Study of 160 MeV Ni ion irradiation effects on electrodeposited polypyrrole films

Conducting polymer polypyrrole thin films doped with LiCF₃SO₃, [CH₃(CH₂)₃]₄NBF₄ and [CH₃(CH₂)₃]₄NPF₆ have been electrodeposited potentiodynamically on ITO coated glass substrate. The polymer films are irradiated with 160 MeV Ni¹²⁺ ions at three different fluences of 5 × 10¹⁰, 5 × 10¹¹ and 3 × 10¹² ions cm⁻². An increase in dc conductivity of polypyrrole films from 100 S/cm to 170 S/cm after irradiation with highest fluence is observed in four-probe measurement. X-ray diffractogram shows increase in the crystallinity of the polypyrrole films upon SHI irradiation, which goes on increasing with the increase in fluence. Absorption intensity increase in the higher wavelength region is observed in the UV–Vis spectra. The SEM studies show that the cauliflower like flaky microstructure of the surface of polypyrrole films turns globular upon SHI irradiation at fluence 5 × 10¹¹ ions cm⁻² and becomes smooth and dense at the highest fluence used. The cyclic voltammetry studies exhibit that the redox properties of the polypyrrole films do not change much on SHI irradiation.     

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.     

Investigation of the radiation hardness on semiconductor devices using the ion micro-beam

Variation of the ion beam induced charge (IBIC) pulse heights due to ion irradiation was investigated on a Si pn diode and a 6H-SiC Schottky diode using a 2 Mev He⁺ micro-beam. Each diode was irradiated with a focused 2 MeV He⁺ micro-beam to a fluence in the range of 1×10⁹–1×10¹³ ions/cm². Charge pulse heights were analyzed as a function of the irradiation fluence. After a 2 MeV ion irradiation to the Si pn junction diode, the IBIC pulse height decreased by 15% at 9.2×10¹² ions/cm². For the SiC Schottky diode, with a fluence of 6.5×10¹² ions/cm², the IBIC pulse height decreased by 49%. Our results show that the IBIC method is applicable to evaluate irradiation damage of Si and SiC devices and has revealed differences in the radiation hardness of devices dependent on both structural and material.     

Magnetic force microscopy studies on the magnetic ordering in organic materials induced by high-energy proton irradiation

In this study, ferromagnetic microstructures in highly oriented pyrolytic graphite and superparamagnetic spots in polyimide foils were created by 2.25 MeV proton microbeam irradiation and characterized using atomic and magnetic force microscopy. For this purpose, graphite samples were irradiated with cross-like patterns of 15 μm × 15 μm size using ion fluences in the range of (0.003–2.5) × 10¹⁸ cm⁻². The irradiated crosses showed strong magnetic signals and a complex domain structure in the magnetic images depending on the geometrical dimensions of the crosses. Furthermore, polyimide foils were irradiated with microspots and fluences in the range of (0.016–3.1) × 10¹⁹ cm⁻². Magnetic force microscopy shows very strong phase shifts in these irradiated areas.     

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.     

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.     

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).     

Low temperature fast-neutron and gamma irradiation of glass fiber-epoxy composite. Part 2: Structure and chemistry

Structure and chemistry of S2-glass fiber-epoxy composite to fast-neutron and gamma irradiation at 4.2 K have been studied. Fast-neutron fluence ranged from 0.9 × 10²² to 1 × 10²³ n/m². At the neutron fluence of 3.1 × 10²² n/m², ordering of the amorphous S2-glass structure intervened. Ordering was followed by partial crystallization at the neutron fluence of 1 × 10²³ n/m². Although the epoxy matrix retained its amorphous structure, reactor irradiation induced crosslink formation and hydrogen evolution. These processes became significant at neutron fluences equal to or higher than 1.8 × 10²² n/m². No evidence has been found for hydrogen bubble or void nucleation at the glass-epoxy interface at the neutron fluence of 3.1 × 10²² n/m². Futhermore, sharp compositional changes measured at the glass-epoxy interface preclude an extended irradiation-induced atom mixing at this neutron fluence.     

Ion implantation doping and electrical conductivity enhancement of C60 films

Pristine C₆₀ films sublimed onto sheet mica were implanted with 20 keV K⁺ ions and I⁺ ions at doses of 1.0 × 10¹⁶/cm², 3.0 × 10¹⁶/cm² and 5.0 × 10¹⁶/cm², and with 20 keV Ar⁺ ions at a dose of 5.0 × 10¹⁶/cm². The distributions of dopants were studied using Rutherford backscattering spectrometry (RBS). The temperature dependence of sheet resistivity of the films was investigated applying a four-probe system. It was proposed that the conductivity enhancement of K⁺ implanted C₆₀ films was due to the implanted ions in the films, while for I⁺ implanted C₆₀ films, both implanted I⁺ ions and irradiation effects of the ions contributed to the enhancement of conductivity.     

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.     

Pumping experiment of water on B and LaB6 films with an electron beam evaporator

The pumping characteristic of water vapor on boron and lanthanum hexaboride films formed with an electron beam evaporator have been investigated in high vacuum between 10⁻⁴ and 10⁻³ Pa. The measured initial maximum pumping speeds of water for the fresh B or LaB₆ films with a deposition amount from 2.3 × 10²¹ to 6.7× 10²¹ molecules/m² separately formed on a substrate are 3.2–4.9 m³/sm², and the saturation values of adsorbed water on these films are 2.1 ×10²⁰−1.3 × 10²¹ H₂O molecules/m².     

Vacancy defects induced in the track region of 132 MeV C irradiated SiC

Positron annihilation lifetime spectroscopy (PALS) and electron paramagnetic resonance (EPR) have been used in this work to investigate vacancy defects induced in the track region of 132 MeV ¹²C irradiated silicon carbide. Irradiations have been performed at room temperature at a fluence of 2.5 × 10¹⁴ cm⁻² in N-low doped 6H–SiC and 3C–SiC monocrystals. Silicon monovacancies have been detected in both polytypes using EPR. Their charge state and concentration have been determined in the track and cascade region of the C⁺ ions. PALS measurements performed as a function of temperature have shown the presence of V_Si–C divacancies in the track region for both polytypes.     

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.     

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.     

Heavy ion irradiation effects in the rare-earth sesquioxide Dy2O3

Polycrystalline pellets of the rare-earth sesquioxide Dy₂O₃ with cubic C-type rare-earth structure were irradiated with 300 keV Kr²⁺ ions at fluences up to 5 × 10²⁰ Kr/m² at cryogenic temperature. Irradiation-induced microstructural evolution is characterized using grazing incidence X-ray diffraction (GIXRD) and transmission electron microscopy (TEM). In previous work, we found a phase transformation from a cubic, C-type to a monoclinic, B-type (C2/m) rare-earth structure in Dy₂O₃ during Kr²⁺ ion irradiation at a fluence of less than 1 × 10²⁰ Kr/m². In this study, we find that the crystal structure of the top and middle regions of the implanted layer transform to a hexagonal, H-type (P6₃/mmc) rare-earth structure when the irradiation fluence is increased to 5 × 10²⁰ Kr/m²; the bottom of the implanted layer, on the other hand, remains in a monoclinic phase. The irradiation dose dependence of the C-to-B-to-H phase transformation observed in Dy₂O₃ appears to be closely related to the temperature and pressure dependence of the phases observed in the phase diagram. These transformations are also accompanied by a decrease in molecular volume (or density increase) of approximately 9% and 8%, respectively, which is an unusual radiation damage behavior.     

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.     

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.     

Effect of tin on the irradiation growth of polycrystalline zirconium

Measurements of irradiation growth of polycrystalline Zr-1.5% Sn and Zr-0.1% Sn alloys at 353 K and 553 K have been made following fast neutron irradiation with fluences up to 3.1 × 10²⁵ n/m². At 353 K, growth of Zr-1.5% Sn virtually saturated at a strain of 4.5 × 10⁻⁴ after a fluence of ˜10²⁴ n/m². At this temperature, Zr-0.1% Sn continued to grów until ˜ 2 × 10²⁵ n/m², when the strain levelled off at ˜ 1.2×10⁻³. At 553 K, Zr-1.5% Sn initially grew about twice as fast as the 0.1% Sn alloy, but both eventually reached the same steady state rate of ˜ 2.4 × 10⁻²⁹ m²/n. Comparison of the data for the 1.5% Sn material with those for Zircaloy-2 from earlier work reveals that at 353 K, growth is suppressed by the presence of Sn atoms, which may serve as vacancy traps. However, at 553 K, minor additions and impurities in Zircaloy-2 (such as Fe, Ni, Cr and O) play an important role and cannot be neglected. The growth behaviour of Zr-0.1% Sn is similar to that of pure polycrystalline zirconium, especially at 353 K, indicating that the addition of Sn at this concentration does not strongly influence the growth of zirconium.