Ion beam synthesis and recrystallization of amorphous SiGe/SiC structures

Si_1−xGe_x amorphous layers implanted with different doses of carbon (between 5 × 10¹⁵ and 2 × 10¹⁷ cm⁻² and annealed at 700°C and 900°C have been analyzed by Raman and Infrared spectroscopies, electron microscopy and Auger electron spectroscopy. The obtained data show the synthesis of amorphous SiC by implanting at the highest doses. In these cases, recrystallization only occurs at the highest annealing temperature (900°C). The structure of the synthesized SiC strongly depends on the implantation dose, in addition to the anneal temperature. For the highest dose (2 × 10¹⁷ cm⁻²), crystalline β-SiC is formed. Finally, a strong migration of Ge towards the Si substrate is observed from the region where SiC precipitation occurs.     

EXAFS studies of thermal annealing effects on the local environment of erbium implanted in LiNbO3

X-ray absorption spectroscopy (XAS) has been applied to the study of thermal annealing effects on the local environment of erbium ions implanted at 300 keV (2 × 10¹⁶ ions/cm²) in LiNbO₃. The radial distribution functions change dramatically as a function of temperature and duration of annealing in air. The best simulations of the shells surrounding Er have been obtained with the Nb and Li site positions for Er after annealing at 500°C for 20 h and 1100°C for 100 h, respectively. Moreover, a shared site (Li, Nb) has to be considered after high temperature annealing for 20 h.     

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.     

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.     

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.     

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.     

Isothermal release of tritium from neutron-irradiated Li17Pb83

Isothermal release experiments were carried out to study the tritium recovery from lithium-lead alloy Li₁₇Pb₈₃ in which tritium was produced by irradiation with thermal neutrons. The experimental results indicate that the tritium recovery was incomplete within two hours at 200 °C. At temperatures above the melting point, the tritium release rates have been significantly increased and found to be controlled by the diffusion in the alloy. The determined diffusion coefficients of tritium in the alloy are 6.6 × 10⁻⁶, 7.8 × 10⁻⁶ and 9.5 × 10⁻⁶ cm²/s at 300, 400 and 500°C, respectively.     

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.     

Investigations of lattice location and mobility of carbon in GaAs using the channeling technique

In order to get information about the lattice location and the mobility of ¹²C in GaAs wafers, the channeling technique in combination with nuclear reaction analysis (NRA) is a powerful method. The targets were implanted with ¹²C ions (2.6 × 10¹³−2.6 × 10¹⁵cm⁻²) at energies between 60 and 3000 keV. This corresponds to implantation depths of about 0.1 to 3 μm. Using the nuclear reaction ¹²C(d, p)¹³C a depth distribution of the implanted carbon is obtained. The relationship between the concentration of ¹⁴C in random and along the 100 and 110 axial directions gives information about the substitutional lattice location of carbon within the GaAs crystal. In addition, we measured lattice defect depth distributions with a 1.5 MeV ⁴He⁺ beam before and after thermal annealing at temperatures up to 600°C.     

The formation of compound layers in silicon by ion beam synthesis

The technique of ion beam synthesis (IBS) using high doses of energetic ions has been successfully implemented to produce a variety of compounds, the physical properties of which are dependent on the implanted species and range from insulators, e.g. SiO₂, through semiconductors, e.g. SiC, to conductors, e.g. CoSi₂. In this paper we study the evolution of these compounds and compare and contrast their methods of formation. To demonstrate the versatility of the technique we look at three examples of IBS layers: (1) To date most of the interest in IBS has concentrated on the production of buried oxide layers for silicon-on-insulator (SOI) device applications. Recently it has been shown that by using a series of sequential implants and high-temperature anneals the defect density in the silicon overlayer can be dramatically reduced. To study how this process occurs, we followed the redistribution of the implanted species during implantation and annealing using both ¹⁶O⁺ and ¹⁸O⁺. (2) Buried CoSi₂ layers can be fabricated in (100) single-crystal silicon by implanting high doses of energetic cobalt ions at elevated temperatures. For the higher doses (≥ 4 × 10¹⁷ O⁺/cm² at 350 keV), a continuous coherent layer of CoSi₂ grows epitaxially during implantation. For lower doses, precipitates of both A- and B-type CoSi₂ are observed. After annealing at 1000° C for 30 min, single-crystal aligned layers are produced for the higher doses, while for lower doses discrete octahedral A-type precipitates are formed. (3) The microstructures of synthesized SiC layers are more complex than analogous synthesized oxide or silicide layers. Unlike buried oxide layers, the carbon concentration at the peak of the implanted distribution does not saturate at a value equivalent to that in the stoichiometric compound, but continues to rise, reflecting the lower diffusivity of the C in the synthesized compound layer. To achieve chemical segregation of the implanted carbon, very-high-temperature (≥ 1300°C), long-time (typically 20 h) anneals are required. At the interface with the silicon substrate the synthesized layer grows with a degree of epitaxy. This is also found to occur during implantation if the temperature is ≥ 650° C.     

Time scales of transient enhanced diffusion: free and clustered interstitials

Transient enhanced diffusion (TED) and electrical activation after nonamorphizing Si implantations into lightly B-doped Si multilayers shows two distinct timescales, each related to a different class of interstitial defect. At 700°C, ultrafast TED occurs within the first 15 s with a B diffusivity enhancement of > 2 × 10⁵. Immobile clustered B is present at low concentration levels after the ultrafast transient and persists for an extended period ( 10²–10³ s). The later phase of TED exhibits a near-constant diffusivity enhancement of ≈ 1 × 10⁴, consistent with interstitial injection controlled by dissolving {113} interstitial clusters. The relative contributions of the ultrafast and regular TED regimes to the final diffusive broadening of the B profile depends on the proportion of interstitials that escape capture by {113} clusters growing within the implant damage region upon annealing. Our results explain the ultrafast TED recently observed after medium-dose B implantation. In that case there are enough B atoms to trap a large proportion of interstitials in Si---B clusters, and the remaining interstitials contribute to TED without passing through an intermediate {113} defect stage. The data on the ultrafast TED pulse allows us to extract lower limits for the diffusivities of the Si interstitial (D_I > 2 × 10⁻¹⁰ cm²s⁻¹) and the B interstitial(cy) defect (D_Bi > 2 × 10⁻¹³ cm²s⁻¹) at 700°C.     

RBS studies of the lattice damage caused by 1 Me V Si implantation into Al0.3Ga0.7As/GaAs superlattices at elevated temperature

The lattice damage accumulation in GaAs and Al_0.3Ga_0.7As/GaAs superlattices by 1 MeV Si⁺irradiation at room temperature and 350°C has been studied. For irradiations at 350°C, at lower doses the samples were almost defect-free after irradiation, while a large density of accumulated defects was induced at a higher dose. The critical dose above which the damage accumulation is more efficient is estimated to be 2 × 10¹⁵ + Si/cm² for GaAs, and is 5 × 10¹⁵ Si/cm² for Al_0.8Ga_0.7As/GaAs superlattice for implantation with 1.0 MeV Si ions at 350°C. The damage accumulation rate for 1 MeV Si ion implantation in Al_0.3Ga_0.7As/GaAs superlattice is less than that in GaAs.     

Surface regrowth of Sb ion implanted Si(100)

Thermal regrowth of a Si(100) surface, damaged by 80 keV Sb implantation, was monitored by angular resolved photoemission (ARUPS), Rutherford backscattering (RBS) and channelling. It was found that regrowth in UHV at 650°C does not result in a well ordered surface. Annealing at higher temperatures (700–1100°C) results in densities of surface defects of (2.5 ± 0.4) × 10¹⁵ at./cm². A well ordered Si(100)2 × 1 reconstructed surface can be formed only after removal of a 10 nm thick layer by Ne ion bombardment, and heat treatment at 600°C. These observations can be explained by the formation of a surface layer with misoriented domains simultaneously with the solid phase epitaxy.     

Carbon ion-implanted optical waveguides in Nd:YLiF4 crystal: Refractive index profiles and thermal stability

We report on the optical planar waveguides in Nd:YLiF₄ laser crystals fabricated by 6.0 MeV C³⁺ ion implantation at doses of 1 × 10¹⁵ or 2.5 × 10¹⁵ ions/cm², respectively. The refractive index profiles, which are reconstructed according to the measured dark mode spectroscopy, show that the ordinary index had a positive change in the surface region, forming non-leaky waveguide structures. The extraordinary index is with a typical barrier-shaped distribution, which may be mainly due to the nuclear energy deposition of the incident ions into the substrate. In order to investigate the thermal stability of the waveguides, the samples are annealed at temperature of 200–300 °C in air. The results show that waveguide produced by higher-dose carbon implantation remains relatively stable with post-irradiation annealing treatment at 200 °C in air.     

Elemental dissolution study of Pu-bearing borosilicate glasses

Single-pass flow-through tests were conducted to study the effects of self-radiation damage from alpha decay on dissolution kinetics of three radiation-aged Pu-bearing (1 mass% PuO₂) borosilicate glasses over a pH interval of 9–12 at 80–88 °C. The chemical compositions of the glasses were identical except the ²³⁹Pu/²³⁸Pu isotopic ratio, which was varied to yield accumulated doses of 1.3 × 10¹⁶, 2.9 × 10¹⁷ and 2.6 × 10¹⁸ -decays/g at the time of testing. Release of Al, B, Cs, Na, Si and U to solution increased with increasing pH, whereas Ca, Pu and Sr were invariant over the pH interval. Average dissolution rates, based on B release, were identical within experimental uncertainty for all three glass compositions and increased from 0.17 ± 0.07 at pH(23 °C) 9 to 10.6 ± 2.7 (g/(m² d¹)) at pH(23 °C) 12. Release rates of Pu were 10²- to 10⁵-fold slower compared to all other elements and were not affected by isotopic composition, self-radiation damage sustained by the glass, or pH. These data demonstrate that self-radiation damage does not affect glass dissolution rates, despite exposure to internal radiation doses for >20 years.     

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.     

Thermal recovery of defects in neutron irradiated UO2

Thermal recovery of both lattice and volume expansions of UO₂ irradiated to a dose of less than 9.97 × 10¹⁷ fissions/cm³ was studied in a temperature range from 200 to 1000°C. Two or three steps were observed in the recovery of lattice expansion. Volume expansion was also recovered in two or three steps. Recovery behavior of volume expansion of the specimen irradiated to 9.97 × 10¹⁷ fissions/cm³ was different from those irradiated to lower doses, and an abrupt volume increase was observed in the temperature range from 500 to 700 °C. This behavior might be related to the bubble swelling due to fission product gases. From the results on the recovery of lattice and volume expansions, the behavior of lattice point defects and defect clusters was discussed.     

Damage distributions in LiNbO3 crystal induced by MeV F tilted implantations

X-cut LiNbO₃ crystals have been implanted by 0.8, 1.0 and 1.2 MeV F⁺ tilted at angles of 15°, 45° and 60° with doses of 5 × 10¹⁴, 7 × 10¹⁴ and 5 × 10¹⁴ ions/cm², respectively. The Rutherford backscattering (RBS)/channeling technique was used to investigate the induced damage distributions. The damage profiles were deconvoluted from the measured spectra after considering the energy spread due to the different stopping power of channeled and nonchanneled ions. Good agreements were obtained between the measured damage profiles and the calculated defect profiles by TRIM'90 (transport of ions in matter, version 1990), except that the measured damage concentration was enhanced in the near-surface region. Information on the lateral and longitudinal damage spread in LiNbO₃ crystals was obtained from the damage profiles induced by tilted ion implantations and compared with TRIM'90 calculation.     

Photoluminescence of Au formed in 12CaO · 7Al2O3 single crystal by Au-implantation

Au⁺ ion implantation with fluences from 1 × 10¹⁴ to 3 × 10¹⁶ cm⁻² into 12CaO · 7Al₂O₃ (C12A7) single crystals was carried out at a sample temperature of 600 °C. The implanted sample with the fluence of 1 × 10¹⁵ cm⁻² exhibited photoluminescence (PL) bands peaking at 3.1 and 2.3 eV at 150 K when excited by He–Cd laser (325 nm). This was the first observation of PL from C12A7. These two PL bands are possibly due to intra-ionic transitions of an Au⁻ ion having the electronic configuration of 6s², judged from their similarities to those reported on Au⁻ ions in alkali halides. However, when the concentration of the implanted Au ions exceeded the theoretical maximum value of anions encaged in C12A7 (2.3 × 10²¹ cm⁻³), surface plasmon absorption appeared in the optical absorption spectrum, suggesting Au colloids were formed at such high fluences. These observations indicate that negative gold ions are formed in the cages of C12A7 by the Au⁺ implantation if an appropriate fluence is chosen.     

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.