High gamma dose response of the electrical properties of polyethylene terephthalate thin films

Electrical properties of polyethylene terephthalate (PET), irradiated with gamma rays, have been investigated. The PET films were irradiated with high gamma dose levels in the range from 100 to 2000 kGy. The changes in the DC (σ_DC) and the ac (σ_ac) conductivities, with the dose, have been performed. The effect of gamma irradiation on the dielectric constant (ε′) and loss (ε″) has been determined. Also, the dose dependence of the frequency exponent index (S), the resonance frequency (Fc) and the hopping frequency (ω_P) have been obtained. The obtained results show that increasing gamma dose leads to slight increase in σ_DC, σ_ac and ε′, while no change was observed in ε″ value. Meanwhile, S, Fc and ω_P are inversely proportional to the dose. Accordingly, the study suggests the possibility of using PET films in electronic components (capacitors, resistors, etc.), especially that operate at high gamma dose environments for the frequency independent applications.     

Vitamin C hinders radiation cross-linking in aqueous poly(vinyl alcohol) solutions

Poly(vinyl alcohol) (PVA) is a promising semi-crystalline material for biomedical applications. It is soluble in water and can be formed into hydrogels by freezing and thawing or crystallizing from an aqueous theta solution such as that of polyethylene glycol (PEG). Radiation cross-linking caused by sterilization or high dose irradiation of concentrated PVA solutions could compromise some properties of these hydrogels. Therefore, we hypothesized that radiation cross-linking of PVA solutions and PVA-PEG theta gels could be prevented by using the antioxidant vitamin C as an anticross-linking agent. Our hypothesis tested positive. Vitamin C concentrations of 0.75 and 4.5 mol/mol of PVA repeating unit could prevent cross-linking in 17.5 wt/v% PVA solutions made with PVA molecular weight of 115,000 g/mol irradiated to 25 and 100 kGy, respectively. Vitamin C also prevented cross-linking in 25 kGy irradiated PVA-PEG theta gels containing up to 5 wt% PEG and decreased the viscosity of those up to 39 wt%.     

Method to measure composition modifications in polyethylene terephthalate during ion beam irradiation

Matter losses of polyethylene terephthalate (PET, Mylar) films induced by 1600 keV deuteron beams have been investigated in situ simultaneously by nuclear reaction analysis (NRA), deuteron forward elastic scattering (DFES) and hydrogen elastic recoil detection (HERD) in the fluence range from 1 × 10¹⁴ to 9 × 10¹⁶ cm⁻². Volatile degradation products escape from the polymeric film, mostly as hydrogen-, oxygen- and carbon-containing molecules. Appropriate experimental conditions for observing the composition and thickness changes during irradiation are determined. ¹⁶O(d,p₀)¹⁷O, ¹⁶O(d,p₁)¹⁷O and ¹²C(d,p₀)¹³C nuclear reactions were used to monitor the oxygen and carbon content as a function of deuteron fluence. Hydrogen release was determined simultaneously by H(d,d)H DFES and H(d,H)d HERD. Comparisons between NRA, DFES and HERD measurements show that the polymer carbonizes at high fluences because most of the oxygen and hydrogen depletion has already occured below a fluence of 3 × 10¹⁶ cm⁻². Release curves for each element are determined. Experimental results are consistent with the bulk molecular recombination (BMR) model.     

An intense channeling radiation source

A non-conventional X-ray source which is based on the production of electron channeling radiation in a diamond crystal has been installed at the radiation source ELBE. The brilliant electron beam with an average current of up to 200 μA allows to reach photon rates of quasi-monochromatic channeling radiation between 10¹⁰ s⁻¹ and 10¹¹ s⁻¹ per 10% bandwidth. The photon energy can be tuned by variation of the beam energy. On-line X-ray monitoring was realised at high beam currents using a Compton spectrometer. Monochromisation of channeling radiation and bremsstrahlung background reduction has been investigated applying X-ray diffraction at a highly ordered pyrolytic graphite crystal.     

Modelling swift heavy ion irradiation in iron

Swift heavy ions moving in metals lose most of their energy to inelastic scattering of electrons. The energy deposited in the electronic system is transferred into the atomic system via electron-ion interactions and can lead to melting and creation of new damage and also annealing of pre-existing atomic defects. Using a combination of molecular dynamics and a consistent treatment of electron energy transfer and transport we have modelled experiments performed in Fe to investigate the annealing effect and damage creation under electronic excitations. We observe both annealing and new damage creation at low and high electronic stopping, respectively. Rapid separation of interstitial atoms and vacant lattice sites is seen due to efficient transport via replacement collision sequences. Our results suggest that the role of electronic excitation can be significant in modeling of the behaviour of metals under swift heavy ion irradiation and attempts to modify metals via ion implantation.     

Track-etched nanopores in spin-coated polycarbonate films applied as sputtering mask

Thin polycarbonate films were spin-coated on silicon substrates and subsequently irradiated with 1-GeV U ions. The ion tracks in the polymer layer were chemically etched yielding nanopores of about 40 nm diameter. In a second process, the nanoporous polymer film acted as mask for structuring the Si substrate underneath. Sputtering with 5-keV Xe ions produced surface craters of depth ∼150 nm and diameter ∼80 nm. This arrangement can be used for the fabrication of track-based nanostructures with self-aligned apertures.     

Initial stage of etching through pores in PET films irradiated by Ar ions

Changes in the diameters and depths of pores were studied in the process of etching polyethyleneterephthalate (PET) films irradiated by Ar ions having an energy of 1 MeV/n. Information about the pore diameters and lengths was obtained with JSM-840 and TEM-125 electron microscopes. The solutions of NaOH (0.5 mol/dm³ and 2 mol/dm³) were used as etchants. Etching was performed at 55 °C and 70 °C. Two methods of sensitization were used: the first one by UV illumination and treatment in dimethylformamide (DMF), the second method just by UV illumination. It was found that the diameters and the depths of pores are larger in films treated according to the first sensitization method. Etching duration (breakthrough time), which leads to through-going pores of the minimal radius, was established. After sensitization according to the first method the track etch rate grows quicker than the transverse etch rate. This gives a possibility to obtain through pores with diameters ranging from 50 nm to several micrometers.     

Modification of a shell model for the study of the radiation effects in BaTiO3

In order to study the radiation effects in BaTiO₃ ferroelectric crystal, a previously developed shell model is modified. The modifications include adding the ZBL universal potentials at short distances and distance-dependent spring constants for core-shell interactions. The phase transition sequences in BaTiO₃ were correctly reproduced using molecular dynamics simulations with this modified shell model. Also, the calculated Frenkel pair formation energies agree well with results obtained by first principles calculations, which suggests that this model is suitable for the simulation of the radiation effects in BaTiO₃. The dependence of polarization on the number of oxygen vacancies was also studied.     

Ion track formation in low temperature silicon dioxide

Low temperature silicon dioxide layers (LTO), deposited on crystalline silicon substrates, and thermally densified at 750 °C for 90 min or 900 °C for 30 min, jointly with thermally grown silicon dioxide layers, were irradiated with low fluence 11 MeV Ti ions. A selective chemical etch of the latent tracks generated by the passage of swift ions was performed by wet or vapour HF solution. The wet process produced conically shaped holes, while the vapour procedure generated almost cylindrical nanopores. In both cases thermal SiO₂ showed a lower track etching velocity V_t, but with increasing the densification temperature of the LTO samples, the V_t differences reduced. LTO proved to be suitable for wet and vapour ion track formation, and, as expected, for higher densification temperatures, its etching behaviour approached that of thermal silicon dioxide.     

Spectrum and polarization of coherent and incoherent radiation and the LPM effect in oriented single crystal

The spectrum and the circular polarization of radiation from longitudinally polarized high-energy electrons in an oriented single crystal are considered using the method which permits inseparable consideration of both the coherent and the incoherent mechanisms of photon emission. The spectral and polarization properties of radiation are obtained and analyzed. It is found that in some part of the spectral distribution the influence of multiple scattering (the Landau-Pomeranchuk-Migdal (LPM) effect) attains the order of 7%. The same is true for the influence of multiple scattering on the polarization part of the radiation intensity. The degree of the circular polarization of the total intensity of radiation is found. It is shown that the influence of multiple scattering on the photon polarization is similar to the influence of the LPM effect on the total intensity of radiation: it appears only for relatively low energies of radiating electron and has the order of 1%, while at higher energies the crystal field action excludes the LPM effect.     

Vibrational contributions to the stability of point defects in bcc iron: A first-principles study

The purpose of this study is to investigate the modes of vibration of the self-interstitial atoms and the vacancy in bcc iron and to estimate how the vibrational properties can affect the stability of these defects. The phonon density of states of the vacancy and the self-interstitials have been calculated within the quasi harmonic approximation using density functional theory calculations. It was observed that self-interstitial atoms have several localized high frequency modes of vibration related to the stretching of the dumbbell bond, but also soft modes favoring their migration. From the phonon density of states, the vibrational contributions to the free energy have been estimated for finite temperatures. Results are compared to previous work performed by others using empirical potentials. We found a rather large formation entropy for the vacancy, k_B. Our results show that the vibrational entropy can have a significant influence on the formation of the point defects even at moderate temperature. Possible consequences on the mobility of these defects are also discussed.     

Irradiation-induced precipitation modelling of ferritic steels

In high strength low alloy (HSLA) steels typically used in reactor pressure vessels (RPV), irradiation-induced microstructure changes affect the performance of the components. One such change is precipitation hardening due to the formation of solute clusters and/or precipitates which form as a result of irradiation-enhanced solute diffusion and thermodynamic stability changes. The other is irradiation-enhanced tempering which is a result of carbide coarsening due to irradiation-enhanced carbon diffusion. Both effects have been studied using a recently developed Monte Carlo based precipitation kinetics simulation technique and modelling results are compared with experimental measurements. Good agreements have been achieved.     

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.     

Ion irradiation effects on surface mechanical behavior and shrinkage of hybrid sol-gel derived silicate thin films

A study of the effects of ion irradiation on the surface mechanical behavior and shrinkage of organic/inorganic modified silicate thin films was performed. The films were synthesized by sol-gel processing from tetraethylorthosilicate (TEOS) and methyltriethoxysilane (MTES) precursors and spin-coated onto Si substrates. The sol viscosity and the spin velocity were adjusted so that the films produced had a final thickness ranging from 580 to 710 nm after heat treatment. The ion species and incident energies used were selected such that the projected ion range was greater than the film thickness, resulting in fully irradiated films. After heat treatment at 300 °C for 10 min, the films were irradiated with 125 keV H⁺, 250 keV N²⁺ and 2 MeV Cu⁺ ions with fluences ranging from 1 × 10¹⁴ to 1 × 10¹⁶ ions/cm². Both hardness and reduced elastic modulus were seen to exhibit a monotonic increase with fluence for all three ion species. Also, H loss was found to increase monotonically with increase in fluence, while the film thickness was found to decrease with increase in fluence.     

Gamma irradiation of PolyEthyleneTerephthalate and PolyEthyleneNaphthalate

The effect of gamma irradiation in air is investigated in two thermoplastic polyesters (PET and PEN), in order to evaluate the influence of aromatic density and the role of oxygen on radiation resistance. EPR measurements were carried out to detect radical stability against oxygen permeation and to provide radical characterization. Viscometric data reveal a different behaviour between films and thick samples. Positron annihilation spectra show a decrease of ortho-positronium intensity, which is more marked in film samples. ortho-positronium lifetime does not depend on the radiation dose.     

Neutron irradiation-induced dimensional changes in MEMS glass substrates

A study is made of radiation-induced expansion/compaction in Pyrex^® (Corning 7740) and Hoya SD-2^® glasses, which are used as substrates for MEMS devices. Glass samples were irradiated with a neutron fluence composed primarily of thermal neutrons, and a flotation technique was employed to measure the resulting density changes in the glass. Transport of Ions in Matter (TRIM) calculations were performed to relate fast (∼1 MeV) neutron atomic displacement damage to that of boron thermal neutron capture events, and measured density changes in the glass samples were thus proportionally attributed to thermal and fast neutron fluences. Pyrex was shown to compact at a rate of (in Δρ/ρ per n/cm²) 8.14 × 10⁻²⁰ (thermal) and 1.79 × 10⁻²⁰ (fast). The corresponding results for Hoya SD-2 were 2.21 × 10⁻²¹ and 1.71 × 10⁻²¹, respectively. On a displacement per atom (dpa) basis, the compaction of the Pyrex was an order of magnitude greater than that of the Hoya SD-2. Our results are the first reported measurement of irridiation-induced densification in Hoya SD-2. The compaction of Pyrex agreed with a previous study. Hoya SD-2 is of considerable importance to MEMS, owing to its close thermal expansivity match to silicon from 25 to 500°C.     

Positron annihilation study and computational modeling of defect production in neutron-irradiated reactor pressure vessel steels

Positron annihilation spectroscopy (PAS) and a computer simulation were used to investigate a defect production in reactor pressure vessel (RPV) steels irradiated by neutrons. The RPV steels were irradiated at 250 °C in a high-flux advanced neutron application reactor. The PAS results showed that mainly single vacancies were created to a great extent as a result of a neutron irradiation. Formation of vacancies in the irradiated materials was also confirmed by a coincidence Doppler broadening measurement. For estimating the concentration of the point defects in the RPV steels, we applied computer simulation methods, including molecular dynamics (MD) simulation and point defect kinetics model calculation. MD simulations of displacement cascades in pure Fe were performed with a 4.7 keV primary knock-on atom to obtain the parameters related to displacement cascades. Then, we employed the point defect kinetics model to calculate the concentration of the point defects. By combining the positron trapping rate from the PAS measurement and the calculated vacancy concentrations, the trapping coefficient for the vacancies in the RPV steels was determined, which was about 0.97 × 10¹⁵ s⁻¹. The application of two techniques, PAS and computer simulation, provided complementary information on radiation-induced defect production.     

Investigation by slow positron beam of defects in CLAM steel induced by helium and hydrogen implantation

Hydrogen and helium ion beams delivering different doses are used in the ion implantation, at room temperature, of China Low Activation Martensitic (CLAM) steel and the induced defects studied by Doppler broadening of gamma-rays generated in positron annihilation. Defect profiles are analysed in terms of conventional S and W parameters, measures of relative contributions of low and high-momentum electrons in the annihilation peak, as functions of incident positron energies E up to 30 keV. The behaviours of the S-E, W-E and S-W plots under different implantation doses indicate clearly that the induced defect size has obvious variation with depth, taking values that interpolate between surface and bulk values, and depend mainly on helium ion fluences. The S-W plot indicates that two types of defects have formed after ion implantation.     

Ion beam radiation effects in monazite

Monazite is a potential matrix for conditioning minor actinides arising from spent fuel reprocessing. The matrix behavior under irradiation must be investigated to ensure long-term containment performance. Monazite compounds were irradiated by gold and helium ions to simulate the consequences of alpha decay. This article describes the effects of such irradiation on the structural and macroscopic properties (density and hardness) of monazites LaPO₄ and La_0.73Ce_0.27PO₄. Irradiation by gold ions results in major changes in the material properties. At a damage level of 6.7 dpa, monazite exhibits volume expansion of about 8.1%, a 59% drop in hardness, and structure amorphization, although Raman spectroscopy analysis shows that the phosphate-oxygen bond is unaffected. Conversely, no change in the properties of these compounds was observed after He ion implantation. These results indicate that ballistic effects predominate in the studied dose range.     

Low temperature resistivity study of nanostructured polypyrrole films under electronic excitations

The synthesis of nanostructured polypyrrole (Ppy) films by electrochemical process and their modifications by electronic excitations induced by swift heavy ion irradiations is reported in this paper. The electrical property of ion beam irradiated polypyrrole was investigated at low temperature by resistivity measurements. The structural and optical properties were also studied using X-ray diffraction (XRD), UV-vis spectroscopy and scanning electron microscopy (SEM). At low temperature, the polypyrrole films show the metallic behaviour after ion beam irradiation. UV-vis spectroscopy shows a red shift in the absorbance edge and thus reduction in band gap with increasing ion fluence. The structural studies show that the percentage crystallinity improves with increase in ion fluence. The SEM study corroborates the results of structural analysis and shows the formation of rod type structures along with the evolution of amorphous phase with increasing ion fluence.