The role of nitrogen in the preferential chromium segregation on the ferritic stainless steel (1 1 1) surface

The temperature dependence on the segregation behavior of the ferritic stainless steel single crystal (1 1 1) surface morphology has been examined by scanning tunneling microscopy (STM), Auger electron spectroscopy (AES), and low energy electron diffraction (LEED). AES clearly showed the surface segregations of chromium and nitrogen upon annealing. Nanoscale triangular chromium nitride clusters were formed around 650 °C and were regularly aligned in a hexagonal configuration. In contrast, for the ferritic stainless steel (1 1 1) surface with low-nitrogen content, chromium and carbon were found to segregate on the surface upon annealing and Auger spectra of carbon displayed the characteristic carbide peak. For the low-nitrogen surface, LEED identified a facetted surface with (2 × 2) superstructure at 650 °C. High-resolution STM identified a chromium carbide film with segregated carbon atoms randomly located on the surface. The facetted (2 × 2) superstructure changed into a (3 × 3) superstructure with no faceting upon annealing at 750 °C. Also, segregated sulfur seems to contribute to the reconstruction or interfacial relaxation between the ferritic stainless steel (1 1 1) substrate and chromium carbide film.     

Laser pulse heating of steel surface and flexural wave analysis

Laser gas-assisted material processing finds wide application in industry. The modelling of heating, elastic response of the substrate material, and the wave analysis gives insight into the laser workpiece interaction. In the present study, laser gas-assisted heating of steel is considered. The normal component of the thermal stress is taken as the source of load for the flexural wave generation in the material. The flexural wave generated is simulated and the wave characteristics are analyzed at four locations at the workpiece surface. The numerical scheme employing a control volume approach is introduced when solving the governing equations of flow and heat transfer while finite element and spectran element methods are used when solving the stress and wave equations. It is found that the normal component of the stress is tensile. The dispersion effect of the workpiece material, interference of the reflected beam, and partial overlapping of second mode of the travelling wave enable to identify a unique pattern in the travelling wave in the substrate.     

X-ray photoelectron spectroscopy investigation of the carburization of 310 stainless steel

The surface of 310 stainless steel (310SS) samples was investigated by X-ray photoelectron spectroscopy (XPS) after 500 h cyclic exposure to two carburizing atmospheres: CH₄ (2%)–H₂ (98%) at 800 °C, and CH₄ (10%)–H₂ (90%) at 1100 °C. The depth distribution of various elements in the surface region was obtained by XPS after successive cycles of argon etching. The microstructure of the alloy was observed by scanning electron microscopy (SEM) and the phases formed during the exposure were analyzed by X-ray diffraction (XRD). The results showed that the major phases that were formed within few micrometer depth during exposure at 800 °C include both iron and chromium carbides. (Mn, Cr) oxide was also formed as a result of the reaction with the residual oxygen of the atmosphere. A region of few microns width that was relatively depleted of chromium was formed under the surface as a result of the outwards diffusion of chromium. The exposure to the reducing atmosphere at 1100 °C led to the formation of various iron and chromium carbides. No oxide was formed during exposure. In all exposed samples, the surface was Cr enriched while nickel remained buried under the surface region that reacted with the atmosphere.     

Surface composition of the steel powders pre-alloyed with manganese

The determination of the surface oxide layer composition is vital to facilitate the adjustment of the sintering conditions for sufficient removal of the surface oxides for providing strong metal bonding between the metal particles during sintering. To systematically investigate the composition, morphology and thickness of the surface oxide the influence of manganese content from 0.3 to 1.8 wt.% on the surface products composition in the case of water atomized steel powder was evaluated. Analysis of the powder surfaces by X-ray photoelectron spectroscopy and high-resolution scanning electron microscopy in combination with X-ray microanalysis showed that powder particles in all cases are covered by heterogeneous oxide layer, composed of particulate features of thermodynamically stable oxides (Cr-Mn-Si) and homogeneous iron surface oxide layer in between. For increasing alloying content the fraction of stable oxide cations in the surface layer increases linearly, whereas the thickness of the iron oxide layer decreases. Moreover, from the investigation of the sintering and degassing behavior by thermal analysis coupled with mass-spectrometry (TG/DTA + MS), three different stages of carbothermal reduction process were observed and their correlation with surface oxides composition was established during sintering in argon.     

激光触发真空沿面闪络开关的初步实验研究

 介绍了沿面闪络开关的发展状况和基本原理，实验研究了真空条件下激光触发介质沿面闪络特性。实验采用固体Nd:YAG纳秒激光器作为触发源，对试样施加正直流高压，电压范围1～6 kV，试样绝缘子为直径50 mm的尼龙6。通过研究不同激光能量、波长和聚焦形状对介质闪络的影响，总结出适用于沿面闪络开关的激光触发形式。实验表明：在一定电场和真空度下闪络的时延和抖动将随着输入激光能量的提高而减小，而激光可触发的电压范围将提高；激光波长减小有助于提高触发的稳定性；激光焦斑的形状是沿面闪络触发的最大影响因素，采用具有一定能量密度、焦斑横跨两电极的带状激光来触发闪络是闪络开关的理想选择。     

Temperature-dependent modifications in the surface composition of Finemet: A ToF-SIMS study

Time-of-flight secondary ion mass spectrometry (ToF-SIMS) was employed as an in situ tool to study the temperature-induced alteration of the surface composition of amorphous Finemet, Fe₇₃Si_15.8B_7.2Cu₁Nb₃. Temperature was changed reversibly by cooling from room temperature to 118 K and warming back to room temperature. As a general result, the ion intensities and, consequently, the surface concentrations of the alloy constituents were found to vary non-monotonously. Therefore segregation processes were in operation the extent of which was element-specific. Most importantly, while cycling the temperature hysteresis behaviour was observed with concentration of Fe developing just opposite to that of the alloying elements. Accordingly, on cooling the alloy, the surface enrichment with B, Si, Nb, Cu attained first a maximum in the range of 248-193 K before the segregation changed the trend to establish appreciable depletion of these elements at 118 K (as compared to room temperature). By contrast, the surface iron content developed inversely and decreased first to a minimum at ∼223 K before reaching enrichment at 118 K. During warming, a maximum segregation of boron and silicon was observed at about 223 K - similar as on cooling - so that this temperature can be considered characteristic of the segregation process. Dissociative adsorption of water from the residual atmosphere occurring at low temperatures was responsible for the formation of surface hydroxides of iron, silicon and niobium; an enhanced adsorption of molecular water was observed at temperatures below 153 K. The temperature-dependent segregation and adsorption-desorption processes were found to be largely reversible, so that the surface composition of Finemet was practically restored after finishing the cooling-warming cycle. The processes and factors governing the non-monotonous temperature dependence of the surface segregation in the amorphous alloy are discussed within the frame of segregation theory and the influence of temperature-induced tensile stress on segregation.     

New developments in the surface analysis of solids

In both fundamental and applied surface physics, it is essential to know as much as possible about the chemical composition of the outer atomic layers of solids. Rapid progress has recently been made in the development of analytical methods which could be used in surface analysis. All utilize some type of emission (photons, electrons, atoms, molecules, ions), caused by excitation of the surface states. Both the “excitation” and emission processes must meet certain basic requirements as regards information depth, form in which the information is obtained, sensitivity, changes in the surface layer during analysis, etc. The more important of the methods that qualify, namely Auger-Electron Spectroscopy (AES), photo-Electron Spectroscopy for Chemical Analysis (ESCA) and the static method of Secondary-Ion Mass Spectrometry (SIMS), are discussed and their potentialities and limitations illustrated by characteristic examples.     

Inhibition of initial surface oxidation by strongly bound hydroxyl species and Cr segregation: H2O and O2 adsorption on Fe-17Cr

The initial stages of surface oxidation of Fe-17Cr (ferritic stainless steel) were investigated at 323 K by X-ray photoelectron spectroscopy (XPS) and inelastic electron background analysis. The results indicated the formation of a mixed iron-chromium oxide layer upon O₂ exposure and the formation of a thin chromium oxyhydroxide layer upon H₂O exposure. The oxidation of Fe did not occur in the latter case. Moreover, it was found that pre-exposing the Fe-17Cr surface to H₂O significantly hinders subsequent oxidation by O₂, thus providing a way to control the formation of nanoscale oxides on stainless steel materials. It was concluded that the formation of strongly bound hydroxyl species together with adsorbate-induced segregation of Cr severely limits the reaction between O₂/H₂O and Fe from the alloy.     

An XPS round robin investigation on analysis of wood pulp fibres and filter paper

X-ray photoelectron spectroscopy (XPS) has been applied to pulp and paper research for decades. However, there has been no attempt to standardise or even systematically compare experimental and analysis procedures, even though it is known that fibrous, nature-derived and insulating fibre materials pose remarkable challenges to reliable surface analysis. The experimental problems are mainly linked with neutralisation, energy resolution, contamination and X-ray induced degradation.We have tested applicability, reliability and reproducibility of XPS analysis on real pulp samples with varying lignin and extractives contents in a small round robin investigation. We also tested the instrumental set-ups with an acetone-extracted filter paper, used as a reference sample. The data, collected at four different laboratories with state-of-the-art instruments indicate that reproducible results can be obtained, despite minor differences in experimental and analysis procedures. However, we found that a specified sample handling procedure and limited X-ray exposure are crucial for reproducible, reliable data.Based on the round robin data we recommend dose restricted monochromatic measurements, a cellulosic in situ reference and a consistent sample handling procedure. The data confirms that a paper-based reference material and the correlation of high-resolution C 1s data with O/C atomic ratios can be used in testing instruments and experimental set-ups for pulp and paper materials.     

Influence of CrN surface compound on the initial stages of high temperature oxidation of ferritic stainless steel

Segregation phenomena and formation of surface compounds on Fe-17Cr (ferritic stainless steel) were studied at temperatures up to 800 °C upon annealing and kinetically controlled oxidation by photoelectron spectroscopy and inelastic electron background analysis. The results revealed the formation of a chromium nitride surface compound during annealing in ultrahigh vacuum at temperatures exceeding 527 °C. Surface enrichment of P, As, and other trace elements became more prominent at higher temperatures approaching 800 °C. It was found that nitrogen was buried below the surface oxide layer during oxygen exposure, yet it had little effect on the rate of oxidation. However, the formation of CrN surface compound promoted the selective oxidation of Cr initially, which is of great importance in processing and application environments involving high temperature and controlled atmosphere conditions.     

Comparison of F-12 aramid fiber with domestic armid fiber III on surface feature

A comparison of F-12 aramid fiber with domestic armid fiber III (DAF III) on surface feature was carried out by scanning electron microscope (SEM), atomic force microscopy (AFM), elements analysis and X-ray Photoelectron Spectroscopy (XPS) analysis. It is found that the two aramid fibers are of “skin-core” structure and fibrillar structure. The microfibrils orient along the fiber axis and rather poorly bond in transverse direction. Many defects exist on the surface of two fibers. Carbon, hydrogen, nitrogen and oxygen are the major elements of two aramid fiber. The element content of the same aramid fiber from surface to interior is different. The surface carbon contents of F-12 aramid fiber and DAF III are increased by 10.75% and 9.95% than those in fiber interior respectively, the surface nitrogen content decreased by 9.72% and 27.02% respectively, and the surface oxygen content increased by 13.99% and 37.95% respectively.     

The influence of UV irradiation on surface composition of collagen/PVP blended films

The surface chemical composition and surface properties of collagen/poly(vinyl pyrrolidone) (PVP) blended films before and after UV irradiation (λ = 254 nm) were investigated using X-ray Photoelectron Spectroscopy (XPS), FTIR-ATR spectroscopy and Atomic Force Microscopy (AFM).The XPS results showed that collagen is enriched on the surface of the collagen/PVP blend. The surface composition of the collagen film was changed more by UV irradiation than the surface composition of the collagen/PVP blend.FTIR-ATR spectra showed that the positions of the amide bands in collagen are more altered after UV irradiation than those for the collagen/PVP blends.AFM images showed that the collagen surface is ordered contrary to PVP. The blend surface was similar to the pure collagen surface and confirms that there is more collagen present at the surface (higher concentration of collagen at the surface compared to PVP). UV irradiation caused only the small changes in the surface morphology of the collagen/PVP films. All of the results confirm that the surface of the collagen/PVP blend is more photoresistant than collagen.     

Evolution of vacuum ultraviolet emission in dual-frequency capacitively coupled plasmas

In plasma material processing, vacuum ultraviolet (VUV) emission is released from gas discharges, leading to undesirable results. Energetic VUV photons enable the creation of an electron-hole pair current when their energy is larger than the bandgap energy of the plasma-facing top layer during plasma material processing. For example, the high energy of VUV photons from helium (21.2 eV), argon (11.6 eV), and oxygen (13.6 eV) is sufficient to generate induced currents in SiO₂ thin films. These feedstock gases are widely used in many procedures utilizing low-temperature industrial plasmas. Thus, the VUV emission evolution with both the power ratio between high (60 MHz) and low (2 MHz) frequencies and pulse duty ratio of the low-frequency radio frequency (rf) power in a dual-frequency capacitively coupled plasma, which is indispensable in modern plasma etching processes, was investigated. Both the power ratio between high and low frequencies and the pulse duty ratio changed the electron temperature, leading to evolution of the VUV emission intensity.     

Liquid surface and liquid/liquid interface energies of binary subregular alloys and wetting transitions

Energetics and chemistry of liquid surfaces and liquid/liquid interfaces of binary A-B alloys are calculated using a subregular solution model. In this model, two macroscopic energetic parameters are used to produce an asymmetric miscibility gap. They are related to two microscopic parameters which describe the interaction energy between two atoms as a function of the composition of the first coordination shell of each atom. The impact of the asymmetry of the A-B interactions on the surface and interfacial energies and adsorption are analyzed by comparing the results obtained with this subregular model to those calculated for a regular solution. The role of the asymmetry on the prewetting and wetting transitions are also discussed. Calculations performed in the Co-Cu system are in good agreement with experimental data of surface energy.     

Surface roughness influence on the pull-in voltage of microswitches in presence of thermal and quantum vacuum fluctuations

In this work we investigate the influence of the combined effect from random self-affine roughness, finite conductivity, and finite temperature on the pull-in voltage in microswitches influenced by thermal and quantum vacuum fluctuations through the Casimir force and electrostatic forces. It is shown that for separations within the micron or sub-micron range the roughness influence plays a dominant role, while temperature starts to show its influence well above micron separations. Indeed, increasing the temperature leads to higher pull-in voltages since it leads to an increased Casimir force. The temperature influence is more significant for relatively large roughness exponent H ∼ 1, while its influence is significantly lower with increasing lateral roughness correlation length ξ or due to long wavelength surface smoothness.     

ARXPS study of a plasma-treated polymer surface: An example of Case II diffusion?

The Laplace transform of the Wang, Kwei and Frisch equation for the concentration depth profile of a diffusant in a glassy polymer has been derived and applied to the interpretation of ARXPS data obtained on a polystyrene film exposed to a helium/oxygen plasma. It was found that the best fit to the data was given by a rectangular oxygen profile that would be characteristic of Case II diffusion. The reliability of this finding is discussed in terms of the uniqueness of the fitted profile.     

A method for the study of surface segregation in multicomponent alloys

A simple algorithm for the determination of segregation profiles in multicomponent systems based on a mean field formalism and a quantum approximate method for the energetics is introduced. The method is described and applied to two ternary systems, concentrating on the changes in segregation patterns relative to the corresponding binary cases.     

真空冷却过程中真空室内温度变化的实验研究

以熟肉为实验材料,对真空冷却过程中真空室内温度变化进行了实验研究。结果发现:真空冷却过程中真空室内的温度会出现一些波动,其变化过程可以分为四个阶段:真空室内的温度从15.8℃一直降低到10.7℃;然后从10.7℃升到最高的19.1℃;随着产品温度的降低以及真空室内压力的降低,真空室内的温度从最高的19.1℃降低到最低的6.1℃;最后,由于真空室内放气阀的开启,使得真空室的温度从最低的6.1℃升高到最终的13.1℃,一直保持在真空冷却过程结束。     

Structure and composition of the NiPd(1 1 0) surface

The NiPd(1 1 0) alloy surface was studied using low energy electron diffraction to measure the structure and composition of the first three atomic layers. The surface layer is highly enriched in Pd and has a significantly buckled structure. The second layer is also buckled, with displacements even larger than the surface layer. The second layer also exhibits intralayer segregation (chemical ordering), with alternate close-packed rows of atoms being Ni enriched and Pd enriched. The third layer has a structure and composition close to that of the bulk alloy. These results are compared with results for the other low index faces of NiPd, the extensive literature on NiPt alloy surfaces, and the growing body of theoretical literature for NiPd alloy surfaces.     

Comparative study of morphology and surface composition of Al–Cr–Fe alloy powders produced by water and gas atomisation technologies

The morphology and surface composition of Al–Cr–Fe alloy powders of 0–63 and 63–100 μm size fractions, produced by gas and water atomisation, have been studied by scanning electron microscopy and Auger electron spectroscopy. While gas atomised particles are of spherical shape, water atomised powders are usually irregular in shape with a complex branched relief. The morphology and composition of surface oxides have been estimated. The surface oxide film is composed of aluminium oxides/hydroxides and contains no Fe and Cr atoms. Two to five water molecules are associated with one Al₂O₃ molecule on the surface of powders. The surface oxide film has a non-uniform thickness, with thick oxide islands separated by thinner oxide film. The parameters of the surface film morphology, such as the island coverage, the oxygen content and the thin film thickness, depend on the atomisation technology used and powder size fraction. Heavily and weakly oxidised powder groups present in all powder fractions are distinguished by Auger spectra analysis. Relationships between heavily and weakly oxidised powder groups are discussed as a function of atomisation technology and size fraction.