Lithium diffusion in polyether ether ketone and polyimide stimulated by in situ electron irradiation and studied by the neutron depth profiling method

Diffusion of lithium from a LiCl aqueous solution into polyether ether ketone (PEEK) and polyimide (PI) assisted by in situ irradiation with 6.5?MeV electrons was studied by the neutron depth profiling method. The number of the Li atoms was found to be roughly proportional to the diffusion time. Regardless of the diffusion time, the measured depth profiles in PEEK exhibit a nearly exponential form, indicating achievement of a steady-state phase of a diffusion–reaction process specified in the text. The form of the profiles in PI is more complex and it depends strongly on the diffusion time. For the longer diffusion time, the profile consists of near-surface bell-shaped part due to Fickian-like diffusion and deeper exponential part.     

Effects of passage of 200 MeV Ag9+ ions in indium phosphide at different depths

Indium phosphide sample was irradiated with 200?MeV Ag⁹⁺ ions for the fluence of 2?×?10¹³?ions?cm^?2. The sample was chemically etched down up to 240?nm depth to investigate the distribution of defects at different regions. Raman scattering and glancing incidence X-ray diffraction spectra were recorded at different depths. The stress estimated from Raman shift was found to increase with depth up to 160?nm and thereafter it decreased and at a depth of 224?nm sample did not show any stress. Phonon coherence length estimated from the Phonon Confinement Model was found to vary between 43 and 18?nm with respect to depth. Glancing incidence X-ray diffraction results revealed the decrease in crystallite size from 16.12 to 1.00?nm in different depth regions.     

Effect of MeV electron irradiation on the free volume of polyimide

The free volume of the microvoids in the polyimide samples, irradiated with 6 MeV electrons, was measured by the positron annihilation technique. The free volume initially decreased the virgin value from ～13.70 to ～10.98 Å³ and then increased to ～18.11 Å³ with increasing the electron fluence, over the range of 5?×?10¹⁴ – 5?×?10¹⁵ e/cm². The evolution of gaseous species from the polyimide during electron irradiation was confirmed by the residual gas analysis technique. The polyimide samples irradiated with 6 MeV electrons in AgNO₃ solution were studied with the Rutherford back scattering technique. The diffusion of silver in these polyimide samples was observed for fluences >2?×?10¹⁵ e/cm², at which microvoids of size ≥3 Å are produced. Silver atoms did not diffuse in the polyimide samples, which were first irradiated with electrons and then immersed in AgNO₃ solution. These results indicate that during electron irradiation, the microvoids with size ≥3 Å were retained in the surface region through which silver atoms of size ～2.88 Å could diffuse into the polyimide. The average depth of diffusion of silver atoms in the polyimide was ～2.5 μm.     

50 MeV Li3+ ion irradiation effect on structural, electrical, and dielectric properties of PVA-based nanocomposite polymer electrolytes

Nanocomposite polymer electrolyte thin films of polyvinyl alcohol (PVA)-orthophosphoric acid (H₃PO₄)-Al₂O₃ have been prepared by solution cast technique. Films are irradiated with 50 MeV Li³⁺ ions having four different fluences viz. 5?×?10¹⁰, 1?×?10¹¹, 5?×?10¹¹, and 1?×?10¹² ions/cm². The effect of irradiation on polymeric samples has been studied and characterized. X-ray diffraction spectra reveal that percent degree of crystallinity of samples decrease with ion fluences. Glass transition and melting temperatures have been also decreased as observed in differential scanning calorimetry. A possible complexation/interaction has been shown by Fourier transform infrared spectroscopy. Temperature-dependent ionic conductivity shows an Arrhenius behavior before and after glass transition temperature. It is observed that ionic conductivity increases with ion fluences and after a critical fluence, it starts to decrease. Maximum ionic conductivity of ～2.3?×?10^?5 S/cm owing to minimum activation energy of ～0.012 eV has been observed for irradiated electrolyte sample at fluence of 5?×?10¹¹ ions/cm². The dielectric constant and dielectric loss also increase with ion fluences while they decrease with frequency. Transference number of ions shows that the samples are of purely ionic in nature before and after ion irradiation.     

Effect of proton irradiation on the physical properties of PC/PBT blends

Samples from polycarbonate/poly (butylene terephthalate) (PC/PBT) blends film have been irradiated using different fluences (1?×?10¹⁵– 5?×?10¹⁷ H⁺/cm²) of 1?MeV protons at the University of Surrey Ion Beam Center, UK. The structural modi?cations in the proton irradiated samples have been studied as a function of fluence using different characterization techniques such as X-ray diffraction and UV spectroscopy. The results indicate that the proton irradiation reduces the optical energy gap that could be attributed to the increase in structural disorder of the irradiated samples due to crosslinking. Furthermore, the color intensity ΔE, which is the color difference between the non-irradiated sample and those irradiated with different proton fluences, increased with increasing the proton fluence up to 5?×?10¹⁷ H^+/cm², convoyed by an increase in the red and yellow color components. In addition, the resultant effect of proton irradiation on the thermal properties of the PC/PBT samples has been investigated using thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). It is found that the PC/PBT decomposes in one weight loss stage. Also, the variation of transition temperatures with proton fluence has been determined using DSC. The PC/PBT thermograms were characterized by the appearance of two endothermic peaks due to the glass transition and melting temperatures. The melting temperature of the polymer, T_m, was investigated to probe the crystalline domains of the polymer, since the proton irradiation destroys the crystalline structure so reducing the melting temperature.     

Effect of swift heavy ion irradiation on dilute Fe-doped Sb0.95Se0.05 magnetic semiconductor

A thin film of dilute Fe (0.008)-doped Sb_0.95Se_0.05 alloy was grown on silicon substrate using the thermal evaporation technique. This film was irradiated with swift heavy ions (SHIs) Ag⁺¹⁵ having 200?MeV energy at ion fluences of 1?×?10¹² and 5?×?10¹² ions per cm², respectively. The thickness of the thin film was ～500?nm. We study the effect of irradiation on structural, electrical, surface morphology and magnetic properties of this film using grazing angle XRD (GAXRD), DC resistivity, atomic force microscopy (AFM) and magnetic force microscopy (MFM), respectively. GAXRD suggests that no significant change is observed in this system due to SHI irradiation. The average crystallite size increases with fluence, whereas the AFM image shows the rms roughness decreases due to irradiation with respect to the un-irradiated thin film. The MFM image shows that the magnetic interaction in irradiated film decreases due to the irradiation effect. Although the un-irradiated sample shows metal to semiconducting transition, but after irradiation with fluence of 5?×?10¹² ions per cm², the sharpness of the metal to semiconducting phase transition is observed to increase dramatically at ～300?K. This characteristic of the thin film makes it a promising candidate for an electrical switching device after irradiation.     

Au5+ ion implantation induced structural phase transitions probed through structural,microstructural and phonon properties in BiFeO3 ceramics,using synergistic ion beam energy

Implanted Au⁵⁺-ion-induced modification in structural and phonon properties of phase pure BiFeO₃ (BFO) ceramics prepared by sol–gel method was investigated. These BFO samples were implanted by 15.8?MeV ions of Au⁵⁺ at various ion fluence ranging from 1?×?10¹⁴ to 5?×?10¹⁵?ions/cm². Effect of Au⁵⁺ ions’ implantation is explained in terms of structural phase transition coupled with amorphization/recrystallization due to ion implantation probed through XRD, SEM, EDX and Raman spectroscopy. XRD patterns show broad diffuse contributions due to amorphization in implanted samples. SEM images show grains collapsing and mounds’ formation over the surface due to mass transport. The peaks of the Raman spectra were broadened and also the peak intensities were decreased for the samples irradiated with 15.8?MeV Au⁵⁺ ions at a fluence of 5?×?10¹⁵?ion/cm². The percentage increase/decrease in amorphization and recrystallization has been estimated from Raman and XRD data, which support the synergistic effects being operative due to comparable nuclear and electronic energy losses at 15.8?MeV Au⁵⁺ ion implantation. Effect of thermal treatment on implanted samples is also probed and discussed.     

Electrical characteristics of etched ion-tracks in polyimide filled with silver nanoparticles

Silicon ions, of energy 150?MeV and fluence ～10¹²?ions/cm², were used to register latent tracks in 40?µm thick polyimide samples. Different sizes of tracks were obtained by etching the ion irradiated polyimide samples, in chemical solutions, by varying the temperature and etching period. Silver nanoparticles were diffused into the etched tracks by immersing the polyimide samples in silver solution and then irradiating with 6.5?MeV electrons at different fluences varying from 1?×?10¹⁵ to 5?×?10¹⁵?cm^?2. Results of morphological and elemental analysis, carried out by Scanning Electron Microscopy and Energy Dispersive X-ray. Analysis revealed that the conical tracks could be fully filled with silver nanoparticles at electron fluence of 5?×?10¹⁵?cm^?2. The minimum d. c. resistance of an array of tracks, filled with silver nanoparticles and measured across the polyimide film, was orders of magnitude higher as compared to that of silver wires of equivalent sizes connected in parallel. In addition, these silver nanoparticles filled tracks exhibited rectifying I–V behavior and frequency dependent a. c. resistance, characteristic of metal–polymer nano-composites. Possible mechanisms have been discussed, which can justify the asymmetric current–voltage characteristics in such nano-composites.     

Swift heavy ion provoked structural, optical and electrical properties in SnO2 thin films

SnO₂ thin films grown on glass substrates at 300 ^°C by reactive thermal evaporation and annealed at 600 ^°C were irradiated by 120 MeV Ag⁹⁺ ions. Though irradiation is known to induce lattice disorder and suppression of crystallinity, we observe grain growth at a certain fluence of irradiation. X-ray diffraction (XRD) revealed the crystalline nature of the films. The particle size estimated by Scherrer’s formula for the irradiated films was in the range 10–25 nm. The crystallite size increases with increase in fluence up to 1×10¹² ions?cm^?2, whereas after that the size starts decreasing. Atomic force microscope (AFM) results showed the surface modification of nanostructures for films irradiated with fluences of 1×10¹¹ ions?cm^?2 to 1×10¹³ ions?cm^?2. The UV–visible spectrum showed the band gap of the irradiated films in the range of 3.56 eV–3.95 eV. The resistivity decreases with fluence up to 5×10¹² ions?cm^?2 and starts increasing after that. Rutherford Backscattering (RBS) reveals the composition of the films and sputtering of ions due to irradiation at higher fluence.     

Surface Modification of Poly (ether ether ketone) with a Medlite C6 (ND-YAG Q-Switched) Skin Treatment Laser

Poly ether ether ketone (PEEK), a synthetic polymer, is expected to be useful as a biomaterial due to its appropriate mechanical, chemical, and biocompatibility properties. However, this polymer is biologically inert, requiring surface modification to improve its adhesion to bone cells for use as a bone substrate. Surface properties, such as roughness and hydrophilicity, are important factors in the adhesion of biomaterials to the surrounding tissue; therefore, in this study, laser treatment was performed for surface modification. The aim of the research described here was to investigate the effect of two laser parameters, fluency and wavelength, on the surface roughness and hydrophilicity to determine the optimum parameters for improving surface adhesion. The surface topography and average roughness (R_a) were investigated by atomic force microscopy (AFM). Surface morphology was also observed with an optical microscope, and the hydrophilicity of the surfaces was investigated with static contact angle tests. The results obtained showed that the samples treated at the wavelength of 532?nm with fluency of 8?J/cm², compared to fluencies of 4 and 12?J/cm², showed improved surface properties. However, in terms of radiation wavelength, the wavelength of 1064?nm at these three fluencies showed the most promising results for enhancing the surface properties of PEEK for bone implant applications.     

Influence of 120 MeV Si9+ ion irradiation on ZnTe semiconductor thin films

ABSTRACT

ZnTe (Zinc Telluride) is a potential semiconducting material for many optoelectronic devices like solar cells and back contact material for CdTe-based solar cells. In the present study, ZnTe thin films were prepared by thermal evaporation technique and then irradiated with 120?MeV Si⁹⁺ ions at different fluences. These films are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and UV–Visible spectroscopy techniques. XRD study confirms increased crystallinity and grain growth for post-irradiated ZnTe thin films for fluences, up to 1?×?10¹¹ ions cm^?2. However, the grain size and crystallinity decreased for higher fluence-exposed samples. SEM images confirm the observed structural properties. Modification of the surface morphology of the film due to the ion irradiation with different fluences is studied. Optical band gap of film is decreased from 2.31?eV (pristine) to 2.17?eV after irradiation of Si⁹⁺ ions.     

Clusterization of vacancy defects in ZnO irradiated with 2 MeV O

Slow positrons have been used to study ZnO layers grown on a-axis sapphire and irradiated by 2 MeV O⁺ ions to fluences from 10¹² cm⁻² to 10¹⁷ cm⁻². At low fluences Zn vacancies are observed, and their introduction rate is estimated as 2000 cm⁻¹. At the highest fluences of 10¹⁶-10¹⁷ cm⁻² vacancy clusters are formed. The extent of the primary damage and its recovery is discussed.     

Positron annihilation in electron-irradiated n-type gap crystals

Abstract

The defects in n-GaP crystals irradiated by 2.3 MeV electrons up to 1 × 10¹⁹ cm^?2 at RT were studied by means of positron annihilation (angular correlation) and electrical property measurements. It was found that positrons are trapped in some radiation-induced vacancy-type defects (acceptors) but that the effect saturates at high electron fluences (D1 × 10¹⁸ cm^?2). The trapping rate in irradiated samples increases with temperature in the range 77–300 K. Post-irradiation isochronal annealing reveals the positron traps clustering at about 200–280°C. All positron sensitive radiation-induced defects disappear upon annealing up to 500°C.     

Formation of bubbles and blisters in hydrogen ion implanted polycrystalline tungsten

ABSTRACT

Tungsten (W) has been regarded as one of the most promising plasma facing materials (PFMs) in fusion reactors. The formation of bubbles and blisters during hydrogen (H) irradiation will affect the properties of W. The dependence of implantation conditions, such as fluence and energy, is therefore of great interest. In this work, polycrystalline tungsten samples were separated into two groups for study. The thick samples were implanted by 18?keV H₃⁺ ions to fluences of 1?×?10¹⁸, 1?×?10¹⁹ and 1?×?10²⁰ H⁺/cm², respectively. Another thick sample was also implanted by 80?keV H₂⁺ ions to a fluence of 2?×?10¹⁷ H⁺/cm² for comparison. Moreover, the thin samples were implanted by 18?keV H₃⁺ ions to fluences of 9.38?×?10¹⁶, 1.88?×?10¹⁷ and 5.63?×?10¹⁷ H⁺/cm², respectively. Focused ion beam (FIB) combined with scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used for micro-structure analysis, while time-of-flight ion mass spectrometry (ToF-SIMS) was used to characterize the H depth profile. It is indicated that bubbles and blisters could form successively with increasing H⁺ fluence. H bubbles are formed at a fluence of ～5.63?×?10¹⁷ H⁺/cm², and H blisters are formed at ～1?×?10¹⁹ H⁺/cm² for 18?keV H₃⁺ implantation. On the other hand, 80?keV H₂⁺ ions can create more trapping sites in a shallow projected range, and thus enhancing the blisters formation with a relatively lower fluence of 2?×?10^17?H⁺/cm². The crack-like microstructures beneath the blisters are also observed and prefer to form on the deep side of the implanted range.     

Depth profiling of ion-induced damage in D9 alloy using X-ray diffraction

The ion-induced depthwise damage profile in 35?MeV α-irradiated D9 alloy samples with doses of 5?×?10¹⁵?He²⁺/cm², 6.4?×?10¹⁶?He²⁺/cm² and 2?×?10¹⁷?He²⁺/cm² has been assessed using X-ray diffraction technique. The microstructural characterisation has been done along the depth from beyond the stopping region (peak damage region) to the homogeneous damage region (surface) as simulated from SRIM. The parameters such as domain size and microstrain have been evaluated using two different X-ray diffraction line profile analysis techniques. The results indicate that at low dose the damage profile shows a prominent variation as a function of depth but, with increasing dose, it becomes more homogeneous along the depth. This suggests that enhanced defect diffusion and their annihilation in pre-existing and newly formed sinks play a significant role in deciding the final microstructure of the irradiated sample as a function of depth.     

Investigation of energetic ion-induced mixing in Bi/Ge system

The present study is carried out for the investigation of energetic ion beam mixing in the Bi/Ge system, induced by electronic excitation. The system Ge/Bi/C was deposited on Si substrate at room temperature in the high vacuum deposition system and irradiated using Au ions of 120?MeV at the fluences 1?×?10¹³, 5?×?10¹³ and 1?×?10¹⁴?ions/cm². The top layer of carbon was deposited as the protecting layer to avoid oxidation. The swift heavy ions (SHI)-induced interface mixing was studied by Rutherford backscattering spectroscopy (RBS) for depth profiles and compositions, grazing incidence X-ray diffraction (GIXRD) for phase identification and atomic force microscopy (AFM) for surface roughness. We have calculated the mixing rate, mixing efficiency and inter-diffusion coefficient for the Bi/Ge system. We observed that the thickness of the mixed region increased with increasing fluence. In the GIXRD pattern, no new crystalline phase formation was observed after irradiation, the mixed region may be in an amorphous form. The mixing effect is explained in the framework of the thermal spike model.     

Anti-biofilm efficiency of 120 MeV Fe+9 SHI-irradiated polyimide film

ABSTRACT

Polyimide (PI) films were irradiated by 120 MeV iron (Fe⁺⁹) ions and variations in its optical, chemical, surface morphology and anti-bacterial properties were studied. UV-Visible spectroscopic results showed the decrease in the optical band gap of PI after irradiation due to the chain scission mainly at the carbonyl group which is corroborated by Fourier Transform Infrared spectroscopic results. The scanning electron microscopic results showed the surface roughening, surface structure broken and micro-porous formation in PI after irradiation. These results are also corroborated by the decrease in contact angle as studied by the contact angle measurement. PI films irradiated by 120 MeV Fe⁺⁹ ions showed increased anti-biofilm efficacy against the human pathogen, Salmonella typhi. In addition to this, the morphological changes were also observed due to the stress of Fe-irradiated PI. Biofilm formation was inhibited ≈ 35% at 1?×?10¹¹ ion/cm² and 80% at 5?×?10¹² ion/cm² in irradiated PI films. Thus, surface modification of PI films help in the inhibition of biofilm formation.

Highlights

1. Polyimide (PI) films were irradiated by 120?MeV Fe⁺⁹ ions.

2. Optical band gap of PI decreased after ion irradiation.

3. Surface roughening and micro-pores formation in PI after ion irradiation.

4. Surface modification of PI films helps in the inhibition of bio-film formation.

     

Tomographic study of the three-dimensional distribution of a high-fluence implant in a polymer

6 Li⁺ ions were implanted into PMMA at high flux up to fluences of 1×10¹⁵ cm^-2 under angles of 0° to 70° towards the surface normal. The Li depth distributions were determined by means of neutron depth profiling, and compared with theoretical simulations. The three-dimensional Li distribution was reconstructed from the one-dimensional depth profiles by means of a tomographic technique. It turned out that the measured Li depth distributions can be described by a superposition of Gaussian and exponential functions. This points at considerable Li mobility during or after the ion implantation, with trapping in unsaturable traps in the ion-irradiated region which roughly follow the electronic energy transfer distribution. The Li redistribution is more pronounced along the track direction than transversely to it. The normalized Li distributions in various implantation directions were fed into our tomographic program to reconstruct the three-dimensional distribution of the deposited lithium. As expected, the lithium preferentially distributes along the ion tracks. This work is another hint that mobility of implanted ions in solids does not proceed isotropically, but is strongly influenced by the radiation-damage distributions. Received: 11 May 1998 / Accepted: 9 September 1998 / Published online: 24 February 1999     

Non-equilibrium plasma production by pulsed laser ablation of gold

A gold target has been irradiated with a Q-switched Nd:Yag laser having 1064?nm wavelength, 9?ns pulse width, 900?mJ maximum pulse energy and a maximum power density of the order of 10¹⁰?W/cm². The laser–target interaction produces a strong gold etching with production of a plasma in front of the target. The plasma contains neutrals and ions having a high charge state. Time-of-flight (TOF) measurements are presented for the analysis of the ion production and ion velocity. A cylindrical electrostatic deflection ion analyzer permits measurement of the yield of the emitted ions, their charge state and their ion energy distribution. Measurements indicate that the ion charge state reaches 6⁺ and 10⁺ at a laser fluence of 100?J/cm² and 160?J/cm², respectively. The maximum ion energy reaches about 2?keV and 8?keV at these low and high laser fluences, respectively. Experimental ion energy distributions are given as a function of the ion charge state. Obtained results indicate that electrical fields, produced in the plume, along the normal to the plane of the target surface, exist in the unstable plasma. The electrical fields induce ion acceleration away from the target with a final velocity dependent on the ion charge state. The ion velocity distributions follow a “shifted Maxwellian distribution”, which the authors have corrected for the Coulomb interactions occurring inside the plasma.     

Structure of defects in Pt induced by neutron and ion irradiation

The effect of formation of a nanocrystalline structure in the near-surface layer of platimun (99.99%) as a result of 30-keV Ar ion bombardment up to fluences of 10¹⁶–10¹⁷ cm^?2 was discovered by the direct method of field ion microscopy. The spatial distribution and structure of radiation damage in Pt was established in the case where Pt is bombarded by fast neutrons (E > 0.1 MeV) up to fluences of 6.7 × 10¹⁷ and 3.5 × 10¹⁸ cm^?2 in the RWW-2M reactor at a temperature of ～310 K.