Superior tolerance of Ag/Ni multilayers against Kr ion irradiation: an in situ study

Monolithic Ag and Ni films and Ag/Ni multilayers with individual layer thickness of 5 and 50?nm were subjected to in situ Kr ion irradiation at room temperature to 1 displacement-per-atom (a fluence of 2?×?10¹⁴?ions/cm²). Monolithic Ag has high density of small loops (4?nm in diameter), whereas Ni has fewer but much greater loops (exceeding 20?nm). In comparison, dislocation loops, ～4?nm in diameter, were the major defects in the irradiated Ag/Ni 50?nm film, while the loops were barely observed in the Ag/Ni 5?nm film. At 0.2?dpa (0.4?×?10¹⁴?ions/cm), defect density in both monolithic Ag and Ni saturated at 1.6 and 0.2?×?10²³/m³, compared with 0.8?×?10²³/m³ in Ag/Ni 50?nm multilayer at a saturation fluence of ～1?dpa (2?×?10¹⁴?ions/cm²). Direct observations of frequent loop absorption by layer interfaces suggest that these interfaces are efficient defect sinks. Ag/Ni 5?nm multilayer showed a superior morphological stability against radiation compared to Ag/Ni 50?nm film.     

Effects of damage rate on Cu precipitation in Fe–Cu model alloys under neutron irradiation

The formation of Cu precipitates and point defect clusters was investigated in two Fe–Cu binary model alloys, Fe–0.3Cu and Fe–0.6Cu, irradiated at 573?K at three different damage rates, namely 3.8?×?10^?10, 1.5?×?10^?8 and 5?×?10^?8?dpa (displacements per atom)/s, up to about 1.6?×?10^?2?dpa. Results of positron annihilation experiments indicated that Cu precipitates were formed in these irradiations with different damage rates. The growth of Cu precipitates does not increase monotonously with increasing irradiation dose, but it rather depends on the nucleation and growth of microvoids. It is also clear that the nucleation and growth of microvoids are influenced by the irradiation dose rate.     

Secondary X-rays emitted from foils upon transmission

Relative intensities of secondary X-rays induced by an isotope source in Fe and Cu foils with different thicknesses have been measured upon transmission through a foil using a Si(Li) detector. The experi-mental results indicate that (1) the intensity of secondary X-rays was raised with the increase of the foil’s thickness, which ranged from 5×10^?6 to 1×10^?4 m; (2) the higher Z the foil material had, the more characteristic X-rays would be excited from them; and (3) the intensity of secondary X-rays was related to the activity and energy of the excitation source, as well as the way of foil’s formation. The ‘model of effective neighboring excitation’ has been suggested. The calculation of elemental Cu based on the model described earlier agrees well with experimental data.     

Transformation characteristics in thin foils of a nickel-titanium alloy

Transformation behaviour in thin foils of a Ni-12 at.% Ti alloy was investigated by means of in situ aging and electron irradiation experiments inside a high voltage electron microscope. It is shown experimentally that the mode or the morphology of precipitation and ordering reactions in the thin foils differ somewhat from that observed in the bulk material. In the thicker part of the thin foils aged in situ at 873–973 K, a periodic modulated structure is observed to consist of a periodic array of cuboidal coherent particles along the [100] crystallographic directions. The development of ordering within the solute enriched particles appears to be much slower than in the bulk specimen In the thinner part of the foil or in the near-surface regions, no precipitation or ordering occurs and so-called precipitate-free zones (PFZs) are observed. At a higher temperature of 1073 K, precipitation takes place preferentially at the foil surfaces Electron irradiation at elevated temperatures is found to disturb the formation and growth of a metastable modulated structure. and alter the distribution and the morphology of precipitate particles initially present.

The observed transformation characteristics in the thin foil can be understood in terms of the proximity of external surfaces which act as dominant sinks for point defects or solute atoms in a thin foil. Electron irradiation affects the sink efficiency of the foil surfaces as a result of the radiation-enhanced diffusion.     

Effect of dose on irradiation-induced loop density and Burgers vector in ion-irradiated ferritic/martensitic steel HT9

Samples of F/M steel HT9 were irradiated to 20?dpa at 420°C, 440°C and 470°C in a transmission electron microscope with 1?MeV Kr ions so that the microstructure evolution could be followed in situ and characterised as a function of dose. Dynamic observations of irradiation-induced defect formation and evolution were made at the different temperatures. Irradiation-induced loops were characterised in terms of their Burgers vector, size and density as a function of dose and similar observations and trends were found at the three temperatures: (i) both a/2 <111> and a <100> loops are observed; (ii) in the early stage of irradiation, the density of irradiation-induced loops increases with dose (0–4?dpa) and then decreases at higher doses (above 4?dpa), (iii) the dislocation line density shows an inverse trend to the loop density with increasing dose: in the early stages of irradiation, the pre-existing dislocation lines are lost by climb to the surfaces while at higher doses (above 4?dpa), the build-up of new dislocation networks is observed along with the loss of the radiation-induced dislocation loops to dislocation networks; (iv) at higher doses, the decrease of number of loops affects more the a/2 <111> loop population; the possible loss mechanisms of the a/2 <111> loops are discussed. Also, the ratio of a <100> to a/2 <111> loops is found to be similar to cases of bulk irradiation of the same alloy using 5?MeV Fe²⁺ ions to similar doses of 20?dpa at similar temperatures.     

Microstructural evolution and changes in mechanical property of irradiated Fe–0.6Cu alloy under uniaxial tension stress in reactor

Structural materials for commercial reactor are usually used under conditions of stress. However, the evaluation of the microstructural evolution and the changes in the mechanical property induced by the neutron irradiation in structural materials does not typically consider the effect of stress since it is difficult to carry out neutron irradiation testing under conditions of stress. In this study, a model alloy (Fe–0.6Cu) of reactor pressure vessels was irradiated by neutrons at 573?K with a dose of about 3.2?×?10²¹?neutrons/m² (E?>?0.1?MeV), corresponding to 5.2?×?10^?4?dpa (displacement per atom), with and without tension stress. The tension stress caused elastic deformation in the specimens. The size of microvoids in the irradiated sample with tension stress was larger than that in the sample without tension stress. However, the effects of stress on the formation of Cu precipitates and the changes in the mechanical property were not clear.     

Effect of simultaneous helium implantation on the microstructure evolution of Inconel X-750 superalloy during dual-beam irradiation

This study focuses on investigation into the effect of helium implantation on microstructure evolution in Inconel X-750 superalloy during dual-beam (Ni⁺/He⁺) irradiation. The 1 MeV Ni⁺ ions with the damage rate of 10^?3 dpa/s as well as 15 keV He⁺ ions using rate of 200 appm/dpa were simultaneously employed to irradiate specimens at 400 °C to different doses. Microstructure characterization has been conducted using high-resolution analytical transmission electron microscopy (TEM). The TEM results show that simultaneous helium injection has significant influence on irradiation-induced microstructural changes. The disordering of γ′ (Ni₃ (Al, Ti)) precipitates shows noticeable delay in dose level compared to mono heavy ion irradiation, which is attributed to the effect of helium on promoting the dynamic reordering process. In contrast to previous studies on single-beam ion irradiation, in which no cavities were reported even at high doses, very small (2–5 nm) cavities were detected after irradiation to 5 dpa, which proved that helium plays crucial role in cavity formation. TEM characterization also indicates that the helium implantation affects the development of dislocation loops during irradiation. Large 1/3 〈1?1?1〉 Frank loops in the size of 10–20 nm developed during irradiation at 400 °C, whereas similar big loops detected at higher irradiation temperature (500 °C) during sole ion irradiation. This implies that the effect of helium on trapping the vacancies can help to develop the interstitial Frank loops at lower irradiation temperatures.     

Mixing of Au in Si induced by secondary and high-order recoil implantation

The mixing of Au in Si induced by secondary and high-order recoil implantation was investigated using 350 keV Ar⁺ and 350 keV Kr⁺ ions to fluences from 1?×?10¹⁶ to 3?×?10¹⁶ ions/cm² at room temperature. The thickness of the Au layer evaporated on Si substrate was ～2400 Å.The ranges of the Ar and Kr ions were chosen to be lower than the thickness of the Au layer in order to avoid the ballistic mixing produced by the primary knock-on atoms. Rutherford backscattering spectrometry (RBS) experiments were carried out to study the effects induced by Ar and Kr irradiation at the interface of Au–Si system. We observed that in the case of the irradiation with Ar⁺ ions, a broadening of the Au–Si interface occurred only at the fluence of 3?×?10¹⁶ Ar⁺/cm² and it is attributed to the surface roughening induced by ion bombardment. In contrast, the RBS analysis of a sample irradiated with 2?×?10¹⁶ Kr⁺/cm² clearly showed, in addition to the broadening effect, the formation of a mixed zone of Au and Si atoms at the interface. The mixing of Au in Si atoms can be explained by the secondary and high-order recoil implantation followed by subsequent collision cascades.     

Heavy ion irradiation-induced phase transformation in polycrystalline Dy2O3

Radiation damage effects in polycrystalline pellets of the rare earth sesquioxide Dy₂O₃ irradiated with 300?keV Kr²⁺ ions were studied by combining grazing incidence X-ray diffraction (GIXRD) with transmission electron microscopy (TEM). Radiation damage was introduced using 300?keV Kr²⁺ ions to fluences up to 1?×?10²⁰?Kr?m^?2 at cryogenic temperature. GIXRD and cross-sectional TEM observations revealed that the crystal structure of the irradiated Dy₂O₃ transformed from a cubic, so-called C-type rare earth sesquioxide structure to a monoclinic, B-type rare earth sesquioxide structure upon ion irradiation. In addition, TEM and high-resolution electron microscopy (HREM) indicated that the transformed surface Dy₂O₃ layer adopts an epitaxial orientation relationship with the substrate Dy₂O₃.     

Migration behaviour of vacancies and damage structure recovery in a Fe-based Fe-Cr-Mn-Cu-Mo multi-component alloy

ABSTRACT

A Fe-based multi-component alloy, 60Fe-12Cr-10Mn-15Cu-3Mo, which presents higher yield stress than typical stainless steels (such as 304, 316, and 340), was used to investigate the thermal stability of irradiation-induced defects. Neutron irradiation was carried out at approximately 323 and 643?K using up to 1.3 × 10^?3 and 4.5 × 10^?4 dpa (displacements per atom), respectively. While no defects were accumulated at the high temperature of 643?K, single vacancies were formed after irradiation at the low temperature of 323?K to 1.3 × 10^?3 dpa, and the vacancies became mobile at 423?K. As a result, vacancy clusters were formed. However, as the annealing temperature increased the size of vacancy clusters decreased. Coincidence Doppler broadening measurements indicated that Cu precipitates were the sites of vacancy cluster formation, and the recovery of vacancy clusters became prominent while annealing the irradiated sample at temperatures higher than 423?K. Recovery of vacancy clusters at 573?K, which was not a high temperature, was also observed even in the sample that was irradiated using 2.5?MeV Fe ions at room temperature to 0.6 dpa at damage peak.     

Recrystallization of hexagonal silicon carbide after gold ion irradiation and thermal annealing

Silicon carbide (SiC) single crystals with the 6H polytype structure were irradiated with 4.0-MeV Au ions at room temperature (RT) for increasing fluences ranging from 1?×?10¹² to 2?×?10¹⁵ cm^?2, corresponding to irradiation doses from ~0.03 to 5.3 displacements per atom (dpa). The damage build-up was studied by micro-Raman spectroscopy that shows a progressive amorphization by the decrease and broadening of 6H-SiC lattice phonon peaks and the related growth of bands assigned to Si–Si and C–C homonuclear bonds. A saturation of the lattice damage fraction deduced from Raman spectra is found for ~0.8?dpa (i.e. ion fluence of 3?×?10¹⁴ cm^?2). This process is accompanied by an increase and saturation of the out-of-plane expansion (also for ~0.8?dpa), deduced from the step height at the sample surface, as measured by phase-shift interferometry. Isochronal thermal annealing experiments were then performed on partially amorphous (from 30 to 90%) and fully amorphous samples for temperatures from 200 °C up to 1500 °C under vacuum. Damage recovery and densification take place at the same annealing stage with an onset temperature of ~200 °C. Almost complete 6H polytype regrowth is found for partially amorphous samples (for doses lower than 0.8 dpa) at 1000 °C, whereas a residual damage and swelling remain for larger doses. In the latter case, these unrelaxed internal stresses give rise to an exfoliation process for higher annealing temperatures.     

Effect of swift heavy ion irradiation on dilute Fe-doped Sb0.95Se0.05 magnetic semiconductor

A thin film of dilute Fe (0.008)-doped Sb_0.95Se_0.05 alloy was grown on silicon substrate using the thermal evaporation technique. This film was irradiated with swift heavy ions (SHIs) Ag⁺¹⁵ having 200?MeV energy at ion fluences of 1?×?10¹² and 5?×?10¹² ions per cm², respectively. The thickness of the thin film was ～500?nm. We study the effect of irradiation on structural, electrical, surface morphology and magnetic properties of this film using grazing angle XRD (GAXRD), DC resistivity, atomic force microscopy (AFM) and magnetic force microscopy (MFM), respectively. GAXRD suggests that no significant change is observed in this system due to SHI irradiation. The average crystallite size increases with fluence, whereas the AFM image shows the rms roughness decreases due to irradiation with respect to the un-irradiated thin film. The MFM image shows that the magnetic interaction in irradiated film decreases due to the irradiation effect. Although the un-irradiated sample shows metal to semiconducting transition, but after irradiation with fluence of 5?×?10¹² ions per cm², the sharpness of the metal to semiconducting phase transition is observed to increase dramatically at ～300?K. This characteristic of the thin film makes it a promising candidate for an electrical switching device after irradiation.     

Studies of some physical properties of PrFe0.7Ni0.3O3 thin films after 200 MeV Ag15+ irradiation

PrFe_0.7Ni_0.3O₃ thin films (thickness ~ 200 nm) were prepared by pulsed laser ablation technique on LaAlO₃ substrate. These films were irradiated with 200?MeV Ag¹⁵⁺ ions at various fluencies, ranging from 1 × 10¹¹ to 1 × 10¹² ions/cm². These irradiated thin films were characterized by using X-ray diffraction, dc conductivity, dc magnetization and atomic force microscopy. These films exhibit orthorhombic structure and retain it even after irradiations. The crystallite size (110–137?nm), micro strain (1.48 × 10^?2–1.75 × 10^?2 line^?2?m^?4) and dislocation density (79.7 × 10¹⁴–53.2 × 10¹⁴ line/m²) vary with ion fluencies. An enhancement in resistivity at certain fluence and then a decrease in its value (0.22175–0.21813?Ω?cm) are seen. A drastic change in observed magnetism after ion irradiation is seen. With ion irradiation, an increase in surface roughness, due to the formation of hillocks and other factors, is observed. Destruction of magnetic domains after irradiation can also be visualized with magnetic force microscopy and is in close agreement with magnetization data. The impact on various physical properties in these thin films after irradiation indicates a distortion in the lattice structure and consequently on single-particle band width caused by stress-induced defects.     

Heavy-ion irradiations of Fe and Fe–Cr model alloys Part 1: Damage evolution in thin-foils at lower doses

The evolution of radiation damage in Fe and Fe–Cr alloys under heavy-ion irradiation was investigated using transmission electron microscopy. Thin foils were irradiated with 100 or 150 keV Fe⁺ and Xe⁺ ions at room temperature (RT) and 300°C. Dynamic observations followed the evolution of damage and the early stages in damage development are reported. Small (2–5 nm) dislocation loops first appeared at doses between 10¹⁶ and 10¹⁷ ions m^?2 in all materials. Loop number densities depended strongly on the foil orientation in pure Fe but not in Fe–Cr alloys. Number densities did not depend strongly on Cr content. For a given material, defect yields were higher for Xe⁺ ions than for Fe⁺ ions, and were higher at RT than at 300°C. Loops with both ?100? and ½?111? Burgers vectors were identified. The proportion of ?100? loops was larger, especially in pure Fe. Dynamic observations showed that: the contrast of some new loops developed over intervals as long as 0.2 s; hopping of ½?111? loops was induced by the ion and electron beams and was pronounced in ultra-pure iron; and many loops were lost during and after ion irradiation by glide to the foil surface. The number of loops retained was strongly dependent on the foil orientation in Fe, but less so in Fe–Cr alloys. This is due to lower loop mobility in Fe–Cr alloys, probably due to pinning by Cr atoms. Reduced loop loss probably explains the higher loop number densities in Fe–Cr alloys compared with pure Fe.     

Synthesis and characterization of p-GaSe thin films and the analyses of I–V and C–V measurements of p-GaSe/p-Si heterojunction under electron irradiation

Gallium Selenide (GaSe) thin films were grown by the electrochemical deposition (ECD) technique on Indium tin oxide (ITO) and p-Si (100) substrates. The Electron paramagnetic resonance (EPR) spectrum of GaSe thin films’ growth on ITO was recorded at room temperature. According to EPR results, the g value of an EPR signal obtained for GaSe deposited on ITO is 2.0012?±?0.0005. In/GaSe/p-Si heterojunction was irradiated with high-energy (6?MeV) and low-dose (1.53?×?10¹⁰?e^??cm^?2) electrons. The ideality factor of the In/GaSe/p-Si device was calculated as 1.24 and barrier height was determined as 0.82?eV from I–V measurements before irradiation. Acceptor concentration, built-in potential and barrier height of the In/GaSe/p-Si device were also obtained as 0.72?×?10^14?cm^?3, 0.65?eV and 0.97?eV from C–V measurements, respectively. After irradiation, the ideality factor n and barrier height Φ_b values of the In/GaSe/p-Si device were calculated as 1.55 and 0.781?eV, respectively. Acceptor concentration, the built-in potential and barrier height values of the In/GaSe/p-Si device have also shown a decrease after 6?MeV electron irradiation. This change in heterojunction device parameters shows that current transport does not obey thermionic emission, and thus tunneling could be active due to the defects formed by irradiation at the In–GaSe interface.     

Features of degradation and recovery of the optical properties of coatings based on ZnO powder modified with nanoparticles after irradiation

The effect of electron irradiation with energy of 30?keV and fluence up to 7?×?10¹⁶?cm^?2 on diffuse reflection spectra in situ of coatings based on ZnO powders unmodified and modified with zirconium dioxide and aluminum oxide nanopowders was investigated. The higher radiation stability of coatings based on modified pigments in comparison to unmodified pigments has been established. A significant recovery of the reflection spectra of irradiated coatings after exposure to residual vacuum and air was shown.     

Sol-hydrothermally derived gadolinium oxide (Gd2O3) nanorods and tamarind-like shape evolution under 80 MeV C6+ ion impact

The present work highlights swift heavy ion irradiation-induced shape evolution of gadolinium oxide (Gd₂O₃) nanorods synthesized via a sol-hydrothermal route. Upon dispersing Gd₂O₃ nanorods in the polyvinyl alcohol matrix, thin solid films were cast on borosilicate glass substrates. The films were then exposed to 80?MeV carbon-ion irradiation, while fluence was varied in the range of 1×10¹¹–3×10¹²?ions/cm². The post analyses were carried out by using X-ray diffraction, high resolution transmission electron microscopy (TEM) and Raman spectroscopy studies. An apparently observable shortening of length (L) and diameter (D) of the nanorods can be revealed through the TEM imaging analyses. Moreover, while exhibiting an aspect ratio (L/D) between 3.3 and 4.7, the nanorods were found to exist in the form of bunching at higher fluences. The irradiation-induced tamarind-like shape evolution at higher fluences was attributed to the overlapping of ion impacts on certain regions of the nanorods. The most intense Raman active peak of the pristine sample located at ～360?cm^?1 was seen to experience blue-shifting (～375?cm^?1) when irradiated at the highest fluence (～3×10¹²?ions/cm²). An altered shape evolution of a thermally and mechanically stable oxide system by the energetic ion impact would bring in new insights as regards construction of surface patterns and their potential use in miniaturized devices.     

Characterization of a LiCoO2 thin film cathode grown by pulsed laser deposition

A highly (003)-oriented pure LiCoO₂ thin film cathode, without Co₃O₄ impurities, was grown on a stainless steel substrate by pulsed laser deposition and characterized by electrochemical testing, scanning electron microscopy (SEM), ex situ X-ray diffraction (XRD), Raman and X-ray photoelectron spectroscopy (XPS). The initial reversible discharge capacity of the LiCoO₂ thin film cathode reached 52.5?μAh/cm²µm and capacity loss was about 0.18% per cycle at a current density of 12.74?μA/cm². The chemical diffusion coefficient of the Li⁺ ion was estimated to be about 4.7?×?10^?11?cm²/s from cyclic voltammetric (CV) scans. Ex situ XRD revealed that the spacing of crystalline planes expanded about 0.09?Å when charged to 4.2?V, corresponding to Li_0.5CoO₂, lower than the value for composite powder LiCoO₂ electrodes. XPS results showed that the number of low-coordinated oxygen ions increased relative to the removal of Li⁺ ions.     

Protons and carbon ions acceleration in the target-normal-sheath-acceleration regime using low-contrast fs laser and metal-graphene targets

fs pulsed lasers at an intensity of the order of 10¹⁸ W/cm², with a contrast of 10⁻⁵, were employed to irradiate thin foils to study the target-normal-sheath-acceleration (TNSA) regime. The forward ion acceleration was investigated using 1/11 µm thickness foils composed of a metallic sheet on which a thin reduced graphene oxide film with 10 nm thickness was deposited by single or both faces. The forward-accelerated ions were detected using SiC semiconductors connected in time-of-flight configuration. The use of intense and long pre-pulse generating the low contrast does not permit to accelerate protons above 1 MeV because it produces a pre-plasma destroying the foil, and the successive main laser pulse interacts with the expanding plasma and not with the overdense solid surface. Experimental results demonstrated that the maximum proton energies of about 700 keV and of 4.2 MeV carbon ions and higher were obtained under the condition of the optimal acceleration procedure. The measurements of ion energy and charge states confirm that the acceleration per charge state is measurable from the proton energy, confirming the Coulomb–Boltzmann-shifted theoretical model. However, heavy ions cannot be accelerated due to their mass and low velocity, which does not permit them to be subjected to the fast and high developed electric field driving the light-ion acceleration. The ion acceleration can be optimized based on the laser focal positioning and on the foil thickness, composition, and structure, as it will be presented and discussed.     

Irradiated rare‐earth‐doped powellite single crystal probed by confocal Raman mapping and transmission electron microscopy

The irradiation‐induced damages and structure modifications of rare earths doped powellite single crystal have been precisely studied using optical and electron microscopy techniques, including optical interferometry, confocal micro‐Raman spectroscopy and transmission electron microscopy. The surface of powellite crystal pops out anisotropically after exposing under Ar ion beam, with a saturation swelling value of 2.0% along a‐axis and 1.3% along the c‐axis of powellite at high dose. Raman mapping on focused ion‐beam sections (5 × 3 µm²) perpendicular to the irradiated surface reveals that irradiation damage induces orientation‐dependent compressive stresses in powellite. However, no significant anisotropic effect has been found on the irradiation‐induced structural disorder in powellite. At low dose (0.012 dpa), the main irradiation‐induced defects created in powellite crystal are small defect clusters. By comparison, the dominant kinds of defects in high‐dose (5.0 dpa) sample are dislocations loops and networks. Copyright © 2014 John Wiley & Sons, Ltd.