Physical and thermal properties of 8 MeV electron beam irradiated HPMC polymer films

Microstructural modification in hydroxypropyl methylcellulose (HPMC) polymer films induced by electron irradiation is studied. Irradiation was performed in air at room temperature using a 8 MeV electron accelerator at doses of 25, 50, 75 and 100 kGy. Irradiation can be used to crosslink or degrade the desired component or to fix the polymer morphology. Changes in microstructural parameters, crystallinity and thermal properties in virgin and irradiated HPMC films have been studied using wide angle X-ray scattering data and differential scanning calorimetry. The heat of fusion and the degree of crystallinity are found to be highest for unirradiated HPMC and the crystallite size is larger in virgin HPMC films.     

Photoconduction investigations in 75 MeV oxygen ion irradiated kapton-H polyimide

Photoconduction behaviour of 75 MeV oxygen ion irradiated (Fluences: 1.8 × 10¹¹, 1.8 × 10¹² and 1.8 × 10¹³ ions/cm²) kapton-H polyimide film in the visible region has been investigated at different temperatures ranging 400-2500 °C and at various electric fields ranging 40-600 kV/cm. A photoinduced exciton formation is the major source for providing charge carriers through thermolization and field-assisted dissociation processes. An attempt has been made to fit the field dependence of the steady state photocurrent to one of the several possible conduction mechanisms. In the high and low fluence (1.8 × 10¹³ and 1.8 × 10¹¹ ions/cm²) irradiated samples there exists a possibility of Poole-Frankel type of photoconduction mechanism, whereas at intermediate fluence (1.8 × 10¹² ions/cm²) a Schottky type photoconduction mechanism may be operative. The log I_ps versus 1/T plots consist of two straight lines with a knee point around 800-1000 °C. The activation energy estimated from the slope of these lines is field dependent varying from 0.40 to 0.73 eV and 0.18 to 0.23 eV above and below the knee point, respectively. This indicates the presence of more than one type of trapping levels in irradiated kapton-H polyimide.     

Oxygen defects created in CeO2 irradiated with 200 MeV Au ions

CeO₂ films were irradiated with 200 MeV Au ions in order to investigate the damages created by electronic energy deposition. In the Raman spectra of the ion-irradiated films, a broad band appears at the higher frequency side of the F_2g peak of CeO₂. The band intensity increases as ion fluence increases. Furthermore, the F_2g peak becomes asymmetric with a low-frequency tail. In order to understand the origin of these spectral changes, an unirradiated CeO₂ film was annealed in vacuum at 1000 °C. By comparing the results for the irradiation and for the annealing, it is concluded that the broad band obtained for irradiated samples contains the peak observed for the annealed sample. The F_2g peak becomes asymmetric with a low-frequency tail by the irradiation as well as the annealing. Therefore, the above-mentioned changes in the Raman spectra caused by 200 MeV Au irradiation is closely related to the creation of oxygen vacancies.     

Irradiation effects of a 10 MeV neutron beam on a Nd-Fe-B permanent magnet

The effects of irradiation of a Nd-Fe-B permanent magnet by fast neutrons was investigated. The decrease in measured magnetic flux density at the center of the magnets were 0.6%, 6.9%, 25.2% and 47.3% after continuous irradiation of 1.1 kGy, 3.7 kGy, 5.6 kGy and 7.4 kGy, respectively. On the other hand, the decrease due to non-continuous irradiation, in which the magnet was first irradiated at 3.7 kGy, then irradiated again at 3.7 kGy nine months later, was 14% smaller than that of continuous irradiation, even for the same total dose. The temperature coefficient of the magnetization did not change with irradiation. Some radioactive materials, such as ¹⁴⁷Nd, ¹⁵¹Pm, and ⁵⁴Mn, were detected in the magnet after irradiation.     

8 MeV electron irradiation effects in silicon photo-detectors

Results of investigations on the electrical properties of n⁺-p-p⁺ silicon (Si) photo-detectors irradiated with 8 MeV electrons are presented. The photo-detectors were irradiated with electrons of doses up to 100 kGy. Current-voltage (I-V) and capacitance-voltage (C-V) characteristics under dark conditions were measured as a function of dose. A significant change in the diffusion component of the saturation current is observed after irradiation, while the generation-recombination component of the saturation current remains almost unchanged. The series resistance is found to increase with increasing dose while the shunt resistance and carrier concentration decrease with dose. Optoelectronic properties, namely short circuit current I_sc, open circuit voltage V_oc under air mass zero illumination and spectral response, were measured at various doses. From the spectral responses of the devices, the minority carrier diffusion length was estimated.     

Neutron interrogation of high-enriched uranium by a 4 MeV linac

For revealing unauthorized transport (illicit trafficking) of nuclear materials, a non-destructive method reported earlier, utilizing a 4 MeV linear accelerator for photoneutron interrogation, was further developed. The linac served as a pulsed neutron source for assay of highly enriched uranium. Produced in beryllium or heavy water by bremsstrahlung, neutrons subsequently induced fission in the samples. Delayed neutrons were detected by a newly designed neutron collar built up of 14 ³He counters embedded in a polyethylene moderator. A PC controlled multiscaler served as a time analyzer, triggering the detector startup by the beam pulse. Significant progress was achieved in enhancing the detector response, hence the sensitivity for revealing illicit material. A lower sensitivity limit of the order of 10 mg ²³⁵U was determined in a 20 s measurement time with a reasonable amount of beryllium (170 g) or of heavy water (100 g) and a mean electron current of 10 μA. Sensitivity can be further enhanced by increasing the measurement time.     

Redeposition of amorphous hydrogenated carbon films during thermal decomposition

Thermally induced decomposition of hard and soft amorphous hydrocarbon films was investigated by thermal effusion spectroscopy. Released species were detected by a sensitive quadrupole mass spectrometer using two different experimental setups for thermal effusion. Species released in a molecular beam setup were detected in direct line of sight to the sample surface, while species released in a remote UHV oven had no direct line of sight to the mass spectrometer. Soft, hydrogen-rich carbon films exhibit a desorption maximum at T ≈ 740 K while hard films with a low hydrogen content have their maximum at T ≈ 870 K. Additionally, the spectrum of released species differs dramatically between hard and soft films. We found a significant redeposition of species released from soft films. From the redeposited fraction of material we estimated an average redeposition probability of about 50% for species released from soft films.     

Study of electron beam curing process using epoxy resin system

Polymeric matrix composite (PMC) has been used in engineering applications instead of metal in the last few years, due to its corrosion resistance and excellent relation between tensile strength/density and elastic modulus/density. However, PMC materials cured by thermal process require high temperature and are time-consuming. The electron beam (EB) curing technology allows its use at room temperature and reduced curing times, and this is one of the main advantages over thermal technology. The aim of this work is to investigate electron beam curable epoxy formulations to use in filament winding processes to produce composite material with similar or better properties than thermal curable composites. The study has been made with commercial epoxy resins and cationic initiators. The epoxy resin samples were irradiated for few minutes with total dose of 150 kGy. The glass transition temperatures (T_g) were determined by dynamic mechanical analyzer (DMA) and the result was 137 °C. The thermal process was carried out in a furnace following three steps: 4 h at 90 °C, increasing temperature from 90 °C to 130 °C during 4 h and 12 h at 130 °C. The total process time was 20 h. The T_g of this sample was 102 °C.     

Structural, thermal and optical behavior of 84 MeV oxygen and 120 MeV silicon ions irradiated PES

In order to study structural, thermal and optical behavior, thin flat samples of polyethersulfone were irradiated with oxygen and silicon ions. The changes in properties were analyzed using different techniques viz: X-ray diffraction, thermo-gravimetric analysis, Fourier transform infrared, UV-visible and photoluminescence spectroscopy. A noticeable increase in the intensity of X-ray diffraction peaks was observed after irradiation with 84 MeV oxygen ions at low and medium fluences, which may be attributed to radiation-induced cross-linking in polymer. Fourier transform infrared and thermo-gravimetric analysis corroborated the results of X-ray diffraction analysis. No noticeable change in the Fourier transform infrared spectra of oxygen ion irradiated polyethersulfone were observed even at the highest fluence of 1 × 10¹³ ions cm⁻², but after irradiation with silicon ions, a reduction in intensity of almost all characteristic bands was revealed. An increase in the activation energy of decomposition of polyethersulfone was observed after irradiation with 84 MeV oxygen ions up to medium fluences but degradation was revealed at higher fluences. Similar trends were observed by photoluminescence analysis.     

Electron beam irradiation effects on the mechanical, thermal and surface properties of a fluoroelastomer

Fluoroelastomer can be used as a sealing material for different purposes. The aim of this work is the evaluation of the effects of the ionizing radiation of an electron beam (EB) on the mechanical, thermal and surface properties of a commercial fluoroelastomer containing carbon black and inorganic fillers. The material was irradiated with overall doses between 10 and 250 kGy. Tensile strength (stress and strain at break), hardness (Shore A) and compression set were evaluated. Thermal behavior was evaluated by thermogravimetric analysis and differential scanning calorimetry. Surface modifications were inspected using scanning electron microscopy (SEM) and optical microscopy. The experiments have shown that EB irradiation promotes beneficial changes in the fluoroelastomer tensile strength behavior while compression set remain constant and the glass transition temperature increases. The SEM micrographs have shown compactness in the irradiated samples, although optical observations showed no surface morphology changes.     

Photoneutron interrogation of low-enriched uranium induced by bremsstrahlung from a 4 MeV linac

Revealing smuggled nuclear material by passive γ-detection is hindered, because the weak radiation can easily be shielded. Neutrons, as penetrate shielding, represent a detection potential, by inducing fission in the nuclear material. A 4 MeV linear accelerator was used as a pulsed neutron source for active interrogation of U-bearing material. Produced in heavy water by bremsstrahlung, neutrons subsequently induced fissions in UO₂ samples. Delayed fission neutrons were detected in a neutron collar built up by ³He counters in a polyamide container. The counters were gated to be detached from high voltage during the electron pulse. Irradiation-measurement cycles were carried out with a 25 Hz pulse repetition rate as optimum setting. The time analyser start-up was externally triggered and synchronised by the electron beam pulse. The response of the system was studied as a function of the intensity of the electron current, the amount of heavy water, U enrichment, and total U content. Sensitivity limit was achieved as 0.5 g ²³⁵U and/or 30 g ²³⁸U in a 20 s measurement time (500 cycles) with the amount of heavy water of 100 g and a mean electron current of 2 μA. Because of the long decay time of the prompt (interrogating and fission) neutron pulse, about a half of the time interval (40 ms) between pulses is only available for counting delayed neutrons.     

Performance of the SIRAD ion electron emission microscope

An axial ion electron emission microscope (IEEM) is now working at the SIRAD irradiation facility of the INFN Laboratories of Legnaro (Italy). The IEEM is used to precisely reconstruct the impact points of single ions, information that may be used to determine the areas of a microelectronic device under test that are sensitive to single event effects (SEE). After describing the setup briefly reviewing its working principles, we show our first time resolved ion induced electron emission images of standard calibration targets. We also discuss a preliminary measurement of ion impact detection efficiency of the IEEM system and the available trigger signals for SEE studies. We finally make an assessment of ion electron emission microscopy at SIRAD and indicate future developments.     

Thermal and structural properties of low-fluence irradiated graphite

The release of Wigner energy from graphite irradiated by fast neutrons at a TRIGA Mark II research reactor has been studied by differential scanning calorimetry and simultaneous differential scanning calorimetry / synchrotron powder X-ray diffraction between 25 and 725 °C at a heating rate of 10 °C min⁻¹. The graphite, having been subject to a fast-neutron fluence from 5.67 × 10²⁰ to 1.13 × 10²² n m⁻² at a fast-neutron flux (E > 0.1 MeV) of 7.88 × 10¹⁶ n m⁻² s⁻¹ and at temperatures not exceeding 100 °C, exhibits Wigner energies ranging from 1.2 to 21.8 J g⁻¹ and a Wigner energy accumulation rate of 1.9 × 10⁻²¹ J g⁻¹ n⁻¹ m². The differential-scanning-calorimeter curves exhibit, in addition to the well known peak at ∼200 °C, a pronounced fine structure consisting of additional peaks at ∼150, ∼230, and ∼280 °C. These peaks correspond to activation energies of 1.31, 1.47, 1.57, and 1.72 eV, respectively. Crystal structure of the samples is intact. The dependence of the c lattice parameter on temperature between 25 and 725 °C as determined by Rietveld refinement leads to the expected microscopic thermal expansion coefficient along the c axis of ∼26 × 10⁻⁶ °C⁻¹. At 200 °C, coinciding with the maximum in the differential-scanning-calorimeter curves, no measurable changes in the rate of thermal expansion have been detected - unlike its decrease previously seen in more highly irradiated graphite.     

Experimental study of the residual activity induced by 950 MeV/u uranium ions in stainless steel and copper

As a preparatory work for constructing the FAIR facility at GSI, samples of stainless steel and copper were irradiated by 950 MeV/u ²³⁸U ions and depth-profiles of residual activity were measured by gamma-ray spectroscopy. The isotopes with dominating contribution to the residual activity were identified and their contributions were quantified. In contrast to the previous study performed at lower energies, the activities could no longer be determined from the full-assembly target measurements. Depth-profiling of residual activity of all identified isotopes had to be completed by measurements of individual target foils. The activity contributions were then obtained by integration of the depth-profiles.     

Effect of 50 MeV Li ion irradiation on electrical, optical and mechanical properties of 4,4′-dimethylbenzophenone

4,4′-Dimethylbenzophenone (DMBP) single crystals were irradiated at room temperature and at liquid nitrogen temperature with 50 MeV Li³⁺ ions at fluences 1 × 10¹² and 1 × 10¹³ ions/cm². The dielectric constant and dielectric loss as a function of frequency of the applied ac field in the range from 20 Hz to 1 MHz and at temperatures ranging from 313 to 353 K were analyzed. The dielectric constant decreases with increase in frequency for all the temperatures. The dielectric constant and dielectric loss increase with fluence. Optical absorption was measured at different conditions. UV-Vis studies reveal the decrease in bandgap. The unirradiated as well as irradiated crystals were characterized by photoluminescence. Ion-induced changes were also studied with respect to their mechanical response using the Vicker’s microhardness technique and parameters including fracture toughness, brittleness index and yield strength are calculated.     

Electron beam modification and functionalization of MWNT for covalent dispersion into polymeric systems

The development of nanotube-based polymer composites with improved mechanical properties and electrical conductivity requires the covalent dispersion of carbon nanotubes to utilize their stress transfer capabilities. Covalent dispersion of nanotubes therefore requires the functionalization of their surface to interact with solvents or monomers. In this work, we have developed a novel method of nanotube surface modification in which dry MWNT are irradiated with a high-energy electron beam (EB) in ambient air environment. Raman spectroscopy was performed to characterize the influence of EB irradiation on nanotubes, namely, variance of the disorder, or D band (∼1360 cm⁻¹) with respect to the graphitic, or G, band (∼1580 cm⁻¹). Raman spectra show increased deformation to the graphitic structure, as well as increased strain on the carbon-carbon bonds, weakening the nanotube. Transmission electron microscopy (TEM) confirms that nanotubes remain intact despite high EB dose. In addition, minimal surface deformation and length reduction occurred on irradiated MWNT.     

Effects of 0.28-2.80 MeV proton irradiation on GaInP/GaAs/Ge triple-junction solar cells for space use

GaInP/GaAs/Ge triple-junction solar cells were irradiated with 0.28, 0.62 and 2.80 MeV protons with fluences ranging from 1 × 10¹⁰ cm⁻² to 1 × 10¹³ cm⁻². Their performance degradation is analyzed using current-voltage characteristics and spectral response measurements. The degradation rates of the short circuit current, open circuit voltage, and maximum power output increase with fluence, but decrease with increasing proton energy. It was also observed that the spectral response of the GaAs middle cell degrades more significantly than that of the GaInP top cell.     

DSC studies of retrogradation and amylose-lipid complex transition taking place in gamma irradiated wheat starch

The effect of gamma irradiation (⁶⁰Co) with doses of 5-30 kGy on the amylose-lipid complex transition and retrogradation occurring in gels containing ca. 50% and ca. 20% wheat starch was studied by differential scanning calorimetry (DSC) during heating-cooling-heating cycles (up to three cycles). Transition of the amylose-lipid complex occurs in all the irradiated samples at a lower temperature as compared to the non-irradiated starch. That effect was larger when the radiation dose was higher. A further thermal treatment causes a decrease of the transition temperature in the irradiated samples, with no effect or increase of that temperature observed for the non-irradiated ones. Irradiation hinders retrogradation taking place in 50% gels but facilitates the process occurring in 20% gels. The differences between the irradiated and the non-irradiated samples are more evident in the every next heating or cooling cycle as well as after storage and in the case of ca. 50% suspensions as compared to ca. 20% suspensions. The results point out to the deterioration of the structure of the complexes formed in the irradiated starch as compared to the non-irradiated one.     

Surface roughness of ion-bombarded Si(1 0 0) surfaces: Roughening and smoothing with the same roughness exponent

We have carried out scanning tunneling microscopy experiments under ultrahigh vacuum condition to study the roughness of pristine as well as ion-bombarded Si(1 0 0) surfaces and of ultrathin Ge films deposited on them. One half of a Si(1 0 0) sample (with native oxide layer) was irradiated at room temperature using 45 keV Si⁻ ions at a fluence of 4 × 10¹⁵ ions/cm² while the other half was masked. STM measurements were then carried out on the unirradiated as well as the irradiated half of the sample. Root-mean-square (rms) roughness of both the halves of the sample has been measured as a function of STM scan size. Below a length scale of ∼30 nm we observe surface smoothing and surface roughening is observed for length scales above this value. However, the surface is self-affine up to length scales of ∼200 nm and the observed roughness exponent of 0.46 ± 0.04 is comparable to earlier cases of ion sputtering studies where only roughening [J. Krim, I. Heyvart, D.V. Haesendonck, Y. Bruynseraede, Phys. Rev. Lett. 70 (1993) 57] or only smoothing [D.K. Goswami, B.N. Dev, Phys. Rev. B 68 (2003) 033401] was observed. Preliminary results involving morphology for Ge deposition on clean ion-irradiated and pristine Si(1 0 0) surfaces are presented.     

Strain-driven (0 0 2) preferred orientation of ZnO nanoparticles in ion-implanted silica

We present an experimental and theoretical study on the structural properties of ZnO nanoparticles embedded in silica. The ZnO-SiO₂ nanocomposite was prepared by ion implanting a Zn⁺ beam in a silica slide and by annealing in oxidizing atmosphere at 800 °C. From an experimental point of view, the structural properties of the ZnO-SiO₂ nanocomposite were studied by using glancing incidence X-ray diffraction. According to the results, zinc crystalline nanoclusters with an average diameter of 13 nm are in the as-implanted sample. The annealing in oxidizing atmosphere promotes the total oxidation of the Zn nanoclusters and increases their size until to an average of 22 nm. Moreover, the formed ZnO nanocrystals have a preferential (0 0 2) crystallographic orientation. From a theoretical point of view, the preferential orientation of the ZnO nanoparticles can be explained satisfactory by the minimization of the strain energy of the nanoparticles placed in proximity of the surface of the matrix.