Compositional and structural medium energy ion scattering study of the temperature mediated diffusion determination at the Co/V interface in Co/V/MgO(100)

The impact of annealing at 300 °C on the elemental composition and the atomic structure of the Co/V interface in the 2.5 Å Co/70 Å V/MgO (100) system has been investigated by medium energy ion scattering (MEIS) using 100 keV He⁺ ions. By combining the experimental MEIS results with simulations we show that, while the Co/V interface is abrupt for the system kept at room temperature, annealing at 300 °C induces a strong interdiffusion leading to a Co_0.5V_0.5 surface bcc alloy with a high degree of disorder. Additionally, the MEIS data suggest that the surface of the annealed system is slightly rumpled by ~ 0.2 Å.     

Nanostructures on GaAs surfaces due to 60 keV Ar+-ion beam sputtering

The effect of 60 keV Ar⁺-ion beam sputtering on the surface topography of p-type GaAs(1 0 0) was investigated by varying angle of incidence of the ion (0–60°) with respect to substrate normal and the ion fluence (2 × 10¹⁷–3 × 10¹⁸ ions/cm²) at an ion flux of 3.75 × 10¹³ ions/cm²-s. For normal incidence and at a fluence of 2 × 10¹⁷ ions/cm², holes and islands are observed with the former having an average size and density of 31 nm and 4.9 × 10⁹ holes/cm², respectively. For 30° and 45° off-normal incidence, in general, a smooth surface appears which is unaffected by increase of fluence. At 60° off-normal incidence dots are observed while for the highest fluence of 3 × 10¹⁸ ions/cm² early stage of ripple formation along with dots is observed with amplitude of 4 nm. The applicability and limitations of the existing theories of ion induced pattern formation to account for the observed surface topographies are discussed.     

Simulation and measurement of AES depth profiles; a case study of the C/Ta/C/Si system

A multilayer sample (C (23.3 nm)/Ta (26.5 nm)/C (22.7 nm)/Si substrate) was submitted to AES depth profiling by Ar⁺ ions of energy 1 keV and angles of incidence of 72°, 78°, and 82°. The shapes of the as-measured depth profiles were strongly different emphasizing that the ion-bombardment conditions strongly affects the shapes of measured depth profiles. We simulated the depth profile measured at an angle of incidence of 72° by calculating the backscattering factor, applying attenuation lengths available in the literature, and simulating the ion-bombardment-induced specimen alteration with a TRIDYN simulation and a trial and error method. The good agreement between the calculated and measured depth profiles justified the method applied.     

Measurement of the sputter yield after mild ion erosion of a pristine Cu(001) surface

Using the STM technique we have determined the sputter yield on a pristine Cu(001) surface after mild (fluence less than 0.044 ions per surface atom) bombardment of the pristine surface with 800 eV Ar⁺ions at normal incidence. The experiments have been performed at substrate temperatures ranging from 200 to 350 K. Making use of the positional correlation of adatoms and surface vacancies, at 200 K and 325 K, we concluded that about 1/3 of the surface adatoms originate from interstitials arriving at the surface and they give a direct indication of the buried bulk vacancies. A careful analysis of the different areas for surface vacancies and adatom then allowed a quantitative evaluation of the sputter yield at 1.2 Cu atoms per 800 eV Ar⁺ ion.     

Silver sulphide growth on Ag(111): A medium energy ion scattering study

The interaction of S₂ with Ag(111) under ultra-high vacuum conditions has been investigated by medium energy ion scattering (MEIS). 100 keV He⁺ MEIS measurements provide a direct confirmation of a previous report, based on thermal desorption, that the growth of multilayer films of Ag₂S occurs through a continuous corrosion process. These films show a commensurate (√7 × √7)R19° unit mesh in low energy electron diffraction, consistent with the epitaxial growth of (111) layers of the high-temperature F-cubic phase of Ag₂S. The substantial range of co-existing film thicknesses found indicates that the growth must be in the form of variable-thickness islands. The use of 100 keV H⁺ incident ions leads to a very rapid decrease in the sulphide film thickness with increasing exposure that we attribute to an unusual chemical leaching, with implanted H atoms interacting with S atoms and desorption of H₂S from the surface.     

Relation between surface structures and sputtering ratios of copper single crystals

Polished (100) Cu crystals have been bombarded at target temperatures of 204 K, 294 K and 456 K by 10 and 20 keV Ne⁺ ions up to a total dose of 1.7 × 10¹⁹ ions/cm². The plane of incidence was chosen to be a {100} plane perpendicular to the surface. Measurements have been performed for incident angles between 36° and 44° with respect to the surface normal. In this angular interval the sputtering ratio and the surface structure have been studied by weightloss and replica electron microscope techniques respectively. At target temperatures of 204 K and 294 K an anomaly was observed in the curve of the sputtering ratio versus angle of incidence. A small peak appears where the curve slopes towards the 〈110〉 minimum. The position and height of the peak is a function of target temperature and ion energy.

This sputtering submaximum is accompanied by the formation of {100} orientated furrows perpendicular to the ion beam. The nucleation of this relief is tentatively discussed in terms of local deviations from perfection of the surface, which might be due to a singularity in the production of focusing collisions influencing the damage structure. The growth of the furrows and the submaximum in the sputtering ratio are discussed in terms of the angle between the ion beam and the characteristic {110} side of the furrows.

These sputtering and faceting phenomena have not been observed at 20 keV Ar⁺ ion bombardment nor generally under bombardment at a target temperature of 456 K.     

Dependence of the AES backscattering correction factor on the experimental configuration

We present an analysis of the dependence of the backscattering correction factor (BCF) in Auger-electron spectroscopy (AES) on the analyzer acceptance angle. Illustrative BCF calculations are presented for Pd M₅N₄₅N₄₅ Auger electrons as a function of primary-electron energy for primary-electron angles of incidence, θ₀, of 0° and 80° and for various values of the analyzer acceptance angle. It was necessary to generalize the BCF definition for the case of an analyzer with an arbitrarily large acceptance angle; this was done with a new function, the integral emission depth distribution function. BCFs calculated from an advanced model of electron transport in the surface region of the Pd sample varied weakly with analyzer half-cone angle for θ₀ = 0° but more strongly for θ₀ = 80° where there were BCF differences varying between 19% at a primary energy of 1 keV and 6% at a primary energy of 5 keV. These BCF differences are due in part to variations of the BCF with emission angle and in part to variations of the density of inner-shell ionizations within the information depth for the detected Auger electrons. The latter variations are responsible for differences larger than 10% between BCFs from the widely used simplified BCF model and those from the more accurate advanced model for primary energies less than about 5 keV for θ₀ = 80°. For normal incidence of the primary beam, differences greater than 10% between BCFs from the simplified and advanced models were found for primary energies between 1 keV and 4 keV. These BCF differences indicate that the simplified model can provide only approximate BCF values. In addition, the simplified model does not provide any BCF dependence on Auger-electron emission angle or analyzer acceptance angle.     

ISS measurement of surface composition of AuCu alloys by simultaneous ion bombardments with Ar+ and He + ions

Surface composition of Au-Cu(43 at%) alloy under 1.5–5 keV argon ion bombardment has been investigated by ion scattering spectroscopy (ISS). In this experiment, we adopted a specific technique to use mixed He⁺ and Ar⁺ ions as primary beam in order to perform sputtering (Ar⁺) and ISS measurement (He⁺) simultaneously. The outermost atom layer of Au-Cu alloys under Ar⁺ ion bombardment is Au-rich leading to the conclusion that Ar⁺ ion bombardment of AuCu alloys causes the preferential sputtering of Cu atoms, resulting in a Au-rich outermost atom layer and a depletion layer of Au atoms beneath the outermost atom layer due to ion-beam-enhanced surface segregation. This result explains the experimental results obtained by AES as well.     

Structural characterization of Pb nanoislands in SiO2/Si interface synthesized by ion implantation through MEIS analysis

Medium energy ion scattering (MEIS) measurements and transmission electron microscopy (TEM) observations are applied to characterize a buried Pb nanoparticle (NP) system synthesized by ion implantation. The NPs are located at the SiO₂/Si film interface, forming a dense two-dimensional array. Full 2D (energy and angle) experimental MEIS spectra are compared with Monte Carlo simulated ones. The results demonstrate that MEIS measurements provide microstructural information (mean NP volume of about 150 nm³ and areal density of about 4 × 10¹¹ NP/cm²), but no accurate information on the NP geometrical shape.     

A comparison of radiation from sputtered atoms with radiation from projectiles scattered on oxidized magnesium at varying angle of incidence

The intensity of light emitted from sputtered atoms and neutralized, scattered primary ions, excited during 4 keV Ne⁺ and Ar⁺ bombardment of oxidized magnesium has been measured as a function of the incidence angle. It was found that the photon yield of sputtered atoms increases with the angle of incidence much more rapidly than the theoretical sputtering yield and the photon yield of scattered projectiles. In order to explain the experimental results a numerical approach was made based on the following assumptions: (1) the sputtered atom can be excited when it crosses the surface after getting the momentum from the collision cascade; (2) at oblique incidence the sputtered excited atom can be directly emitted after a gentle collision between the incident ion and the surface atom; (3) the neutralized primary ion can only be excited in a violent collision with the surface atom.     

Incident angle and temperature dependence of WSi wire-grid polarizer

The dependences of the incident angle and thermal durability of a tungsten silicide (WSi) wire-grid polarizer were examined. A WSi grating with a 0.5 fill factor, 260 nm depth, and 400 nm period was formed on a Si surface using two-beam interference and dry etching. The TM transmission spectrum of the fabricated element was greater than 60% at the incident angle of θ = 40° (the angle between the incident direction and the perpendicular axis to the grating direction) in the 4–10 μm wavelength range. An extinction ratio of 22.2 dB was achieved at 2.5 μm wavelength. Additionally, results show that this polarizer has higher thermal resistance than that of commercial infrared polarizers. Therefore, this polarizer is effective for taking a polarized thermal image of high temperatures.     

Highly sensitive hydrogen detection by medium energy Ne+ impact

Hydrogen atoms on solid surfaces were measured directly by elastic recoil detection analysis (ERDA) using medium energy (100–150 keV) Ne⁺ ions with an excellent sensitivity of (～ 1 × 10¹² H/cm²) without any absorber foils and time-of-flight techniques. An electrostatic toroidal analyzer acquired H⁺ ions with energy around 11 keV recoiled from Si(111)-1 × 1-H surfaces. The H⁺ fraction strongly depends upon emerging angle and takes a value more than 50% at the angle below 70° and a saturated value of 17% at the angle above 80° with respect to surface normal. We detected H atoms on the reduced TiO₂(110) exposed to water molecules at room temperature (2 L) and estimated the absolute amount of H to be ～ 2.0 × 10¹⁴ H/cm² corresponding to ～ 38% (～ 0.38 ML) of the bridging oxygen atoms.     

Interaction of HNCO with Au(111) surfaces

The surface chemistry of isocyanic acid, HNCO, and its dissociation product, NCO, was studied on clean, O-dosed and Ar ion bombarded Au(111) surfaces. The techniques used are high resolution energy loss spectroscopy (HREELS) and temperature-programmed desorption (TPD). The structure of Ar ion etched surface is explored by scanning tunneling microscopy (STM). HNCO adsorbs molecularly on Au(111) surface at 100 K yielding strong losses at 1390, 2270 and 3230 cm^? 1. The weakly adsorbed HNCO desorbs in two peaks characterized by T_p = 130 and 145 K. The dissociation of the chemisorbed HNCO occurs at 150 K to give NCO species characterized by a vibration at 2185 cm^? 1. The dissociation process is facilitated by the presence of preadsorbed O and by defect sites on Au(111) produced by Ar ion bombardment. In the latter case the loss feature of NCO appeared at 2130 cm^? 1. Isocyanate on Au(111) surface was found to be more stable than on the single crystal surfaces of Pt-group metals. Results are compared with those obtained on supported Au catalysts.     

Comparison of the higher diffraction order images in methyl-red-doped liquid crystal films

We investigate the change of higher diffraction order images in holographic image storage and reconstruction process. In experiments, an s-polarized Ar⁺ laser (488.0 nm) was used to record permanent grating in the dye-doped liquid crystal, 4,4′-n-entylcyanobiphenyl (5CB) doped with 1 wt% methyl-red (MR), at a small incident angle. Higher diffraction order images were observed when the signal beam was focused in front of and behind the film. Then the film was illuminated by an s-polarized He–Ne laser (632.8 nm) in the direction perpendicular to the surface. The higher diffraction order images were reconstructed. A theory about the change of higher diffraction order images is developed, which is in good agreement with experimental results. The results show that the higher diffraction order provides a useful method for optical information processing.     

Sputtering of highly oriented pyrolytic graphite with 30 keV Argon ions

The influence of the incidence angle of 30 keV Ar⁺ ions, ion fluence and target temperature on the sputtering yield and surface microgeometry of highly oriented pyrolytic graphite (UPV-1T) samples was experimentally studied. It was found that at fluences more than 5 × 10¹⁹ ion cm^?2 the sputtering yield at room temperature in the range of the ion incidence angle from 0° to 80° is twice as small as the corresponding experimental data for both polycrystalline graphite and glassy carbon. The analysis of ion-induced relief permits us to suppose the topographical suppression mechanism of highly oriented pyrolytic graphite sputtering.     

Modelling the directional and energy dependence of 5–10 keV Ar+ ion-induced secondary electron yields from Cu crystals

The primary ion directional effects observed in secondary electron yields induced by ion bombardment [5 keV Ar⁺ → Cu(100)] are simulated using a semi-empirical molecular dynamics model. The directional effects are presumed to arise from inelastic energy transfers that take place in close binary atomic encounters. The latter are estimated using the Oen-Robinson model, in combination with a critical apsidal distance (R_c). The connection between the measured kinetic electron emission (KEE) yields (γ_KEE) and the predicted inelastic energy loss in a binary atomic collision (ΔE_i) is established through a semi-empirical fitting procedure involving R_c and other parameters in the following model: γ_e = γ₀ + γ_KEE = γ₀ + 〈ΔE_i(z)exp(? z/λ)〉, where z is the collision depth. The directional effects are best reproduced by fitting the model to Ar–Cu inelastic collisions for two azimuthal incident directions: R_c is estimated to be 0.47 ± 0.03 Å; the parameter, λ (an effective electron attenuation length), is estimated to be 18 ± 2 Å. The same model also describes the γ_KEE energy dependence for 5–10 keV Ar⁺ normally incident on low-index Cu crystal targets [Phys. Rev. 129 (1963) 2409]. The spatial and temporal distributions of the hard collisions that initiate KEE are discussed on the basis of the model.     

Preferential sputtering of TIC under keV Ar+ ion bombardment: Simultaneous sputtering-ISS measurement with He+ and Ar+ ions

The composition change of the outermost atom layer of TiC(110) under ion bombardment with 1.5–3 keV He⁺ and He⁺ + Ar⁺ ions has been measured by ion scattering spectroscopy with He⁺ ions at different sample temperatures. It has been found that the preferential sputtering of C atoms takes place for both the He⁺ and Ar⁺ ion bombardment, however the preferred sputtering is more pronounced for Ar⁺ ions than for He⁺ ions. The ion bombardment with He⁺ ions at elevated sample temperatures hardly results in any change in surface composition below ～800°C, while Ar⁺ ion bombardment results in C enrichment for elevated temperatures as reported so far.     

Self-assembly of well-ordered and highly uniform nanoripples induced by focused ion beam

Well-ordered and highly uniform nanoripple structures on the surface of single crystal LaAlO₃ (1 0 0), SrTiO₃ (1 0 0) and Al₂O₃ (0 0 0 1) were formed via self-assembly (not by beam writing) by focused ion-beam bombardment. The morphology and topography of nanoripple structures were characterized using in-situ focused ion-beam/scanning electron microscope, as well as ex-situ atomic force microscopy. Under off-normal bombardment without sample rotation, the characteristic wavelength of nanoripples varying from 248 to 395 nm on the LaAlO₃ (1 0 0) surface can be obtained by changing ion fluence and incident angle. When all sputtering parameters except the ion fluence are constant, the wavelength of nanoripples is increased with the enhanced ion fluence. These results demonstrate the potential application of using ion sputtering method for fabricating the well-ordered and highly uniform nanoripples which can be used in nanodevices.     

Metal–insulator transition induced by non-stoichiometry of surface layer and molecular reactions on single crystal KTaO3

In the study we present results on topography, morphology, chemical composition, electronic structure and electrical properties of the (100) surface layer of KTaO₃ single crystal caused by sputtering with Ar⁺ ion beam with energy of 1 keV. Several surface sensitive techniques, i.e. X-ray photoelectron spectroscopy (XPS), local conductivity of atomic force microscopy (LC-AFM), and Kelvin Probe Force Microscopy (KPFM) were used. The observed changes in the electronic structure were explained as a result of the chemical decomposition of the surface layer. A correlation between the electronic states which appeared in the energy gap and the changes in charge state of Ta ions was found. The activation energy related to averaged local conductivity temperature dependence was estimated from Arrhenius plot. It was also found, that variations in the local contact potential difference (LCPD) indicated changes in the chemical composition in nano-scale. The chemical reconstruction of the KTaO₃ surface modified by Ar⁺ ion beam was deduced. This non-homogeneity corresponded to 2-D non-homogeneity of the local electric conduction (LC-AFM), which occurred within nano-areas after sputtering. Chemical reactivity of the modified surface with CO₂ and O₂ was observed. The reversibility of the Ar⁺ induced loss of oxygen non-stoichiometry was observed after the sample was exposed to various doses of O₂. The successful reversibility occurred after oxidation process at high temperature, i.e. 300 °C.     

3C-SiC(001)-3 × 2 reconstructed surface analyzed by high-resolution medium energy ion scattering

The atomic structure of the 3C-SiC(001)-3 × 2 reconstructed surface was analyzed precisely by high-resolution medium energy ion scattering (MEIS). The present MEIS analysis unambiguously shows that the (3 × 2) surface consists of Si adatoms (1/3 ML, 1 ML = 1.05 × 10¹⁵ atoms/cm²) on top and underlying Si adlayer (2/3 ML) on the bulk truncated Si plane. As the result, the most probable structure is focused on the Two Adlayer Asymmetric Dimer Model predicted by ab initio calculations and the modified versions with alternating long and short dimers in the 2nd adlayer proposed by photoelectron diffraction (PED) and by grazing incidence X-ray diffraction (GIXRD) analyses. Observed MEIS spectra are well reproduced by the structure relatively close to that determined by PED rather than GIXRD. Interestingly, the first principle calculations using VASP (Vienna ab initio simulation package) prefer symmetric dimers in the second Si adlayer and non-relaxed interplanar distance between the top Si and 2nd C plane of the bulk-truncated surface, which are, however, unable to reproduce the observed MEIS spectra. The distorted 2nd adlayer (asymmetric dimers) may correlate with the compressed interplanar distance between the underlying Si and C planes.