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.     

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.     

Optical absorption of metallic Zn nanoparticles in Zn ion implanted sapphire

Zn⁺ ion implantation (48 keV) was performed at room temperature up to a fluence of 5 × 10¹⁷ cm⁻² in -Al₂O₃ single crystals. X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM) and optical absorption spectroscopy were utilized to characterize the optical properties, chemical charge states and the microstructure of embedded metallic Zn nanoparticles, respectively. XPS analysis indicated that implanted Zn ions are in the charge state of metallic Zn⁰. TEM analysis revealed the metallic Zn nanoparticles of 3–10 nm in the as-implanted sample at a fluence of 1 × 10¹⁷ cm⁻². A selected area electron diffraction (SAD) pattern indicates the random orientation of the Zn nanoparticles. A clear absorption peak appeared gradually in the optical absorption spectra of the as-implanted crystals, due to surface plasma resonance (SPR) of Zn nanoparticles. The wavelength of the absorption peak shifted from 260 nm to 285 nm with the increasing ion fluence, ascribed to the growth of Zn nanoparticles.     

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.     

Mechanism of irradiation assisted stress corrosion crack initiation in thermally sensitized 304 stainless steel

Thermally sensitized 304 stainless steels, irradiated up to 1.2 × 10²¹ n/cm² (E > 1 MeV), were slow-strain-rate-tensile tested in 290 °C water containing 0.2 ppm dissolved oxygen (DO), followed by scanning and transmission electron microscopic examinations, to study mechanism of irradiation-assisted-stress-corrosion-crack (IASCC) initiation. Intergranular (IG) cracking behaviors changed at a border fluence (around 1 × 10²⁰ n/cm²), above which deformation twinning were predominant and deformation localization occurred earlier with increasing fluence. The crack initiation sites tended to link to the deformation bands, indicating that the crack initiation may be brought about by the deformation bands interacted with grain boundaries. Thus the border fluence is equivalent to the IASCC threshold fluence for the sensitized material, although the terminology of IASCC is originally given to the non-sensitized materials without microstructural definition. The IASCC threshold fluence was found to change with irradiation conditions. Changes in IASCC susceptibility and IASCC threshold fluence with fluence and DO were further discussed.     

Helium retention of vanadium alloy after energetic helium ion irradiation

Helium irradiation experiments of V–4Ti alloy were conducted in an ECR ion irradiation apparatus by using helium ions with energy of 5 keV. The ion fluence was in the range from 1 × 10¹⁷ He/cm² to 8 × 10¹⁷ He/cm². After the helium ion irradiation, the helium retention was examined by using a technique of thermal desorption spectroscopy (TDS). After the irradiation, the blisters with a size of about 0.1 μm were observed at the surface, and the blister density increased with the ion fluence. Two desorption peaks were observed at approximately 500 and 1200 K in the thermal desorption spectrum. When the ion fluence was low, the retained helium desorbed mainly at the higher temperature regime. As increase of the ion fluence, the desorption at the lower temperature peak increased and the retained amount of helium saturated. The saturated amount was approximately 2.5 × 10¹⁷ He/cm². This value was comparable with those of the other plasma facing materials such as graphite.     

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.     

Heavy-ion-induced luminescence of amorphous SiO2 during nanoparticle formation

Silica glass was implanted with negative 60 keV Cu ions at an ion flux from 5 to 75 μA/cm² up to a fluence of 1 × 10¹⁷ ions/cm² at initial sample temperatures of 300, 573 and 773 K. Spectra of ion-induced photon emission (IIPE) were collected in situ in the range from 250 to 850 nm. Optical absorption spectra of implanted specimens were ex situ measured in the range from 190 to 2500 nm.

IIPE spectra showed a broad band centered around 560 nm (2.2 eV) that was assigned to Cu⁺ solutes. The band appeared at the onset of irradiation, increased in intensity up to a fluence of about 5 × 10¹⁵ ions/cm² and then gradually decreased indicating three stage of the ion beam synthesis of nanoclusters: accumulation of implants, nucleation and growth nanoclusters. The IIPE intensity normalized on the ion flux is independent on the ion flux below 20 μA/cm²at higher fluences. The intensity of the band increased with increasing samples temperature, when optical absorption spectra reveal the increase of Cu nanoparticles size.     

Radiation effects on MgAl2O4–yttria stabilized ZrO2 composite material irradiated with Ne ions at high temperatures

Spinel (MgAl₂O₄) and yttria stabilized ZrO₂ (YSZ) are candidates for fuel materials for use in nuclear reactors and the optical and insulating materials for fusion reactors. In our previous studies, the amorphization of spinel under 60 keV Xe ion irradiation at RT was observed. On the other hand, amorphization could not be confirmed in YSZ single crystals under the same irradiation conditions. In the present study, the damage evolution process of polycrystalline spinel–YSZ composite materials has been studied by in situ TEM observation during ion irradiation. The irradiation was performed with 30 keV Ne⁺ ions at a flux of 5 × 10¹³ ions cm⁻² s⁻¹ at 923 K and 1473 K, respectively. The observed results revealed a clear difference in morphology of damage depending on irradiation temperature and crystal grains. In the irradiation at 923 K, defect clusters and bubbles were formed homogeneously in YSZ grains. On the other hand, at 1473 K, only bubble formation was observed. The bubbles grew remarkably with increasing ion fluence in both grains. Even though the growth of the bubbles was observed in both grains, the average diameter of grown bubbles in spinel grains was larger than those in YSZ ones. The bubbles tended to form along the grain boundary at both temperatures.     

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.     

Optical and structural behaviour of Mn implanted sapphire

Sapphire single crystals were implanted at room temperature with 180 keV manganese ions to fluences up to 1.8 × 10¹⁷ cm⁻². The samples were annealed at 1000 °C in oxidizing or reducing atmosphere. Surface damage was observed after implantation of low fluences, the amorphous phase being observed after implantation of 5 × 10¹⁶ cm⁻², as seen by Rutherford backscattering spectroscopy under channelling conditions. Thermal treatments in air annealed most of the implantation related defects and promoted the redistribution of the manganese ions, in a mixed oxide phase. X-ray diffraction studies revealed the presence of MnAl₂O₄. On the contrary, similar heat treatments in vacuum led to enhanced out diffusion of Mn while the matrix remained highly damaged. The analysis of laser induced luminescence performed after implantation showed the presence of an intense red emission.     

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.     

Study of radiation-induced degradation of RPV steels and model alloys by positron annihilation and Mössbauer spectroscopy

The influence of different microstructural processes on the degradation due to radiation embrittlement has studied by positron annihilation and Mössbauer spectroscopy. The materials studied consisted of WWER-440 base (15Kh2MFA) and weld (10KhMFT) RPV steels which were neutron-irradiated at fluence levels of 0.78 × 10²⁴ m⁻², 1.47 × 10²⁴ m⁻² and 2.54 × 10²⁴ m⁻²; WWER-1000 base (15Kh2NMFAA) and weld (12Kh2N2MAA) irradiated at a fluence level 1.12 × 10²⁴ m⁻²; three different model alloys implanted with protons at two dose levels (up to 0.026 dpa), finally the base metal of WWER-1000 (15Kh2NMFAA) was thermally treated with the intention to simulate the P-segregation process. It has been shown possible to correlate the values of parameters obtained by such techniques and data of mechanical testing (ductile-to-brittle transition temperature and upper shelf energy).     

Structural characterization of amorphous Fe–Si and its recrystallized layers

We have synthesized amorphous Fe–Si thin layers and investigated their microstructure using transmission electron microscopy (TEM). Si single crystals with (1 1 1) orientation were irradiated with 120 keV Fe⁺ ions to a fluence of 4.0 × 10¹⁷ cm⁻² at cryogenic temperature (120 K), followed by thermal annealing at 1073 K for 2 h. A continuous amorphous layer with a bilayered structure was formed on the topmost layer of the Si substrate in the as-implanted specimen: the upper layer was an amorphous Fe–Si, while the lower one was an amorphous Si. After annealing, the amorphous bilayer crystallized into a continuous β-FeSi₂ thin layer.     

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.     

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.     

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.     

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.     

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.     

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.