Localization by TEM and EELS of deuterium trapping sites in CFC exposed to plasma irradiation in Tore Supra

Carbon fiber composite (CFC) Sepcarb^® N11 is used in the tokamak Tore Supra as plasma-facing components. To investigate the fuel retention capability of this material, a mobile sample holder was used to expose CFC N11 samples to direct irradiation by the scrape-off layer plasma of Tore Supra at fluences up to 1 × 10²⁵ m⁻². Deuterium (D) elemental mapping using nuclear reaction analysis for the most-exposed CFC sample showed that D retention occurs at depths greater than 8 μm due to the presence of deep (>3.5 μm) local retention sites. In this work, combining transmission electron microscopy (TEM) and electron energy-loss spectroscopy (EELS), we describe at a high spatial resolution where and how D atoms are trapped in these sites. TEM experiments performed on thin cross-sections of the plasma-modified surface show evidence of the presence of a 3.5 μm-thick deuterated amorphous carbon layer deposited on the CFC surface. We show that specific localized retention sites correspond to the filling of relatively large (∼3 μm.) and deep (at least 3 μm below the initial CFC surface) cracks between fibres and matrix by the deuterated amorphous carbon layer.     

Effect of swift heavy ion irradiation on hydrothermally synthesized hydroxyapatite ceramics

The effect of swift heavy ion irradiation on hydroxyapatite (HAp) ceramic - a bone mineral was investigated. The irradiation experiment was conducted using oxygen ions at energy of 100 MeV with three different fluences of 10¹², 10¹³, 10¹⁴ ions/cm². The irradiated samples were characterized by glancing angle X-ray diffraction (GXRD), atomic force microscopy (AFM), dynamic light scattering (DLS), photoluminescence spectroscopy (PL), scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDAX). GXRD confirmed incomplete amorphisation of HAp with increase in fluence. There was considerable reduction in particle size on irradiation leading to nanosized HAp (upto 53 nm). PL studies showed emission in the visible wavelength region. The irradiated samples exhibited better bioactivity than the pristine HAp.     

The effect of ion sputtering of silicon substrates on the catalyst morphology and growth of carbon nanotube arrays

Polished Si substrates are sputtered by He⁺ ions, and carbon nanotube arrays are prepared on the Fe-coated substrates by heat chemical vapor deposition from acetylene. Scanning electron microscopy and atomic force microscopy are employed to examine the morphologies of sputtered substrates, catalyst and carbon nanotube arrays. It is found that ion sputtering is effective in increasing the roughness of Si substrates, and helpful in obtaining higher density Fe catalyst particles and better-aligned carbon nanotube arrays.     

Electron beam modification and functionalization of MWNT for covalent dispersion into polymeric systems

The development of nanotube-based polymer composites with improved mechanical properties and electrical conductivity requires the covalent dispersion of carbon nanotubes to utilize their stress transfer capabilities. Covalent dispersion of nanotubes therefore requires the functionalization of their surface to interact with solvents or monomers. In this work, we have developed a novel method of nanotube surface modification in which dry MWNT are irradiated with a high-energy electron beam (EB) in ambient air environment. Raman spectroscopy was performed to characterize the influence of EB irradiation on nanotubes, namely, variance of the disorder, or D band (∼1360 cm⁻¹) with respect to the graphitic, or G, band (∼1580 cm⁻¹). Raman spectra show increased deformation to the graphitic structure, as well as increased strain on the carbon-carbon bonds, weakening the nanotube. Transmission electron microscopy (TEM) confirms that nanotubes remain intact despite high EB dose. In addition, minimal surface deformation and length reduction occurred on irradiated MWNT.     

Surface molecular degradation of high performance carbon/bismaleimide composites induced by proton irradiation

This work aims to identify and describe the effects of proton irradiation in ultra high vacuum environment on the surface degradation of high performance carbon/bismaleimide composites used in aerospace. The changes in surface molecular structure and surface chemical composition with increasing irradiation fluence were studied by Attenuated total reflection Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy, respectively. The evolution of surface morphology and surface roughness were characterized by atomic force microscopy. The results indicated that the proton irradiation caused surface degradation of the carbon/bismaleimide composites by altering their surface chemical structure and surface morphology. The surface chemical bonds were broken largely and the extent of carbonification at the surface layer of the composites was enhanced with increasing irradiation fluence. The increment in the carbon concentration and the sharp reduction in the oxygen and nitrogen concentration with increasing irradiation fluence were caused by the emission of some oxygen-containing and nitrogen-containing small molecules from the material surface under high vacuum environment. The surface roughness firstly increased under the fluence lower than 5 × 10¹⁵ cm⁻², and then decreased after the irradiation fluence increased to some extent.     

Morphological change in FePt nanogranular thin films induced by swift heavy ion irradiation

We have investigated morphology change of FePt nanogranular films (FePt)₄₇(Al₂O₃)₅₃ under irradiation with 210 MeV Xe ions. Here, electron tomography technique was extensively employed to clarify three-dimensional (3D) structure in irradiated specimens, in addition to conventional transmission electron microscopy (TEM) techniques such as bright-field observation and scanning TEM energy dispersive X-ray spectroscopy (STEM-EDX) analysis. The ion irradiation induces the coarsening of FePt nanoparticles with elongation along the beam direction. Electron tomography 3D reconstructed images clearly demonstrated that when the fluence achieves 5.0 × 10¹⁴ ions/cm², well-coarsened FePt balls have been formed on the irradiated surface, and the particles in the film interior have been deformed into rods along the ion trajectory. The alloy particles become inhomogeneous in composition after prolonged irradiation up to 1.0 × 10¹⁵ Xe ions/cm². The particle center is enriched with Pt, while Fe is slightly redistributed to the periphery.     

A direct current glow discharge plasma source for inner surface modification of metallic tube

A dc glow discharge plasma source was developed for inner surface modification of metallic tubes with an inner diameter of 10 mm. A tungsten wire of 30 μm thick was stretched inside the tube to form coaxial electrodes. DC glow discharge plasma was generated inside the tube by applying a negative high dc voltage to the tube. It was found that the length of the cylindrical plasma bulk depends linearly on the applied voltage. The electron excitation temperature of Ar plasma was measured as 12830 ± 550 K by optical emission spectroscopy method. As a preliminary application, diamond-like carbon (DLC) films were deposited onto the inner surface of stainless steel tube of 100 mm in length and 10 mm in inner diameter by using CH₄/Ar mixture with 40% CH₄ at 40 Pa pressure. The chemical structure of the DLC film deposited on the substrate was analyzed by Raman spectroscopy. The integrated intensity ratio (I_D:I_G) was obtained as 1.62 from the Raman spectra. The thickness of the DLC film deposited on the substrate was estimated as 1.5 μm by scanning electron microscopy (SEM) observation.     

Secondary electron yield of Au and Al2O3 surfaces from swift heavy ion impact in the 2.5-7.9 MeV/amu energy range

We report on the secondary electron yields of Au and oxidized aluminum (Al₂O₃) by impact of heavy ions with energies ranging from 7.92 MeV/amu (¹²C₆) to 2.54 MeV/amu (¹⁰⁷Ag₄₇). The obtained results, the first in this energy range using medium-heavy ions, extend the validity of proposed scaling laws obtained with lighter ions. Measurements have been performed using the SIRAD irradiation facility at the 15 MV Tandem of the INFN Laboratory of Legnaro (Italy), to evaluate the performance of ion electron emission microscopy at SIRAD.     

Oxygen ion irradiation effect on corrosion behavior of titanium in nitric acid medium

The corrosion assessment and surface layer properties after O⁵⁺ ion irradiation of commercially pure titanium (CP-Ti) has been studied in 11.5 N HNO₃. CP-Ti specimen was irradiated at different fluences of 1 × 10¹³, 1 × 10¹⁴ and 1 × 10¹⁵ ions/cm² below 313 K, using 116 MeV O⁵⁺ ions source. The corrosion resistance and surface layer were evaluated by using potentiodynamic polarization, electrochemical impedance spectroscopy (EIS), scanning electron microscopy (SEM) and glancing-angle X-ray diffraction (GXRD) methods. The potentiodynamic anodic polarization results of CP-Ti revealed that increased in ion fluence (1 × 10¹³-1 × 10¹⁵ ions/cm²) resulted in increased passive current density due to higher anodic dissolution. SEM micrographs and GXRD analysis corroborated these results showing irradiation damage after corrosion test and modified oxide layer by O⁵⁺ ion irradiation was observed. The EIS studies revealed that the stability and passive film resistance varied depending on the fluence of ion irradiation. The GXRD patterns of O⁵⁺ ion irradiated CP-Ti revealed the oxides formed are mostly TiO₂, Ti₂O₃ and TiO. In this paper, the effects of O⁵⁺ ion irradiation on material integrity and corrosion behavior of CP-Ti in nitric acid are described.     

Behavior of tungsten with exposure to deuterium plasmas

Four kinds of tungsten (W) materials, i.e. (1) foil of 50 μm thick (f-W), (2) polycrystalline (Pc-W) with grain size of ∼3 μm, (3) recrystallized (Re-W) with grain size of ∼50 μm and (4) vacuum plasma spraying (VPS-W) coatings, were irradiated employing linear plasma generators, with fluxes ?1 × 10²² D/m²/s and energies ?100 eV/D. Scanning electron microscopy (SEM) was used to observe blister formation at the surfaces. The SEM surface morphology and cross section observation indicates that blister formation is related to the microstructure and surface state of different material grades. Results of trapping and deuterium retention measured by thermal desorption spectroscopy (TDS) and nuclear reaction analysis (NRA) show also a close correlation between the retention and the microstructure and surface state.     

Structural and optical study of irradiation effect in GaN epilayers induced by 308 MeV Xe ions

Wurtzite GaN epilayers irradiated at room temperature with 308 MeV ¹²⁹Xe³⁵⁺ ions to fluences of 1 × 10¹³ and 3 × 10¹³ cm⁻² have been studied by contact mode atomic force microscopy (AFM), high-resolution X-ray diffraction (HRXRD), micro-Raman scattering and photoluminescence (PL) spectroscopy. The AFM images showed that the surface of GaN films was etched efficiently due to the Xe ion irradiation. The initial step-terrace structure on GaN surface was eliminated completely at a fluence of 3 × 10¹³ cm⁻². HRXRD and Raman results indicated that the Xe ion irradiation led to a homogenous lattice expansion throughout the entire ∼3 μm-thick GaN films. The lattice expansion as well as the biaxial compressive stress of the films was increasing with the increase of ion fluence. PL measurements showed that a dominant yellow luminescence band in the as-grown GaN films disappeared, but a blue and a green luminescence bands were produced after irradiation. Based on these results, the strong electronic excitation effect of 308 MeV Xe ions in GaN is discussed.     

Evidence of nanostructure formation in Ge oxide by crystallization induced by swift heavy ion irradiation

Ge oxide films were irradiated with 150 MeV Ag ions at fluences varying between 10¹² and 10¹⁴ ions/cm². The irradiation-induced changes were monitored by FT-IR spectroscopy, atomic force microscopy, X-ray diffraction and photoluminescence spectroscopy. The FT-IR spectra indicate stoichiometric changes and an increase in Ge content on irradiation. X-ray diffraction shows a crystallization of the irradiated films and presence of both Ge and GeO₂ phases. The Ge nanocrystal size, as calculated from Scherrer’s formula, was around 30 nm. The morphological changes, observed in atomic force microscopy, also indicate formation of nanostructures upon ion irradiation and a uniform growth is observed for a fluence of 1 × 10¹⁴ ions/cm².     

The morphology and structure of one-dimensional carbon-carbon composite under high-fluence ion irradiation

The temperature dependences of the ion-induced electron emission yield γ(T), the crystal structure, and the morphology of a surface layer of the one-dimensional carbon fiber composite KUP-VM (1D) under high-fluence (10¹⁸-10¹⁹ ion/cm²) irradiation with 30 keV ions at normal incidence both perpendicular and parallel to the fiber directions have been studied. The target temperature has been varied during continuous irradiation from T = −180 to 400 °C. The surface analysis has been performed by the RHEED, SEM and RBS techniques. The surface microgeometry was studied using laser goniophotometry (LGP). It has been found that ion irradiation results in a loss of anisotropy of the surface layer structure because of amorphization at room temperature or recrystallization at a temperature higher than the ion-induced annealing temperature. The fiber morphology anisotropy remains under ion irradiation.     

PL and XPS study of radiation damage created by various slow highly charged heavy ions on GaN epitaxial layers

Photoluminescence (PL) spectrum, in conjunction with X-ray photoelectron spectroscopy (XPS) is used to evaluate the surface damage of GaN layer by highly-charged Xe^q+ (18 ? q ? 30), Ar^q+ (6 ? q ? 16) and Pb^q+ (q = 25,35) ions. The intensity of PL emission of GaN layer, including near band-edge peak and yellow luminescence, decreases with increasing fluence and charge state of the incident ions. Finally the PL emission is completely quenched after irradiation to high fluences at high charge state. A new peak at 450 nm appeared in PL spectra of the specimens irradiated with Xe¹⁸⁺, Ar⁶⁺ and Ar¹¹⁺, indicating that radioactive recombination within donor-acceptor pairs (DAPs) during irradiation. After irradiation, XPS spectra show N deficient or Ga rich on GaN surface and XPS spectra of Ga3d core levels indicate spectral peak evidently shifts from a Ga-N to Ga-Ga and Ga-O bond. The relative content of Ga-N bond decreases and the content of Ga-Ga bond increases with the increase of ion fluence and ion charge state. The binding energy of Ga3d_5/2 electron corresponding to Ga-Ga bond of the irradiated GaN film is found to be smaller than that of metallic Gallium (Ga⁰), which can be attributed to irradiation damage.     

Radiation tolerance of Cu/W multilayered nanocomposites

Magnetron sputtered Cu/W multilayer samples with individual layer thicknesses from 2.5 to 50 nm were irradiated by 50 keV He⁺ ions at ion fluences from 7 × 10²⁰ to 6 × 10²¹ m⁻² at room temperature. Evolution of the interfacial structure during irradiation is monitored by X-ray diffraction and cross-sectional transmission electron microscopy. Moreover, radiation responses on the individual layer thickness and He⁺ ion irradiation fluence are revealed. The highly morphological stability of the multilayered structure suggests that the interfacial structure and grain boundary can serve as sinks for radiation-induced defects.     

Clarification of high density electronic excitation effects on the microstructural evolution in UO2

In order to understand the properties of ion tracks and the microstructural evolution under accumulation of ion tracks in UO₂, 100 MeV Zr¹⁰⁺ and 210 MeV Xe¹⁴⁺ ions irradiation examinations have been done at a tandem accelerator facility of JAEA-Tokai, and it has been observed the microstructure by means of a transmission electron microscope (TEM) and a scanning electron microscope (SEM) in CRIEPI.Comparison of the diameter of ion tracks between UO₂ and CeO₂ under irradiation with 100 MeV Zr¹⁰⁺ and 210 MeV Xe¹⁴⁺ ions at room temperature clarify that the sensitivity on high density electronic excitation of UO₂ is much less than that of CeO₂. By the cross-sectional observation of UO₂ under irradiation with 210 MeV Xe¹⁴⁺ ions at 300 °C, elliptical changes of fabricated pores that exist till ∼6 μm depth and the formation of dislocations have been observed in the ion fluence over 5 × 10¹⁴ ions/cm². The drastic changes of surface morphology and inner structure in UO₂ indicate that the overlapping of ion tracks will cause the point defects, enhance the diffusion of point defects and dislocations, and form the sub-grains at relatively low temperature.     

New separator prepared by electron beam irradiation for high voltage lithium secondary batteries

Grafted separators, for which poly(ethylene glycol) borate acrylate (PEGBA) was grafted onto polyethylene (PE) separator, were newly prepared by electron beam irradiation. The grafted separators were characterized by FT-IR, energy dispersive X-ray spectrometer (EDS). The morphological changes of the grafted separators were investigated by scanning electron microscopy (SEM). The degree of grafting was increased with irradiation doses. The ionic conductivity of the grafted separator showed the highest value of 6.24 × 10⁻⁴ S cm⁻¹ at 10 kGy. In addition, its lithium ion transference number and electrochemical stability were enhanced to 0.53 and 4.8 V, respectively owing to anion trapping effect of the grafted unit. The Li ion cells using the grafted separator showed better cycle performances than that using conventional PE separator at various C-rates and high voltage operation conditions. It is suggested that this grafted separator can be a promising candidate for high voltage operation of lithium secondary batteries.     

Light ion irradiation-induced phase transformation in the monoclinic polymorph of zirconia

Ion irradiation damage experiments were performed at ∼80 K on polycrystalline samples of monoclinic, slightly sub-stoichiometric zirconia (ZrO_1.98). Following irradiation with 150 keV Ne⁺ ions, the monoclinic phase was gradually replaced by a new phase. Transmission electron microscopy (TEM) observations in cross-sectional geometry and electron microdiffraction (μD) measurements revealed that the irradiated layer in a sample irradiated to a fluence of 5 × 10²⁰ Ne/m² is partially transformed to a higher symmetry phase of high crystallinity. This phase transformation is accompanied by reduction of the initial micron-sized, highly-twinned grain distribution, to a nano-phased grain structure. Grazing incidence X-ray diffraction (GIXRD) measurements revealed that the radiation-induced phase is a tetragonal polymorph of zirconia. This was verified by the existence of strong (1 0 1) diffraction maxima and weak (1 0 2) reflections (body-centered cell). Raman spectroscopy (RS) measurements were also performed in an attempt to corroborate GIXRD results obtained from the irradiated material. RS measurements in the confocal geometry agreed with GIXRD measurements, although RS was not as definitive as GIXRD. In addition to RS showing the existence of a band corresponding to a tetragonal structure at 262 cm⁻¹, a new mystery band appeared at 702 cm⁻¹ that increased in intensity as a function of irradiation fluence.     

Cross-section transmission electron microscopy of the ion implantation damage in annealed diamond

It has formerly been shown that low-damage levels, produced during the implantation doping of diamond as a semiconductor, anneal easily while high levels “graphitize” (above about 5.2 × 10¹⁵ ions/cm²). The difference in the defect types and their profiles, in the two cases, has never been directly observed. We have succeeded in using cross-section transmission electron microscopy to do so. The experiments were difficult because the specimens must be polished to ∼40 μm thickness, then implanted on edge and annealed, before final ion beam thinning to electron transparency. The low-damage micrographs reveal some deeply penetrating dislocations, whose existence had been predicted in earlier work.     

Angular distributions of high energy protons channeled in long (10, 10) single-wall carbon nanotubes

In this work we study the angular distributions of 1 GeV protons channeled in long (10, 10) single-wall carbon nanotubes. The nanotube length, L, is varied between 10 and 100 μm. The angular distributions of channeled protons are obtained using the numerical solution of the proton equations of motion in the transverse plane and the Monte Carlo method. The effects of proton energy loss and scattering angle dispersion caused by its collisions with the nanotube electrons are taken into account. Analysis shows that for L < 30 μm, the transverse structure of the nanotube could be deduced from the angular distribution. For L ? 40 μm, the angular distribution contains the concentric circular ridges whose number increases and the average distance between them decreases when L increases. A possible application of the obtained results for characterization of carbon nanotubes is discussed.