Structural evolution in Fe ion implanted Si upon thermal annealing

We have performed high-dose Fe ion implantation into Si and characterized ion-beam-induced microstructures as well as annealing-induced ones using transmission electron microscopy (TEM) and grazing-incidence X-ray diffraction (GIXRD). Single crystals of Si(1 0 0) substrate were irradiated at 623 K with 120 keV Fe⁺ ions to a fluence of 4 × 10¹⁷ cm⁻². The irradiated samples were then annealed in a vacuum furnace at temperatures ranging from 773 K to 1073 K. Cross-sectional TEM observations and GIXRD measurements revealed that a layered structure is formed in the as-implanted specimen with ε-FeSi, β-FeSi₂ and damaged Si, as component layers. A continuous β-FeSi₂ layer was formed on the topmost layer of the Si substrate after thermal annealing.     

Electron-beam radial distribution analysis of irradiation-induced amorphous SiC

Advanced electron microscopy techniques have been employed to examine atomistic structures of ion-beam-induced amorphous silicon carbide (SiC). Single crystals of 4H-SiC were irradiated at a cryogenic temperature (120 K) with 300 keV Xe ions to a fluence of 10¹⁵ cm⁻². A continuous amorphous layer formed on the topmost layer of the SiC substrate was characterized by energy-filtering transmission electron microscopy in combination with imaging plate techniques. Atomic pair-distribution functions obtained by a quantitative analysis of energy-filtered electron diffraction patterns revealed that amorphous SiC networks contain heteronuclear Si–C bonds, as well as homonuclear Si–Si and C–C bonds, within the first coordination shell. The effects of inelastically-scattered electrons on atomic pair-distribution functions were discussed.     

Spectroscopic and microscopic study of the corrosion of iron–silicon steel by lead–bismuth eutectic (LBE) at elevated temperatures

The performance of iron–silica alloys with different silicon composition was evaluated after exposure to an isothermal bath of lead–bismuth eutectic (LBE). Four alloys were evaluated: pure iron, Fe–1.24%Si, Fe–2.55%Si and Fe–3.82%Si. The samples were exposed to LBE in a dynamic corrosion cell for periods from 700 to 1000 h at a temperature of 550 °C. After exposure, the thickness and composition of the oxide layer were examined using optical microscopy, scanning electron microscopy (SEM) and X-ray photoelectron spectrometry (XPS), including sputter depth profiling. Particular attention was paid to the role, spatial distribution, and chemical speciation of silicon. Low-binding-energy silicon (probably silicates or ) was found in the oxide; while elemental silicon (Si) was found in the metal as expected, and silica (SiO₂) was found at the bottom of the oxide layer, consistent with the formation of a layer between the oxide and the metal. Alloys with low concentrations of Si contained only silicate in the oxide. Alloys with higher concentrations of Si contained a layer of silica at the boundary between the oxide and the bulk metal. All of the alloys examined showed signs of oxide failure. This study has implications for the role of silicon in the stability of the oxide layer in the corrosion of steel by LBE.     

The excitation power density effect on the Si nanocrystals photoluminescence

In the present work we have studied the photoluminescence (PL) behavior from Si nanocrystals (NCs) as a function of the excitation power density and annealing time. The NCs were produced in a SiO₂ matrix by Si implantations from room temperature (RT) up to 700 °C, followed by post-annealing in N₂ atmosphere at high temperature. With this aim we have changed the excitation power density (from 2 × 10⁻³ W/cm² up to 15 W/cm²) and the annealing time (from 10 min up to 15 h). The strong PL signal, which at 15 W/cm² is composed by a single-peak structure (650–1000 nm) centered at around 780 nm, expands up to 1200 nm showing a two-peak structure when measured at 20 × 10⁻³ W/cm². The peak structure located at the short wavelength side is kept at 780 nm, while the second peak, starting at around 900 nm, redshifts and increases its intensity with the implantation temperature and annealing time. The effect of the annealing time on the PL spectra behavior measured at low excitation power agrees by the first time with the Si NC growth according to quantum confinement effects.     

Defect evolution during ion bombardment of amorphous Si probed by in situ conductivity measurements

In this work we use in-situ conductivity measurements during ion irradiation as a sensitive probe of the defect structure of amorphous Si. Electronic transport in amorphous Si occurs by hopping at the high density ( 10²⁰ cm⁻³ eV⁻¹) of deep lying localized states introduced by the defects in the band gap. In-situ conductivity measurements allow to follow directly the defect generation and annihilation kinetics during and after ion bombardment of the material. Amorphous Si layers, patterned to perform conductivity measurements, were annealed at 500°C in order to reduce the defect density by about a factor of 5. Defects were subsequently reintroduced by high energy ion irradiation at different temperatures (77–300 K). During irradiation the conductivity of the layer increases by several orders of magnitude and eventually saturates. Turning off the beam results in a decrease of the conductivity by a factor of 2 in times as long as a few hours even at 77 K. The effects of different ions (He, C, Si, Cu, and Au) and different ion fluxes (10⁹–10¹² ions/cm² s) on these phenomena have been explored. These data give a hint on the mechanisms of defect production and annihilation and demonstrate a strong correlation between electrical and structural defects in amorphous silicon.     

Radiation damage induced by 5 keV Si ion implantation in strained-Si/Si0.8Ge0.2

The damage distributions induced by ultra low energy ion implantation (5 keV Si⁺) in both strained-Si/Si_0.8Ge_0.2 and normal Si are measured using high-resolution RBS/channeling with a depth resolution better than 1 nm. Ion implantation was performed at room temperature over the fluence range from 2 × 10¹³ to 1 × 10¹⁵ ions/cm². Our HRBS results show that the radiation damage induced in the strained Si is slightly larger than that in the normal Si at fluences from 1 × 10¹⁴ to 4 × 10¹⁴ ions/cm² while the amorphous width is almost the same in both strained and normal Si.     

Effect of GeV-Ion irradiation on magnetic properties of Fe–Ni invar alloys

High-energy ion irradiation was performed using a ring-cyclotron installed at the Institute of Physical and Chemical Research (RIKEN). The incident ions were Ta with the energy of 3.71 GeV, and the fluence was fixed to 5 × 10¹² ions/cm². As a target, three sheets of square plates of Fe–30.2 at.% Ni invar alloys were put one upon another. The shift of the Curie temperature T_C of the first sample was 14 K, while that of the second one was 22 K. Comparing these two, the shift was as large as 46 K in the last sample in which ions stopped in the middle. It was concluded that there are at least two different mechanisms that contribute to the shift of T_C.     

Effect of Si implantation on the microstructure of silicon nanocrystals and surrounding SiO2 layer

Si nanocrystals (Si-nc) embedded in a SiO₂ layer have been characterized by means of transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). For local Si concentration in excess  8 × 10²¹ Si⁺/cm³, the size of the Si-nc was found to be 3 nm and comparatively homogeneous throughout the whole implanted layer. For local Si concentration in excess of 2.4 × 10²² Si⁺/cm³, the Si-nc diameter ranges from 2 to 12 nm in the sample, the Si-nc in the middle region of the implanted layer being bigger than those near the surface and the bottom of the layer. Also, Si-nc are visible deeper than the implanted depth. Characterization by XPS shows that a large quantity of oxygen was depleted from the first 25 nm in this sample (also visible on TEM image) and most of the SiO₂ bonds have been replaced by Si–O bonds. Experimental and simulation results suggest that a local Si concentration in excess of 3 × 10²¹ Si/cm³ is required for the production of Si-nc.     

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.     

Plasma nitridation of thin SiO2 films: AES, ELS and IR study

Auger electron spectroscopy, low-energy electron loss spectroscopy and infrared spectroscopy are used to investigate the nitridation of thin (10–22 nm) thermal SiO₂ in RF soft NH₃ plasma. It is found that plasma action at a substrate temperature of 573 K can completely nitridate the thermal oxide to an oxynitride layer. The layers obtained are macroscopic mixtures of two phases SiO₂ and Si₃N₄, rather than amorphous polymers of Si, O and N.     

High resolution channeling contrast microscopy and channeling analysis of SiGe quantum well structures

High resolution channeling contrast microscopy (CCM) and channeling measurements were carried out to characterize SiGe quantum well structures on micron thick graded layers (i.e. virtual substrates). The virtual substrates were grown by gas source molecular beam epitaxy at a pressure of 10⁻⁵ mbar and low pressure chemical vapor deposition at 10⁻² mbar on boron doped Si(0 0 1) substrates respectively. A homoepitaxial silicon buffer layer was grown prior to the deposition. The nominal structure is a 20 nm Si_0.75Ge_0.25 layer at the surface, followed by 10 nm pure Si, 500 nm Si_0.75Ge_0.25 and a 1000 nm thick graded SiGe (0–26%) layer. RBS was used to measure the depth profiles, and angular scans around the (1 0 0) axis were carried out to assess crystal and interface quality. CCM was used to acquire depth resolved images of micron-sized lateral inhomogenities (‘cross-hatch') present on both samples.     

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.     

Low temperature epitaxial regrowth of mercury implanted sapphire

Hg ions were implanted into sapphire at room temperature and 80 keV energy to a fluence of 1 × 10¹⁵ Hg⁺ / cm². This fluence was enough to produce an amorphous surface layer. The annealing behaviour was studied combining RBS/channeling and hyperfine interaction techniques. Surprisingly, the RBS/channeling results show there is an epitaxial regrowth of the damaged layer after annealing at 800°C for 20 min. Although some of the implanted Hg segregates to the surface during the epitaxial regrowth, a significant fraction is incorporated into regular sites along the c-axis. The hyperfine interactions results, obtained after implantation of a dose of 5 × 10¹² Hg⁺ / cm², show that a small fraction of Hg is probably bound to oxygen. This result is in agreement with the RBS/channeling measurements which also show that the system formed after annealing is stable even at high temperatures.     

Effect of annealing on the optical absorption of Ni nanoparticles in MgO single crystals

Ni⁺ ion implantation with an energy of 64 keV in MgO single crystals was conducted at room temperature up to a fluence of 1 × 10¹⁷ ion/cm². The as-implanted crystals were annealed isochronally at temperatures up to 900 °C. Optical absorption spectroscopy, X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) have been utilized to characterize the changes of optical properties and the microstructure of the annealed samples. XPS results showed that the charge state of implanted Ni was still mainly in metallic Ni⁰ after annealing at 900 °C. TEM analysis revealed metallic Ni nanoparticles with depth-dependant dimensions of 1–10 nm in the annealed sample. Optical absorption spectroscopy indicated that the Ni nanoparticles exhibited a broad surface plasmon resonance absorption band in annealed samples and the band shifted to a longer wavelength with the increasing annealing temperature.     

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.     

Separation of plutonium from lanthanum by electrolysis in LiCl–KCl onto molten bismuth electrode

This work presents a study on the electroseparation of plutonium from lanthanum using molten bismuth electrodes in LiCl–KCl eutectic at 733 K. The reduction potentials of Pu³⁺ and La³⁺ ions were measured on a Bi thin film electrode using cyclic voltammetry (CV). A difference between the peak potentials for the formation of PuBi₂ and LaBi₂ of approximately 100 mV was found. Separation tests were then carried out using different current densities and salt phase compositions between a plutonium rod anode and an unstirred molten Bi cathode in order to evaluate the efficiency of an electrolytic separation process. At a current density of 12 mA/cm²/wt% (Pu³⁺), only Pu³⁺ ions are reduced into the molten Bi electrode, leaving La³⁺ ions in the salt melt. Similar results were found at two different Pu/La concentration ratios ([Pu]/[La] = 4 and 10). At a current density of 26 mA/cm²/wt% (Pu³⁺), co-reduction of Pu and La was observed as expected by the large negative potential of the Bi cathode during the separation test.     

Temperature dependence of the chemical sputtering of amorphous hydrogenated carbon films by hydrogen

The temperature dependence of chemical erosion and chemical sputtering of amorphous hydrogenated carbon films due to exposure to hydrogen atoms (H⁰) alone and combined exposure to argon ions and H⁰ was measured in the temperature range from 110 to 950 K. The chemical erosion yield for H⁰ alone is below the detection limit for temperatures below about 340 K. It increases strongly with increasing temperature, goes through a maximum around 650–700 K and decreases again for higher temperatures. Combined exposure to Ar⁺ and H⁰ results in substantial chemical sputtering yields in the temperature range below 340 K. In this range the yield does not depend on temperature, but it increases with energy from about 1 (eroded carbon atoms per impinging Ar⁺ ion) to about 4 if the ion energy is increased from 50 to 800 eV. For temperatures above 340 K the measured erosion rates show the same temperature dependence as for the H⁰-only case, but they are higher than for H⁰-only. The difference between the Ar⁺ and H⁰ and the H⁰-only cases increases monotonically with increasing ion energy.     

On the useful range of application of molecular dynamics simulations in the recoil interaction approximation

The validity of the binary collision (BC) approximation and of the so-called recoil interaction approximation (RIA) in ion–solid interactions at low energies is investigated by comparison with molecular dynamics (MD) simulations. The systems studied are channeling through a (1 1 0) oriented layer of Si, implantation into a (1 0 0)-Si target, and reflection from (1 0 0)-Si. It is found that the BC approximation does not introduce significant errors in the case of channeling simulations even at very low energies. Under non-channeling conditions an upper limit to the break-down energy of the BC approximation in Si is given by 30M₁^0.55 eV, taking 5% deviation in the projected range as the criterion.     

Ion beam mixing of Au marker in Pt and Pt marker in Au by 7 MeV Ag ions

Mixing of a thin Au layer in Pt and in reversed conditions mixing of a thin Pt layer in Au due to bombardment with 7 MeV Ag ions has been measured. The Pt-Au multilayers deposited on a Si substrate were irradiated to doses of 1–6 × 10¹⁵ ions cm⁻² at room temperature. The mixed profiles were measured using a SIMS apparatus with O₂⁺ sputter ions at energy 2.5 keV. The width of the Pt marker increased from 90 to 260 Å with increasing dose. The width of the Au marker increased from 80 to 90 Å, respectively. The corresponding mixing efficiencies are 5 ± 3 (Au marker) and 90 ± 30 Å⁵/eV (Pt marker). The experimental results are compared with simulations based on a model which describes the atomic transport from the initial collisional phase to the late thermalized stage. The calculated values for mixing efficiencies agree reasonably well with experimental values.     

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.