus the deterioration in the protective ability of passive film.     

Influence of isovalent ion substitution on the electrochemical performance of LiCoPO4

LiCo_1−xM_xPO₄ (M = Mg²⁺, Mn²⁺ and Ni²⁺; 0 ≤ x ≤ 0.2) compounds have been synthesized by solid-state reaction method and studied as cathode materials for secondary lithium batteries. LiCoPO₄ exhibits a discharge plateau at ∼4.7 V with an initial discharge capacity of 125 mAh/g and on cycling capacity falls. Substitution of Co²⁺ with Mg²⁺/Mn²⁺/Ni²⁺ in LiCoPO₄ has an influence on the initial discharge capacity and on cycling behaviour. The capacity retention of LiCoPO₄ is improved by manganese substitution. Among the manganese substituted phases, LiCo_0.95Mn_0.05PO₄ shows good reversible capacity of ∼50 mAh/g.     

Synthesis and electrochemical properties of Co3O4 nanofibers as anode materials for lithium-ion batteries

Co₃O₄ nanofibers as anode materials for lithium-ion batteries were prepared from sol precursors by using electrospinning. The morphology, structure and electrochemical properties of Co₃O₄ nanofibers were characterized by atomic force microscopy (AFM), scanning electron microscopy (SEM), X-ray diffraction (XRD) and charge-discharge experiments. The results show that Co₃O₄ nanofibers possessed typical spinel structure with average diameter of 200 nm. The initial capacity of Co₃O₄ nanofibers was 1336 mAhg^− 1 and the capacity reached 604 mAhg^− 1 up to 40 cycles. It was suggested that the high reversible capacity could be ascribed to the high surface area offered by the nanofibers' structure.     

Microstructure evolution and mechanical properties of linear friction welded S31042 heat-resistant steel

S31042 heat-resistant steel was joined by linear friction welding(LFW) in this study. The microstructure and the mechanical properties of the LFWed joint were investigated by optical microscopy, scanning electronic microscopy, transmission electron microscopy, hardness test and tensile test. A defect-free joint was achieved by using LFW under reasonable welding parameters. The dynamic recrystallization of austenitic grains and the dispersed precipitation of NbCrN particles resulting from the high stress and high temperature in welding, would lead to a improvement of mechanical property of the welded joint.With increasing the distance from the weld zone to the parent metal, the austenitic grain size gradually increases from ~1μm to ~150μm, and the microhardness decreases from 301 HV to 225 HV. The tensile strength(about 731 MPa) of the welded joint is comparable to that of the S31042 in the solution-treated state.     

Fe3B基纳米复合永磁材料的微结构和性能

利用差热(扫描)分析、X射线、透射电镜、振动样品磁强计研究了添加Co、Dy对Fe3B／Nd2Fe14B 纳米复合永磁材料的微结构和性能的影响．结果表明：添加适当的微量元素可以提高Nd4．5Fe77B18．5纳米复合永磁材料的内禀磁性,改进微结构,从而提高材料的永磁性能．在Nd4．5Fe77B18．5中添加1％-3％(原子分数)的Co、Dy明显地降低材料的晶化温度和最佳热处理温度、提高了2：14：1相的居里温度、改善了纳米复合永磁材料的微观结构,从而提高材料的永磁性能．与Nd4．5Fe77B18．5相比,Nd3．5Fe74Co3DylBl8.5的永磁性能为：Br=1.06T,jHc=328kA／m,(BH)max=108．9kJ／m^3,分别提高了26％,17％和104％．     

共沉淀制备不同粒径Fe3O4纳米颗粒及磁性能的研究

以氯化铁(FeCl3·6H2O)和氯化亚铁(FeCl2·4H2O)为原料,氢氧化钠(NaOH)为沉淀剂,在无表面活性剂作用下共沉淀制备出了不同粒径的Fe3O4纳米颗粒.采用X射线衍射(XRD)、透射电子显微镜(TEM)和振动样品磁强计(VSM)对产物的晶体结构、形貌、粒径及磁性能进行了表征.实验结果表明,n(Fe2+)...     

多元醇法制备纳米Fe3O4及其静磁性能的研究

以氯化亚铁为前驱物,1,2-丙二醇为还原剂,采用多元醇法意外获得Fe3O4纳米粒子.通过X射线衍射分析标定了获得样品的物相为面心立方结构的Fe3O4,用透射电镜观察了样品的形貌,颗粒形貌为球形,大小为50～70nm,反应机理的研究表明,Fe2 发生了歧化反应,反应主要向氧化的方向进行.用振动样品磁强计表征了样品的静磁性能,测得的饱和磁化强度为74.30A·m2/kg,矫顽力仅为102.68A/m,粒子具有超顺磁性.     

镁含量对Al-Zn-In-Mg-Ti-Ga-Mn合金牺牲阳极组织和性能的影响

采用金相显微、扫描电镜以及电化学测试等方法,研究了合金元素Mg含量对Al-Zn-In-Mg-Ti-Ga-Mn牺牲阳极组织及电化学性能的影响.结果表明:随着Mg含量的增加,合金阳极中偏析相逐渐增多,牺牲阳极晶间腐蚀倾向增加,阳极性能降低.当阳极中Mg含量低于2％时,合金中偏析相适中,阳极性能优异.     

达克罗涂层的组织结构及电化学特性研究

研究了达克罗涂层的组织结构和电化学特征以揭示其耐蚀机理,达克罗涂层中锌粉和铝粉层层叠加的结构能保证其耐蚀性的稳定,EDS和XRD分析表明Cr的氧化物弥散分布,阻抗谱解析表明自腐蚀电位下稳态时的极化阻力主要来自扩散阻力,极化曲线测试表明,达克罗涂层通过降低氧的极限扩散电流密度而降低自腐蚀电流密度。     

Facile preparation and electrochemical characterization of graphene/ZnO nanocomposite for supercapacitor applications

Graphene/ZnO nanocomposites were successfully synthesized by microwave-assisted method. The structure, morphology, optical and composition of the obtained samples were characterized using XRD, FT-IR, laser Raman, UV–Vis spectroscopy and XPS analysis. XRD analysis confirmed the presence of graphene/ZnO nanocomposite. FE-SEM image reveals that the homogenous distribution of ZnO nanoparticles on the graphene nanosheets. The electrochemical properties of the graphene/ZnO electrodes were analyzed by cyclic voltammetry and impedance spectroscopy. The results confirmed that the incorporation of ZnO nanoparticles enhanced the capacitive performance of graphene electrode. Graphene/ZnO nanocomposite electrode showed higher capacitance value of 109 F g⁻¹ at a scan rate of 5 mV s⁻¹ in 1 M KCl solution as compared to the graphene electrodes. These results demonstrated the importance and great potential of graphene based composites in the development of high-performance energy-storage systems.     

The preparation of nanoporous gold electrodes by electrochemical alloying/dealloying process at room temperature and its properties

A novel method of preparing nanoporous gold has been developed: nanoporous gold materials have been prepared on the bulk gold substrates by galvanostatic electrochemical alloying and galvanostatic electrochemical dealloying processes at 0.05 mA in 1 M LiPF₆, EC/DMC(1:1, v/v) solution at room temperature. The result shows that the particle size ranges from 50 nm to 100 nm on the surface of the prepared nanoporous gold by Quanta 200FEG scanning electron microscope. And it is determined that the maximum anodic current for the nanoporous gold electrode is 50 times higher than that of the polished gold electrode in 0.5 M KOH by the cyclic voltammograms.     

Crystal structure and lithium electrochemical extraction properties of olivine type LiFePO4

Lithium iron phosphate (LiFePO₄) cathode material has been synthesized by a solid-state reaction. The XRD patterns and SEM images of the samples show that the LiFePO₄ compounds prepared at 650 °C by using carbon gel in reaction have a single-phase, small grain-size and regular shapes. By using Rietveld refinement method, we calculated the Li–O interatomic distance in LiO₆ octahedra and the cross section area of the lithium ion one-dimension tunnel, and analyze the reason of the improvement of the Lithium ion diffusion. The electrochemical test results of the sample show the LiFePO₄ prepared by using carbon gel exhibits excellent electrochemical properties. Such a significant improvement in electrochemical performance should be partly related to the enhanced Lithium ion diffusion and electric conductivity due to the use of carbon gel.     

Fabrication of precisely controlled silicon wire and cone arrays by electrochemical etching

There is an exponentially growing need for well-oriented, vertical silicon nano/micro-structure arrays, particularly in high-density integrated electronic devices. Here, we demonstrate that precisely controlled vertical arrays of silicon wires and cones can be fabricated by a combined treatment strategy of electrochemical and chemical etchings. First, a periodically ordered array of silicon wires was readily fabricated at microscale by simple electrochemical etching in which the current density played a critical role in determining the wire diameter and interspacing. The microstructures fabricated by electrochemical etching were more precisely tuned by further chemical etching, thereby transforming into cone arrays with extremely sharp tips where the cone height was controlled by the etching time. This approach could have broad utility in many electronics requiring miniaturization and high-density integration such as field emitters, photovoltaic and thermoelectric devices.     

Microstructure and mechanical properties of Mg-Al-Zn alloy under a low-voltage pulsed magnetic field

Effect of a low-voltage pulsed magnetic field on the solidified microstructure and mechanical properties of Mg-Al-Zn alloy has been investigated. When the low-voltage pulsed magnetic field is applied during solidification, the as-cast microstructure is significantly refined and α-Mg is modified from developed dendrite to fine rosette. This morphology modification is caused by the accumulation of Joule heat on the dendrite tip. The yield strength is improved with the application of the low-voltage pulsed magnetic field under normal casting and semi-continuous casting conditions. The ultimate tensile strength is decreased slightly under normal casting condition due to the occurrence of plenty of shrinkage under the low-voltage pulsed magnetic field. The shrinkages are removed and the yield strength and ultimate tensile strength are increased under semi-continuous casting condition with low-voltage pulsed magnetic field.