A comparative study of single crystal magnesium oxide and oxidised magnesium by auger electron spectroscopy

In a study by AES of the surfaces of single crystal magnesium oxide and magnesium after various stages of oxidation, it has been shown that Auger energy shifts are produced by surface charging. Recognition of the charging effects has enabled the peak in the low energy spectrum of magnesium oxide crystal to be assigned. The low energy secondary electron spectra of both MgO crystal and oxidised magnesium are complicated by the presence of extra features which arise from diffraction of true secondary electrons, and in particular for oxidised magnesium a cross-transition occurring at the metal-oxide interface. Oxidation studies of sodium also reveal transitions arising from a similar process.     

The bonding state of carbon segregated to α-iron surfaces and on iron carbide surfaces studied by electron spectroscopy

Segregated carbon on the Fe(100) surface has been studied by means of X-rayand ultraviolet photoelectron (XPS, UPS), Auger electron (AES) and electron energy loss spectroscopy (ELS). For comparison, the surfaces of polycrystalline graphite and of iron carbides stabilized by chromium or manganese additions have been investigated. On the iron surface, carbon exists as a chemisorbed state or graphitic multilayer. The two states exhibit different energy positions in XPS, and are different in energy positions and lineshapes in AES and ELS. During the transition of graphitic carbon to chemisorbed carbon on Fe(100) a novel coverage-dependent Auger feature is reported. The spectra of graphitic carbon on the iron surface always coincide with those of solid graphite. The carbon Auger transitions of chemisorbed carbon and of iron carbides exhibit very similar lineshapes, but the energy positions of both states differ in AES as well as XPS.     

Quantitative Auger electron spectroscopy analysis with co-evaporated AuCu films

A method for the quantitative Auger electron spectroscopy (AES) analysis by using a co-evaporation technique is extended to the AuCu system following the previous work. The calibration curves for lower Auger energy have peaks at 60 eV for Cu and at 69 eV for Au, and for higher Auger energy peaks at 239 eV for Au and at 920 eV for Cu. It is found that a simple linear relation does not exist in the results for AES measurements and the bulk analysis by atomic absorption spectroscopy (AAS) because of the back-scattering effect and the overlap of the spectra at lower energies in the Au-Cu system. It is also found that the adsorption of oxygen caused by electron beam bombardment has a significant influence on the AES results. The calibration curves obtained after a correction for oxygen adsorption are successfully applied to the determination of the composition at the surface of a sputtered AuCu alloy.     

Structure and surface layers of Mg-C nanocomposites produced by ball milling

X-ray diffractometry (XRD), X-ray photoelectron spectrometry (XPS), Auger electron spectrometry (AES) and transmission electron microscopy (TEM) were used to investigate the structure and surface layers properties of nanocomposites produced by the mechanical activation (ball milling) of elemental magnesium with carbon materials (amorphous carbon and graphite). Amorphous carbon was synthesized by electric discharge treatment in kerosene. It was shown that ball milling, the allotropic form of carbon materials, and features of hydrogenation have a considerable effect on the structure, surface layer properties, and hydrogen adsorption of a formed composition. XPS and Auger spectroscopy revealed the surface layer of the composite particles to be enriched with carbon. In addition, there were oxide layers on their surfaces due to the particles’ interaction with the environment.     

Metallization of the Ge(111) surface at high-temperature probed by energy-loss and Auger spectroscopies

We present new electron energy-loss spectroscopy (EELS) and Auger (AES) experiments aimed to study the structural transition of the Ge(111) surface taking place at high temperatures. Our advanced high-temperature set-up allowed us to collect accurate EELS spectra near the M_2,3 excitation edges and AES MMV and MVV spectra, corresponding to different probing depths ranging from 4 to 10 Å. The metallization of the surface has been clearly detected by the shift of the M_2,3 edge and of the MMV, MVV Auger energies. A detailed study of the transition has been performed using a fine temperature step under thermal equilibrium conditions. The AES and EELS experiments show that a sudden semiconductor-metal transition takes place at about 1000 K involving mainly the topmost layers. Deeper layers within 10 Å are also involved in the metallization process (in a range of 10 above 1010 K) and a smooth change in the topmost layers is also observed at higher temperatures up to 1070 K. These transitions are not fully reversible upon cooling (down to 870 K). Structural and electronic characteristics of the surface transition are discussed in light of available models.     

Ion scattering spectroscopy studies of barium and oxygen on tungsten and tungsten-based dispenser cathodes

In order to use Ion Scattering Spectroscopy (ISS) for studies of tungsten dispenser cathodes, the relevant ISS sensitivities must be measured. Calibrations have been made using a polycrystalline tungsten ribbon with controlled coverages of oxygen, barium and combinations thereof. Auger Electron Spectroscopy (AES) was used to monitor these controlled surfaces and the escape depths of the tungsten Auger electrons in barium and oxygen have been measured. The absolute ISS sensitivities of all three elements were found to be strongly dependent on the barium coverage of the tungsten surface. This effect has been attributed to the lowering of the work function of the tungsten surface caused by the barium adsorption. However, the relative ISS sensitivities of the three elements are not affected in this way when both barium and oxygen (or oxygen alone) are present on the tungsten surface. ISS spectra of such surfaces have been analyzed quantitatively and found to be in reasonable agreement with AES measurements. The analysis has also been applied to ISS spectra of uncoated tungsten matrix dispenser cathodes in an active state and following exposure to oxygen. Compared to AES, these spectra indicate less oxygen on the active cathode surfaces as a result of the oxygen (associated with barium) not contributing to the oxygen ISS signal. Comparisons of the spectra from the active and oxygen poisoned cathodes suggest that oxygen adsorbed during the oxygen exposure sits on the topmost barium layer whereas the oxygen on the active cathode surface does not.     

Characterisation of nickel silicide thin films by spectroscopy and microscopy techniques

This article discusses the formation and detailed materials characterisation of nickel silicide thin films. Nickel silicide thin films have been formed by thermally reacting electron beam evaporated thin films of nickel with silicon. The nickel silicide thin films have been analysed using Auger electron spectroscopy (AES) depth profiles, secondary ion mass spectrometry (SIMS), and Rutherford backscattering spectroscopy (RBS). The AES depth profile shows a uniform NiSi film, with a composition of 49-50% nickel and 51-50% silicon. No oxygen contamination either on the surface or at the silicide-silicon interface was observed. The SIMS depth profile confirms the existence of a uniform film, with no traces of oxygen contamination. RBS results indicate a nickel silicide layer of 114 nm, with the simulated spectra in close agreement with the experimental data. Atomic force microscopy and transmission electron microscopy have been used to study the morphology of the nickel silicide thin films. The average grain size and average surface roughness of these films was found to be 30-50 and 0.67 nm, respectively. The film surface has also been studied using Kikuchi patterns obtained by electron backscatter detection.     

Auger and electron energy loss spectra of adsorbed species: α and β states of carbon monoxide and nitrogen on W(100)

Auger and electron energy loss spectra have been recorded for both α and β chemisorbed states of carbon monoxide and nitrogen on W(100). The α state spectra have been analysed with reference to results for the gas phase molecules, those for the β states have been analysed following a quasi-atomic final state model. The results illustrate both the potential and the limitations of AES and ELS in surface chemical analysis.     

Study of the chemical bonding of titanium with silicon and oxygen by AES and SEELS

Auger electron Spectroscopy (AES) and slow electron energy loss Spectroscopy (SEELS) have been employed to study the electronic structure of Ti, TiSi₂ and TiO₂. The changes in the Auger and loss spectra when Ti chemically binds with silicon to form TiSi₂ and with oxygen to form TiO₂ have been understood as manifestations of changes in electronic participation. AES spectra show distinct changes in line shapes of transitions involving the Ti valence electrons. The SEELS spectra provide information regarding shallow core levels, valence band and the collective excitation energies of the volume and surface plasmons. By monitoring the changes in the Auger peak at 387 eV and the 3p→ 3d quasiatomic transition (at about 45 eV), the role of d-orbital occupancies are studied in Ti and its compounds. The SEELS studies in the 0-80 eV range have enabled the authors to observe the behaviour of the 3p → 3d quasiatomic transition in Ti, which persists after oxidation but almost disappears during TiSi₂ formation. The values of the plasmon losses are related to the collective behaviour of conduction electrons.     

X-ray photoelectron and auger spectroscopy analysis of Ge:Mn-based magnetic semiconductor layers

Thin (～60 nm) germanium layers supersaturated with a manganese impurity of 10–16 at % have been studied by x-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES). The layers have been fabricated by pulsed laser deposition onto a semi-insulating single-crystal GaAs substrate. The results of XPS analysis of the Ge:Mn layers reveal a change in the line shape of germanium and manganese (2p) in the surface region compared to deeper layers, which indicates a transition from the oxidized form of the base material (Ge²⁺ and Ge¹⁺) and impurity (Mn²⁺) near the surface to the unoxidized state of germanium (Ge ⁰) and manganese (Mn⁰) in the interior of the layer. The XPS spectra of the valence electrons of the Ge:Mn structure indicate that the density of states in the valence band of the ferromagnetic Ge:Mn structures is caused not only by mechanical mixing of germanium and manganese. The composition of heterogeneous inclusions in Ge:Mn films has been studied using scanning Auger microscopy.     

The adsorption of Xe and CO on Ag(111)

The adsorption of Xe and CO on Ag(111) in the range 66 to 123 K and 10^?7 to 10^?1 Pa has been studied by surface potential, low energy electron diffraction (LEED), Auger electron spectroscopy (AES) and electron energy loss spectroscopic (EELS) measurements. Isotherms derived from both surface potential and AES measurements for submonolayer Xe adsorption reveal successive stages and a two-dimensional phase change. Isosteric heats were 18 ± 1 kJ mol^?1. Temkin isotherms were observed for CO, the heat falling linearly with coverage from an initial value of 27 ± 1.5 kj mol^?1. No ordered CO overlayer structure could be detected. EEL spectra of clean Ag(111) agree with previous studies. Additional loss peaks were recorded for Xe and CO overlayers, and the assignment of the substrate loss features is discussed in relation to the effects of adsorption.     

AES studies of palladium films formed on copper and mica

Thin epitaxial films of palladium were grown on epitaxial copper films and cleaved mica in ultra high vacuum. The growth modes of these films were investigated by Auger electron spectroscopy (AES), low energy electron diffraction (LEED), transmission electron microscopy (TEM), and TEM replica techniques. Layer by layer growth of Pd on Cu and mica was observed and inelastic mean free paths of Auger electrons for energies of 60 eV (Cu MMM) and 329 eV (Pd MNN) were calculated. These values were 5.7 and 6.9 Å respectively. The thermal stability of monocrystalline and polycrystalline Pd/Cu bilayer films at 483 K was also investigated by AES and TEM. It was found that Pd agglomerates on the Cu at this temperature to form a Stranski-Krastanov growth morphology. The agglomeration is much more rapid on polycrystalline films, suggesting that high surface diffusivity paths (grain boundaries and possibly other defects) enhance the surface diffusion of Pd on Cu.     

Low-energy electron diffraction and auger electron spectroscopy study of the oxidation of Ti {0001} at room temperature

The reaction of a clean Ti (0001) surface with oxygen gas at low pressure and room temperature has been studied with low-energy electron diffraction (LEED) and Auger electron spectroscopy (AES). At low exposures (about 1 Langmuir) ap(2×2) superstructure is observed which gradually converts to 1×1 at high exposures (about 100 Langmuirs). The LEED spectra confirm that the final 1×1 structure is different from that of clean Ti (0001), while the AES spectra indicate that the final oxide is probably TiO, not TiO₂. The plausibility of this indication is discussed.     

Growth of Ag thin films on ZnO(0 0 0 −1) investigated by AES and STM

The growth of Ag films on ZnO(0 0 0 −1) has been investigated by Auger electron spectroscopy (AES) and scanning tunneling microscopy (STM). A high density of islands is nucleated at the earliest stages of the growth. An upstepping mechanism causes these islands to coalesce while the uncovered fraction of the ZnO surface remains constant (30%).     

Yttrium ion implantation on the surface properties of magnesium

Owing to their excellent physical and mechanical properties, magnesium and its alloys are receiving more attention. However, their application has been limited to the high reactivity and the poor corrosion resistance. The aim of the study was to investigate the beneficial effects of ion-implanted yttrium using a MEVVA ion implanter on the surface properties of pure magnesium. Isothermal oxidation tests in pure O₂ at 673 and 773 K up to 90 min indicated that the oxidation resistance of magnesium had been significantly improved. Surface morphology of the oxide scale was analyzed using scanning electron microscope (SEM). Auger electron spectroscopy (AES) and X-ray diffraction (XRD) analyses indicated that the implanted layer was mainly composed of MgO and Y₂O₃, and the implanted layer with a duplex structure could decrease the inward diffusion of oxygen and reduce the outward diffusion of Mg²⁺, which led to improving the oxidation resistance of magnesium. Potentiodynamic polarization curves were used to evaluate the corrosion resistance of the implanted magnesium. The results show yttrium implantation could enhance the corrosion resistance of implanted magnesium compared with that of pure magnesium.     

Inelastic effects and structure in the auger electron emission spectra of V2O5(010) and V(100) surfaces: Study of chemical shifts

Characteristic ionization losses and plasma losses occurring in the AES spectra of V₂O₅ (010) and V(100) surfaces are discussed. The former are used to evaluate chemical shifts of the VL₂ and VL₃ levels in V₂O₅. Values of approximateley 2.5 eV are found. These are smaller than the values obtained with ESCA (± 5 eV). It is described how the electron beam used in AES is thought to be responsible for this effect. ESCA data from partly reduced V₂O₅ samples tend to confirm the proposed model, based on oxygen loss and decomposition of V₂O₅ single crystals under the influence of the electron beam.The plasma losses of the larger Auger peaks are discussed. It is shown how some fine structure in the spectra can be partly explained by their presence. The plasma losses were simulated with numerical techniques based on the use of a signal averager.Signal averaging, curve fitting and related numerical techniques improve the resolution of AES spectra. Spectra of V₂O₅(010) and V(100) obtained in this manner are discussed. With respect to the transitions involving the valence band it is shown that the complex valence band structure is one of the causes of the observed discrepancies between theoretical and experimental AES data. Furthermore there is an uncertainty concerning the way in which ionization correction should be applied in this case. This correction is thought to increase with the degree of localization of the valence electrons.Auger peak intensities in function of the primary energy were found to show a maximum at about 3.5 times the critical potential, as was expected from theory if a moderate amount of backscattering is taken into account. Finally the intensity variations of the Auger peaks under continuous electron bombardment show the rate of oxygen loss at a V₂O₅ surface due to the primary beam.     

Initial interaction of oxygen with aluminium single crystal faces: A LEED,AES and work function study

Auger electron spectroscopy (AES), low energy electron diffraction (LEED) and work function (Kelvin probe) measurements have been used to study the initial interaction of clean Al(111), (100) and (110) surfaces with oxygen at room temperature. The oxidation process was found to be surface orientation dependent, but a common feature has been always observed on the three low-index surfaces: they show two distinct phases, i.e. a chemisorbed phase followed then by an oxidized phase. From analysis of AES, LEED and Kelvin probe results, an adsorption mechanism of O on Al for each surface orientation is proposed.     

Electron irradiation effect on the surface composition of Ar+ ion bombarded Si-nitride and Si-oxinitride

Auger electron spectroscopy (AES) and electron energy loss spectroscopy (ELS) have been used to study the surface composition of the Si-nitride and Si-oxinitride prepared by low pressure chemical vapor deposition. Ion bombardment has been shown to result in appearance of the “free” silicon on the surface. Electron irradiation of the samples preliminary bombarded by Ar⁺ ions has led to disappearance of the “free” silicon. This process is assumed to be connected with electron stimulated desorption of the “free” silicon.     

Electron beam-adsorbate interactions on silicon surfaces

The interactions which occur between electron beams in the energy range 0.5–2.5 keV, with currents of 0.1–1.0 microA and various adsorbates (H₂, CO, CH₄ and C₂H₄) on silicon surfaces have been investigated. The accumulation of beam induced dissociation products on the surface has been monitored by Auger spectroscopy, and the extent of electron stimulated desorption of neutral molecules has been determined mass spectroscopically. Thermal desorption spectra for various gases have also been obtained in order to compare adsorption behaviour with and without the presence of an electron beam. It is concluded that serious experimental errors may occur when LEED and AES are used in adsorption studies, particularly where comparatively weak binding energies are involved.     

Oxygen exposure of Sm,Gd and Tb studied by Auger electron spectroscopy

The present paper treats the characteristics of the Auger transitions out of the valence band of the lanthanides Sm, Gd and Tb engaging in a chemical compound. These facts have been observed by AES on the basis of a slow oxidation process for these elements. The appearing Auger transitions have been identified as far as possible and compared with studies of density of states. The changes in the Auger spectra and the oxidation rate have been discussed.