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.     

Xenon-ion-induced and thermal mixing of Co/Si bilayers and their interplay

Studies on ion-irradiated transition-metal/silicon bilayers demonstrate that interface mixing and silicide phase formation depend sensitively on the ion and film parameters, including the structure of the metal/Si interface. Thin Co layers e-gun evaporated to a thickness of 50 nm on Si(1 0 0) wafers were bombarded at room temperature with 400-keV Xe⁺ ions at fluences of up to 3 × 10¹⁶ cm⁻². We used either crystalline or pre-amorphized Si wafers the latter ones prepared by 1.0-keV Ar-ion implantation. The as-deposited or Xe-ion-irradiated samples were then isochronally annealed at temperatures up to 700 °C. Changes of the bilayer structures induced by ion irradiation and/or annealing were investigated with RBS, XRD and HRTEM. The mixing rate for the Co/c-Si couples, Δσ²/Φ = 3.0(4) nm⁴, is higher than the value expected for ballistic mixing and about half the value typical for spike mixing. Mixing of pre-amorphized Si is much weaker relative to crystalline Si wafers, contrary to previous results obtained for Fe/Si bilayers. Annealing of irradiated samples produces very similar interdiffusion and phase formation patterns above 400 °C as in the non-irradiated Co/Si bilayers: the phase evolution follows the sequence Co₂Si → CoSi → CoSi₂.     

High fluence nitrogen implantation in Al/Ti multilayers

We have studied the effects of high fluence nitrogen ion implantation on the structural changes in Al/Ti multilayers, with the aim of achieving multilayered metal-nitrides. The starting structures consisted of 10 alternate sputter-deposited Al and Ti films, with a total thickness of 270 nm, on (1 0 0) Si substrates. They were implanted with 200 keV , to 1 × 10¹⁷ and 2 × 10¹⁷ at/cm², the projected range being around half-depth of the multilayers. Structural characterization was performed by Rutherford backscattering, Auger electron spectroscopy and transmission electron microscopy. It was found that ion implantation to the higher fluence induces a full intermixing of Al/Ti layers, resulting in a multilayered structure with different content of Al, Ti and N. The applied method can be interesting for preparation of graded (Al,Ti)N multilayers, with a controlled content of nitrogen and a controlled level of Al-Ti intermixing within the structures.     

Ion irradiation effects on tungsten-oxide films and charge state effect on electronic erosion

We have studied electronic- and atomic-structure modifications of polycrystalline WO₃ films (bandgap of ∼3 eV) by ion irradiation. WO₃ films were prepared by oxidation of W films on MgO substrates and of W sheets. We find disordering or amorphization, the lattice expansion of ∼1.5% and bandgap increase of 0.2 eV after 90 MeV Ni ion irradiation at ∼3 × 10¹² cm⁻². A broad peak of optical absorption appears around 1.6 μm by ion irradiation. We also find that the erosion yield by high-energy ions with the equilibrium charge exceeds 10⁴ and that the erosion yield under ion impact with non-equilibrium charge (90 MeV Ni⁺¹⁰) is ∼1/5 of that with the equilibrium charge (89 MeV Ni⁺¹⁹). Effects of depth dependence of the ion mean charge on the erosion yields are discussed. The erosion yield by low-energy ions is also presented.     

RBS study of Ti/ZnO interface

We have studied the interface stability of the Ti(overlayer)/ZnO(substrate) system. Ti thin film was grown on the Zn face of single crystal ZnO(0 0 0 1) substrate by the vacuum deposition technique. The Ti film thickness was typically 16 nm. Then the samples were annealed in air at 300 and 400 °C for 15 min, respectively. The deposition and annealing effects on the interface structure were investigated with Rutherford backscattering and channeling spectroscopy using 2 MeV He⁺ ion beam. After Ti deposition the minimum yield from the ZnO substrate increased from 2% to 7%. This suggests severe damage caused by deposition, i.e. the interface reaction between Ti and ZnO (even at room temperature). A significant amount of Zn (approximately 6.4 × 10¹⁶ atoms/cm²) moved onto the surface after post-annealing at 400 °C. Since Ti has a stronger tendency to react with O than Zn, it is expected that Ti reacts with substrate oxygen leaving behind free Zn atoms, which can easily migrate onto the surface. We discuss how the Ti/ZnO interface reaction in detail, and seek to find another good metallic contact for ZnO devices, which are attracting much attention recently for practical applications as well as scientific aspects.     

Xenon-ion irradiation of Co/Si bilayers: Effects of interface structure and ion energy

Heavy-ion irradiation of ferromagnetic thin layers changes their micromagnetic and microstructural properties, due to the production of defects, relaxation or build-up of stress, or changes of grain size. When the ion range exceeds the layer thickness, ion mixing processes take place, leading to the formation of silicide phases. The present study deals with Co(30 or 55 nm)/Si bilayers irradiated at room temperature with 100- or 200 keV Xe ions to fluences of up to 15 × 10¹⁵/cm². The Si(1 0 0) wafers were either crystalline or pre-amorphized by 1 keV Ar⁺ implantation. Rutherford backscattering spectroscopy, in-plane magneto-optical Kerr effect, and X-ray diffraction served to analyse the samples before and after irradiation. The results will be compared with those obtained for other heavy-ions for Co/Si bilayers and in similar studies on Fe/Si bilayers.     

Medium energy ion irradiation capability for studies of radiation damage effects over a wide temperature range

In this report, we present preliminary ion irradiation experiments performed using a new medium energy (up to ∼20 MeV), high temperature ion irradiation capability that we developed at Los Alamos National Laboratory. Details of ion fluence and irradiation temperature (including ion beam heating) control, measurements procedure and accuracy are described. In particular, we investigated irradiation-induced atomic intermixing in a layered structure composed of MgO and HfO₂ thin films deposited on a sapphire substrate. This multi-layered structure represents a dispersion nuclear fuel form surrogate. To simulate a nuclear reactor environment, we performed ion irradiation using 10 MeV Au ions to a fluence of 5 × 10¹⁵ cm⁻² at a substrate temperature of 1000 °C. The degree of atomic intermixing was assessed from depth profiles of Mg, Hf, and Al atoms, which were obtained using Rutherford backscattering spectrometry. We found considerable interlayer mixing for sample regions in close proximity to the sapphire substrate.     

Krypton irradiation damage in Nd-doped zirconolite and perovskite

Understanding the effect of radiation damage and noble gas accommodation in potential ceramic hosts for plutonium disposition is necessary to evaluate their long-term behaviour during geological disposal. Polycrystalline samples of Nd-doped zirconolite and Nd-doped perovskite were irradiated ex situ with 2 MeV Kr⁺ at a dose of 5 × 10¹⁵ ions cm⁻² to simulate recoil of Pu nuclei during alpha decay. The feasibility of thin section preparation of both pristine and irradiated samples by Focused Ion Beam sectioning was demonstrated. After irradiation, the Nd-doped zirconolite revealed a well defined amorphous region separated from the pristine material by a thin (40-60 nm) damaged interface. The zirconolite lattice was lost in the damaged interface, but the fluorite sublattice was retained. The Nd-doped perovskite contained a defined irradiated layer composed of an amorphous region surrounded by damaged but still crystalline layers. The structural evolution of the damaged regions is consistent with a change from orthorhombic to cubic symmetry. In addition in Nd-doped perovskite, the amorphisation dose depended on crystallographic orientation and possibly sample configuration (thin section or bulk). Electron Energy Loss Spectroscopy revealed Ti remained in the 4+ oxidation state but there was a change in Ti coordination in both Nd-doped perovskite and Nd-doped zirconolite associated with the crystalline to amorphous transition.     

Change in magnetic properties of MgB2 thin films after irradiation by 200 MeV Au ion beam

The SHI irradiation induced effects on magnetic properties of MgB₂ thin films are reported. The films having thickness 300-400 nm, prepared by hybrid physical chemical vapor deposition (HPCVD) were irradiated by 200 MeV Au ion beam (S_e ∼ 23 keV/nm) at the fluence 1 × 10¹² ion/cm². Interestingly, increase in the transition temperature T_c from 35.1 K to 36 K resulted after irradiation. Substantial enhancement of critical current density after irradiation was also observed because of the pinning provided by the defects created due to irradiation. The change in surface morphology due to irradiation is also studied.     

Structural studies of silicon oxynitride layers formed by low energy ion implantation

Silicon oxynitride (Si_xO_yN_z) layers were synthesized by implanting ¹⁶O₂⁺ and ¹⁴N₂⁺ 30 keV ions in 1:1 ratio with fluences ranging from 5 × 10¹⁶ to 1 × 10¹⁸ ions cm⁻² into single crystal silicon at room temperature. Rapid thermal annealing (RTA) of the samples was carried out at different temperatures in nitrogen ambient for 5 min. The FTIR studies show that the structures of ion-beam synthesized oxynitride layers are strongly dependent on total ion-fluence and annealing temperature. It is found that the structures formed at lower ion fluences (∼1 × 10¹⁷ ions cm⁻²) are homogenous oxygen-rich silicon oxynitride. However, at higher fluence levels (∼1 × 10¹⁸ ions cm⁻²) formation of homogenous nitrogen rich silicon oxynitride is observed due to ion-beam induced surface sputtering effects. The Micro-Raman studies on 1173 K annealed samples show formation of partially amorphous oxygen and nitrogen rich silicon oxynitride structures with crystalline silicon beneath it for lower and higher ion fluences, respectively. The Ellipsometry studies on 1173 K annealed samples show an increase in the thickness of silicon oxynitride layer with increasing ion fluence. The refractive index of the ion-beam synthesized layers is found to be in the range 1.54-1.96.     

Barrier modification of Au/n-GaAs Schottky diode by swift heavy ion irradiation

The effect of swift heavy ion (72.5 MeV ⁵⁸Ni⁶⁺) irradiation on Au/n-GaAs Schottky barrier characteristics is studied using in situ current-voltage measurements. Diode parameters are found to vary as a function of ion irradiation fluence. The Schottky barrier height (SBH) is found to be 0.55(±0.01) eV for the as deposited diode, which decreases with ion irradiation fluence. The SBH decreases to a value of 0.49(±0.01) eV at the highest ion irradiation fluence of 5 × 10¹³ ions cm⁻². The ideality factor is found to be 2.48 for unirradiated diode, and it increases with irradiation to a value of 4.63 at the highest fluence. The modification in Schottky barrier characteristics is discussed considering the energy loss mechanism of swift heavy ion at the metal-semiconductor interface.     

Ion energy dependence of interface parameters of ion beam sputter deposited W/Si interfaces

W thin films and W/Si/W tri-layer samples have been deposited on c-Si substrates in a home-made ion beam sputtering system at 1.5 × 10⁻³ Torr Ar working pressure, 10 mA grid current and at different Ar⁺ ion energies between 600 and 1200 eV. Grazing incidence X-ray reflectivity (GIXR) measurements in specular and diffused (detector scan) geometry have been carried out on the above samples. The measured GIXR spectra were fitted with theoretically simulated spectra and the different interface parameters viz., interface width, interface roughness and interface diffusion have been estimated for both Si-on-W and W-on-Si interfaces in the above samples. The variation of the above interface parameters as a function of ion energy used for W sputtering has been studied.     

Fabrication and nuclear analysis of isotopic N and N ion-implanted silicon standards

The fabrication of reliable isotopic nitrogen standards is achieved in Si through ¹⁴N and ¹⁵N ion implantation. 60 keV and ions were implanted at 400 °C up to ∼60% peak atomic concentration, yielding nitrogen-saturated silicon layers as measured using resonant nuclear reaction analysis. No isotopic effect has been observed. The nitrogen standards are validated by measurements of stability under ion irradiation. No significant desorption of nitrogen is observed either under a ⁴He⁺ ion fluence of 3.36 × 10¹⁶ cm⁻² or under a ¹H⁺ ion fluence of 8.60 × 10¹⁷ cm⁻², giving strong evidence that isotopic nitrogen standards can be achieved.     

Grazing-incidence electron microscopy of surface blisters in single- and polycrystalline tungsten formed by H, D and He irradiation

Blisters on single- and polycrystalline tungsten surfaces formed by hydrogen and helium ion irradiation were investigated by grazing-incidence electron microscopy (GIEM) with an ultra-high-voltage transmission electron microscope. It was found that the blister skin thickness formed by D⁺ irradiation of polycrystalline tungsten (PCW) was considerably larger than the calculated ion range of the implants; however, this skin thickness (or blister depth) is not related to the pre-existing grain boundaries in the PCW. Blister formation was also observed with GIEM for single crystal tungsten (SCW) irradiated with H⁺, D⁺, and He⁺. The critical ion fluence for blister formation in SCW is estimated to be ∼10²³ H⁺(D⁺)/m² for H(D) and ∼10²¹ He⁺/m² for He. The size of the blisters and their skin structure depends on the irradiating conditions. Typical skin thickness was about 50-150 nm. Based on the assumption that gas particles (H₂, D₂, and He) accumulate within the blisters during H⁺, D⁺, and He⁺ irradiation, the GIEM measurements provide a means to derive an estimate of the amount of gas so accumulated, by reproducing the observed blister shapes with finite element method (FEM) calculations. From the GIEM images and FEM calculations we have estimated the number of implanted ions being retained in the blisters, and compared these amounts with published retention measurements. A mechanism for the blister formation is proposed based on the present results.     

Effect of ion beam irradiation on magnetic and structural properties of Pt/Cr/Co multilayers

This paper discusses the effect of ion beam irradiation on the magnetic and structural properties of Pt/Cr/Co multilayers. We observe Co-Cr-Pt ternary alloy phase formation in 1 MeV N⁺ ion irradiated [Pt (2.5 nm)/Cr (0.8 nm)/Co (3.0 nm)]_×6/Si multilayers for a fluence of 1 × 10¹⁶ ions cm⁻² and beyond. The observed phase formation is accompanied by an enhancement in the average grain size, surface roughness and coercivity. Monte Carlo simulation has been performed to study ion-induced defect evolution and atomic displacements to correlate the above observed effects.     

Study of 200 MeV Ag ion induced amorphisation in nickel ferrite thin films

Thin films of nickel ferrite of thickness ∼100 and 150 nm were deposited by pulsed laser deposition. The films were irradiated with a 200 MeV Ag¹⁵⁺ beam of three fluences 1 × 10¹², 2 × 10¹² and 4 × 10¹² ions/cm². X-ray diffraction showed a decrease in the intensity of peaks indicating progressive amorphisation with increased irradiation fluence. Fourier transform infra-red and Raman spectra of pristine and irradiated films were also recorded which showed a degradation of the crystallinity of the samples after irradiation. The damage cross section of the infra-red bands was determined. It was found that the two bands at 557 and 614 cm⁻¹ did not show similar behaviour with fluence.     

Mixing of Cr and Si atoms induced by noble gas ions irradiation of Cr/Si bilayers

Cr/Si bilayers were irradiated at room temperature with 120 keV Ar, 140 keV Kr and 350 keV Xe ions to fluences ranging from 10¹⁵ to 2 × 10¹⁶ ions/cm². The thickness of Cr layer evaporated on Si substrate was about 400 Å. Rutherford backscattering spectrometry (RBS) was used to investigate the atomic mixing induced at the Cr-Si interface as function of the incident ion mass and fluence. We observed that for the samples irradiated with Ar ions, RBS yields from both Cr layer and Si substrate are the same as before the irradiation. There is no mixing of Cr and Si atoms, even at the fluence of 2 × 10¹⁶ ions/cm². For the samples irradiated with Kr ions, a slight broadening of the Cr and Si interfacial edges was produced from the fluence of 5 × 10¹⁵ ions/cm². The broadening of the Cr and Si interfacial edges is more pronounced with Xe ions particularly to the fluence of 10¹⁶ ions/cm². The interface broadening was found to depend linearly on the ion fluence and suggests that the mixing is like a diffusion controlled process. The experimental mixing rates were determined and compared with values predicted by ballistic and thermal spike models. Our experimental data were well reproduced by the thermal spikes model.     

Physical and chemical response of 145 MeV Ne ion irradiated polymethylmethacrylate (PMMA) polymer

Characterization of ion induced modifications in the physical, chemical and structural properties of polymethylmethacrylate (PMMA) polymer induced by 145 MeV Ne⁶⁺ ions has been carried out by FTIR, UV-Visible, Differential scanning calorimetry (DSC) and X-ray diffraction. Heavy ion irradiation was carried out under a vacuum of ∼10⁻⁶ torr at Variable Energy Cyclotron Centre, Kolkata, India using a low beam current (∼15 nA). Ion fluences of 10¹⁰, 10¹¹, 10¹², 10¹³ ions/cm² were used. The optical band gap (E_g), calculated from the absorption edge of the UV-Vis spectra of these films in 200-800 nm region varied from 2.167 eV to 1.512 eV for virgin and irradiated samples. In FTIR spectra appreciable changes have been observed after irradiation, indicating the molecular fragmentation, cross-linking, formation of unsaturated groups and free radicals. DSC thermograms give information about the thermal stability and type of thermal reactions (exothermic/endothermic) on the application of heat to the polymer. XRD analyses show slight shift of peak position and significant changes in peak intensity. XRD results show a decrease of ∼4.12% in crystallite size of irradiated sample at the higher fluence of 10¹² ions/cm².     

Sputtering and crystalline structure modification of bismuth thin films deposited onto silicon substrates under the impact of 20-160 keV Ar ions

The sputtering of bismuth thin films induced by 20-160 keV Ar⁺ ions has been studied using Rutherford backscattering spectrometry, scanning electron microscopy and X-ray energy dispersive and diffraction spectroscopy. These techniques revealed increasing modifications of the Bi film surfaces with increasing both ion beam energy and fluence up to their complete deterioration under irradiation conditions E = 160 keV and φ = 1.5 × 10¹⁶ cm⁻², leaving isolated islands of preferred (0 1 2) orientation on the Si substrate. The observed surface morphology and crystalline structure evolutions are likely due to a complex interplay of interaction mechanisms involving both elastic nuclear collisions and inelastic electronic ones. The measured Bi sputtering yields versus Ar⁺ ion fluence for a fixed ion energy exhibit a significant depression at very low φ-values followed by a steady state regime above ∼2.0 × 10¹⁴ cm⁻². Measured sputtering yields versus Ar⁺ ion energy with fixing ion fluence to 1.2 × 10¹⁶ cm⁻² in the upper part of the yield saturation regime are also reported. Their comparison to theoretical model and SRIM 2008 Monte Carlo simulation predictions is discussed.     

Sputtering and surface state evolution of Bi under oblique incidence of 120 keV Ar ions

The sputtering and surface state evolution of Bi/Si targets under oblique incidence of 120 keV Ar⁺ ions have been investigated over the range of incidence angles 0° ? θ_i ? 60°. Increasing erosion of irradiated samples (whose surface thickness reduced by ∼3% at normal incidence up to ∼8% at θ = 60°) and their surface smoothing with reducing grain sizing were pointed out using Rutherford backscattering (RBS), atomic force (AFM) and X-ray diffraction (XRD) techniques. Measured sputtering yield data versus θ_i with fixed ion fluence to ∼1.5 × 10¹⁵ cm⁻² are well described by Yamamura et al. semi-empirical formula and Monte Carlo (MC) simulation using the SRIM-2008 computer code. The observed increase in sputter yield versus incidence angle is closely correlated to Bi surface topography and crystalline structure changes under ion irradiation.