Ion bombardment induced surface electrical degradation monitoring by means of luminescence in aluminas

Oxide ceramics for use as electrical insulators in future fusion devices, will be exposed to ionization and displacement damage (neutrons, gammas, ion bombardment). Enhanced oxygen loss due to ion bombardment increases surface electrical conductivity, and at the same time the surface emits light due to ion beam induced luminescence (IBIL). Results for 3 types of α-alumina and sapphire measuring electrical surface conductivity and IBIL as a function of dose at different temperatures between 20 and 200 °C, show a clear correlation between luminescence and surface electrical degradation. This indicates the potential to remotely monitor insulating material degradation not only in ITER and beyond, but also in the more immediate in-reactor experiments required for materials testing. Partial reduction of degradation by heating in air suggests the possibility for in situ recovery of the insulating properties.     

Recovery of fused silica surface damage resistance by ion beam etching

An increase of photoluminescence induced by laser irradiation in vacuum was observed for the fused silica. The degradation of transmittance and damage resistance performance of fused silica surfaces may be due to substoichiometric silica and a sufficient defect population introduced in the near surface. When the laser-irradiated surface layers were removed by ion beam etching, the laser-induced damage threshold recovered to that of un-irradiated samples. The photoluminescence also decreased after ion beam etching. According to the calculated etching depth, the laser-induced defects formed in the surface layer of 10-20 nm when different parameters used during vacuum exposure. In addition, the evolution of surface root-mean-square microroughness as a function of ion beam etching time was studied by the optical interferometric technique and atomic force microscopy.     

Ionoluminescence decay measured with single ions

A new ion beam analysis-based, single ion technique called the time to first photon has been developed to measure the decay of the luminescence signal of phosphors. Such measurements are currently needed to study luminescence decay mechanisms following high-density excitations and to identify strongly luminescent phosphor coatings with short lifetimes for ion photon emission microscopy (IPEM). The samples for this technique consist of thin phosphor layers placed or coated on the surface of PIN diodes. Single ions from an accelerator strike this sample and simultaneously create ion beam induced luminescence (IBIL) from the phosphor that is measured by a single-photon-detector, and an ion beam induced charge collection (IBICC) signal in the PIN diode. In this case, the IBICC signal provides the start pulse and the IBIL signal the stop pulse to a time to amplitude converter. It is straightforward to show that this approach also measures a signal proportional to activity versus time with an accuracy of 5% as long as the number of detected photons per ion is less than 0.1, which usually requires the use of absorbers for the IBIL detector or electronic discrimination for the IBIL signals. Details of the new analysis are given together with examples of luminescence decay measurements of several ceramic phosphors being considered to coat IPEM samples. IPEM is currently being developed at Sandia National Laboratory (SNL), the University of North Texas in Denton, and the Universities and INFN of Padova and Torino.     

An inelastic thermal spike model to calculate ion induced desorption yields

Ion induced desorption is a severe luminosity limitation for low charge state heavy ion accelerators. Therefore, it was intensively investigated in dedicated experiments during recent years. Several experimental results were obtained providing numerous desorption yields for different ion beam parameters and different materials as well as surface treatments. The heavy ion induced desorption was identified as a pure surface cleaning effect. Nevertheless it was shown that the yields have a strong link to the irradiated material. The initial desorption yield decreases during the irradiation reaching a dynamic equilibrium. Desorption yields of several hundred molecules per incident ion from one monolayer adsorbed gas can not be explained with the geometrical cross section of the projectile. Therefore we have expanded the inelastic thermal spike model to describe the process as thermal desorption from a microscopic heated region. The obtained results of this extended model represent very well the numbers from many experimental studies.     

Ion beam induced luminescence of polyethylene terephthalate foils under MeV H and He ion bombardment

The evolution of the ion beam induced luminescence (IBIL) of the polyethylene terephthalate (PET) foils was studied under the irradiation of H and He ions of MeV energy. The optical and chemical changes of the samples were also examined by photo-stimulated luminescence and optical absorption measurements after the irradiation. A prominent broad emission peak of IBIL appeared at around 380 nm, and its intensity monotonically decreased during the ion irradiation. The decay curves of the emission intensity were quantitatively explained as a function of the electronic energy deposition of the incident H and He ions. On the contrary, to the decrease of the main emission peak, a growth of new peaks was observed in the wavelengths between 500 and 600 nm.     

The electrical conductivity of carbon nanotube sheets by ion beam irradiation

A method for improving the electrical conductivity of carbon nanotube (CNT) sheets by ion beam irradiation is reported. CNT sheets prepared by a vacuum filtration method were irradiated by Ar and H ion beams at different temperatures. The electrical conductivity of the irradiated CNT sheets at a temperature of 800 K can be improved. The conductivity improvement can be ascribed to the formation of covalent bond crosslinks between CNTs induced by the ion beam irradiation at the elevated temperature.     

Roughening of silicon (1 0 0) surface during low energy Cs ion bombardment

Nowadays, the use of low energy ion bombardment in secondary ion mass spectrometry (SIMS) is a mandatory step to obtain high depth resolution for the characterization of ultra shallow junctions. However, increment of roughness during ion bombardment leads to the degradation of depth resolution. The evolution of surface roughening and ripple formation on silicon at ambient temperature under 1 keV Cs⁺ ion bombardment with and without sample rotation has been studied by means of atomic force microscopy.Ripple formation with a perpendicular orientation with respect to the Cs⁺ beam direction has been detected, and their wavelength and correlation length have been monitored as a function of the experimental conditions. Roughness and wavelength increased with increasing ion fluence, while variations of ion flux showed little effect. The effect of sample rotation during ion bombardment led to a critical reduction of the surface roughness and disappearance of ripples.     

Radiation hardness of polysiloxane scintillators analyzed by ion beam induced luminescence

The radiation hardness of polysiloxane based scintillators has been measured by ion beam induced luminescence (IBIL). The light intensity as a function of the irradiation fluence with an He⁺ beam at 1.8 MeV (1.0 μA/cm²) has been measured on undoped polymers synthesized with different amounts of phenyl units and on polysiloxanes doped with two different dye molecules (BBOT and Lumogen Violet) sensitizing the scintillation yield.     

Aperture edge scattering in focused MeV ion beam lithography and nuclear microscopy: An application for the GEANT4 toolkit

Collimators are widely used to define MeV ion beams. Recent studies have shown the capability of combinations of collimators and lenses to define beams of MeV ions with sub-100 nanometre dimensions. Such nanometre beams have potential applications in MeV ion beam lithography, which is the only maskless technique capable of producing extremely high aspect ratio micro- and nano-structrures, as well as in high resolution MeV ion beam based imaging. The ion scattering from the collimator-edges can be a resolution restricting factor in these applications. Scattering processes at edges are difficult to study using conventional simulation codes because of the complicated geometry. In this work we overview the possibilities and pitfalls in using the GEANT4 toolkit as a simulation tool for studying the behaviour of ions impinging onto, or in close proximity to aperture edges. Results from simulations of scattering of 2 MeV protons incident on a 5 mm in diameter cylindrical beam defining tungsten carbide (WC) aperture blade, such as used in nuclear micro- and nanobeams as object and scraper apertures, are presented. The bubble formation at the aperture edges due to the implantation of H was first believed to cause edge roughening and hence the beam quality degradation. The concentration profile of implanted H in a WC cylinder shows that the bubble formation is not likely to be the edge roughening factor, but rather other mechanisms of beam induced topographical changes such as ion beam induced morphological changes and cracking of hydrocarbons.     

Photoluminescence and photoluminescence excitation studies in 80 MeV Ni ion irradiated MOCVD grown GaN

We report damage creation and annihilation under energetic ion bombardment at a fixed fluence. MOCVD grown GaN thin films were irradiated with 80 MeV Ni ions at a fluence of 1 × 10¹³ ions/cm². Irradiated GaN thin films were subjected to rapid thermal annealing for 60 s in nitrogen atmosphere to anneal out the defects. The effects of defects on luminescence were explored with photoluminescence measurements. Room temperature photoluminescence spectra from pristine sample revealed presence of band to band transition besides unwanted yellow luminescence. Irradiated GaN does not show any band to band transition but there is a strong peak at 450 nm which is attributed to ion induced defect blue luminescence. However, irradiated and subsequently annealed samples show improved band to band transitions and a significant decrease in yellow luminescence intensity due to annihilation of defects which were created during irradiation. Irradiation induced effects on yellow and blue emissions are discussed.     

On the understanding of positive and negative ionization processes during ToF-SIMS depth profiling by co-sputtering with cesium and xenon

In this paper, ionization processes of secondary ions during ToF-SIMS dual beam depth profiling were studied by co-sputtering with 500 eV cesium and xenon ions and analyzing with 25 keV Ga⁺ ions. The Cs/Xe technique consists in diluting the cesium sputtering/etching beam with xenon ions to control the cesium surface concentration during ToF-SIMS dual beam depth profiling. Several depth profiles of a H-terminated silicon wafer were performed with varying Cs beam concentration and the steady state Si, Xe and Cs surface concentrations were measured in situ by Auger electron spectroscopy. It was found that the implanted Cs surface concentration increases with the Cs fraction in the beam from 0% for the pure Xe beam to a maximum Cs surface concentration for the pure Cs beam. Secondly, the variation of the silicon work function, due to the Cs implantation, was measured in situ and during depth profiling as the shift of the secondary ion kinetic energy distributions. Finally, the positive and negative elemental ion yields generated by the Ga analysis beam were recorded and modeled with respect to varying Cs/Xe mixture. We found that the Si⁻ and the Cs⁻ yields increase exponentially with the decrease of the silicon’s work function while that of Cs⁺ and Si⁺ decrease exponentially, as expected by the electron tunneling model.     

A track detector technique for determining ion source emission profiles

Solid state nuclear track detectors have been used to directly measure for an ion source the beam emission cross sections along the ion beam trajectory. Results are demonstrated for an ion source of the surface ionization type using solid source materials to obtain ¹⁴⁷Sm or ⁶Li isotopes. Cellulose nitrate LR 115 was used as the detector to register the alpha tracks from the radioactive decay of the implanted ¹⁴⁷Sm and from the ⁶Li (n, α) reaction induced by thermal neutrons in a nuclear reactor.     

Application of the thin layer activation technique to study surface erosion under high voltage electrical spark discharges

The thin layer activation technique using a heavy ion beam has been applied to measure the erosion loss of materials by electrical spark discharges with a discharge current in the mA range. Since the range of heavy ions such as ¹⁴N, ¹⁶O and ²⁰Ne, is about one order less than that of light ions such as p, d and α, the total activity can be generated within a narrow layer by activation with heavy ions. In the present work, a narrow layer of activity of ∼27 μm thickness was produced in copper-based materials by heavy ion induced nuclear reactions using 110 MeV ¹⁶O ions to measure the surface erosion in the range of hundreds of nanometers to few microns. The sensitivity can be enhanced to tens of nanometers using suitable heavy ions.     

Evolution of surface morphology of nano and micro structures during focused ion beam induced growth

We report on the morphological studies of C, Pt and W nanopillars fabricated by focused ion beam chemical vapor deposition (FIB-CVD) process. The pillars have large base size as compared to the tip and they exhibit a rough morphology with whisker like structures protruding out of the surface. The whiskers have thickness of about 100 nm and their length varies upto 1 μm. The dimensions of these protrusions depend on the location of the protrusions on the pillar surface and show a systematic variation and saturation of growth as a function of ion flux. The growth of protrusions has been explained on the basis of formation of crystalline seeds on the surface due to ion beam induced temperature rise and cracking of the precursor gas in the vicinity of the seeds due to the secondary ion and electron impact. Pillars having smooth surfaces can be achieved by milling the edges of these structures.     

Low-energy unstable nuclear beam channel “SLOW” at the RIKEN ring cyclotron

A new type of low-energy radioactive nuclear beam channel “SLOW” has been constructed at the RIKEN ring cyclotron facility, intended not only for the study of emission mechanisms of various low-energy radioactive as well as stable isotope ions from a characterized surface of the primary target, but also for the generation of useful radioactive ion beams for surface-physics studies of the secondary target.

In the commissioning experiment of the SLOW beam channel, the reaction products of a heavy-ion induced nuclear reaction have been observed after surface ionization at a hot tungsten target.     

Electrical and optical surface degradation of silica due to superficial He implantation

Different oxides will be used in ITER and future fusion reactors for electrical insulation and optical components. The vacuum face of these materials will be subjected not only to neutron and gamma irradiation, but also to particle bombardment, due mainly to ionization of the residual gas and acceleration of the resulting ions by local electric fields. Previous work showed that silica suffers electrical and optical degradation when subjected to He bombardment with energies from 300 keV down to 27 keV. As the He ion energy may extend down to some few keV, or less, further work has been performed to study possible degradation for energies from 21 keV down to 5 keV. The results show that both surface and optical degradation occur at these low energies, more rapidly for the lowest energy (5 keV) ions. They also suggest that the superficial narrow implanted He profile plays an important role in the surface degradation.     

The ionoluminescence apparatus at the LABEC external microbeam facility

In this paper, we describe the main features of the ionoluminescence (IL) apparatus recently installed at the external scanning microbeam facility of the 3 MV Tandetron accelerator of the INFN LABEC Laboratory in Firenze. The peculiarity of this IL set-up resides in the fact that the light produced by the ion irradiation of the specimen is collected by a bifurcated optical fiber, so that photons are shunted both to a CCD spectrometer, working in the 200-900 nm wavelength range, and to a photomultiplier (PMT). The accurate focusing of the optical system allows high photon collection efficiency and this results in rapid acquisition of luminescence spectra with low ion currents on luminescent materials; simultaneously, luminescence maps with a spatial resolution of 10 μm can be acquired through the synchronization of PMT photon detection with the position of the scanning focused ion beam. An optical filter with a narrow passband facing the photomultiplier allows chromatic selectivity of the luminescence centres.The IL apparatus is synergistically integrated into the existing set-up for ion beam analyses (IBA). The upgraded system permits simultaneous IL and PIXE/PIGE/BS measurements. With our integrated system, we have been studying raw lapis lazuli samples of different known origins and precious lapis lazuli artworks of the Collezione Medicea of Museum of Natural History, University of Firenze, aiming at characterising their composition and provenance.     

Production behavior of irradiation defects in vitreous silica under ion beam irradiation

The production behavior of irradiation defects in vitreous silica was studied by an in situ luminescence measurement technique under ion beam irradiation of H⁺ and He⁺. No apparent difference was observed in the luminescence spectra of specimens of different OH contents. The temperature dependence of the luminescence intensity at 280 and 460 nm was measured, and analyzed by considering the production mechanisms and kinetics of the irradiation defects of oxygen deficiency centers.     

Possibility of Radiation-Induced Degradation of Concrete by Alkali-Silica Reaction of Aggregates

The effect of Ar ion irradiation on the reactivity of crystalline and amorphous quartz to alkali has been examined for clarifying whether radiation from nuclear reactors accelerates the degradation of concrete by inducing alkali-silica reaction of aggregates. Distorted amorphous quartz generated on the surface of quartz by irradiation of a 200 keV Ar ion beam is at least 700 times and 2.5 times more reactive to alkali than crystalline and regular amorphous quartz, respectively. The high reactivity of the distorted amorphous quartz indicates that the degradation of concrete by alkalsilica reaction is possible to be induced by nuclear radiation even the aggregates are inert to alkali before the irradiation. The critical radiation doses for the degradation of aggregates containing crystalline quartz are estimated to be 5 × 10¹⁹ n/cm² for fast neutrons with energy >0.1 MeV, and 5×10¹¹ Gy for beta and gamma rays. They are 1×10¹⁹ n/cm² and 0.5tiems;10¹¹ Gy, respectively for aggregates containing amorphous quartz.     

Ion beam characterization of advanced luminescent materials for application in radiation effects microscopy

The ion photon emission microscope (IPEM) is a technique developed at Sandia National Laboratories (SNL) to study radiation effects in integrated circuits with high energy, heavy ions, such as those produced by the 88” cyclotron at Lawrence Berkeley National Laboratory (LBNL). In this method, an ion-luminescent film is used to produce photons from the point of ion impact. The photons emitted due to an ion impact are imaged on a position-sensitive detector to determine the location of a single event effect (SEE). Due to stringent resolution, intensity, wavelength, decay time, and radiation tolerance demands, an engineered material with very specific properties is required to act as the luminescent film. The requirements for this material are extensive. It must produce a high enough induced luminescent intensity so at least one photon is detected per ion hit. The emission wavelength must match the sensitivity of the detector used, and the luminescent decay time must be short enough to limit accidental coincidences. In addition, the material must be easy to handle and its luminescent properties must be tolerant to radiation damage. Materials studied for this application include plastic scintillators, GaN and GaN/InGaN quantum well structures, and lanthanide-activated ceramic phosphors. Results from characterization studies on these materials will be presented; including photoluminescence, cathodoluminescence, ion beam induced luminescence, luminescent decay times, and radiation damage. Results indicate that the ceramic phosphors are currently proving to be the ideal material for IPEM investigations.