Surface analysis and oxidation behavior of Y-ion implanted AZ31 magnesium alloys

AZ31 samples were implanted with yttrium ions with fluences of 5 × 10¹⁶, 1 × 10¹⁷ and 5 × 10¹⁷ ions/cm², using a metal vapor vacuum arc source at an extraction voltage of 45 kV. The surfaces of the implanted samples were then analyzed by Auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS). It was found that after treatment a pre-oxidation layer was formed, and the higher the fluence, the thicker the pre-oxidation layer was. The valence states showed that yttrium existed in the form of Y₂O₃. Isothermal oxidation tests have been conducted in pure oxygen at 773 K for 90 min to evaluate the oxidation behavior of the implanted samples. The results indicate that after implantation the oxidation resistance of the samples was significantly improved. Moreover, the greater the fluence, the better the oxidation resistance has been achieved. The characterization of the implanted layers after isothermal oxidation was examined by SEM, AES and XPS. From the results, it can be found that the thickness of the oxide scale formed on the implanted surfaces have been greatly decreased, and there is no obvious change for both the thickness of the pre-oxidation layer and the valence states of the elements after oxidation.     

XPS study of SnTe(1 0 0) oxidation by molecular oxygen

The interaction between the (1 0 0) surface of SnTe single crystal and molecular oxygen was studied by means of X-ray photoelectron spectroscopy (XPS). Analysis of the obtained spectra shows that the mechanism of surface oxidation does not change in the range of oxygen exposure 10⁸-10¹³ L. During the oxidation an additional component shifted 1.1 eV towards higher binding energies appears in the Sn 3d spectra. The Te 3d_5/2 spectra fitting reveals two additional components with binding energies close to Te⁰ and Te⁺⁴. The dependence of the additional components fraction in both Sn 3d and Te 3d_5/2 spectra on the oxygen exposure is semi-logarithmic. On the base of the experimental data two possible mechanisms are proposed.     

A study of the formation and oxidation of PtSi by SR-PES

In the paper we present the results on the formation of platinum silicide (PtSi) by means of synchrotron radiation photoelectron spectroscopy (SR-PES) and show the effect of a Pt/Si sample exposure to both a low and high-pressure oxygen atmosphere at the end of an annealing process. We have carried out a detailed analysis of high resolution photoelectron spectra of the Pt 4f and Si 2p peaks which were taken during the sample annealing at specific temperatures. In addition to the generally known Pt₂Si and PtSi phases we have recognized an additional intermediate phase during the formation of Pt₂Si and attributed it to the Pt₃Si phase. We have proved that silicon diffuses towards the sample surface. The results of a low-pressure oxygen experiment have shown that oxygen binds only to surface silicon, however, in the case of a PtSi sample prepared externally in the ON Semiconductor labs under nitrogen/oxygen atmosphere oxygen binds not only to surface silicon but also takes over Si atoms out of the PtSi phase which results in the formation of a SiO₂ layer on almost pure platinum.     

Influence of titanium ions implantation on corrosion behavior of zirconium in 1 M H2SO4

In order to study the effect of titanium ion implantation on the aqueous corrosion behavior of zirconium, specimens were implanted with titanium ions with fluence ranging from 1 × 10¹⁶ to 1 × 10¹⁷ ions/cm², using a metal vapor vacuum arc (MEVVA) source at an extraction voltage of 40 kV. The valence states and depth distributions of elements in the surface layer of the samples were analyzed by X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES), respectively. The potentiodynamic polarization technique was employed to evaluate the aqueous corrosion resistance of implanted zirconium in a 1 M H₂SO₄ solution. It was found that a significant improvement was achieved in the aqueous corrosion resistance of zirconium implanted with titanium ions. The larger the fluence, the better is the corrosion resistance of implanted sample. Finally, the mechanism of the corrosion behavior of titanium-implanted zirconium was discussed.     

Surface composition modification of high-carbon low-alloy steels oxidized at high temperature in air

Segregating alloys across a metal/oxide interface, which occurs when an iron alloy is heated at high temperature in air, was studied on five high-carbon low-alloy steels. The metallographic analyses showed differences between the oxidation kinetics, the decarburisation rates of the surfaces and the number of surface defects. The results of the AES analyses enabled the characterization of the concentration profiles of the alloy elements and to explain the differences observed between the oxidation kinetics, the decarburisation rates and the number of surface defects. All the concentration profiles are discussed and possible mechanisms are proposed in order to understand the profiles obtained.     

Effect of copper ions implantation on corrosion behavior of zircaloy-4 in 1 M H2SO4

In order to study the effect of copper ion implantation on the aqueous corrosion behavior, samples of zircaloy-4 were implanted with copper ions with fluences ranging from 1 × 10¹⁶ to 1 × 10¹⁷ ions/cm², using a metal vapor vacuum arc source (MEVVA) operated at an extraction voltage of 40 kV. The valence states and depth distributions of elements in the surface layer of the samples were analyzed by X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES), respectively. Glancing angle X-ray diffraction (GAXRD) was employed to examine the phase transformation due to the copper ion implantation. The potentiodynamic polarization technique was employed to evaluate the aqueous corrosion resistance of implanted zircaloy-4 in a 1 M H₂SO₄ solution. It was found that a significant improvement was achieved in the aqueous corrosion resistance of zircaloy-4 implanted with copper ions when the fluence is smaller than 5 × 10¹⁶ ions/cm². The corrosion resistance of implanted samples declined with increasing the fluence. Finally, the mechanism of the corrosion behavior of copper-implanted zircaloy-4 was discussed.     

Role of chromium ion implantation on the corrosion behavior of zirconium in 1N H2SO4

In order to study the effect of chromium ion implantation on the aqueous corrosion behavior of zirconium, specimens were implanted by chromium ions with a dose range from 1×10¹⁶ to 1×10¹⁷ ions/cm², using MEVVA source at an extracted voltage of 40 kV. The valence and elements penetration distribution of the surface layer were analyzed by X-ray photoelectron spectroscopy (XPS) and auger electron spectroscopy (AES), respectively. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to examine the micro-morphology and microstructure of chromium-implanted samples. The potentiodynamic polarization measurement was employed to value the aqueous corrosion resistance of zirconium in a 1N H₂SO₄ solution. It was found that a significant improvement was achieved in the aqueous corrosion resistance of zirconium compared with that of as-received zirconium. The mechanism of the corrosion resistance improvement of chromium-implanted zirconium is probably due to the addition of the chromium oxide dispersoid into the zirconium matrix.     

Determination of growth modes via spectroscopy: new simple analytical models

Analytical models for the determination of thin film growth modes were developed on the basis of the simultaneous multilayer (SM) growth model. The models take into account up-step and down-step diffusion, enabling quick identification of the growth modes from experimentally obtained spectroscopic data. We tested the models by applying them to growth data from the literature that had been recorded via Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS), and low-energy ion scattering (LEIS). We discuss the applicability of the new analytical models in comparison with the diffusion-corrected simultaneous multilayer (DCSM) model.     

The effect of gold on platinum oxidation in homogeneous Au-Pt electrocatalysts

Oxidation of Au-Pt thin films was carried out in ambient air at room temperature and characterized by X-ray photoelectron spectroscopy. The homogeneous films were prepared by RF co-sputtering with concentrations varying from Au₉Pt₉₁ to Au₈₉Pt₁₁ and compared to pure Pt and Au thin films. Spectral deconvolution of the Au 4f and Pt 4f core levels revealed linear peak shifts for both the Au-Au and Pt-Pt bonding components as a function of alloy mixture and metallic component peak asymmetry that remained constant for all alloy stoichiometries. The predominant oxidation products were PtO and PtO₂ and were characterized by stable core level binding energies for all films. A gradual decline in the Pt-O_x products and corresponding levels of elemental oxygen was observed with increasing Au content but was similar in proportion to the metallic Pt components. Based on these results, variations in Pt oxide phases and/or concentration do not appear to contribute to enhanced electrocatalytic activity for oxygen reduction observed for the intermediate alloy stoichiometries.     

Near surface composition of some alloys by X-ray photoelectron spectroscopy

Chemical compositions of the alloys of CuNi (Cu_0.10Ni_0.90, Cu_0.30Ni_0.70, Cu_0.70Ni_0.30) and BiSb (Bi_0.80Sb_0.20, Bi_0.64Sb_0.34, Bi_0.55Sb_0.45) are determined by X-ray photoelectron spectroscopy. The stoichiometries are determined and are compared with the bulk compositions. Possible sources of systematic errors contributing to the results are discussed. Errors arising out of preferential etching in these alloys have been investigated. It has been inferred from such studies that the preferential etching does not enrich the surface composition with a particular component for the two systems reported here. Quantitative results of CuNi system indicate that the surface regions of the Cu_0.70Ni_0.30 alloy is Cu-rich, although no such evidence is observed in case of BiSb system.     

X射线光电子能谱

X射线光电子能谱（X-ray photoelectron spectroscopy，XPS）技术也被称作用于化学分析的电子能谱（electron spectroscopy for chemical analysis，ESCA）．XPS属表面分析法，它可以给出固体样品表面所含的元素种类、化学组成以及有关的电子结构重要信息，在各种固体材料的基础研究和实际应用中起着重要的作用．文章简要介绍了XPS仪器的工作原理和分析方法，并给出了XPS在科学研究工作中的应用实例．     

Core level spectroscopy and RHEED analysis of KGd0.95 Nd0.05(WO4)2 surface

A study of the surface structure and electronic properties of (010) KGd_0.95Nd_0.05(WO₄)₂ (Nd:KGW) using RHEED analysis and XPS is presented. It is shown that Nd doping has a negligible effect on the core levels of the basic elements. A bombardment of the Nd:KGW crystal with 3-keV Ar ions results in surface amorphization accompanied by the generation of tungsten ions in lower valence states.     

The effect of Pt on Ni3Al surface oxidation at low-pressures

The fully-oxidized surface that forms on (1 1 1) oriented Ni₃Al single crystals, with and without Pt addition, at 300-900 K under oxygen pressures of ca. 10⁻⁷ Torr was studied using XPS, AES, and LEIS. Two main types of surfaces form, depending upon oxidation temperature. At low-temperature, the predominant oxide is NiO, capped by a thin layer of aluminum oxide, which we refer to generically as Al_xO_y. At high-temperature (i.e., 700-800 K), NiO is replaced by a thick layer of Al_xO_y. By comparing samples that contain 0, 10 and 20 at.% Pt in the bulk, we find that the effect of Pt is to: (1) reduce the maximum amount of both NiO and Al_xO_y; and (2) shift the establishment of the thick Al_xO_y layer to lower temperatures. Platinum also decreases the adsorption probability of oxygen on the clean surface.     

Luminescence characterization and electron beam induced chemical changes on the surface of ZnAl2O4:Mn nanocrystalline phosphor

Luminescence characteristics and surface chemical changes of nanocrystalline Mn²⁺ doped ZnAl₂O₄ powder phosphors are presented. Stable green cathodoluminescence (CL) or photoluminescence (PL) with a maximum at ∼512 nm was observed when the powders were irradiated with a beam of high energy electrons or a monochromatic xenon lamp at room temperature. This green emission can be attributed to the ⁴T₁ → ⁶A₁ transitions of the Mn²⁺ ion. Deconvoluted CL spectra resulted in two additional emission peaks at 539 and 573 nm that may be attributed to vibronic sideband and Mn⁴⁺ emission, respectively. The luminescence decay of the Mn²⁺ 512 nm emission under 457 nm excitation is single exponential with a lifetime of 5.20 ± 0.11 ms. Chemical changes on the surface of the ZnAl₂O₄:Mn²⁺ phosphor during prolonged electron beam exposure were monitored using Auger electron spectroscopy. The X-ray photoelectron spectroscopy (XPS) was used to determine the chemical composition of the possible compounds formed on the surface as a result of the prolonged electron beam exposure. The XPS data suggest that the thermodynamically stable Al₂O₃ layer was formed on the surface and is possibly contributing to the CL stability of ZnAl₂O₄:Mn phosphor.     

Surface characterisation of ethylene-propylene-diene rubber upon exposure to aqueous acidic solution

Two types of pure ethylene propylene diene rubbers were exposed to two different acids for varying period of time. Surface characterisation was carried out using X-ray photoelectron spectroscopy (XPS). Two EPDM rubbers selected for this study were comparable in co-monomer compositions but significantly different with respect to molar mass and the presence of long chain branching. Both rubbers contained 5-ethylidene-2-norbornene (ENB) as diene. Solution cast films of pure EPDM samples were exposed in two different acidic solutions, viz. chromosulphuric (Cr (VI)/H₂SO₄) and sulphuric acid (H₂SO₄) (20%, v/v) at ambient temperature from 1 to 12 weeks. XPS analysis indicated that several oxygenated species were formed on the surface of both rubbers after exposure. It was postulated from the XPS analyses that both aqueous acidic solutions attacked the olefinic double bonds (CC) of ENB. Furthermore, 20% Cr (VI)/H₂SO₄ also attacked the allylic carbon-hydrogen (CH) bonds of ENB resulting in more oxygenated species on the surface compared to 20% H₂SO₄ under identical conditions. Cr (VI) in the 20% Cr (VI)/H₂SO₄ was found to play an important role in alteration of surface chemistry. Studies using a model system consisting of EPDM mixed with Cr (VI) and Cr (III) salts revealed that the change of oxidation state from Cr (VI) to Cr (III) as a consequence of direct involvement of Cr (VI) in the chemical alteration of EPDM surfaces. Interestingly, the presence of long chain branching and molar mass did not significantly influence the chemical processes owing to the acid treatment.     

Interfacial bonding characteristic of nanoclay/polymer composites

Using a small amount of nanoclay (montmorillonite (MMT)) can significantly enhance the thermal and mechanical properties of polymer-based composites. Therefore, an in depth understanding of the bonding characteristic between the nanoclay and its surrounding matrix is essential. In this study, Fourier Transform Infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS) were conducted to analyze the chemical composition between epoxy matrix and nanocomposite. These experiments revealed that a chemical bonding at an interface between the matrix and nanoclay of the composites did exist. Thus, such bonding can enhance the mechanical and thermal properties of resultant polymer composites as reported in many literatures.     

Surface cleaning procedures for thin films of indium gallium nitride grown on sapphire

Surface preparation procedures for indium gallium nitride (InGaN) thin films were analyzed for their effectiveness for carbon and oxide removal as well as for the resulting surface roughness. Aqua regia (3:1 mixture of concentrated hydrochloric acid and concentrated nitric acid, AR), hydrofluoric acid (HF), hydrochloric acid (HCl), piranha solution (1:1 mixture of sulfuric acid and 30% H₂O₂) and 1:9 ammonium sulfide:tert-butanol were all used along with high temperature anneals to remove surface contamination. X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM) were utilized to study the extent of surface contamination and surface roughness, respectively. The ammonium sulfide treatment provided the best overall removal of oxygen and carbon. Annealing over 700 °C after a treatment showed an even further improvement in surface contamination removal. The piranha treatment resulted in the lowest residual carbon, while the ammonium sulfide treatment leads to the lowest residual oxygen. AFM data showed that all the treatments decreased the surface roughness (with respect to as-grown specimens) with HCl, HF, (NH₄)₂S and RCA procedures giving the best RMS values (∼0.5-0.8 nm).     

Dissociative adsorption of NO on TiO2(1 1 0) argon ion bombarded surfaces

The interaction of NO with TiO₂(1 1 0) Ar⁺-ion-bombarded surfaces has been studied by X-ray photoelectron spectroscopy, ultraviolet photoelectron spectroscopy, Auger electron spectroscopy. Surfaces with different degrees of defects have been characterized by monitoring the evolution of the electronic structure of the surface, with the aim of studying the influence of the surface defects on the interaction with NO. The interaction was studied for exposures up to 500 L. However, the main effects occur already in the first 10 L. The exposure of the surfaces to NO resulted in the removal of defect sites without adsorption of N.     

Structural and compositional stability of Co oxide grown on (001) bct Co

Room temperature (RT) adsorption of oxygen on the (001) surface of metastable, cubic Co film epitaxially grown on a Fe substrate results in the formation of about 7 monolayers (ML) crystalline CoO film, in the typical rocksalt structure 45° rotated with respect to the square unit mesh of the underlying Co film. We investigated the stability of this oxide layer upon annealing in the RT–620 K temperature range, by means of primary-beam diffraction modulated electron emission (PDMEE), and X-ray photoelectron spectroscopy (XPS). For temperatures up to 570 K, film thickness and local order are preserved, in spite of an increasing number of Co and O atoms bonded in sites of reduced coordination. For larger temperatures, thickness also reduces, but the oxide film is still characterized by a high degree of CoO-like local order.     

铜导线短路熔痕的XPS研究

利用氩离子溅射对熔痕样品进行了深度刻蚀,同时利用Cu的俄歇谱线和计算的俄歇参数值,对不同环境形成的铜导线短路痕迹的物相及元素分布规律进行了分析。根据刻蚀时间可将一次短路熔痕表面膜层分为三部分,即C含量迅速减少的近表面层;O含量变化不大,C含量逐渐消失且有Cu₂O相的中间层;无Cu₂O相,O含量显著减少的过渡层。而将二次短路熔痕表面膜层分为两部分：C含量迅速减少的近表面层;无Cu₂O相,C和O量逐渐减少层。由此可见,一次短路熔痕的表面膜层与基体分界明显,有显著的过渡层,而二次短路熔痕的表面膜层与基体分界不明显,无过渡层。综上所述,可以根据两种短路熔痕是否含有Cu₂O相以及定量分析结果来区分两种熔痕,为判断火灾原因提供新的技术依据。