Surface morphology of the Ar ion-irradiated Ag/Si(1 1 1) system

In the present study, a 500 Å thin Ag film was deposited by thermal evaporation on 5% HF etched Si(1 1 1) substrate at a chamber pressure of 8×10⁻⁶ mbar. The films were irradiated with 100 keV Ar⁺ ions at room temperature (RT) and at elevated temperatures to a fluence of 1×10¹⁶ cm⁻² at a flux of 5.55×10¹² ions/cm²/s. Surface morphology of the Ar ion-irradiated Ag/Si(1 1 1) system was investigated using scanning electron microscopy (SEM). A percolation network pattern was observed when the film was irradiated at 200°C and 400°C. The fractal dimension of the percolated pattern was higher in the sample irradiated at 400°C compared to the one irradiated at 200°C. The percolation network is still observed in the film thermally annealed at 600°C with and without prior ion irradiation. The fractal dimension of the percolated pattern in the sample annealed at 600°C was lower than in the sample post-annealed (irradiated and then annealed) at 600°C. All these observations are explained in terms of self-diffusion of Ag atoms on the Si(1 1 1) substrate, inter-diffusion of Ag and Si and phase formations in Ag and Si due to Ar ion irradiation.     

Ion beam enhanced etching of LiNbO3

Single crystals of z- and x-cut LiNbO₃ were irradiated at room temperature and 15 K using He⁺- and Ar⁺-ions with energies of 40 and 350 keV and ion fluences between 5 × 10¹² and 5 × 10¹⁶ cm⁻². The damage formation investigated with Rutherford backscattering spectrometry (RBS) channeling analysis depends on the irradiation temperature as well as the ion species. For instance, He⁺-irradiation of z-cut material at 300 K provokes complete amorphization at 2.0 dpa (displacements per target atom). In contrast, 0.4 dpa is sufficient to amorphize the LiNbO₃ in the case of Ar⁺-irradiation. Irradiation at 15 K reduces the number of displacements per atom necessary for amorphization. To study the etching behavior, 400 nm thick amorphous layers were generated via multiple irradiation with He⁺- and Ar⁺-ions of different energies and fluences. Etching was performed in a 3.6% hydrofluoric (HF) solution at 40 °C. Although the etching rate of the perfect crystal is negligible, that of the amorphized regions amounts to 80 nm min⁻¹. The influence of the ion species, the fluence, the irradiation temperature and subsequent thermal treatment on damage and etching of LiNbO₃ are discussed.     

Defect and void evolution in oxide dispersion strengthened ferritic steels under 3.2 MeV Fe ion irradiation with simultaneous helium injection

In an attempt to explore the potential of oxide dispersion strengthened (ODS) ferritic steels for fission and fusion structural materials applications, a set of ODS steels with varying oxide particle dispersion were irradiated at 650°C, using 3.2 MeV Fe⁺ and 330 keV He⁺ ions simultaneously. The void formation mechanisms in these ODS steels were studied by juxtaposing the response of a 9Cr–2WVTa ferritic/martensitic steel and solution annealed AISI 316LN austenitic stainless steel under the same irradiation conditions. The results showed that void formation was suppressed progressively by introducing and retaining a higher dislocation density and finer precipitate particles. Theoretical analyses suggest that the delayed onset of void formation in ODS steels stems from the enhanced point defect recombination in the high density dislocation microstructure, lower dislocation bias due to oxide particle pinning, and a very fine dispersion of helium bubbles caused by trapping helium atoms at the particle–matrix interfaces.     

The annealing of damage in U3Si: Electrical resistivity studies

The annealing of damage in quenched and in irradiated samples of U₃Si was studied by measuring changes in electrical resistivity at 4.2°K. No significant changes in resistivity were introduced by quenching from temperatures just below and from above the allotropie transformation from tetragonal to cubic at 760°C. Large increases in electrical resistivity were caused by irradiation below 100°C to produce either the disordered cubic or amorphous structures. While all the damage annealed by 600°C, there were distinct differences in annealing behaviour of cubic and amorphous samples. The kinetics of each annealing stage has been identified and discussed making reference to the results of similar studies based on electron microscopy, density and X-ray diffraction techniques.     

Formation of cavities in GaAs and InGaAs

The ion implantation of He is examined as a means to form thermally stable cavities in GaAs. Room-temperature implantation of 2–10 × 10¹⁶ He/cm² at 40 or 50 keV forms bubbles, but subsequent annealing at 250°C or above leads to exfoliation of the implanted surface layer. The exfoliation appears related to the agglomeration of bubbles on dislocations at the back of the layer; evidence suggests these may be misfit dislocations formed to relieve compressive stress in the implanted layer. Implantation of He at 150°C produces similar results, whereas the He diffuses out of GaAs without forming cavities during implantation at 300°C. However, implantations of immobile Ar followed by He at 400°C produce extended defects with bubbles in the implanted layer; the He can be degassed by subsequent annealing at 400°C to produce 1.5–3.5 nm cavities that are stable at this temperature. The same treatment applied to an In_0.10Ga_0.90As/GaAs heterostructure produces larger cavities preferentially located on dislocations at the interface, with only slight reduction in strain of the epitaxial layer. The microstructures of both GaAs and the heterostructure clearly demonstrate an attractive interaction between bubbles or cavities and dislocations.     

Ion beam induced amorphization and recrystallization of Si/SiC/Si layer systems

Epitaxial, buried silicon carbide (SiC) layers have been fabricated in (100) and (111) silicon by ion beam synthesis (IBS). In order to study the ion beam induced epitaxial crystallization (IBIEC) of buried SiC layers, the resulting Si/SiC/Si layer systems were amorphized using 2 MeV Si²⁺ ion irradiation at 300 K. An unexpected high critical dose for the amorphization of the buried layers is observed. Buried, amorphous SiC layers were irradiated with 800 keV Si⁺ ions at 320 and 600°C, respectively, in order to achieve ion beam induced epitaxial crystallisation. It is demonstrated that IBIEC works well on buried layers and results in epitaxial recrystallization at considerably lower target temperatures than necessary for thermal annealing. The IBIEC process starts from both SiC/Si interfaces and may be accompanied by heterogenous nucleation of poly-SiC as well as interfacial layer-by-layer amorphization, depending on irradiation conditions. The structure of the recrystallized regions in dependence of dose, dose rate, temperature and crystal orientation is presented by means of TEM investigations.     

Bubbles in SiC crystals formed by helium ion irradiation at high temperatures

Helium bubbles were found to be formed in SiC crystals by irradiation with He⁺ ions at 1000 to 1200° C. The size of bubbles increased with increasing irradiation temperatures.

The density of helium atoms in the bubbles was measured to be about 10²⁸ atoms/m³ by EELS measurement in combination with electron microscopic observation in the same selected areas, and the internal pressure of the bubbles was estimated therefrom to be on the order of 10⁸ Pa at room temperature.     

Analysis of annealing and ion implantation effects in Ti/TiN contacts on silicon

The effects of thermal annealing and 350 keV As⁺ ion implantation on interdiffusion processes in a c-Si/Ti/TiN system were analysed. The Ti/TiN contacts were deposited by sputtering (Ti, 100 nm) and by reactive sputtering (TiN, 50 nm) on (111) n-Si wafers. Characterization included RBS, SEM and XRD analysis and electrical measurements. During vacuum annealing, interdiffusion is observed at the Si/Ti interface, where intermixing and growth of silicides takes place at 600° C and at higher temperatures. Annealing in a nitrogen atmosphere induces changes in surface morphology and stoichiometry of TiN, which does not affect the reaction at Si/Ti. Implantation of As⁺ to doses above 3.9 × 10¹⁴ ions/cm² enhances intermixing at the Si/Ti interface during post-implantation annealing, while the TiN overlayer is unaffected in structure and morphology.     

Influence of SHI irradiation on the formation of buried SiC

Silicon carbide (SiC) precipitates buried in Si(1 0 0) substrates were synthesized by ion implantation of 50 keV and 150 keV C⁺ ions at different fluences. Two sets of samples were subsequently annealed at 850 °C and 1000 °C for 30 min. Fourier transform infrared (FTIR) spectroscopy studies and X-ray diffraction (XRD) analysis confirmed formation of β-SiC precipitates in the samples. Ion irradiation with 100 MeV Ag⁷⁺ ions at room temperature does not induce significant change in the precipitates. It could be interpreted from the FTIR observations that ion irradiation may induce nucleation in Si + C solution created by ion implantation of C in Si. Modifications induced by swift heavy ion irradiation are found to be dependent on implantation energy of C⁺ ions.     

Ion beam induced nucleation in amorphous GaAs layers during MeV implantation

To investigate the nonlinear dose dependence of the thickness of the recrystallized layer during ion beam induced epitaxial recrystallization at amorphous/crystalline interfaces GaAs samples were irradiated with 1.0 MeV Ar⁺, 1.6 MeV Ar⁺ or 2.5 MeV Kr⁺ ions using a dose rate of 1.4 × 10¹² cm⁻² s⁻¹ at temperatures between 50°C and 180°C. It has been found that the thickness of the recrystallized layer reaches a maximum value at T_max = 90°C and 135°C for the Ar⁺ and Kr⁺ implantations, respectively. This means that the crystallization rate deviates from an Arrhenius dependence due to ion beam induced nucleation and growth within the remaining amorphous layer. The size of the crystallites depends on the implantation dose. This nucleation and growth of the crystallites disturbes and at least blocks the interface movement because the remaining surface layer becomes polycrystalline. Choosing temperatures sufficiently below T_max the thickness of the recrystallized layer increases linearly with the implantation dose indicating that the irradiation temperature is too low for ion induced nucleation.     

Irradiation induced growth of CoSi2 precipitates in Si at 650°C: An in situ study

Crystalline Si samples were implanted at 350°C with 50 keV Co⁺ ions to a fluence of 10¹⁵ Co cm⁻². Small CoSi₂ precipitates were formed. We studied the precipitate growth, via in situ transmission electron microscopy, under irradiation with 100 keV Si ions at 650°C. We deduce the precipitate growth processes involved. Irradiation-induced (or enhanced) Ostwald ripening is the main growth mechanism. We also find an instability of the B-type precipitates, which leads to their transformation into A-type precipitates above a critical size. These preliminary results show that direct comparisons with kinetic Monte Carlo modelling of the precipitate growth is at hand.     

X-ray irradiation of ion-implanted MOS capacitors

He⁺ ion-implanted metal-oxide-semiconductor (MOS) capacitors with two different oxide thickness have been irradiated by X-rays and the depth distribution of the implant damage in the Si–SiO₂ structures have been examined. The efficiency of X-ray annealing of electronic traps caused by implantation and changes in charge populations are reported. The experiment shows that (in the case when defects introduced by implantation are located at the Si–SiO₂ interface) only defects corresponding to the deep levels in the Si can be affected by X-ray irradiation. When defects introduced by ion implantation are located deeper within the Si substrate complete annealing of these defects is observed.     

A TEM study of D -implanted Cu following Ar-ion milling: Microstructure and epitaxial Cu2O formation

In examining the microstructure of TEM specimens prepared from D⁺-implanted Cu for the presence of bubbles it was found that cuprous oxide (Cu₂O) layers had formed over large areas of the specimen surfaces. The Cu was irradiated at normal incidence with 200 keV D⁺ ions at a temperature of 120 K to a dose of ˜2 × 10²¹ D⁺/m². Ar⁺ ion milling at 330 K was used to erode irradiated surfaces to various depths prior to chemical back-thinning in a jet electropolishing bath. There was no evidence for the formation in the Cu of bubbles of either deuterium or argon, but dislocations at high density and planar defects were evident. Lattice fringes from {110}, {111} and {200} planes in Cu₂O and moiré patterns formed by double diffraction in the Cu and overlaid Cu₂O film were obvious features in bright-field micrographs. The moiré patterns include examples of magnified images of lattice defects.     

Carbon clustering in Si1−xCx formed by ion implantation

Silicon-carbon alloys were formed by multiple energy implantation of C⁺ ions in silicon and in Silicon on Sapphire (SOS). The ion fluence ranged between 5 × 10¹⁶ − 3 × 10¹⁷ ions/cm² and the energy between 10–30 keV in order to obtain constant carbon concentration into a depth of 100 nm. The carbon atomic fraction (x) was in the range 0.22–0.59 as tested by Rutherford backscattering spectrometry (RBS). Thermal annealing of the implanted films induced a transition from amorphous to a polycrystalline structure at temperatures above 850°C as detected by Infrared spectrometry (IR) in the wavenumber range 600–900 cm⁻¹. The optical energy gap and the intensity of the infrared signal after annealing at 1000°C depended on the film composition: they both increased linearly with carbon concentration reaching a maximum at the stoichiometric composition (x = 0.5). At higher carbon concentration the IR intensity saturated and the optical energy gap decreased from the maximum value of 2.2 to 1.8 eV. The behaviour at the high carbon content has been related to the formation of graphitic clusters as detected by Raman spectroscopy.     

Effect of Auger neutralization on yields of He ions backscattered and alkali ions sputtered from the surface of alkali halides by keV He ion impact

The yields of ions and neutrals backscattered and alkali ions sputtered from LiF crystals by keV He⁺ ion impact have been measured by means of the coaxial impact collision ion scattering spectroscopy in time of flight analysis mode using the charging-up effect. It is found that as the charging-up potential increases due to continuous irradiation of the pulsed ion beam, the time of flight of the He⁺ ions backscattered shifts toward the shorter time, while that of the neutrals backscattered shifts toward the longer, and that of Li ions sputtered also shifts much more clearly toward the shorter. The charging-up potential has been estimated as a function of irradiation time of the pulsed ion beam from the time of flight data and the ion to neutral ratio in the backscattering yields is estimated to be about 0.15. The mechanisms for ionization on He and sputtering of alkali ions are discussed in terms of charging-up and trion (bihole and electron) produced by Auger neutralization of keV He⁺ ions at the target surface.     

Radiation damage and annealing behaviour of Ge-implanted SiC

In recent years, single-crystal SiC has become an important electronic material due to its excellent physical and chemical properties. The present paper reports a study of the defect reduction and recrysallisation during annealing of Ge⁺-implanted 6H-SiC. Implants have been performed at 200 keV with doses of 1 × 10¹⁴ and 1 × 10¹⁵ cm⁻². Furnace annealing has been carried out at temperatures of 500, 950 and 1500°C. Three analytical techniques including Rutherford backscattering spectrometry in conjunction with channelling (RBS/C), positron annihilation spectroscopy (PAS) and cross-sectional transmission electron microscopy (XTEM) have been employed for sample characterisation. It has been shown that damage removal is more complicated than in ion-implanted Si. The recrystallisation of amorphised SiC layers has been found to be unsatisfactory for temperatures up to 1500°C. The use of ion-beam-induced epitaxial crystallisation (IBIEC) has been more successful as lattice regrowth, although still imperfect, has been observed to occur at a temperature as low as 500°C.     

Determination of the structure of subsurface layers by means of coaxial time-of-flight scattering and recoiling spectrometry (TOF-SARS)

It is demonstrated that both surface and subsurface structural information can be obtained from Si{100}-(2 × 1) and Si{100}-(1 × 1)-H by coupling coaxial time-of-flight scattering and recoiling spectrometry (TOF-SARS) with three-dimensional trajectory simulations. Experimentally, backscattering intensity versus incident angle scans at a scattering angle of 180° have been measured for 2 keV He⁺ incident on both the (2 × 1) and (1 × 1)-H surfaces. Computationally, an efficient three-dimensional version of the Monte Carlo computer code RECAD has been developed and applied to simulation of the TOF-SARS results. An R (reliability) factor has been introduced for quantitative evaluation of the agreement between experimental and simulated scans. For the case of 2 keV He⁺ scattering from Si{100}, scattering features can be observed and delineated from as many as 14 atomic layers ( 18 Å) below the surface. The intradimer spacing D is determined as 2.2 Å from the minimum in the R-factor versus D plot.     

XPS and optical studies of Xe-implanted and annealed YSZ single crystals

Xe⁺ ion implantation with 200 keV was completed at room temperature up to a fluence of 1 × 10¹⁷ ion/cm² in yttria-stabilized zirconia (YSZ) single crystals. Optical absorption and X-ray photoelectron spectroscopy (XPS) were used to characterize the changes of optical properties and charge state in the as-implanted and annealed crystals. A broad absorption band centered at 522 or 497 nm was observed in the optical absorption spectra of samples implanted with fluences of 1 × 10¹⁶ ion/cm² and 1 × 10¹⁷ ion/cm², respectively. These two absorption bands both disappeared due to recombination of color centers after annealing at 250 °C. XPS measurements showed two Gaussian components of O_1s spectrum assigned to Zr–O and Y–O, respectively, in YSZ single crystals. After ion implantation, these two peaks merged into a single peak with the increasing etching depth. However, this single peak split into two Gaussian components again after annealing at 250 °C. The concentration of Xe decreased drastically after annealing at 900 °C. And the XPS measurement barely detected the Xe. There was no change in the photoluminescence of YSZ single crystals with a fluence of 1 × 10¹⁷ ion/cm² after annealing up to 900 °C.     

He+离子辐照Inconel 718合金表面形貌改变及机理研究

研究了3种不同剂量He⁺离子辐照后Inconel 718合金的形貌变化规律及其形成机理。结果表明,He⁺离子辐照会在合金表面形成纳米多孔结构,其孔径会随辐照剂量的增加而增大。此外,He⁺离子辐照还会破坏合金表面δ相并导致碳化物的持续溅射损耗,且这一现象会随着辐照剂量的增加而愈发严重。由于辐照过程中氦泡间微观应力σ n作用会引起毗邻材料断裂及氦泡合并长大,且辐照溅射作用又会导致氦泡上层薄膜的损耗甚至破裂,因而这也是He⁺离子辐照Inconel 718合金表面纳米多孔结构的形成机制。     

Optical behaviour of Er doped rutile by ion implantation

Rutile single crystals were implanted at room temperature with fluences of 5 × 10¹⁵ Er⁺/cm² ions with 150 keV energy. Rutherford backscattering/channeling along the 0 0 1 axis reveals complete amorphization of the implanted region. Photoluminescence reveals the presence of an optical centre close to the intra-ionic emission of Er³⁺ in the as-implanted samples. After annealing at 800 °C in air no changes were observed in the aligned RBS spectrum. On the contrary, annealing in reducing atmosphere (vacuum) induces the epitaxy of the damage layer. These results are unexpected, since for implantations of other ions under the same conditions, epitaxial recrystallization of the damage region occurs at this temperature. On the other hand, photoluminescence studies show the presence of new Er-related optical centres with high thermal stability in the samples annealed under oxidizing conditions. Annealing at 1000 °C in vacuum leads to the complete recrystallization of the damaged region. At this temperature a large fraction of Er segregates to the surface.