Synthesis and electrode characteristics of the new composite alloys Mg2Ni-xwt.% Ti2Ni

A new composite alloy Mg₂Ni-xwt.% Ti₂Ni has been successfully synthesised using a ‘particle inlaying’ method. Scanning electron microscopy and energy dispersive spectroscopy revealed that very fine Ti₂Ni particles were inlaid onto the surface of Mg₂Ni particles by mechanical treatment and sintering. XRD showed the composite alloys were composed of primary alloys Mg₂Ni, Ti₂Ni and new phases TiNi, Ti---Mg formed in the composite procedure. The electrode characteristics of Mg₂Ni-xwt.% Ti₂Ni alloys in an alkaline solution have been investigated and compared with those of Mg₂Ni. The discharge capacity of the alloy electrode was effectively improved from 8 mA h g¹ of Mg₂Ni to 165 mA h g¹ of Mg₂Ni-40wt.% Ti₂Ni at ambient temperature, which is almost comparable with that of Ti₂Ni electrode (170 mA h g¹). It is believed that the fine Ti₂Ni particles inlaid on the surface of Mg₂Ni particles play a two-fold role: firstly, they hydride-dehydride as hydrogen storage materials themselves: secondly, they provide active sites and pathways for Mg₂Ni hydriding-dehydriding. This is supported by analysis of discharge behaviour and electrochemical impedance spectra studies.     

Hydrogen absorption properties of the slurry system composed of liquid C6H6 and F-treated Mg2Ni

The hydrogenation characteristics of the slurry composed of the NH₄F solution treated Mg₂Ni and liquid C₆H₆ were studied. The F-treatment results in a net-shaped MgF₂ surface and higher nickel content in the sub-layer. It is found that the hydride of the NH₄F treated alloy has a much higher activity for the hydrogenation of benzene. The catalytic activity for hydrogenation of the alloy depended strongly on the surface properties of the catalyst. At 483 K and under a hydrogen pressure of 4.0 MPa, the alloy absorbed hydrogen first, transformed into hydride and then the benzene was hydrogenated to cyclohexane with the hydride as the catalyst. The hydrogen absorption capacity of slurry system composed of 20 wt.% treated alloy and benzene reached 6.4 wt.% and the hydrogenation completed in 20 min. Results of X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM) analysis on the crystal structure, surface composition and surface morphology of the untreated and treated alloy are presented and discussed.     

Preparation of nano-sized SrAl2O4 using an amorphous hetero-nucleus complex as a precursor

Nano-crystalline SrAl₂O₄ with spinel structure was successfully prepared at 700 °C using amorphous SrAl₂(diethylenetriaminepentaacetic acid (DTPA)_1.6)(H₂O)₄ as precursor. The precursor was synthesized by a simple inorganic reaction and decomposed into SrAl₂O₄ at temperatures above 500 °C, which was proved by DTA–TGA and X-ray photoelectron spectroscopy (XPS) analysis. X-ray diffraction (XRD) results illustrated that a crystalline SrAl₂O₄ phase can form at 700 °C, which is about 600 °C lower than that used in the traditional method. The crystalline SrAl₂O₄ prepared at 900 °C for 2 h had a crystal size of about 28 nm and a grain size of about 80 nm, and its BET surface area can reach 28.056 m²/g. Calcination temperature and time had a weak effect on crystal size.     

Ti_（0.10）Zr_（0.15）V_（0.35）Cr_（0.10）Ni_（0.30）-10% LaNi_3复合物的电化学储氢特性及协同效应

为了改善钛钒基固溶体合金的电催化活性和动力学性能,采用两步电弧熔炼法制备储氢复合合金Ti0.10Zr0.15V0.35Cr0.10Ni0.30–10%LaNi3,利用X-射线衍射、场发射扫描电镜-能谱、电化学阻抗谱和恒流充放电测试技术系统研究该储氢复合合金电极的电化学性能与协同效应。结果表明：该复合合金的主相是BCC结构的钒基固溶体相和六方结构的C14Laves相,在复合过程中生成了第二相;复合合金电极的综合电化学性能较母体合金有显著改善;复合合金电极的活化周期为5周,最大放电容量为362.5mA·h/g,在233K时放电能力为65.84%;在活化、复合、任意循环及高、低温和高倍率放电过程中,该储氢复合合金电极的放电容量均存在协同效应;该复合合金电极的电荷转移电阻和交换电流密度均存在协同效应。     

Powder Size Influence on Tensile Properties and Porosity for PM Ti_2AlNb Alloy Prepared by Hot Isostatic Pressing

Pre-alloyed powder of Ti_2AlNb alloy was prepared by electrode induction gas atomization method, and the powder was screened into fi ve kinds of powder size distribution. Fully dense Ti_2AlNb alloy was prepared by powder metallurgy(PM) using hot isostatic pressing. The properties of pre-alloyed powder and PM Ti_2AlNb alloy were tested. Results show that mean grain size of PM Ti_2AlNb alloy is infl uenced by powder particle size, but particle size has no signifi cant infl uence on tensile properties. Finer Ti_2AlNb powder has low Argon gas bubble ratio and high oxygen content, and poor fl owability of fi ner powder increases the degree of diffculty during degassing. As a result, big pores( 50 μm) are observed in PM Ti_2AlNb alloy prepared by fi ner powder and cause plasticity loss of tensile properties. In order to get a better comprehensive properties of PM Ti_2AlNb alloy, powder with an average size(～ 100 μm) is suggested.     

Zn-Co-TiO2纳米复合镀层的光生阴极保护特性

用纳米复合电沉积技术在低碳钢表面制备了Zn-Co-TiO₂纳米复合镀层。用SEM、EDS和XRD等技术手段对样品进行了分析与表征。结果表明,镀层中TiO₂的含量约为12.63%,并均匀分散在镀层中,可以起到细化Zn-Co合金镀层晶粒的作用,并使Zn-Co合金镀层的耐蚀性能得到提高。用紫外光辅助照射电极电位监测方法研究Zn-Co-TiO₂纳米复合镀层光生阴极保护特性。结果表明,在紫外光照射下,镀层的电极电位负移,说明镀层具有光生阴极保护性能;关闭紫外光灯后,其电极电位正移,但仍低于镀层未光照前的电极电位。在400℃下氧化6 h后镀层表面生成了ZnO薄膜,其与TiO₂的协同作用可进一步提高镀层的光生阴极保护性能。     

Effects of H2O2 pretreatment on surface characteristics and bioactivity of NaOH-treated NiTi shape memory alloy

The effects of H₂O₂ pretreatment on the surface characteristics and bioactivity of NaOH-treated NiTi shape memory alloy(SMA) were investigated by scanning electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, Raman spectra, Fourier transform infrared spectroscopy as well as a simulated body fluid(SBF) soaking test. It is found that the H₂O₂ pretreatment can lead to the direct creation of more Ti—OH groups and the decrease in the amount of Ni₂O₃, Na₂TiO₃ and remnant NiTi phases on the surfaces of bioactive NiTi SMA prepared by NaOH treatment. As a result, the induction period of apatite formation is shortened by dispensing with the slow kinetic formation process of Ti—OH groups via an exchange of Na⁺ ions from Na₂TiO₃ phase with H₃O⁺ ions in SBF, which indicates that the bioactivity of NaOH-treated NiTi SMA can be further improved by the H₂O₂ pretreatment.     

Highly enhanced degradation of dye with well-dispersed TiO2 nanoparticles under visible irradiation

TiO₂ nanoparticles were prepared through a facile flame method. The samples were characterized by means of X-ray diffraction, transmission electron microscopy, zeta potential measurement and transmittance spectrum. Compared with TiO₂ P-25, smaller particle size, less agglomeration and well dispersion are shown for the prepared TiO₂ particles. The photosensitized catalytic activity of as-prepared TiO₂ was investigated upon its degradation of Rhodamine B under visible light irradiation. It is found that the optical characteristics of TiO₂ have great influence on the photosensitized catalytic activity due to its crystalline forms, smaller size, higher surface area and well dispersion.     

Characterization of La2MoO6 prepared by the cation complexation technique

The La₂MoO₆ mixed oxide was prepared by the cation complexation technique using citric acid as complexant agent. The main purpose of this work was to obtain a mesoporous powder with relatively high specific surface area. The thermal decomposition behavior of the metal complex was studied by thermal analysis and Fourier transform infrared spectroscopy. A specific surface area value of 15 m² g⁻¹ was obtained by nitrogen adsorption/desorption measurements. X-ray diffraction patterns of calcined mesoporous materials reveal that even though a low degree of crystallinity is attained, this phase may be obtained at low temperatures.     

铝合金Ce-Mn转化膜溶液中HF2-离子作用机理研究

利用电子探针显微分析（EPMA）、X射线衍射（XRD）、能谱仪（EDS）、X射线光电子能谱分析（XPS）对Ce-Mn转化膜膜层进行表面和截面元素分布、相组成分析及沉淀物粉末的物相分析。结果表明,HF₂^-盐作为Ce-Mn转化膜溶液的促进剂,主元素F不是Ce-Mn复合膜层的组成成分,并不参与膜层的生长过程。通过对铝合金基体的腐蚀及其表面氧化膜(Al₂O₃)的溶解,使铝合金阴极区快速暴露,形成的[AlFe₆]^3-总量小于1.8mmol/L,完全溶于溶液。     

Preparation and electrochemical performance of nanosized Co3O4 via hydrothermal method

The hydrotalcite-type cobalt compounds were prepared through oxidation of Co（OH）2 gel using NH4OH as precipitating agent and H2O2 as oxidant. These hydrotalcite-type cobalt compounds were transformed into Co3O4 through hydrothermal decomposition with nanostructural deformation. The precursor and product were characterized by Fourier-transform infrared（FT-IR） spectrum, X-ray diffractometry（XRD） and transmission electron microscopy（TEM）. The electrochemical performances of as-prepared nanosized Co3O4 as anode materials in lithium-ion batteries were tested by charge-discharge test in the voltage range of 0-3.0 V. The influence of morphology of Co3O4 particle on the capacity and cycling performance was studied. The results show that the shape and size of the final product can be controlled by altering cobalt sources. The irregular cubic Co3O4 with the average particle size of about 10 nm shows the best electrochemical performance. After 10 charge-discharge cycles, the specific charge capacity retains 555 mA.h/g.     

pH值对CeO2/SiO2纳米复合磨粒分散性的影响

以胶体SiO₂溶液作硅源,采用均相沉淀工艺制备壳-核结构完整的CeO₂/SiO₂纳米复合磨粒。采用X射线衍射仪和透射电子显微镜对复合磨粒样品进行物相组成分析和微观形貌观察;通过粒径分布、Zeta电位分析,研究水相分散系中pH值对CeO₂/SiO₂复合磨粒分散性的影响。结果表明:所制备的CeO₂/SiO₂复合磨粒为壳-核包覆结构完整的纳米微球,粒径约110 nm,内核为无定形SiO₂,壳层为立方萤石型CeO₂;CeO₂/SiO₂复合磨粒的等电位点pH值约为5,其值由SiO₂等电位点向CeO₂等电位点明显偏移。CeO₂/SiO₂复合磨粒在酸性水相介质中分散性差,容易出现严重的团聚现象;而在碱性环境下,CeO₂/SiO₂复合磨粒分散性良好。      

Preparation of nanocomposite alumina–Sn2Fe by mechanical alloying

Nanocomposites of Al₂O₃ and Sn₂Fe were prepared by ball milling alumina with elemental Sn and Fe. Samples were prepared with molar ratios of Al₂O₃ and Sn₂Fe of 1:1 and 2:1. Materials produced in this way have been characterized by X-ray diffraction techniques as well as ⁵⁷Fe Mössbauer effect spectroscopy as a function of milling time. The nanosized grains show a distribution of particle sizes along with some residual elemental components. Preliminary investigations of electrochemical cells indicate that these materials show promise as possible electrodes for Li-ion cells.     

Oxidation behavior of multiphase Mo5SiB2 （T2）-based alloys at high temperatures

Two MosSiB2 （T2）-based alloys with nominal compositions of Mo-12.5Si-25B and Mo-14Si-28B （molar fraction, %） were prepared in an arc-melting furnace, and their oxidation kinetics from 1 000 to 1 300 ℃ were studied. The microstructures of the alloys were characterized by X-ray diffractometry（XRD） and scanning electron microscopy（SEM） with energy dispersive spectroscopy （EDS）. The oxide scales of both alloys oxidized at 1 200 ℃ for l0 min, 2 h and 100 h were investigated by surface XRD and cross-sectional SEM-EDS. The results show that the matrix of both alloys consists of T2. The dispersions of Mo-12.5Si-25B alloy are Mo and Mo3Si, and the dispersions of Mo-14Si-28B alloy are MosSi3 （T1） and MoB. The cyclic oxidation kinetics data exhibit initial rapid mass loss followed by slow mass loss. The mass loss of Mo-12.5Si-25B alloy is much faster than that of Mo-14Si-28B alloy at 1 200 and 1 300 ~C. For l0 min exposure, both alloys form irregular and porous thin scale. For 2 h exposure, Mo-12.5Si-25B alloy forms irregular thin scale and the scale contains large cracks, and Mo-14Si-28B alloy forms sound and continuous scale. For 100 h exposure, Mo-12.5Si-25B and Mo-14Si-28B alloys form sound and continuous scale about 50-75 μm and 40-45 μm in thickness, respectively. The better oxidation resistance of Mo-14Si-28B alloy is due to a sound and continuous B-SiO2 layer formation in the early stage of oxidation.     

Activation of Zr0.8Ti0.2Mn0.4V0.6Ni electrode by hot-charging treatment and its cycling performance for Ni-MH secondary battery

An electrode with a composition Zr_0.8Ti_0.2Mn_0.4V_0.6Ni was activated by hot-charging treatment at various current densities and for different times, and then its cycling performance was examined. The first discharge capacity increases as the hot-charging times and the current density increase. The hot-charging and the charge–discharge cycling create cracks on the surface of the particles and make the particles smaller, leading to the exposure of the clean surfaces of the particles.

The form of the cycling performance curve of the alloy with small and large particles is suggested. The surface of the electrode, analyzed by energy-dispersive spectrometry (EDS), shows an gradual increase in the atomic ratio of Ni as the number of cycle increases. The electrolyte after 50 cycles analyzed by ICP have relatively large concentrations of V and Zr.     

Effects of sintering on composite metal hydride alloy of Mg2Ni and TiNi synthesized by mechanical alloying

As-milled composite metal hydrides composed of Mg₂Ni and TiNi phases were cold-pressed under a pressure of 490 MPa and sintered for 1 h at 5×10⁻⁶ Torr and 300 °C. Electrochemical characteristics of the sintered composite metal hydride electrode were investigated. The maximum discharge capacity of the sintered composite alloy electrode was 125 mAh/g at a discharge current density of 100 mA/g. This value was similar to that of the as-milled one before sintering. However, the sintered electrode retained 80% of the maximum discharge capacity after 150 cycles, while the as-milled electrode retained only 55%. This is because after the sintering process an interface between Mg₂Ni and TiNi plays a role similar to a diffusion layer of hydrogen. In the sintered composite electrode, when a discharging step proceeds, hydrogen absorbed in a Mg₂Ni particle can move into a TiNi phase through the bonded-interface between Mg₂Ni and TiNi, then discharges at the interface between TiNi and the electrolyte. Also, the electrochemical impedance spectroscopy (EIS) tests showed that the composite alloy electrodes had a lower charge-transfer resistance and a higher hydrogen diffusion coefficient than those in single-phase Mg₂Ni. This indicates that TiNi particles in the composite are the active sites for redox reaction of hydrogen and the pathway for the diffusion of hydrogen     

Preparation and properties of a γ-Al2O3 washcoat deposited on a ceramic honeycomb

Washcoat deposited on ceramic honeycomb was prepared using pseudoboehmite, the CeO₂–ZrO₂–La₂O₃ solid solution, pore enlarger and other additives. The microstructures and surface performances of washcoat/honeycomb were investigated by SEM, BET surface area, XRD, ultrasonic vibration and hot shock simulation. The results show that the performance and loading of washcoat are affected obviously by the properties of slurry gel, such as the apparent viscosity, solid content, particle size and its distribution. When the apparent viscosity of slurry is lower, the gel with a narrow particle size distribution and finer particles can be obtained, with which the coating having an excellent performance can be prepared. Adding a small quantity of the CeO₂–ZrO₂–La₂O₃ solid solution can promote the thermal stability of washcoat, such as, after calcined at 1000 °C for 5 h the sample exhibits mainly the γ-Al₂O₃ phases and the θ-Al₂O₃ -Al₂O₃ and κ-Al₂O₃ phases have not been detected in the XRD spectra. It is found also that the washcoat prepared has excellent properties of the vibration-resistant, heat-resistant and its BET surface area reaches 50 m²/g.     

Electrocatalytic oxidation of methanol on carbon-nanotubes/graphite electrode modified with platinum and molybdenum oxide nanoparticles

Electrochemical codeposition and electrocatalytic properties of platinum and molybdenum oxide nanoparticles(Pt-MoOx) on carbon-nanotubes/graphite electrode for methanol oxidation were investigated.The micrograph and elemental composition of the resulting Pt-MoOx/CNTs/graphite electrode were characterized by scanning electron microscopy(SEM)and energy dispersive X-ray spectroscopy(EDS).The results show that the Pt-MoOx particles with the average size of about 50 nm are highly dispersed on the CNTs surface.The Pt-MoOx/CNTs/graphite electrode delivers excellent electrocatalytic properties for methanol oxidation.The highest mass activity(Am)reaches 264.8 A/g at the loading mass of 159.3μg/cm2.This may be attributed to the small particle size and high dispersion of Pt-MoOx catalysts deposited on the CNTs surface.The kinetic analysis from electrochemical impedance spectroscopy(EIS)reveals that the existed MoOx phase can improve the chemisorptive and catalytic properties for methanol oxidation.     

Preparation and characterization of Y3Al5O12:Ce and Y2O3:Eu phosphors powders by combustion process

A nickel hydroxide, Ni(OH)₂, was prepared by microwave-assisted heating technique from nickel nitrate aqueous solution and sodium hydroxide (assigned as PM). Then, the as-prepared PM was oxidized by liquid oxidation with sodium hypochlorite (assigned as PMO). Further, pure nanocrystalline nickel oxide (NiO) particles were obtained from the as-prepared PMO by calcination at 300, 400, 500, 600, 650 and 700 °C (labeled as C300, C400, C500, C600, C650 and C700, respectively). The as-prepared powders (PM and PMO) and the NiO nanoparticles were characterized by X-ray diffraction (XRD), infrared spectroscopy (IR), temperature-programmed reduction (TPR) and scanning electron microscope (SEM). The results indicated that the particle size of nickel oxide was controlled by the calcined temperature. The average crystal size of the NiO nanoparticles ranges from about 5 to 35 nm at 300–700 °C. Mechanism of nickel oxide nanocrystallite growth during thermal treatment was investigated.     

CaWO4-NaCl-CaCl2体系熔盐电解制备钨粉的表征与电化学分析

通过熔盐电解法从CaWO4-NaCl-CaCl2体系制备出金属钨粉,采用X射线衍射仪(XRD)、电子扫描显微镜(SEM)和能谱分析仪(EDS)对钨粉的形貌和相组成进行表征。在试验数据的基础上计算电流效率,通过分析电解过程中形成的中间产物,讨论电解过程中的电极反应,采用循环伏安法和方波伏安法分析体系的基本热力学性质。结果表明:在750℃、槽电压2.5 V下经5 h以上电解可制备出纯度达到99%、平均粒度低于2μm的金属钨粉,实验中的电流效率可达到80%;电解过程的电极反应不可逆,浓差极化是体系电解速率的主要阻力。