Characterization of silane layers on modified stainless steel surfaces and related stainless steel-plastic hybrids

The aim of this work was to characterize silane layers on the modified stainless steel surfaces and relate it to the adhesion in the injection-molded thermoplastic urethane-stainless steel hybrids. The silane layers were characterized with scanning electron microscope and transmission electron microscope, allowing the direct quantization of silane layer thickness and its variation. The surface topographies were characterized with atomic force microscope and chemical analyses were performed with X-ray photoelectron spectroscopy. The mechanical strength of the respective stainless steel-thermoplastic urethane hybrids was determined by peel test. Polishing and oxidation treatment of the steel surface improved the silane layer uniformity compared to the industrially pickled surface and increased the adhesion strength of the hybrids, resulting mainly cohesive failure in TPU. XPS analysis indicated that the improved silane bonding to the modified steel surface was due to clean Fe₂O₃-type surface oxide and stronger interaction with TPU was due to more amino species on the silane layer surface compared to the cleaned, industrially pickled surface. Silane layer thickness affected failure type of the hybrids, with a thick silane layer the hybrids failed mainly in the silane layer and with a thinner layer cohesively in plastic.     

Electron-beam modification of a surface layer deposited on low-carbon steel by means of arc spraying

State-of-the-art means of physical materials science are used to study the structure, phase composition, defect substructure, and tribological properties of a coating formed on low-carbon Hardox 450 martensite steel via the electrocontact deposition of an Fe–C–Ni–B wire and modified through subsequent irradiation with high-intensity pulsed electron beams. It is shown that electron-beam treatment results in the formation of a modified 50-μm thick surface layer, the main phases of which are the α-phase, iron boride FeB, and boron carbide B₄C. In the layer modified by electron-beam treatment, the transverse size of batch martensite crystals is reduced by a factor of 3, relative to the initial Hardox 450 steel, and ranges from 50 to 70 nm. It is established that the wear resistance of the deposited layer after electron-beam treatment grows by more than 20 times with respect to the wear resistance of Hardox 450 steel, and the friction coefficient is reduced by a factor of 3.5. The microhardness of a deposited layer ~7 mm thick is more than double that of the base metal.     

Surface layer structure degradation of rails in prolonged operation

By methods of optical, scanning and transmission electron microscopy and microhardness measurement the transformation regularities of structure-phase states, defect substructure, fracture surface and mechanical properties of rail surface layer up to 10 mm deep in process of long-term operation (passed tonnage of gross weight 1000 mln. tons) were revealed. According to the character of fracture and level of structure imperfection the three layers were detected: surface, transition and boundary ones. It has been shown that the surface layer ~20 μm in thickness has a multiphase, submicro- and nanocrystalline structure and it contains micropores and microcracks. The increased density of bend extinction contours at 2 mm depth from the tread contact surface was noted, and it was shown that the maximum amplitude of stress fields was formed on the interphase boundary the globular cementite particle–matrix. The evaluation of stress fields was done.     

The influence of compressive stress applied by hard coatings on the power loss of grain oriented electrical steel sheet

To reduce the core loss of electrical steel the vacuum arc ion plating technique has been used to deposit titanium nitride (TiN) layers on highly grain oriented electrical steel sheets. The layer thickness, the stresses of layers and coated sheets and the achieved reduction in core losses have been measured as functions of coating duration and applied bias voltage. Well adhered layers with high compressive stress up to 6.8 GPa have been produced. With increasing bias voltage the layer thickness decreases and the intrinsic stress of the layers increase. A further increase of bias voltage leads to a drop in stress due to thermal relaxation. In general, the tensile stress of the coated sheets rises with increasing layer thickness while the core loss of the coated material decreases with increasing tensile stress of the steel sheet and increasing bias voltage. The highest reduction of core loss has been found to be 28% (from P_1.7=0.86 W/kg for commercially coated HGO electrical steel sheet with glass film to 0.62 W/kg for TiN coated material) and is due to the reduction of excess loss only.     

Prediction of dislocation formation in epitaxial multilayers subject to in-plane loading

A theoretical model is described to predict equilibrium distributions of misfit dislocations in one or more anisotropic epitaxial layers of a multilayered system deposited on a thick substrate. Each layer is regarded as having differing elastic and lattice constants, and the system is subject to biaxial in-plane mechanical loading. A stress transfer methodology is developed enabling both the stress and displacement distributions in the system to be estimated for cases where the interacting dislocations are of a pure edge configuration. Energy methods are used to determine equilibrium distributions of the dislocations for given external applied stress states. It is shown that the new model accurately reproduces known exact analytical solutions for the special case of just one isotropic epitaxial layer applied to an isotropic semi-infinite substrate having the elastic constants of the substrate but differing lattice constants. The model is used to consider equilibrium dislocation distributions in capped epitaxial systems with misfit dislocations. It is shown that the simplifying assumptions often made in the literature, regarding the uniformity of elastic properties and the neglect of anisotropy, can lead to critical thicknesses being underestimated by 15–18%. The application of uniaxial tensile stresses increases the value of critical thicknesses. The model can be used to analyse dislocations in various non-neighbouring layers provided the dislocation density has the same value in all layers in which dislocations have formed. This type of analysis enables the prediction of the deformation of metallic multilayers subject to mechanical and thermal loading.     

金属表面碳涂层对激光等离子体辐射的影响

 阐述了激光诱导击穿光谱技术的基本原理,分析了金属材料表面光学性质与激光诱导等离子体辐射强度的关系,建立了空气中进行等离子辐射研究的试验装置,测量了不同厚度碳层下激光等离子体的发射光谱强度。实验结果表明：当一束近红外高能量脉冲激光（能量为5 J）作用于覆盖有约18 μm厚度碳层的标钢样品时,激光等离子体的发射光谱强度提高了16%～22%;证明了金属样品表面覆盖碳层能够提高激光等离子体辐射强度。     

The influence of low-temperature silver-ion exchange on the spectral-luminescent properties of fluorophosphate glasses doped with PbSe

Changes in the absorption and luminescence spectra of fluorophosphate glasses doped with PbSe caused by low-temperature Ag⁺–Na⁺ ion exchange are considered. It is found that the silver distribution gradient in a near-surface layer about 16 μm thick leads to two different processes of interaction between metal and semiconductor nanoparticles. PbSe molecular clusters and quantum dots more efficiently grow in deep layers with a low silver concentration. The near-surface glass layers with a high silver concentration exhibit formation of Ag metal nanoparticles, on the surface of which interaction with PbSe molecular clusters leads to the formation of Ag–Se–Pb bonds, which transform into Ag₂Se layers in the process of heat treatment. The appearance of the new phase is confirmed by X-ray diffraction.     

Superconducting properties of V/Fe superlattices

We report measurements on the superconducting properties of V/Fe superlattices with various layer thicknesses. These samples were prepared with a novel UHV evaporator which can produce up to twenty different samples in the same run. The Fe layer, a strong pair breaker, suppresses the superconducting transition temperature in a systematic way. When the V layer thickness is on the order of the BCS coherence length and the Fe layer is only a few atomic planes thick, a 2D–3D crossover has been observed in the temperature dependence of the parallel upper critical field H_C2∥. This implies the coexistence of superconductivity and ferromagnetismm. We observe three dimensional behavior for thinner Fe layers (～1 atomic plane) and two dimensional behavior for thicker Fe layers (greater than 10 atomic planes).     

Study of the composition and properties of protective layers formed by the ion-beam-assisted deposition of cadmium,zinc, and aluminum onto steel surfaces

Layers formed by the ion-beam-assisted deposition of cadmium, zinc, and aluminum onto the surface of carbon and stainless steels to protect aluminum and its alloys from corrosion in the case of their contact with steel parts are investigated. The protective layers are created via ion-beam-assisted deposition, in which metal deposition and mixing of the deposited layer with the substrate surface (this process is implemented by accelerated (U = 5 kV) ions of the same metal) occurs, respectively, from a neutral vapor fraction and the vacuum arc plasma of a pulsed electric-arc ion source. The morphology and composition of the generated surface layers are studied by means of scanning electron microscopy, electron-probe microanalysis, and Rutherford backscattering spectrometry. The layer composition is revealed to include atoms of the deposited metal, the substrate material, oxygen, and carbon. The layer thickness varies from ~50 to 80 nm, and the deposited metal content of the layers is ~(1.0–3.5) × 10¹⁷ atom/cm². Corrosion tests of the aluminum and its alloy in contact with the materials under study confirm the efficiency of the ion-beam modification of steel surfaces.     

Investigating <Superscript>64</Superscript>Zn<Superscript>+</Superscript> ion-doped silicon under conditions of hot implantation

The results from visualizing the structure and identifying the composition of surface and the nearsurface layers of CZ n-Si (100) implanted by ⁶⁴Zn⁺ ions with dose of 5 × 10¹⁶ cm^–2 and energy of 50 keV under conditions of a substrate heated to 350°C are presented. It is found that there is no Si amorphization after Zn implantation, and only one layer 200 nm thick forms and is damaged because of radiation-induced defects. Zn nanoparticles 10–100 nm in size are found on a sample’s surface and in its near-surface layer. Computer analysis and mapping of the elemental and phase composition of FIB crater walls and the surface show that the main elements (54%) in the sample near-surface layer are Si, O, and Zn. The presence of ZnO phase is recorded to a depth of 20 nm in the sample.     

Interface effects on Gd induced disordering of Co films on Pt(111)

Amorphization of epitaxial Co thin films grown on top of a Pt(111) surface has been studied by surface X-ray diffraction after deposition of Gd overlayers. The results indicate strong differences of the disordering process depending on the thickness of the Co film. First basic difference is that thick Co films (15 atomic layers) are only partially amorphized by 4 atomic layers of Gd on top of them, whereas thinner Co films (5 atomic layers) are completely disordered by just 2 atomic layers of Gd. Moreover, amorphization by Gd overlayers induces different stress relaxation processes in both cases. For 15 atomic layers thick Co films a preferential amorphization of the more strained Co grains is observed, leading to an effective relaxation of about ? 0.5% of the in-plane lattice parameter during amorphization, approaching its relaxed value. On the contrary, for 5 atomic layers thick Co films, the initial steps of disordering are accompanied by a stronger increase of the in-plane lattice constant, by about 1.4%, typical of Co–Pt interface alloy formation, followed by a complete amorphization. Furthermore, the magnetic characterization, carried out by magneto-optical Kerr effect and resonant magnetic surface X-ray diffraction, strongly supports that the amorphization of thin Co films is changing the nature of the Co/Pt interface. In particular, as Gd overlayers are deposited, and the amorphization proceeds, the structural disordering of the Co/Pt interface flips its characteristic perpendicular magnetic anisotropy toward in-plane orientation before the complete magnetic depolarization of the interface Pt atoms is reached. All these results confirm a marked dependence of amorphization processes on film thickness, which can be related to the enhanced influence of the nearby film/substrate interface.     

Diffuse phase transition in a surface quartz layer with variations in temperature

The temperature dependence of the α-phase concentration in surface layers of a solution-grown quartz crystal has been studied in the range 290–820 K. This has been achieved by measuring the intensity of the 695.1, 785.0, and 1061.5 cm^?1 bands in the ?″(ν) IR damping spectra. It has been found that, in a surface layer ～0.15 μm thick, the concentration of the α-phase behaves with increasing temperature as expected for a first-order phase transition, namely, before 800 K, it remains constant, after which at T → 846 K, tends to zero. At a distance from ～1 to 20 μm from the surface, however, the concentration of the α-phase starts to decrease already at ～350 K, while at 812 K it decreases to one-fifth of the original value. This is paralleled by an increase in the intensity of the 804 cm^?1 band assigned to the β-phase. The diffusive pattern of the α-β phase transition is initiated by distortion of the quartz crystal lattice around growth dislocations. The internal stresses arising in these layers have been estimated from the shift of the band maxima. It has been established that at distances up to ～1 μm from the surface, tensile stresses reaching ～300–400 MPa appear at 400 K. These stresses drive in the surface layer of the macrocrystal microcracks culminating in total destruction of the sample. The appearance of tensile stresses is assigned to an increase in volume of the macrocrystal layer located at a distance from ～1 to 20 μm from the surface and the growth in it of the β-phase concentration. At the same time, compressive stresses develop in a layer ～1 to 20 μm thick at a temperature above 500 K, which reach a maximum at ～650 K, to fall off thereafter with increasing temperature. The compression is caused by vibrations of growth dislocation loops in the temperature range specified.     

Finite amplitude folding of single layers: elastica,bifurcation and structural softening

The amplification of viscous single-layer folds, from infinitesimal amplitudes up to finite amplitudes and large strains, is investigated analytically. Analytical solutions for finite amplitude folding of viscous layers valid for large viscosity contrasts and for post-buckling of elastic columns are shown to be identical. The failure of the classical, exponential amplification solution for folding is quantified using a nonlinear amplification equation similar to the Landau equation. The evolution of fold amplitude–strain for single layers with different initial amplitudes and viscosity contrasts essentially depends on a single parameter rather than three parameters as commonly assumed (strain, initial amplitude and viscosity contrast). This single parameter is constructed by scaling the strain with the crossover strain, which is the specific value of strain at which the linear solutions fail. Scaling the strain with the crossover strain yields a collapse of all amplitude evolution paths for different initial amplitudes and viscosity contrasts onto a single amplification path. Analytical solutions for the evolution of the layer-parallel deviatoric stress within the layer during folding are presented showing a decrease of the layer-parallel deviatoric stress with increasing fold amplitude. All stress–amplitude evolution paths for different initial amplitudes and viscosity contrasts can be collapsed onto a single stress–amplitude evolution path, if the amplitude is scaled by the crossover amplitude. The decrease in stress is proportional to a decrease in effective viscosity of the layer during folding. This decrease in effective viscosity represents structural softening, because the true, Newtonian viscosity of the layer remains constant.     

Acoustic study of adsorbed liquid layers

Interference measurements of small variations in the velocity and attenuation of surface acoustic waves (SAWs) are used to investigate water layers up to 15 nm thick adsorbed on the surface of a lithium niobate crystal. The frequency dependence of the relative variation of the SAW velocity with the adsorption of water vapor is measured in the range from 40 to 400 MHz. Acoustic techniques are used to experimentally estimate the frequency dependence of the dielectric constant of adsorbed water and its dipole relaxation frequency along with the dependence of the adsorption layer thickness on the water vapor pressure in the surrounding medium. A simple expression is proposed for calculating the dispersion of the SAW velocity in a solid loaded with a thin liquid layer.     

Elastic measurements of layered nanocomposite materials by Brillouin spectroscopy

Surface Brillouin spectroscopy makes it possible to measure surface elastic wave propagation parameters at frequencies up to 20 GHz or more. This enables us to measure the elastic properties of surface layers only a small fraction of a micrometre thick. The wavelength and incident angle of the light determine the wavenumber of surface elastic waves (SAW) that scatter the light inelastically, and their frequency can be found by measuring the change in wavelength of the scattered light. By analysing the elastic wave modes present in the surface, the elastic properties can be deduced. We have used this technique to measure the elastic properties of layered nanocomposite materials, which are widely used in the packaging industry. 12 microns polymer films (PET) were coated with glass oxide layers of thickness as little as 25 nm, to give transparent nanocomposite structures with excellent gas barrier properties. In order to understand and model the behaviour of these films under deformation, it is necessary to determine the elastic properties of the different layers. Evaluation of the elastic properties presents several challenges. First, the oxide layers are much thinner than the wavelengths of the surface phonons in surface Brillouin spectroscopy (and hence the depth probed), which usually lie in the range 250-500 nm. The anisotropic elastic properties of the PET substrate must therefore be measured accurately, and this can be done using bulk Brillouin spectroscopy. Second, a thin layer of metal (usually 10-20 nm) must be deposited on the glass surface so that the surface phonons scatter the light effectively. The elastic properties of the glass layer can then be deduced from surface Brillouin spectroscopy measurements, by simulating the surface wave modes of the metal/glass/polymer composite, and adjusting the parameters to give the best fit. In this way it is possible to observe how the properties of the glass vary as a function of thickness, and in turn to understand how to improve systematically the properties under deformation.     

Reaction products and oxide thickness formed by Ti out-diffusion and oxidization in poly-Pt/Ti/SiO2/Si with oxide films deposited

In the paper, we present experimental results to enhance the understanding of Ti out-diffusion and oxidization in commercial poly-Pt/Ti/SiO₂/Si wafers with perovskite oxide films deposited when heat-treated in flowing oxygen ambient. It indicates that when heat-treated at 550 and 600 °C, PtTi₃+PtTi and PtTi are the reaction products from interfacial interaction, respectively; while heat-treated at 650 °C and above, the products become three layers of titanium oxides instead of the alloys. Confirmed to be rutile TiO₂, the first two layers spaced by 65 nm encapsulate the Pt surface by the first layer with 60 nm thick forming at its surface and by the next layer with 35 nm thick inserting its original layer. In addition, the next layer is formed as a barrier to block up continuous diffusion paths of Ti, and thus results in the last layer of TiO_2−x formed by the residual Ti oxidizing.     

P110钢CO2腐蚀产物膜的XPS分析

为了确定CO2腐蚀产物膜的组成及不同层次结构中成分和含量的差异,采用P110钢在高温高压腐蚀静态釜中制备CO2腐蚀产物膜,利用SEM观察了腐蚀产物膜的表面和断面形貌,结合XRD分析结果,通过XPS研究了两层结构膜的化学组成差异。结果表明,腐蚀产物膜断面呈现双层结构;膜层的主要成分是FeCO3,还有少量的CaCO3和铁的氧化物,但内层CaCO3较多且夹杂着Fe3C和单质Fe,外层氧化物稍多;通过内外层Ca^2＋含量差异推断出内层腐蚀膜优先形成。     

Characterization of inhomogeneous colloidal layers using adapted coherence probe microscopy

Colloidal layers play an important role in environmental studies, for example in the movement of radionuclides in nuclear waste management. New characterization techniques are required for studying such complex, porous layers. The purpose of this work is to adapt coherence probe microscopy (CPM), which is typically used for measuring the surface roughness of single surfaces, to the analysis of thick inhomogeneous colloidal layers. Two types of layers, either composed of 80 nm or 400 nm alumina colloidal particles deposited on glass slides by decantation have been studied. One of the problems in performing routine roughness measurements of colloidal layers using CPM is the appearance of apparent pits below the level of the substrate surface. We demonstrate that this is due to partial detection of the buried colloid/substrate interface. Further, we have developed the “Z-scan” technique, which consists of building up an XYZ image stack by scanning the full depth of the sample. Any point in an XY image can then be investigated to study the local buried internal structure, layer thickness, and effective refractive index. Comparison of results with AFM and SEM confirm the structure found with CPM and the new “Z-scan” technique, which opens up new and useful applications.     

Structure and dynamics of ordered water in a thick nanofilm on ionic surfaces

The structure and dynamics of water in a thick film on an ionic surface are studied by molecular dynamic simulations. We find that there is a dense monolayer of water molecules in the vicinity of the surface. Water molecules within this layer not only show an upright hydrogen-down orientation, but also an upright hydrogen-up orientation. Thus, water molecules in this layer can form hydrogen bonds with water molecules in the next layer. Therefore, the two-dimensional hydrogen bond network of the first layer is disrupted, mainly due to the O atoms in this layer, which are affected by the next layer and are unstable. Moreover, these water molecules exhibit delayed dynamic behavior with relatively long residence time compared with those bulk-like molecules in the other layers. Our study should be helpful to further understand the influence of water film thickness on the interfacial water at the solid-liquid interface.     

激光冲击对E690高强钢激光熔覆修复微观组织的影响

为研究激光冲击对E690高强钢激光熔覆修复层微观组织的影响,选用专用金属粉末对E690高强钢试样预制凹坑进行激光熔覆修复,并使用脉冲激光对激光熔覆层进行冲击强化处理,同时采用扫描电镜、透射电镜和X射线应力分析仪分别对激光冲击前后激光熔覆层的微观组织和表面残余应力进行检测。结果表明:激光熔覆修复后,激光熔覆层组织为等轴晶,熔覆层与E690高强钢基体之间冶金结合良好,其表面残余应力为均匀分布的压应力。经激光冲击后,激光熔覆层截面晶粒得到细化,并观察到大量的形变孪晶,互相平行的孪晶界分割熔覆层粗大晶粒,在激光熔覆层的晶粒细化过程中发挥着重要作用;试样表层位错在{110}滑移面上发生交滑移,在晶界周围形成了位错缠结。经激光冲击后,激光熔覆层冲击区域表面残余压应力数值相较于冲击前提升了1.1倍。