Swift heavy ion induced modifications of optical and microstructural properties of silver–fullerene C60 nanocomposite

In this paper, we study the optical and microstructural properties of silver–fullerene C₆₀ nanocomposite and their modifications induced by swift heavy ion irradiation. Silver nanoparticles embedded in fullerene C₆₀ matrix were synthesized by co-deposition of silver and fullerene C₆₀ by thermal evaporation. The nanocomposite thin films were irradiated by 120 MeV Ag ions at different fluences ranging from 1 × 10¹² to 3 × 10¹³ ions/cm². Optical absorption studies revealed that the surface plasmon resonance of Ag nanoparticles showed a blue shift of ～49 nm with increasing ion fluence up to 3 × 10¹³ ions/cm². Transmission electron microscopy and Rutherford backscattering spectroscopy were used to quantify particle size and metal atomic fraction in the nanocomposite film. Growth of Ag nanoparticles was observed with increasing ion fluence. Raman spectroscopy was used to understand the effect of heavy ion irradiation on fullerene matrix. The blue shift in plasmonic wavelength is explained by the transformation of fullerene C₆₀ matrix into amorphous carbon.     

Angular and lateral spreading of ion beams in biomedical nuclear microscopy

Nuclear scattering from target atoms gives rise to a spatial broadening of energetic ion beams penetrating matter. The spatial broadening of the ion beam presents an ultimate limit to the resolving power that can be achieved in nuclear microscopy methods. The pressing of the attainable resolution limit in biomedical nuclear microscopy to dimensions approaching 10 nm, or so, implies the fundamental limitation from ion-target scattering will become increasingly significant. This effect has been investigated by a combined analytical and numerical computational approach to determine the extent and how single and multiple scattering processes limit the resolution for analysis with 2 MeV ⁴He and ¹H ions of realistic biomedical samples. The cases studied were direct-Scanning Transmission Ion Microscopy (direct-STIM), Particle Induced X-ray Emission (PIXE) studies of 20 μm tissue sections and in vivo single-ion irradiation of cells.     

Ion beam mixing in uranium nitride thin films studied by Rutherford Backscattering Spectroscopy

Thickness, composition, concentration depth profile and ion irradiation effects on uranium nitride thin films deposited on fused silica have been investigated by Rutherford Backscattering Spectroscopy (RBS) using 2 MeV He⁺ ions. The films were prepared by reactive DC sputtering at the temperatures of ?200 °C, +25 °C and +300 °C. A perfect 1U:1N stoichiometry with a layer thickness of 660 nm was found for the film deposited at ?200 °C. An increase of the deposition temperature led to an enhancement of surface oxidation and an increase of the thickness of the mixed U–N–Si–O layers at the interface. The sample irradiation by 1 MeV Ar⁺ ion beam with ion fluence of about 1.2–1.7 × 10¹⁶ ions/cm² caused a large change in the layer composition and a large increase of the total film thickness for the films deposited at ?200 °C and at +25 °C, but almost no change in the film thickness was detected for the film deposited at +300 °C. An enhanced mixing effect for this film was obtained after further irradiation with ion fluence of 2.3 × 10¹⁶ ions/cm².     

Evaluation of soft error rates using nuclear probes in bulk and SOI SRAMs with a technology node of 90 nm

The difference of soft error rates (SERs) in conventional bulk Si and silicon-on-insulator (SOI) static random access memories (SRAMs) with a technology node of 90 nm has been investigated by helium ion probes with energies ranging from 0.8 to 6.0 MeV and a dose of 75 ions/μm². The SERs in the SOI SRAM were also investigated by oxygen ion probes with energies ranging from 9.0 to 18.0 MeV and doses of 0.14–0.76 ions/μm². The soft error in the bulk and SOI SRAMs occurred by helium ion irradiation with energies at and above 1.95 and 2.10 MeV, respectively. The SER in the bulk SRAM saturated with ion energies at and above 2.5 MeV. The SER in the SOI SRAM became the highest by helium ion irradiation at 2.5 MeV and drastically decreased with increasing the ion energies above 2.5 MeV, in which helium ions at this energy range generated the maximum amount of excess charge carriers in a SOI body. The soft errors occurred by helium ions were induced by a floating body effect due to generated excess charge carriers in the channel regions. The soft error occurred by oxygen ion irradiation with energies at and above 10.5 MeV in the SOI SRAM. The SER in the SOI SRAM gradually increased with energies from 10.5 to 13.5 MeV and saturated at 18 MeV, in which the amount of charge carriers induced by oxygen ions in this energy range gradually increased. The computer calculation indicated that the oxygen ions with energies above 13.0 MeV generated more excess charge carriers than the critical charge of the 90 nm node SOI SRAM with the designed over-layer thickness. The soft errors, occurred by oxygen ions with energies at and below 12.5 MeV, were induced by a floating body effect due to the generated excess charge carriers in the channel regions and those with energies at and above 13.0 MeV were induced by both the floating body effect and generated excess carriers. The difference of the threshold energy of the oxygen ions between the experiment and the computer calculation might be due to the difference between the designed and real structures.     

Ion implantation into aluminum and copper by a beam of carbon nanoparticles from regenerative sooting discharges

We present a new technique to generate light carbon nanoparticles from regenerative sooting discharges and its use for ion implantation on aluminum and copper surfaces at an energy of 40 keV. Films formed at fluences up to 3 × 10¹⁵ C⁺/cm² for aluminum and 10¹⁶ C⁺/cm² for copper are studied using Raman spectroscopy, X-ray diffraction and atomic force microscopy. Raman spectroscopy reveals the existence of graphite and diamond like structures in all samples. Precipitates of Al₄C₃ of rhombohedral and hexagonal types were found in the nanometer ranges from the X-ray diffraction pattern for aluminum samples and the probable formation of body-centered cubic diamond and hexagonal carbon in copper samples. The average grain sizes of Al₄C₃ were calculated ～40 nm for Al and ～35 nm for Cu. Mass spectra from a graphite hollow cathode duoplasmatron ion source are also presented. Atomic force microscopy images of a Cu sample also support the existence of 46 nm structures. Light carbon nanoparticles are readily available from the ion source in which a special carbonaceous environment creates regenerative soot. Support gas Ar produces more C₃ than Ne.     

Development of a TOF-ERDA measurement system for analysis of light elements using a He beam

A time-of-flight ERDA (TOF-ERDA) measurement system has been developed for the analysis of light elements. He ions are used for the incident beam, and recoil light ions are detected with the system. The system consists of a time detector and a silicon detector, and energy and velocity of recoil ion are measured simultaneously. The depth resolution of 21.6 ± 2.2 nm (FWHM) has been obtained by an ERDA measurement of a thin carbon layer onto a silicon wafer using a 5.7 MeV He beam. The mass resolution is better than 1 for elements up to oxygen. Maximum detectable depth of carbon in a PET film is about 650 nm. An ERDA measurement of implanted carbon in a silicon wafer has been demonstrated.     

Developments in micro-sample 14C AMS at the ANTARES AMS facility

We continue development of micro-sample radiocarbon sample preparation and AMS measurement at the ANTARES AMS facility. We routinely prepare samples containing 10–200 μg of carbon using an iron catalyst with an excess of hydrogen in ～2.5 mL graphitisation reactors. These use a tube furnace to heat the catalyst to 600 °C and a Peltier-cooled water trap. Samples containing just a few micrograms of carbon can be prepared. We describe progress with a 0.5 mL laser-heated ‘microfurnace’ we are developing for the rapid and efficient graphitisation of ～5 μg samples. Following operating experience with a prototype unit, work has commenced on the development of a second-generation device with the goal of fully automated operation with minimal introduction of extraneous carbon.Key to development of micro-sample ¹⁴C AMS is the ability to reliably handle the graphite/iron sample and to mount it in the ion source target holder. We have developed a target holder that permits the sample to be loaded in a 1 mm diameter recess and rear pressed, ensuring a high quality surface finish, at a reproducible depth. Additionally we have developed a method for systematically aligning the sample stage with the cesium beam following ion source servicing.     

Mapping of ion beam induced current changes in FinFETs

We report on progress in ion placement into silicon devices with scanning probe alignment. The device is imaged with a scanning force microscope (SFM) and an aligned argon beam (20 keV, 36 keV) is scanned over the transistor surface. Holes in the lever of the SFM tip collimate the argon beam to sizes of 1.6 μm and 100 nm in diameter. Ion impacts upset the channel current due to formation of positive charges in the oxide areas. The induced changes in the source–drain current are recorded in dependence of the ion beam position with respect to the FinFET. Maps of local areas responding to the ion beam are obtained.     

Controlling the microstructure of ZnO nanoparticles embedded in Sapphire by Zn ion implantation and subsequent annealing

(0 0 0 1) α-Al₂O₃ single crystals (sapphire) were implanted with Zn ions of 60 keV at a fluence of 1 × 10¹⁷ ions/cm². Transmission electron microscopy and optical absorption spectroscopy studies show the formation of ZnO nanoparticles in the sapphire substrate after the implanted sample was annealed at 700 °C in oxygen ambient. The photoluminescence spectrum of the annealed sample indicates the formation of ZnO nanoparticles with perfect lattice structure. The selected-area electron diffraction pattern proves that the ZnO nanoparticles have the (0 0 0 2) orientation which follows the orientation of Al₂O₃ substrate. The result shows that the crystallographic orientation of nanoparticles obtained through ion implantation is defined by the substrate.     

Radiation tolerance of fluorite-structured oxides subjected to swift heavy ion irradiation

Fluorite-structured materials are known to exhibit an excellent structural stability under irradiation. The radiation stability of urania and yttria-stabilised cubic zirconia single crystals submitted to intense electronic excitations induced by 944-MeV Pb⁵³⁺ ions was investigated. Various analytical tools (TEM, AFM, RBS/C, XRD) were employed to examine the modifications induced at the surface and in the crystal bulk. At low fluence irradiation leads to the formation of localised ion tracks whose centre is hollowed in the surface region over a depth of ～100 nm and to the formation of nanometer-sized hillocks. Both features are interpreted as resulting from an ejection of matter in the wake of the projectile. Track overlapping at high fluence results in the formation of micrometer-sized domains (～50 nm) in the crystal bulk characterised by a slight disorientation (～0.2°) with respect to the main crystallographic orientation of the crystal.     

Study and optimization of boronization in Alcator C-Mod using the Surface Science Station (S3)

A Surface Science Station (S³) on the Alcator C-Mod tokamak is used to study and optimize the location and rate of boron film deposition in situ during electron cyclotron (EC) discharge plasmas using 2.45 GHz radio-frequency (RF) heating and a mixture of helium and diborane (B₂D₆) gasses. The radial profile of boron deposition is measured with a pair of quartz microbalances (QMB) on S³, the faces of which can be rotated 360° including orientations parallel and perpendicular to the toroidal magnetic field B_T ～0.1 T. The plasma electron density is measured with a Langmuir probe, also on S³ in the vicinity of the QMBs, and typical values are ～1 × 10¹⁶ m^?3. A maximum boron deposition rate of 0.82 μg/cm²/min is obtained, which corresponds to 3.5 nm/min if the film density is that of solid boron. These deposition rates are sufficient for boron film applications between tokamak discharges. However the deposition does not peak at the EC resonance as previously assumed. Rather, deposition peaks near the upper hybrid (UH) resonance, ～5 cm outboard of the EC resonance. This has implications for RF absorption, with the RF waves being no longer damped on the electrons at the EC resonance. The previously inferred radial locations of critical erosion zones in Alcator C-Mod also need to be re-evaluated. The boron deposition profile versus major radius follows the ion flux/density profile, implying that the boron deposition is primarily ionic. The application of a vertical magnetic field (B_V ～0.01 T) was found to narrow the plasma density and boron deposition profiles near the UH resonance, thus better localizing the deposition. A Monte Carlo simulation is developed to model the boron deposition on the different QMB/tokamak surfaces. The model requires a relatively high boron ion gyroradius of ～5 mm, indicating a B⁺¹ ion temperature of ～2 eV, to match the deposition on QMB surfaces with different orientation to B_T. Additionally, the boron ion trajectories become de-magnetized at high neutral gas throughput (～0.5 Pa m³ s^?1) and pressure (～2 Pa) when the largest absolute deposition rates are measured, resulting in deposition patterns, which are independent of surface orientation to B_T in optimized conditions.     

Design and analysis of the IFMIF–EVEDA beam dump cooling system

The IFMIF–EVEDA beam dump is designed to stop a 9 MeV, 125 mA continuous wave deuteron beam that deposits along its surface a total of 1.125 MW. The beam dump design is based on a 2.5 m long copper cone whose inner surface absorbs the beam. This piece is cooled by water flowing at high velocity through the annular channel formed between it and a second piece (shroud) made of four truncated cones of slightly different slopes.In this paper the beam dump cooling system will be briefly described, and the relevant 1D and 3D results will be presented paying especial attention to the computational fluid dynamics results.     

Imaging of single cells and tissue using MeV ions

With the attainment of sub-100 nm high energy (MeV) ion beams, comes the opportunity to image cells and tissue at nano-dimensions. The advantage of MeV ion imaging is that the ions will penetrate whole cells, or relatively thick tissue sections, without any significant loss of resolution. In this paper, we demonstrate that whole cells (cultured N2A neuroblastoma cells ATCC) and tissue sections (rabbit pancreas tissue) can be imaged at sub-100 nm resolutions using scanning transmission ion microscopy (STIM), and that sub-cellular structural details can be identified. In addition to STIM imaging we have also demonstrated for the first time, that sub-cellular proton induced fluorescence imaging (on cultured N2A neuroblastoma cells ATCC) can also be carried out at resolutions of 200 nm, compared with 300–400 nm resolutions achieved by conventional optical fluorescence imaging. The combination of both techniques offers a potentially powerful tool in the quest for elucidating cell function, particularly when it should be possible in the near future to image down to sub-50 nm.     

Point defects induced in ion irradiated 4H–SiC probed by exciton lines

The defects produced in 4H–SiC epitaxial layers by irradiation with a 200 keV H⁺ ion beam in the fluence range 6.5 × 10¹¹–1.8 × 10¹³ ions/cm² are investigated by Low Temperature Photoluminescence (LTPL–40 K).The defects produced by ion beam irradiation induce the formation of some sharp lines called “alphabet lines” in the photoluminescence spectra in the 425–443 nm range, due to the recombination of excitons at structural defects.From the LTPL lines intensity trend, as function of proton fluence, it is possible to single out two groups of peaks: the P₁ lines (e, f, g) and the P₂ lines (a, b, c, d) that exhibit different trends with the ion fluence. The P₁ group normalized yield increases with ion fluence, reaches a maximum at 2.5 × 10¹² ions/cm² and then decreases. The P₂ group normalized yield, instead, exhibits a formation threshold at low fluence, then increases until a maximum value at a fluence of 3.5 × 10¹² ions/cm² and decreases at higher fluence, reaching a value of 50% of the maximum yield.The behaviour of P₁ and P₂ lines, with ion fluence, indicates a production of point defects at low fluence, followed by a subsequent local rearrangement creating complex defects at high fluence.     

Feasibility of a multi-purpose demonstration neutron source based on a compact superconducting spherical tokamak

Tokamak neutron sources would allow near term applications of fusion such as fusion–fission hybrid reactors, elimination of nuclear wastes, production of radio-isotopes for nuclear medicine, material testing and tritium production. The generation of neutrons with fusion plasmas does not require energetic efficiency; thus, nowadays tokamak technologies would be sufficient for such purposes. This paper presents some key technical details of a compact (～1.8 m³ of plasma) superconducting spherical tokamak neutron source (STNS), which aims to demonstrate the capabilities of such a device for the different possible applications already mentioned. The T-11 transport model was implemented in ASTRA for 1.5 D simulations of heat and particle transport in the STNS core plasma. According to the model predictions, total neutron production rates of the order of ～10¹⁵ s^?1 and ～10¹³ s^?1 can be achieved with deuterium/tritium and deuterium/deuterium respectively, with 9 MW of heating power, 1.4 T of toroidal magnetic field and 1.5 MA of plasma current. Engineering estimates indicate that such scenario could be maintained during ～20 s and repeated every ～5 min. The viability of most of tokamak neutron source applications could be demonstrated with a few of these cycles and around ～100 cycles would be required in the worst cases.     

Study of modifications in Lexan polycarbonate induced by swift O6+ ion irradiation

Swift Heavy Ion (SHI) irradiation of the polymeric materials modifies their physico-chemical properties. Lexan polycarbonate films were irradiated with 95 MeV oxygen ions to the fluences of 10¹⁰, 10¹¹, 10¹², 10¹³ and 2 × 10¹³ ions/cm². Characterization of optical, chemical, electrical and structural modifications were carried out by UV–Vis spectroscopy, FTIR spectroscopy, Dielectric measurements and X-ray Diffraction. A shift in the optical absorption edge towards the red end of the spectrum was observed with the increase in ion fluence. 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 4.12 eV to 2.34 eV for virgin and irradiated samples. The cluster size varied in a range of 69–215 carbon atoms per cluster. In FTIR spectra, appreciable modification in terms of breaking of the cleavaged C–O bond of carbonate and formation of phenolic O–H bond was observed on irradiation. A rapidly decreasing trend in dielectric constant is observed at lower frequencies. The dielectric constant increases with fluence. It is observed that the loss factor increases moderately with fluence and it may be due to scissoring of polymer chains, resulting in an increase in free radicals. A sharp increase in A.C. conductivity in pristine as well as in irradiated samples is observed with frequency and is attributed to scissoring of polymer chains. XRD analyses show significant change in crystallinity with fluence. A decrease of ～9.02% in crystallite size of irradiated sample at the fluence of 2 × 10¹³ ions/cm² is observed.     

Ion beam shaping of Au nanoparticles prepared by micellar technique

Irradiation-induced burrowing and ion-induced shaping effects of Au nanoparticles are investigated. Hexagonally arranged Au nanoparticles prepared by micellar technique with diameter ～10 nm and inter-particle distance of about 80 nm were sequentially irradiated with 200 keV Ar⁺ ions to fluences of 5×10¹⁵ ions/cm². Irradiation with Argon ions causes sinking of the Au nanoparticles into the subjacent SiO₂ layer due to capillary driving forces related to specific wetting conditions while the spherical shape is conserved. Subsequent irradiation with 54 MeV Ag⁸⁺ swift heavy ions of these spherical Au nanoparticles confined within a silica matrix shapes them into prolate nanorods and nanowires whose principal axes are aligned along the beam direction. Above a threshold fluence two deformation regimes have been observed. For relatively low fluences Au nanoparticles elongate into nanorods depending on their volume. For high fluences, the formation of nanowires is observed provided that the inter-particle distance is short enough to allow for an efficient mass transport through the silica matrix.     

Effect of ion-irradiation on the microstructure and microhardness of the W-2Y2O3 composite materials fabricated by sintering and hot forging

A W-2Y₂O₃ material was developed in collaboration with the Plansee Company (Austria). An ingot of the material having approximate dimension of 95 mm × 20 mm was fabricated by mixing the elemental powders followed by pressing, sintering and hot forging. The microstructure of the W-2Y₂O₃ composite was investigated using transmission electron microscopy (TEM). The microhardness was studied using nano-indentation technique. We observed that the W-grains having a mean size of about 1 μm already formed and these grains contain very low density of dislocations. The size of the yttria particles was between 300 nm and 1 μm and the Berkovich hardness was about 4.8 GPa. The specimens were irradiated/implanted with Fe and He ions at JANNuS facility located at Orsay/Saclay, France. The TEM disks kept were irradiated/implanted at 300 and 700 °C using Fe and He ions with an energy of 24 and 2 MeV, respectively. The calculated radiation dose was about 5 dpa produced by Fe ions and total He content is 75 appm at both 300 and 700 °C. From the TEM investigation of irradiated samples, few radiation loops are present on the W grains, whereas on yttria particles, the radiation induced damages appear as voids. Berkovich hardness of the irradiated sample is higher than that of the non-irradiated sample. Results on the microstructure and microhardness of the ion-irradiated W-2Y₂O₃ composites are presented in detail.     

Nanoparticle architecture in carbonaceous matrix upon swift heavy ion irradiation of polymer–metal nanocomposites

Distinct nanoparticle self-organization in the nanocomposites (∼100 nm) of Teflon AF containing different metallic clusters is reported upon swift heavy ion irradiation of 120 MeV Au beams at different ion fluences ranging from 1 × 10¹¹ to 3 × 10¹² ions/cm². Two dimensionally distributed Au clusters are found to be transformed into long cluster chains of seemingly helical pattern in the organic matrix like pearls on a string. Comparatively diluted three dimensionally arranged Ag nanoparticles are observed to be concentrated in the formed mesh of carbon-enriched nanoregions upon irradiation. The nanoparticle self-organization in such carbonaceous nanowires (diameter ∼ 25 nm) finally leads to a quasi-one-dimensional distribution at the highest fluence with several particles apparently being aligned. It appears most probable that a high Au cluster concentration in the polymer matrix leads to direct ion–cluster interaction. This probably initiates irradiation-enhanced and thermally assisted diffusion of the clusters coupled with intermixing in the polymer layers. Moving clusters are assumed to be trapped in the ion beam induced additional free volume leading to a long string of helical-type nanoscale configuration. On the other hand, with diluted clusters arrangement, irradiation induced electronically excited inter-cluster organic regions are interpreted to act as trapping centres for the nanoparticles that self-organize along the ion damaged zones. Transmission electron microscopic investigations have been applied to analyse the irradiated and pristine nanocomposites.     

Er+ medium energy ion implantation into lithium niobate

Erbium-doped lithium niobate (Er:LiNbO₃) is a prospective photonics component, operating at 1.5 μm, which could find its use chiefly as an optical amplifier or waveguide laser. In this study, we have focused on the properties of the optically active Er:LiNbO₃ layers, which are fabricated by medium energy ion implantation under various experimental conditions. Erbium ions were implanted at energies of 330 and 500 keV with fluences of 1.0 × 10¹⁵, 2.5 × 10¹⁵ and 1.0 × 10¹⁶ cm^?2 into LiNbO₃ single-crystalline cuts of various orientations. The as-implanted samples were annealed in air at 350 °C for 5 h. The depth distribution and diffusion profiles of the implanted Er were measured by Rutherford Backscattering Spectroscopy (RBS) using 2 MeV He⁺ ions. The projected range R_P and projected range straggling ΔR_P were calculated employing the SRIM code. The damage distribution and structural changes were described using the RBS/channelling method. Changes of the lithium concentration depth distribution were studied by Neutron Depth Profiling (NDP). The photoluminescence spectra of the samples were measured to determine whether the emission was in the desired region of 1.5 μm. The obtained data made it possible to reveal the relations between the structural changes of erbium-implanted lithium niobate and its luminescence properties important for photonics applications.