Scattering of light molecules from thin Al2O3 films

Molecular oxygen and hydrogen ions were scattered at grazing incidence from various thin Al₂O₃ films. The energy of incident particles was varied from 390 to 1000 eV. For scattered positive oxygen ions, negative ion fractions of up to 17% were recorded. For scattered positive hydrogen ions, the negative ion fractions reached up to 2%. These findings qualify thin films of Al₂O₃ as possible candidates for use as charge state conversion surfaces in neutral particle sensing instruments, which will work in space.     

XRD investigation of ion irradiated Ti3Si0.90Al0.10C2

Ti₃SiC₂ is one of the most promising materials belonging to M_n+1AX_n phases, which exhibit good damage tolerance, thermal stability and mechanical properties.Recently, in the frame of research on future gas cooled fast nuclear reactors, Ti₃SiC₂ has been considered as an innovative candidate material, which could be incorporated in some core components such as fuel cladding. At the present time, however, very few data are available concerning the behaviour of this material after irradiation. In this work, Ti₃Si_0.90Al_0.10C₂ samples were irradiated with high energy Kr and Xe ions and characterized by X-ray diffraction. Patterns were analysed in terms of change in peak intensity, peak position and width. Rietveld refinements were also performed. Increase in micro-strains and lattice parameter with irradiation dose was highlighted. The formation of β-Ti₃SiC₂, which has never been observed by experimental XRD on non irradiated material, was proposed for the highly irradiated samples. A partial recovery of the microstructure with temperature was found.     

Study on the behavior of oxygen atoms in swift heavy ion irradiated CeO2 by means of synchrotron radiation X-ray photoelectron spectroscopy

To study the effects of swift heavy ion irradiation on cerium dioxide (CeO₂), CeO₂ sintered pellets were irradiated with 200 MeV Xe ions at room temperature. For irradiated and unirradiated samples, the spectra of X-ray photoelectron spectroscopy (XPS) were measured. XPS spectra for the irradiated samples show that the valence state of Ce atoms partly changes from +4 to +3. The amount of Ce³⁺ state was quantitatively obtained as a function of ion-fluence. The relative amount of oxygen atom displacements, which are accompanied by the decrease in Ce valence state, is 3-5%. This value is too large to be explained in terms of elastic interactions between CeO₂ and 200 MeV ions. The experimental result suggests the contribution of 200 MeV Xe induced electronic excitation to the displacements of oxygen atoms.     

Ion guiding through capillaries in uncoated Al2O3 membranes

We made an experimental study on ion guiding through capillaries in uncoated Al₂O₃ membranes using a variety of ions such as O¹⁺, O³⁺, and O⁶⁺. The incident energy was varied within the range of 30-150 keV. The results were compared with others using coated PET and Al₂O₃ capillary membranes as well as with the so-called scaling law discovered by Stolterfoht and his co-workers. Good agreement of our results with the scaling law was found. However, our membranes showed extraordinarily strong guiding ability. The reason lies in that our membranes were uncoated. A slower charge drift speed along the insulating capillary wall and a much larger equilibrium charge Q_∞ seems to exist in our experiment.     

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.     

Nuclear tracks in garnets studied by means of Rutherford backscattering and X-ray diffraction

(Y, La)₃(Fe, Ga)₅O₁₂ epitaxial garnet films on (111) Gd₃Ga₅O₁₂ substrates irradiated with ²³⁸U ions of 1.4 MeV/u specific energy in the dose range 10¹⁰ cm^?2 to 3 × 10¹¹ cm^?2 were measured by means of Rutherford backscattering and double-crystal X-ray diffraction before and after thermal annealing in oxygen. The nuclear track diameter of 10 nm confining a cylindrical volume of highly disordered material caused by each ion impact has been deduced from the comparison of the backscattering spectra of the irradiated and unirradiated film areas. The fraction of randomly backscattered ions due to the irradiation-induced damage as well as the lattice expansion perpendicular to the crystal surface caused by irradiation-induced lateral compressive stress are proportional to the ion dose. After thermal annealing the comparison of the almost identical backscattering yield of the irradiated areas and the unirradiated film regions demonstrates a nearly perfect recrystallization of the damaged track volumes.     

Bulk-compositional changes of Ni2Al3 and NiAl3 during ion etching

Bulk-compositional changes of Ni₂Al₃ and NiAl₃ in a Ni-50 wt% Al alloy during ion etching have been investigated by transmission electron microscopy and energy dispersive X-ray spectroscopic analyses. After etching with 7, 5 and 3 keV Ar⁺ ions for 15, 24 and 100 h nickel contents in both Ni₂Al₃ and NiAl₃ exceeded greatly those in the initial compounds and increased with the decrement of the sputtering energy. After 100 h etching with 3 keV Ar⁺ ions the compositions of these two compounds reached a similar value, about Ni_80-83Al_12-15Fe_3-4Cr_1-2 (at%). A synergistic action of preferential sputtering, radiation-induced segregation and radiation-enhanced diffusion enables the altered-layers at the top and bottom of the film extend through the whole film. The bulk-compositional changes are proposed to occur in the unsteady-state sputtering regime of ion etching and caused by an insufficient supply of matter in a thin film.     

Swift heavy ion irradiation-induced microstructure modification of two delta-phase oxides: Sc4Zr3O12 and Lu4Zr3O12

Swift gold ions (185 MeV) were used to systematically investigate the radiation damage response of delta phase compounds Sc₄Zr₃O₁₂ and Lu₄Zr₃O₁₂ in the electronic energy loss regime. Ion irradiation-induced microstructural modifications were examined using X-ray diffraction (XRD) and transmission electron microscopy (TEM). XRD investigations indicate a phase transformation from ordered rhombohedral to disordered fluorite (O-D) in both compounds, with the Sc compound transforming at a higher ion fluence compared with the Lu compound. This result is consistent with our previous study on Sc₄Zr₃O₁₂ and Lu₄Zr₃O₁₂ under displacive radiation environment in which the nuclear energy loss is dominant. High resolution TEM revealed that individual ion tracks maintain crystalline structure, while the core region experiences an O-D phase transformation. TEM observations also suggest that for the doses in which the tracks overlap, the O-D phase transformation occurs across the entire ion range.     

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.     

Amorphisation of ZnAl2O4 spinel under heavy ion irradiation

ZnAl₂O₄ spinels have been irradiated with several ions (Ne, S, Kr and Xe) at the IRRSUD beamline of the GANIL facility, in order to determine irradiation conditions (stopping power, fluence) for amorphisation. We observed by transmission electron microscopy (TEM) that with Xe ions at 92 MeV, individual ion tracks are still crystalline, whereas an amorphisation starts below a fluence of 5 × 10¹² cm⁻² up to a total amorphisation between 1 × 10¹³ and 1 × 10¹⁴ cm⁻². The coexistence of amorphous and crystalline domains in the same pristine grain is clearly visible in the TEM images. All the crystalline domains remain close to the same orientation as the original grain. According to TEM and X-ray Diffraction (XRD) results, the stopping power threshold for amorphisation is between 9 and 12 keV nm⁻¹.     

A cubic-to-monoclinic structural transformation in the sesquioxide Dy2O3 induced by ion irradiation

Polycrystalline pellets of the sesquioxide Dy₂O₃ were irradiated at cryogenic temperature with Kr⁺⁺ ions to a fluence of 1 × 10²⁰ Kr/m². The crystal structure of the irradiated Dy₂O₃ was observed to change from a cubic, so-called C-type rare-earth sesquioxide structure to a monoclinic, B-type rare-earth sesquioxide structure upon ion irradiation. This transformation is accompanied by a decrease in molecular volume (or density increase) of approximately 9%.     

Effects of swift heavy ion irradiation on the structure of Er2O3-doped CeO2

In order to simulate the effects of burnable poison doping on the fission fragment damage of UO₂ nuclear fuels, Er₂O₃-doped CeO₂ pellets were irradiated with 200 MeV Xe¹⁴⁺ ions. The irradiation effect was measured by means of X-ray diffraction (XRD). The expansion of lattice and the disordering of atomic arrangement due to the irradiation become more remarkable with increasing the concentration of the Er₂O₃ dopant.     

A novel method for incorporating fission gas elements into solids

A novel method for the fabrication of test samples for fission gas behavior studies is described. We applied the technique of ion beam assisted deposition (IBAD) as a means to introduce Xe atoms into alumina (Al₂O₃) films. We then investigated the redistribution of Xe atoms and microstructural evolution induced by annealing. Transmission electron microscopy analysis revealed that the microstructure of our Al₂O₃-Xe IBAD films resemble characteristic microstructural features associated with fission gas accumulation in reactor-irradiated nuclear fuels.     

Radiation damage parameters in multicomponent nonmetals

Evaluations of contributions to radiation damage parameters in nonmetals are made for several neutron and gamma-ray interactions. Damage parameters for C, Al₂O₃, Si₃N₄, and MgAl₂O₄ are evaluated for neutron spectra from the EBR-II, ORR, and LPTR reactors, for a hypothetical first-wall fusion spectrum, for a 14-MeV neutron spectrum, and for a neutron spectrum from the Fusion Materials Irradiation Test Facility being built at HEDL.Included in these evaluations are calculations of recoil atom damage initiated by neutrons and gamma-rays, gas production rates, energy absorbed through electronic processes, and displacement damage initiated by repulsion between a recoil atom and atoms it ionizes (ionization-assisted displacements).Evaluations were performed using the damage program DON with either the Robinson form of the Lindhard damage energy function or with special damage energy or displacement functions generated specifically for Al₂O₃, Si₃N₄, and MgAl₂O₄ by Coulter and Parkin.     

In situ studies of ion irradiated inverse spinel compound magnesium stannate (Mg2SnO4)

Magnesium stannate spinel (Mg₂SnO₄) was synthesized through conventional solid state processing and then irradiated with 1.0 MeV Kr²⁺ ions at low temperatures 50 and 150 K. Structural evolutions during irradiation were monitored and recorded through bright field images and selected-area electron diffraction patterns using in situ transmission electron microscopy. The amorphization of Mg₂SnO₄ was achieved at an ion dose of 5 × 10¹⁹ Kr ions/m² at 50 K and 10²⁰ Kr ions/m² at 150 K, which is equivalent to an atomic displacement damage of 5.5 and 11.0 dpa, respectively. The spinel crystal structure was thermally recovered at room temperature from the amorphous phase caused by irradiation at 50 K. The calculated electronic and nuclear stopping powers suggest that the radiation damage caused by 1 MeV Kr²⁺ ions in Mg₂SnO₄ is mainly due to atomic displacement induced defect accumulation. The radiation tolerance of Mg₂SnO₄ was finally compared with normal spinel MgAl₂O₄.     

Impedance studies on high energy Li irradiated PZT thin films

The ferroelectric Pb(Zr_0.48Ti_0.52)O₃ (PZT) thin films prepared by the pulsed laser deposition technique were studied for their response to high energy lithium ion irradiation through impedance spectroscopy. The Debye peaks, observed in the impedance and modulus plots of irradiated films, shifts towards higher frequencies compared to those of unirradiated films. This is equivalent to the trend observed with increase in temperature in the unirradiated films due to the dielectric relaxation. The irradiated films showed a decrease in the grain resistance compared to the unirradiated films. The activation energy of dielectric relaxation increases from 1.25 eV of unirradiated film to 1.62 eV of irradiated film. The observed modifications in the irradiated film were ascribed to the modifications in the grain structure due to the high value of electronic energy loss.     

Damage evolution in Au-implanted Ho2Ti2O7 titanate pyrochlore

Damage evolution at room temperature in Ho₂Ti₂O₇ single crystals is studied under 1 MeV Au²⁺ ion irradiation by Rutherford backscattering spectroscopy along the 〈0 0 1〉 direction. For a better determination of ion-induced disorder profile, an iterative procedure and a Monte Carlo code (McChasy) were used to analyze ion channeling spectra. A disorder accumulation model, with contributions from the amorphous fraction and the crystalline disorder, is fit to the Ho damage accumulation data. The damage evolution behavior indicates that the relative disorder on the Ho sublattice follows a nonlinear dependence on dose and that defect-stimulated amorphization is the primary amorphization mechanism. Similar irradiation behavior previously was observed in Sm₂Ti₂O₇. A slower damage accumulation rate for Ho₂Ti₂O₇, as compared with damage evolution in Sm₂Ti₂O₇, is mainly attributed to a lower effective cross section for defect-stimulated amorphization.     

Tracks of 30-MeV C60 clusters in yttrium iron garnet studied by scanning force microscopy

Yttrium iron garnet (Y₃Fe₅O₁₂ or YIG), an amorphizable ferrimagnetic insulator, is probably the best studied material with respect to track formation and damage morphology. This paper presents first scanning force microscopy (SFM) of surface damage induced by energetic C₆₀ clusters. YIG single crystals were irradiated at normal incidence with 30-MeV C₆₀ cluster ions (kinetic energy ∼0.04 MeV/u) provided by the tandem accelerator of the Institute of Nuclear Physics in Orsay (IPNO). The SFM topographic images show nano-protrusions on the YIG surface; where each hillock is generated by one C₆₀ cluster. The role of stopping power and deposited energy density is discussed in terms of dimensional analysis of the nanostructures. Hillocks created by C₆₀ clusters are compared with those produced by monatomic ions.     

Comparative analysis of the low-energy He+ ions scattering on Al and Al2O3 surfaces

Using the Anderson–Muda–Newns approach, the neutralization rate and the ion survival probability have been calculated for the large angle scattering of low-energy He⁺ ions by Al and by Al₂O₃. The two-band model of the electronic energy spectra is applied for the case of alumina. The electron promotion has been shown to play an important role in the processes of the He⁺ ions scattering by aluminum and alumina. The experimentally observed absence of the matrix effect is discussed on the basis of the obtained results.     

Nanostructuring of BaF2 (1 1 1) surfaces by single slow highly charged ions

The creation of surface nanostructures in BaF₂ (1 1 1) surfaces was studied after irradiation with slow highly charged Xe ions from the Dresden-EBIT (electron beam ion trap). After irradiation, the crystals were investigated by scanning force microscopy (SFM). Using specific ion parameters, the topographic images show nanohillocks emerging from the surface. Additionally, we used the technique of selective chemical etching to reveal the lattice damage created by ion energy deposition below and above threshold needed for surface hillocks formation. The role of both potential and kinetic energy as well as a comparison with results for swift heavy ion irradiations of BaF₂ single crystals are presented.