Image analysis of atmospheric corrosion of field exposure high strength aluminium alloys

The corrosion morphology image acquisition system which can be used in the field was established. In Beijing atmospheric corrosion exposure station, the image acquisition system was used to capture the early stage corrosion morphology of five types of high strength aluminium alloy specimens. After the denoise treatment, wavelet-based image analysis method was applied to decompose the improved images and energies of sub-images were extracted as character information. Based on the variation of image energy values, the corrosion degree of aluminium alloy specimens was qualitatively and quantitatively analyzed. The conclusion was basically identical with the result based on the corrosion weight loss. This method is supposed to be effective to analysis and quantify the corrosion damage from image of field exposure aluminium alloy specimens.     

The effect of grain refining on the microsegregation of aluminium–magnesium alloy 5182

Aluminium alloy 5182 (AA5182) contains approximately 4.5% Mg as its principal alloying addition, and is most commonly used to make the lid of the aluminium can. With a view to the possible future development of a micro-macro model to describe the casting of this alloy, the effect of grain refinement on the microsegregation of magnesium in industrial rolling ingots of AA5182 has been investigated at three different depths beneath the edge of the ingot (and hence three different cooling rates)—60, 140 and 600 mm. The accuracy with which published microsegregation models are able to predict the solute distribution profile is assessed. It has been found that the magnesium segregation range (C_max–C_min) of the grain refined samples actually increases as cooling rate decreases. The range of the non grain refined samples is independent of cooling rate. The solute concentration profiles of the theoretical microsegregation models examined do not correlate well with the experimentally measured profiles. It is concluded that this poor correlation is due to either the effect of post solidification homogenisation or the influence of macroscopic variables during the cast. A more accurate model of post solidification homogenisation is required to assess the relative contribution of each of these factors to the poor correlation. In addition, it is concluded that the measurement of segregation is best done using a combination of EDX mapping and point analysis techniques to locate and quantify the areas of maximum and minimum solute concentration.     

Crystalline Sb–Cu alloy films as anode materials for Li-ion rechargeable batteries

A crystalline Sb–Cu alloy is investigated for use in Li-ion rechargeable batteries, and its structural, electrochemical and thermal properties are characterized. A pulse electrodeposition method is used to prepare Sb–Cu alloy film on Cu foil as a negative electrode. The structure of the alloy film electrode is characterized using XRD, FE-SEM and EDX. The electrochemical behavior of the Sb–Cu alloy film is investigated at the current rate of 0.1C to the cut-off potential range of 1.8 and 0.01 V vs. Li/Li⁺. Our experimental results demonstrate that the initial discharge capacity is 850 mAh g^?1 and that the discharge capacity increases to 1034 mAh g^?1 at the end of the 30th cycle with a stable cycle life. The Coulombic efficiency is approximately 83.5% with good cyclability. Moreover, the crystalline Sb–Cu alloy film has relatively low exothermic properties, and it may be an interesting candidate for use in the negative electrodes of Li-ion batteries.     

用高重频激光剥离-火花诱导击穿光谱分析铝合金样品

为了提高基于等离子体原子发射光谱元素分析技术的分析速度,在高重复频率的前提下建立了一套激光剥离-火花诱导击穿光谱元素分析系统并以铝合金为样品开展了光谱分析。实验以低脉冲能量的声光调Q固体激光脉冲剥离样品,并触发高压火花放电以增强等离子体辐射、提高光谱分析灵敏度。研究结果表明： 在高重频火花放电的作用下,等离子体辐射的峰值强度和弛豫时间分别得到了增强和延长,信号的时间积分强度增强因子可以达到1～2个数量级,且更易于实现时间分辨的信号检测。对铝合金中微量铬元素分析的检出限可达~132 ppm。该研究验证了高重频激光剥离-火花诱导击穿光谱用于分析固体样品元素的可行性,其技术有望在固体样品元素的快速分析中发挥一定的作用。该光谱技术能同时兼顾扫描成像的速度、空间分辨率和光谱分析灵敏度,并为固体样品的二维或者三维元素分布的高分辨快速扫描成像分析提供了一种很好的技术途径。     

A silane pre-treatment for improving corrosion resistance performances of emeraldine base-coated aluminium samples in neutral environment

An aluminium-magnesium alloy AA5182 substrate pre-treated with a 3-aminopropyl-triethoxysilane (APS)-based solution and coated with emeraldine base (EB) showed improved corrosion resistance to neutral salt spray test, compared to samples pre-treated with phosphoric acid-based solutions prior to the EB coating. Scanning electron microscopy (SEM) and energy dispersive X-ray spectrometry (EDX) characterisations of samples pre-treated with APS showed the presence of an uneven silane coating on the aluminium surface according to the surface microstructure. The potentiodynamic study performed on the EB-coated samples showed a noticeable reduction of corrosion current of coupons pre-treated with APS, while no relevant difference in corrosion behaviour was observed between APS and phosphoric acid pre-treated samples prior to the EB coating. The coupling activity of APS between the AA5182 surface and EB coating at the most sensitive corrosion sites could be responsible of an improved adhesion of the EB coating at these points and could explain the observed improved corrosion resistance.     

A microstructure-based yield stress and work-hardening model for textured 6xxx aluminium alloys

The plastic properties of an aluminium alloy are defined by its microstructure. The most important factors are the presence of alloying elements in the form of solid solution and precipitates of various sizes, and the crystallographic texture. A nanoscale model that predicts the work-hardening curves of 6xxx aluminium alloys was proposed by Myhr et al. The model predicts the solid solution concentration and the particle size distributions of different types of metastable precipitates from the chemical composition and thermal history of the alloy. The yield stress and the work hardening of the alloy are then determined from dislocation mechanics. The model was largely used for non-textured materials in previous studies. In this work, a crystal plasticity-based approach is proposed for the work hardening part of the nanoscale model, which allows including the influence of the crystallographic texture. The model is evaluated by comparison with experimental data from uniaxial tensile tests on two textured 6xxx alloys in five temper conditions.     

Hyperfine interaction studies and magnetic properties of FeCoAlN nanocomposite films

Nanogranular magnetic films were produced by specially designed UHV plasma-jet system with DC hollow-cathode discharge. We investigated the properties of these ferromagnetic FeCoAlN-based films. The analyses of the samples were additionally complemented by the study of nuclear magnetic resonance (NMR), Mössbauer spectroscopy, magnetic measurements, and X-ray diffraction.     

Total analysis of surface structure and properties by UHV transfer system

We have developed an ultrahigh-vacuum (UHV) complex sample preparation and analysis system, which realizes a reliable surface science analyzing various characters on an identical surface. The system contains three sample-preparation-and-characterization chambers and five analysis chambers. They are (1) an electronic-properties-characterization chamber, (2) a magnetic-properties-characterization chamber, (3) an organic-molecule chamber, (4) UHV SEM, (5) a high-energy-resolution angle-resolved photoelectron spectrometer, (6) a high-energy-resolution display-type spherical mirror analyzer, (7) a room-temperature (RT) STM, and (8) an optical-properties characterization chamber. A special sample holder is used with six electrodes on it, which enables accurate temperature measurement of a sample by connecting a thermocouple directly to the sample even if it is transferred. Four other electrodes can be used for construction of various circuits including evaporators. Some examples are shown.     

Au80Sn20合金焊料制备工艺

针对高功率二极管激光器的封装要求,通过磁控溅射的方法制备了Au80Sn20合金焊料,使用扫描电子显微镜（SEM）观察其微结构和表面形貌;利用能谱仪（EDX）和X射线荧光测试仪分析其成分;采用差热分析法（DTA）测试其熔化温度,并用制备的Au80Sn20合金焊料进行了可焊性实验。结果表明:磁控溅射法可以制备Au80Sn20合金焊料,其制备的Au80Sn20合金焊料表面无明显缺陷,结构致密;成分与理论值接近;熔点与理论熔点接近;焊接浸润性好,空洞率小,强度大。     

Corrosion of aluminium components studied with MIES, UPS and XPS

We use X-ray photoelectron spectroscopy (XPS), ultraviolet photoelectron spectroscopy (UPS) and metastable impact electron spectroscopy (MIES) to investigate the corrosion of aluminium components. Clean aluminium films were prepared under ultrahigh vacuum (UHV) conditions and exposed to water and NaCl. We attempt to provide a model for the mechanism of this interaction and its effects on the durability of the components.     

The influence of surface microchemistry in protective film formation on multi-phase magnesium alloys

The high strength:weight ratio of magnesium alloys makes them an ideal metal for automotive and aerospace applications where weight reduction is of significant concern. Unfortunately, magnesium alloys are highly susceptible to corrosion particularly in salt-spray conditions. This has limited their use in the automotive and aerospace industries, where exposure to harsh service conditions is unavoidable. The simplest way to avoid corrosion is to coat the magnesium-based substrate by a process such as electroless plating, which is a low-cost, non line of sight process.Magnesium is classified as a difficult to plate metal due to its high reactivity. This means that in the presence of air magnesium very quickly forms a passive oxide layer that must be removed prior to plating. Furthermore, high aluminium content alloys are especially difficult to plate due to the formation of intermetallic species at the grain boundaries, resulting in a non-uniform surface potential across the substrate and thereby further complicating the plating process.The objective of this study is to understand how the magnesium alloy microstructure influences the surface chemistry of the alloy during both pretreatment and immersion copper coating of the substrate.A combination of scanning electron microscopy, energy dispersive spectroscopy and scanning Auger microscopy has been used to study the surface chemistry at the various stages of the coating process. Our results indicate that the surface chemistry of the alloy is different on the aluminum rich β phase of the material compared to the magnesium matrix which leads to preferential deposition of the metal on the aluminum rich phase of the alloy.     

Fabrication,characterization and biocompatibility of TiO2 nanotubes via anodization of Ti6Al7Nb

Ti6Al7Nb has been used as an implant material because of its good corrosion resistance and high mechanical properties. However, the presence of aluminium (Al), which may lead to ostemalacia, anaemia and nervous system disorders, limited its wide clinical use. In this study, a titanium oxide (TiO₂) nanoporous layer was fabricated on a Ti6Al7Nb alloy using an electrochemical anodic oxidation method. The structure of the TiO₂ nanoporous layer was examined by scanning electron microscopy. The chemical compositions of the samples were analysed by X-ray photoelectron spectroscopy (XPS). Biocompatibility was evaluated by culturing rat osteoblast cells. The result showed that TiO₂ nanoporous layers comprise a mixed oxide containing TiO₂ and a small amount of nobium oxides (Nb₂O₅) and almost no elemental aluminium. The outer layer of the TiO₂ nanoporous layer comprises highly ordered nanotubes and the inner layer forms disordered nanopores. The TiO₂ nanoporous layer could support the adhesion, proliferation, differentiation and gene expression of osteoblast cells. Therefore, a TiO₂ nanoporous layer could enhance the biocompatibility of Ti6Al7Nb alloy and is as a promising candidate for Ti6Al7Nb alloy implants.     

FEM study of palladium and molybdenum clusters on an alumina covered field emitter

Palladium and molybdenum polycrystalline layers (clusters) have been deposited in a stainless steel UHV system onto a layer of alumina (Al₂O₃). This layer has been prepared by high temperature oxidation of an aluminium layer. The interaction of this system with nitrogen has been investigated at room temperature by an FEM technique. Under these conditions nitrogen spillover from molybdenum to palladium has been observed.     

Preparation of single-walled nanotubes with the help of a Ni/Cr-based catalyst

The high-yield synthesis of single-walled carbon nanotubes (SWNTs) is carried out in an electric-arc discharge using the Ni-Cr alloy as a catalyst. A new method of introducing the catalyst into the plasma hot region is used in the synthesis. In this method, the anode with a sandwich structure consists of two longitudinal graphite rods of a rectangular cross section, between which the Ni-Cr alloy in the form of a foil having a thickness approximately equal to 0.2 mm is placed. The obtained samples are investigated using transmission electron microscopy (TEM), Raman spectroscopy, and thermogravimetry. According to the results of TEM observations, SWNTs are tied into bundles with a length of several micrometers and a diameter of about 10 nm. The Raman spectra indicate that the diameter distribution of SWNTs lies between 1.2 and 1.5 nm with a peak at approximately 1.24 nm. The SWNT content in the obtained samples is approximately 20%. Heat treatment at various temperatures with a dosed air supply leads to a noticeable mass loss of the sample and to a change in its composition. For example, thus heating to 600 K causes a mass loss of about 40%, leading to an increase in the content of SWNTs up to 35% without their noticeable destruction. Further heating above 600 K leads to a virtually complete thermal decomposition of SWNTs.     

The effect of cerium and lanthanum surface treatments on early stages of oxidation of A361 aluminium alloy at high temperature

X-ray photoelectron spectroscopy analysis has been used to study the surface of A361 aluminium alloy after electrodeposition of cerium and lanthanum compounds followed by oxidation tests in air at 100-500 °C for 2 h. Cerium and lanthanum oxide deposits are found on the β-AlFeSi second phase particles and to a lesser extent on the eutectic Al-Si areas, while the α-Al phase is covered with a thin aluminium oxide film. This uneven deposition may be related either to a preferential nucleation and growth process on active interfaces or to the differing electrical conductivity of the phases and intermetallic compounds of the alloy. Initial stages of oxidation of A361 alloy disclosed thickening of the aluminium oxide layer and Mg enrichment at the surface, especially above 400 °C. Rare earth deposits revealed two different effects: reduced Mg diffusion and enhanced thickening of the aluminium oxide film. A distinctive behaviour of Ce oxide appears at 300-500 °C related with Ce(III) to Ce(IV) transition.     

EDX法分析钼铁中Mo等成分的研究

近期铁合金市场上出现了一些Mo含量很低的高杂质钼铁,采用常规化学法分析,由于杂质元素的共沉淀,Mo的分析结果与冶炼所得钢材的Mo含量相差很大,说明经典的化学法并不适用于高杂质钼铁的Mo含量分析。文章用能量色散X射线荧光法(EDX)分析了钼铁中的Mo等主要成分,研究了制样方法对分析结果的影响,将扫描电镜用于分析样品的表面形貌观察。试验结果表明,EDX可以用于钼铁中Mo和Si的分析,而P,S和Cu未能检出。样品表面形貌对分析结果有一定的影响,通过扫描电子显微镜(SEM)观察发现,将研磨后的钼铁粉末用较大的载荷压成片状样品,变成平坦、光滑的分析表面,可进一步提高Mo的检测精度。     

直流辉光放电等离子体激发光源自动调节控制系统

直流辉光放电过程中需要控制的三个重要工作参数为放电电流、放电电压和放电室内氩气气压.该文介绍了一种应用于直流辉光放电等离子体激发光源的自动调节控制系统,该控制系统在放电电流恒定的情况下调节放电室内氩气气压,实现了对放电电压的信号采集和自动控制.文卷阐述了该控制系统的设计思路、电路原理及控制方案.该自动调节控制系统改善了以往用手动调节时精度低且操作复杂的情况,提高了放电电压的控制精度,缩短了放电电压的稳定时间.文中给出了自动控制方式下激发源放电电压的稳定性测试结果,控制精度由手动调节时的4%FS改善为小于1%FS,放电电压稳定时间由手动时的大于90s缩短到30 s以内.采用该控制系统对中低合金钢和锡肯铜标准样品进行了样品精密度实验.元素含量分析精密度比手动调节方式显著提高,各元素含量测试结果的相对标准偏差(RSD)均优于3.5%.中低合金钢标准样品中Ti,Co,Mn元素含量测试结果的RSD范围由手动时的3.0%～4.3%减小到1.7%～2.4%,S和Mo元素RSD范围由5.2%～5.9%减小到3.3%～3.5%.锡青铜标准样品中Sn,Zn,Al元素RSD范围由2.6%～4.4%减小到1.0%～2.4%,Si,Ni,Fe元素的RSD范围由6.6%～13.9%降低到2.6%～3.5%,并给出了实测数据.     

Characteristics of sealed plasma electrolytic oxidation coatings with electrochemical impedance spectroscopy

<正>Plasma electrolytic oxidation(PEO) coatings are prepared on aluminium with graphite powders added into the electrolyte.The scanning electron microscopy(SEM) coupled with an energy dispersive x-ray analysis system(EDX) is used to characterize the surface and the cross-section morphologies of the coatings.The electrochemical impedance spectroscopy(EIS) is used not only to evaluate the corrosion resistance but also to analyse the structure of the coating. Results show that graphite powders are embedded in the PEO coating.The corrosion resistances of both the inner barrier and the outer porous layer are greatly improved,and the EIS could give some valuable detailed information about the coating structure.     

UHV/CVD硅锗膜的Raman光谱分析

本文提出一种用Raman光谱测量SiGe合金膜中的锗组分及应变的方法,方法是非破坏的。并用这一方法测量了几种不同锗组分和膜厚度的SiGe合金样品,它们都是用UHV／CVD设备生长的,其中两个样品还与X－射线双晶衍射的结果作了比较,两种方法的结果十分一致,这说明本文提出的方法是准确可靠的,这些样品用于制作SiGe/Si异质结PMOSFET,对0．5um 沟长器件,跨导达112ms.mm^-1。     

Characteristics of hydrogen storage alloy electrode with cupric oxide additive

Cupric oxide was used as a novel additive for the hydrogen storage alloy electrode in nickel metal hydride batteries. The influence of the cupric oxide on the discharge storage capacity (DSP) of the hydrogen storage alloy electrode was studied and the electrochemical properties of the electrode were investigated. The cupric oxide was verified to reduce to copper in the first charge and stably existed on the alloy surface in the following cycles. And the hydrogen storage alloy electrode with cupric oxide exhibited better high rate discharge capability and longer cycle life compared with the blank one. The cupric oxide greatly decreases the weight and volume of the hydrogen storage alloy electrode, and make it better meet the requirement as power sources for electric and hybrid vehicles.