Sputter damage in Si surface by low energy Ar+ ion bombardment

The damage distributions in Si(1 0 0) surface after 1.0 and 0.5 keV Ar⁺ ion bombardment were studied using MEIS and Molecular dynamic (MD) simulation. The primary Ar⁺ ion beam direction was varied from surface normal to glancing angle. The MEIS results show that the damage thickness in 1.0 keV Ar ion bombardment is reduced from about 7.7 nm at surface normal incidence to 1.3 nm at the incident angle of 80°. However, the damage thickness in 0.5 keV Ar ion bombardment is reduced from 5.1 nm at surface normal incidence to 0.5 nm at the incident angle of 80°. The maximum atomic concentration of implanted Ar atoms after 1 keV ion bombardment is about 10.5 at% at the depth of 2.5 nm at surface normal incidence and about 2.0 at% at the depth of 1.2 nm at the incident angle of 80°. However, after 0.5 keV ion bombardments, it is 8.0 at% at the depth of 2.0 nm for surface normal incidence and the in-depth Ar distribution cannot be observable at the incident angle of 80°. MD simulation reproduced the damage distribution quantitatively.     

Neutral beam sputtering of positive ion clusters from alkali halides

Neutral argon atom beams of 15 keV energy have been used to sputter alkali halides and the ejected positive ions have been analysed in energy, mass and angular distribution.

The use of a neutral beam, rather than an ion beam, minimizes surface charge and the deflection of ejected ions by electrostatic interaction with a charged incident beam.

A cluster component of the form K₂Cl⁺, K₃Cl⁺ ₂ and higher members of the series is found for all alkali halides studied.     

C60 sputtering of organics: A study using TOF-SIMS, XPS and nanoindentation

Sputtering of organic materials using a C₆₀ primary ion beam has been demonstrated to produce significantly less accumulated damage compared to sputtering with monatomic and atomic-cluster ion beams. However, much about the dynamics of C₆₀ sputtering remains to be understood. We introduce data regarding the dynamics of C₆₀ sputtering by evaluating TOF-SIMS depth profiles of bulk poly(methyl methacrylate) (PMMA). Bulk PMMA provides an ideal test matrix with which to probe C₆₀ sputter dynamics because there is a region of steady-state secondary ion yield followed by irreversible signal degradation. C₆₀ sputtering of PMMA is evaluated as a function of incident ion kinetic energy using 10 keV C₆₀⁺, 20 keV C₆₀⁺ and 40 keV C₆₀⁺⁺ primary ions. Changes in PMMA chemistry, carbon accumulation and graphitization, and topography as a function of total C₆₀ ion dose at each accelerating potential is addressed.     

First μ+SR studies on thin films with a new beam of low energy positive muons at energies below 20 keV

At the Paul Scherrer Institute slow positive muons (μ⁺) with nearly 100% polarization and an energy of about 10 eV are generated by moderation of an intense secondary beam of surface muons in an appropriate condensed gas layer. These epithermal muons are used as a source of a tertiary beam of tunable energy between 10 eV and 20 keV. The range of these muons in solids is up to 100 nm which allows the extension of the μ⁺SR techniques (muon spin rotation, relaxation, resonance) to the study of thin films. A basic requirement for the proper interpretation of μ⁺SR results on thin films and multi-layers is the knowledge of the depth distribution of muons in matter. To date, no data are available concerning this topic. Therefore, we investigated the penetration depth of μ⁺ with energies between 8 keV and 16 keV in Cu/SiO₂ samples. The experimental data are in agreement with simulated predictions. Additionally, we present two examples of first applications of low energy μ⁺ in μ⁺SR investigations. We measured the magnetic field distribution inside a 500-nm thin High-T_C superconductor (YBa₂Cu₃O_7-δ), as well as the depth dependence of the field distribution near the surface. In another experiment a 500-nm thin sample of Fe-nanoclusters (diameter 2.4(4) nm), embedded in an Ag matrix with a volume concentration of 0.1%, was investigated with transverse field μ⁺SR. This revised version was published online in August 2006 with corrections to the Cover Date.     

AES analysis of nitridation of Si(100) by 2–10 keV N+2 ion beams

Ion beam nitridation of Si(100) as a function of N⁺₂ ion energy in the range of 2–10 keV has been investigated by in-situ Auger electron spectroscopy (AES) analysis and Ar⁺ depth profiling. The AES measurements show that the nitride films formed by 4–10 keV N⁺₂ ion bombardment are relatively uniform and have a composition of near stoichiometric silicon nitride (Si₃N₄), but that formed by 2 keV N⁺₂ ion bombardment is N-rich on the film surface. Formation of the surface N-rich film by 2 keV N⁺₂ ion bombardment can be attributed to radiation-enhanced diffusion of interstitial N atoms and a lower self-sputtering yield. AES depth profile measurements indicate that the thicknesses of nitride films appear to increase with ion energy in the range from 2 to 10 keV and the rate of increase of film thickness is most rapid in the 4–10 keV range. The nitridation reaction process which differs from that of low-energy (< 1 keV) N⁺₂ ion bombardment is explained in terms of ion implantation, physical sputtering, chemical reaction and radiation-enhanced diffusion of interstitial N atoms.     

Changes in gold concentration at the surface of a AuCu alloy sputtered at low temperature

A series of depth profiles in Au_0.56Cu_0.44 produced by bombarding at ? 120°C with an argon ion beam of 2 keV energy and current densities of 4, 6, 12 and 24 μA/cm², respectively, are presented. Gold is enriched in the top layer but the concentration rapidly decreases to a minimum at an average depth of about 2 Å, then increases slowly and saturates at about 30 Å. The change in the composition at this point is called a dip. The magnitude of the dip depends on the ion current density, but the depth is nearly independent of it. Segregation and diffusion effects in establishing the surface composition are stressed.     

Depth profiling using C60 SIMS—Deposition and topography development during bombardment of silicon

A C₆₀⁺ primary ion source has been coupled to an ion microscope secondary ion mass spectrometry (SIMS) instrument to examine sputtering of silicon with an emphasis on possible application of C₆₀⁺ depth profiling for high depth resolution SIMS analysis of silicon semiconductor materials. Unexpectedly, C₆₀⁺ SIMS depth profiling of silicon was found to be complicated by the deposition of an amorphous carbon layer which buries the silicon substrate. Sputtering of the silicon was observed only at the highest accessible beam energies (14.5 keV impact) or by using oxygen backfilling. C₆₀⁺ SIMS depth profiling of As delta-doped test samples at 14.5 keV demonstrated a substantial (factor of 5) degradation in depth resolution compared to Cs⁺ SIMS depth profiling. This degradation is thought to result from the formation of an unusual platelet-like grain structure on the SIMS crater bottoms. Other unusual topographical features were also observed on silicon substrates after high primary ion dose C₆₀⁺ bombardment.     

Study of the angular and energy distributions of Na+ and K+ ions which have passed through thin copper films

The angular and energy distributions of alkaline Na⁺ and K⁺ ions which have passed through thin Cu films in different crystal states are studied. The ion energy E₀ is varied from 10 to 40 keV, and the incidence angle. ranges from 0° to 60°. The angular aperture of the detector is ～0.5°, which allows the form of the angular distribution of ions which have passed through the solid thin films as a function of the energy, the angle of primary-ion beam incidence, and the layer thickness to be studied in detail. It is shown that, in the range E₀ = 10.40 keV, the energy loss ΔE of those ions that have passed increases linearly as the energy of incident ions increases. The energy loss increases with increasing ion mass in the case of singly charged ions. The surface amorphization of single- and polycrystalline films leads to an increase (by 150–200 eV) in the energy loss caused by the diffuse propagation of ions and to loss-peak broadening. It is probable that surface amorphization is accompanied by an increase in the number of atoms experiencing multiple collisions with atoms of the film, which leads to an increase in the average energy loss by ions that have passed through films.     

Effet elastique en volume dans le nickel irradie aux electrons a tres basse temperature

Abstract

Experiments designed to determine the damage distribution produced by energetic heavy ions in Si are described. For low ion doses (10¹¹ to 10¹³ cm^?2), the location of the damage peak was determined by changes, which were produced by ion damage, in the electrical properties of thin (0.6 μ), uniformly doped Si layers as a function of depth. The ratio of the peak position in the damage distribution to the peak position in the ion distribution was determined to be approximately 0.6 ± 0.1 for Si²⁹ (150 keV), P³¹ (70, 140, 200 keV), B¹¹ (60 keV), and As⁷⁵ (280 keV). A comparison of carrier removal rates and the number of displaced lattice atoms previously reported from back-scattering experiments with He ions indicates that the nature of damage produced by Si²⁹ and B¹¹ are different. In the former case, cluster damage (amorphous disordered regions) appears to be an important form of radiation damage, while in the latter case, isolated defects are the dominant form of radiation damage for room temperature implantations. Isochronal annealing studies of Si²⁹ and B¹¹ ion damage provide further support for the different nature of radiation defects produced by these species. For high doses (10¹⁴ to 10¹⁶ cm^?2), the growth of a continuous amorphous Si layer was studied with ESR, optical transmission, and visual observation and stripping studies. The ratio of the location of the damage peak to that of the peak ion concentration was determined to be approximately 0.7 for P³¹ (140, 280 keV) and 0.8 for As⁷⁵ (280 keV). From the ESR studies, the number of displaced atoms in amorphous clusters was estimated to be 2800 per 280 keV P³¹ ion.     

Determination of the complex refractive index profiles in P+31 ion implanted silicon by ellipsometry

Ellipsometry was used to determine the complex refractive index profiles in silicon implanted with P⁺₃₁ ions with energies of 35, 52,5 and 70 keV. The profiles were determined both by anodization-stripping of the implanted layer and by numerical fitting of multiple-angle-of-incidence ellipsometer data taken on the as-implanted surface, assuming that the implantation would exhibit a Gaussian distribution. Good correlation was obtained between the two types of profiles, indicating that the non-destructive measurements on the as-implanted surface may be useful in process control. Good agreement with published results was also obtained on the increase in depth with energy of both the damage and the implanted species.     

Physicomechanical properties of the surface of a zirconium alloy modified by a pulsed ion beam

The physicomechanical properties of the surface of the Zr-1% Nb zirconium alloy modified by a pulsed carbon ion beam with a pulse duration of 80 ns, an energy of 200 keV, and a current density of 120 A/cm² are studied at four regimes having different numbers of pulses. Irradiation by a carbon ion beam results in hardening of the surface layer to a depth of 2 μm, grain refinement to 0.15–0.8 μm, zirconium carbide formation, and a decrease in the hydrogen permeability of the zirconium alloy.     

Depth profiles of metal ions implanted in dielectrics at low energies

The depth profiles of Cu⁺, Ag⁺, and Au⁺ ions implanted into amorphous dielectric SiO₂, Al₂O₃, and soda-lime silicate glass (SLSG) are simulated by the DYNA program. The algorithm follows projectile-ion-substrate-atom pair collisions giving rise to a dynamic variation in the phase composition in the surface layer of the irradiated material and takes into account surface sputtering. Ion implantation up to doses of ≤10¹⁶ ion/cm² at low ion energies of 30, 60, and 100 keV is considered. The measured dynamic variation of the depth profiles of implanted ions as a function of the dose is compared with the standard statistical distribution calculated by the TRIM algorithm.     

Structural effects of C60 bombardment on various natural mineral samples—Application to analysis of organic phases in geological samples

Organic phases trapped inside natural mineral samples are of considerable interest in astrobiology, geochemistry and geobiology. Examples of such organic phases are microfossils, kerogen and oil. Information about these phases is usually retrieved through bulk crushing of the rock which means both a risk of contamination and that the composition and spatial distribution of the organics to its host mineral is lost. An attractive of way to retrieve information about the organics in the rock is depth profiling using a focused ion beam. Recently, it was shown that it is possible to obtain detailed mass spectrometric information from oil-bearing fluid inclusions, i.e. small amounts of oil trapped inside a mineral matrix, using ToF-SIMS. Using a 10 keV C₆₀⁺ sputter beam and a 25 keV Bi₃⁺ analysis beam, oil-bearing inclusions in different minerals were opened and analysed individually. However, sputtering with a C₆₀⁺ beam also induced other changes to the mineral surface, such as formation of topographic features and carbon deposition. In this paper, the cause of these changes is explored and the consequences of the sputter-induced features on the analysis of organic phases in natural mineral samples (quartz, calcite and fluorite) in general and fluid inclusions in particular are discussed.The dominating topographical features that were observed when a several micrometers deep crater is sputtered with 10 keV C₆₀⁺ ions on a natural mineral surface are conical-shaped and ridge-like structures that may rise several micrometers, pointing in the direction of the incident C₆₀⁺ ion beam, on an otherwise flat crater bottom. The sputter-induced structures were found to appear at places with different chemistry than the host mineral, including other minerals phases and fluid inclusions, while structural defects in the host material, such as polishing marks or scratches, did not necessarily result in sputter-induced structures. The ridge-like structures were often covered by a thick layer of deposited carbon.Despite the appearance of the sputter-induced structures and carbon deposition, most oil-bearing inclusions could successfully be opened and analysed. However, smaller inclusion (<15 μm) could potentially become entirely covered by sputter-resistant structures and therefore difficult to open. Therefore, it might become necessary, to for example increase the ion energy and rotate the stage to successfully open smaller inclusions for analysis.SIMS, C₆₀, carbon deposition, topography, mineral, fluid inclusions, geological samples, depth profiling.     

Umwandlung von Beryllium in Be2C und BeO durch Elektronenbestrahlung in Anwesenheit von Kohlenwasserstoff-Polymerisaten

The secondary electron yield from beryllium surfaces in presence of residual hydrocarbon vapour at a vacuum of 10^?4 tor decreases with time fromδ=0.45 to 0.25 when the incident primary electrons hit the target with an energy of 28 keV and an incident angle of 60°. Since the yield from the hydrocarbon polymer contamination layer is 0.3, it is concluded that the beryllium surface reacts with the contamination layer. This is confirmed by electron diffraction and electron microscopic observation of thin beryllium layers on different supporting foils, i.e. C-, Al₂O₃, polymeride from gas discharges, and self supporting Be. When a beryllium foil about 500 A. U. in thickness is first irradiated with low intensity (total beam current in the Siemens Elmiskop II<5 μA), a polymeride layer is formed. After increasing the beam current to 30 μA, the micrographs as well as the Debye-Scherrer diagrams show the formation of Be₂C and BeO. It is supposed that the carbon originates from the polymeride layer, and that the oxygen is supplied by the residual gas.     

Interaction of high-power laser pulses with glasses containing implanted metallic nanoparticles

Sodium calcium silicate glasses with Ag⁺ implanted ions are studied. The ion implantation conditions are as follows: the energy is 60 keV, the dose is 7×10¹⁶ cm⁻², and the ion current density is 10 μA/cm². Ion implantation provides the formation of a composite layer that incorporates silver nanoparticles in the surface region of glass. The size distribution of nanoparticles over the depth in the composite layer is strongly nonuniform. The effect of a high-power pulsed excimer laser on the composite layer is investigated. It is found that, under laser irradiation, the size of silver nanoparticles in the implanted layer decreases but the size distribution of nanoparticles over the depth remains nonuniform, even though it becomes slightly narrower compared to that observed prior to irradiation. The experimental results are interpreted in terms of the effects of the melting of glass and metallic particles on a nanosecond scale. __________ Translated from Fizika Tverdogo Tela, Vol. 43, No. 11, 2001, pp. 2100–2106. Original Russian Text Copyright ? 2001 by Stepanov, Popok, Hole, Bukharaev.     

Depth profiling of taxol-loaded poly(styrene-b-isobutylene-b-styrene) using Ga and C60 ion beams

The surface of a triblock copolymer, containing a solid-phase drug, was investigated using 15 keV Ga⁺ and 20 keV C₆₀⁺ ion beams. Overall, the results illustrate the successful use of a cluster ion beam for greatly enhancing the molecular ion and high-mass fragment ion intensities from the surface and bulk of the polymer system. The use of C₆₀⁺ also established the ability to see through common overlayers like poly(dimethyl siloxane) which was not possible using atomic ion sources. Moreover, the use of C₆₀⁺ allowed depth profiles to be obtained using primary ion dose densities in excess of 6 × 10¹⁴ C₆₀⁺/cm². Resulting sputter craters possess relatively flat bottoms without the need for sample rotation and reached depths of ca. 2 μm. AFM results illustrate the more gentile removal of surface species using cluster ions. Specifically, phase contrast and topographic images suggest the relatively high ion doses do not significantly alter the phase distribution or surface topography of the polymer. However, a slight increase in rms roughness was noticed.     

Sputtering yields of PMMA films bombarded by keV C60 ions

A quartz crystal microbalance (QCM) has been used to determine total-mass sputtering yields of PMMA films by 1-16 keV C₆₀^+,2+ ion beams. Quantitative sputtering yields for PMMA are presented as mass loss per incident ion Y_m. Mass-lost rate QCM data show that a 13 keV C₆₀ cluster leads to emission equivalent to 800 PMMA molecules per ion. The power law obtained for the increase in sputtering yield with primary ion energy is in good agreement those predicted by “thermal spike” regime and MD models, when crater sizes are used to estimate sputtering.     

An XPS study on ion beam induced oxidation of titanium silicide

Titanium silicides (TiSi₂) films grown on Si(1 0 0) substrate were investigated by ex situ XPS depth profiling after athermal ion beam induced oxidation (IBO) at 12 keV O₂⁺ incident energy and normal incidence. The composition and stoichiometry of these films were quantitatively determined as chemical state relative concentrations versus sputter time. “In depth” silicon and titanium oxidation states have been obtained after spectra deconvolution, showing a mixture of silicon dioxide, titanium dioxide, titanium suboxides, elemental titanium and residual traces of titanium nitride. Thermochemical data based on the corresponding enthalpies of formation of the oxides cannot explain our experimental results as in the case of low energy IBO, an oxygen defective altered layer is formed, presenting features of a reduced TiO_x phase.     

Formation of silicon carbide and diamond nanoparticles in the surface layer of a silicon target during short-pulse carbon ion implantation

Synthesis of silicon carbide and diamond nanoparticles is studied during short-pulse implantation of carbon ions and protons into a silicon target. The experiments are carried out using a TEMP source of pulsed powerful ion beams based on a magnetically insulated diode with radial magnetic field B _r . The beam parameters are as follows: the ion energy is 300 keV, the pulse duration is 80 ns, the beam consists of carbon ions and protons, and the ion current density is 30 A/cm². Single-crystal silicon wafers serve as a target. SiC nanoparticles and nanodiamonds form in the surface layer of silicon subjected to more than 100 pulses. The average coherent domain sizes in the SiC particles and nanodiamonds are 12–16 and 8–9 nm, respectively.     

The effect of incident angle on the C60 bombardment of molecular solids

The effect of incident angle on the quality of SIMS molecular depth profiling using C₆₀⁺ was investigated. Cholesterol films of ∼300 nm thickness on Si were employed as a model and were eroded using 40 keV C₆₀⁺ at an incident angle of 40° and 73° with respect to the surface normal. The erosion process was characterized by determining at each angle the relative amount of chemical damage, the total sputtering yield of cholesterol molecules, and the interface width between the film and the Si substrate. The results show that there is less molecule damage at an angle of incidence of 73° and that the total sputtering yield is largest at an angle of incidence of 40°. The measurements suggest reduced damage is not necessarily dependent upon enhanced yields and that depositing the incident energy nearer the surface by using glancing angles is most important. The interface width parameter supports this idea by indicating that at the 73° incident angle, C₆₀⁺ produces a smaller altered layer depth. Overall, the results show that 73° incidence is the better angle for molecular depth profiling using 40 keV C₆₀⁺.