Oxygen ion irradiation effect on corrosion behavior of titanium in nitric acid medium

The corrosion assessment and surface layer properties after O⁵⁺ ion irradiation of commercially pure titanium (CP-Ti) has been studied in 11.5 N HNO₃. CP-Ti specimen was irradiated at different fluences of 1 × 10¹³, 1 × 10¹⁴ and 1 × 10¹⁵ ions/cm² below 313 K, using 116 MeV O⁵⁺ ions source. The corrosion resistance and surface layer were evaluated by using potentiodynamic polarization, electrochemical impedance spectroscopy (EIS), scanning electron microscopy (SEM) and glancing-angle X-ray diffraction (GXRD) methods. The potentiodynamic anodic polarization results of CP-Ti revealed that increased in ion fluence (1 × 10¹³-1 × 10¹⁵ ions/cm²) resulted in increased passive current density due to higher anodic dissolution. SEM micrographs and GXRD analysis corroborated these results showing irradiation damage after corrosion test and modified oxide layer by O⁵⁺ ion irradiation was observed. The EIS studies revealed that the stability and passive film resistance varied depending on the fluence of ion irradiation. The GXRD patterns of O⁵⁺ ion irradiated CP-Ti revealed the oxides formed are mostly TiO₂, Ti₂O₃ and TiO. In this paper, the effects of O⁵⁺ ion irradiation on material integrity and corrosion behavior of CP-Ti in nitric acid are described.     

Investigations on the effect of 100 MeV Ni ions irradiated chloride vapour phase epitaxy (Cl-VPE) grown GaN epilayers

Gallium nitride (GaN) epilayers have been grown by chloride vapour phase epitaxy (Cl-VPE) technique and the grown GaN layers were irradiated with 100 MeV Ni ions at the fluences of 5 × 10¹² and 2 × 10¹³ ions/cm². The pristine and 100 MeV Ni ions irradiated GaN samples were characterized using X-ray diffraction (XRD), UV-visible transmittance spectrum, photoluminescence (PL) and atomic force microscopy (AFM) analysis. XRD results indicate the presence of gallium oxide phases after Ni ion irradiation, increase in the FWHM and decrease in the intensity of the GaN (0 0 0 2) peak with increasing ion fluences. The UV-visible transmittance spectrum and PL measurements show decrease in the band gap value after irradiation. AFM images show the nanocluster formation upon irradiation and the roughness value of GaN increases with increasing ion fluences.     

Ion beam modification of strained InGaAs/InP characterized by HRXRD, PL and AFM

Highly tensile strained InGaAs/InP multi quantum wells have been grown by the LP-MOVPE technique. Such samples were subjected to irradiation with 100 MeV Au⁸⁺ ions. These were studied as a function of fluence, then the irradiated samples were annealed by rapid thermal annealing at 700 °C for 60 s in nitrogen atmosphere. We used high resolution X-ray diffraction (HRXRD), photoluminescence (PL) and atomic force microscopy (AFM) characterization techniques to study the interfacial induced changes, band gap modifications and surface morphology. Multi quantum wells were then studied before and after irradiation.     

Structural and optical study of irradiation effect in GaN epilayers induced by 308 MeV Xe ions

Wurtzite GaN epilayers irradiated at room temperature with 308 MeV ¹²⁹Xe³⁵⁺ ions to fluences of 1 × 10¹³ and 3 × 10¹³ cm⁻² have been studied by contact mode atomic force microscopy (AFM), high-resolution X-ray diffraction (HRXRD), micro-Raman scattering and photoluminescence (PL) spectroscopy. The AFM images showed that the surface of GaN films was etched efficiently due to the Xe ion irradiation. The initial step-terrace structure on GaN surface was eliminated completely at a fluence of 3 × 10¹³ cm⁻². HRXRD and Raman results indicated that the Xe ion irradiation led to a homogenous lattice expansion throughout the entire ∼3 μm-thick GaN films. The lattice expansion as well as the biaxial compressive stress of the films was increasing with the increase of ion fluence. PL measurements showed that a dominant yellow luminescence band in the as-grown GaN films disappeared, but a blue and a green luminescence bands were produced after irradiation. Based on these results, the strong electronic excitation effect of 308 MeV Xe ions in GaN is discussed.     

PL and XPS study of radiation damage created by various slow highly charged heavy ions on GaN epitaxial layers

Photoluminescence (PL) spectrum, in conjunction with X-ray photoelectron spectroscopy (XPS) is used to evaluate the surface damage of GaN layer by highly-charged Xe^q+ (18 ? q ? 30), Ar^q+ (6 ? q ? 16) and Pb^q+ (q = 25,35) ions. The intensity of PL emission of GaN layer, including near band-edge peak and yellow luminescence, decreases with increasing fluence and charge state of the incident ions. Finally the PL emission is completely quenched after irradiation to high fluences at high charge state. A new peak at 450 nm appeared in PL spectra of the specimens irradiated with Xe¹⁸⁺, Ar⁶⁺ and Ar¹¹⁺, indicating that radioactive recombination within donor-acceptor pairs (DAPs) during irradiation. After irradiation, XPS spectra show N deficient or Ga rich on GaN surface and XPS spectra of Ga3d core levels indicate spectral peak evidently shifts from a Ga-N to Ga-Ga and Ga-O bond. The relative content of Ga-N bond decreases and the content of Ga-Ga bond increases with the increase of ion fluence and ion charge state. The binding energy of Ga3d_5/2 electron corresponding to Ga-Ga bond of the irradiated GaN film is found to be smaller than that of metallic Gallium (Ga⁰), which can be attributed to irradiation damage.     

Morphological change in FePt nanogranular thin films induced by swift heavy ion irradiation

We have investigated morphology change of FePt nanogranular films (FePt)₄₇(Al₂O₃)₅₃ under irradiation with 210 MeV Xe ions. Here, electron tomography technique was extensively employed to clarify three-dimensional (3D) structure in irradiated specimens, in addition to conventional transmission electron microscopy (TEM) techniques such as bright-field observation and scanning TEM energy dispersive X-ray spectroscopy (STEM-EDX) analysis. The ion irradiation induces the coarsening of FePt nanoparticles with elongation along the beam direction. Electron tomography 3D reconstructed images clearly demonstrated that when the fluence achieves 5.0 × 10¹⁴ ions/cm², well-coarsened FePt balls have been formed on the irradiated surface, and the particles in the film interior have been deformed into rods along the ion trajectory. The alloy particles become inhomogeneous in composition after prolonged irradiation up to 1.0 × 10¹⁵ Xe ions/cm². The particle center is enriched with Pt, while Fe is slightly redistributed to the periphery.     

Evidence of nanostructure formation in Ge oxide by crystallization induced by swift heavy ion irradiation

Ge oxide films were irradiated with 150 MeV Ag ions at fluences varying between 10¹² and 10¹⁴ ions/cm². The irradiation-induced changes were monitored by FT-IR spectroscopy, atomic force microscopy, X-ray diffraction and photoluminescence spectroscopy. The FT-IR spectra indicate stoichiometric changes and an increase in Ge content on irradiation. X-ray diffraction shows a crystallization of the irradiated films and presence of both Ge and GeO₂ phases. The Ge nanocrystal size, as calculated from Scherrer’s formula, was around 30 nm. The morphological changes, observed in atomic force microscopy, also indicate formation of nanostructures upon ion irradiation and a uniform growth is observed for a fluence of 1 × 10¹⁴ ions/cm².     

Effect of swift heavy ion irradiation on structure, optical, and gas sensing properties of SnO2 thin films

Swift heavy ion irradiation has been successfully used to modify the structural, optical, and gas sensing properties of SnO₂ thin films. The SnO₂ thin films prepared by sol-gel process were irradiated with 75 MeV Ni⁺ beam at fluences ranging from 1 × 10¹¹ ion/cm² to 3 × 10¹³ ion/cm². Structural characterization with glancing angle X-ray diffraction shows an enhancement of crystallinity and systematic change of stress in the SnO₂ lattice up to a threshold value of 1 × 10¹³ ions/cm², but decrease in crystallinity at highest fluence of 3 × 10¹³ ions/cm². Microstructure investigation of the irradiated films by transmission electron microscopy supports the XRD observations. Optical properties studied by absorption and PL spectroscopies reveal a red shift of the band gap from 3.75 eV to 3.1 eV, and a broad yellow luminescence, respectively, with increase in ion fluence. Gas response of the irradiated SnO₂ films shows increase of resistance on exposure to ammonia (NH₃), indicating p-type conductivity resulting from ion irradiation.     

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.     

Electronic excitations induced modifications of structural and optical properties of ZnO-porous silicon nanocomposites

The influence of swift heavy ion (SHI) irradiation on structural and photoluminescence (PL) properties of ZnO nanocrystallites deposited into porous silicon (PS) templates by the sol-gel process was studied. The ZnO/PS nanocomposites were irradiated using 120 MeV Au ions at different fluences varying from 1 × 10¹² to 1 × 10¹³ ions/cm². The intensity of the X-ray diffraction peaks is suppressed at the high fluence, without evolution of any new peak. The PL emission from PS around 700 nm is found to decrease with increase in ion fluence, while the PL emission from deep level defects of ZnO nanocrystallites is increased with ion fluence. At the highest fluence, the observation of drastic increase in PL emission due to donor/acceptor defects in the region 400-600 nm and suppressions of XRD peaks could be attributed to the defects induced structural modifications of ZnO nanocrystallites.     

AFM and photoluminescence studies of swift heavy ion induced nanostructured aluminum oxide thin films

E-beam evaporated aluminum oxide films were irradiated with 120 MeV swift Au⁹⁺ ions in order to induced nanostructure formation. Atomic force microscope (AFM) results showed the formation of nanostructures for films irradiated with a fluence of 1 × 10¹³ ions cm⁻². The particle size estimated by section analysis of the irradiated film was in the range 25-30 nm. Glancing angle X-ray diffraction (GAXRD) revealed the amorphous nature of the films. Two strong Photoluminescence (PL) emission bands with peaks at ∼430 nm and ∼645 nm besides a shoulder at ∼540 nm were observed in all irradiated samples. The PL intensity is found to increase with increase of ion fluence.     

In vitro degradation properties of ion-beam irradiated poly(lactide-co-glycolic acid) mesh

Scaffolds for tissue regeneration must be biocompatible and biodegradable. Ion-beam irradiation is useful for making polymers biocompatible, but the process by which the irradiated polymers biodegradable is not yet well understood. We investigated this phenomenon by Kr⁺-irradiated poly(lactide-co-glycolic acid) (PLGA) mesh substrate at an acceleration energy of 50 keV with fluences of 1 × 10¹³ and 1 × 10¹⁴ ions/cm². We then measured the electronic states of the constituent elements on the irradiated surface by X-ray photoelectron microscopy (XPS) and evaluated the hydrolytic degradation properties (weight loss, media pH, and tensile strength) of the mesh in phosphate buffer solution. New functional groups and carbonization were induced on the irradiated surface. Degradation rate and tensile strength remain unchanged by ion-beam irradiation. Ion-beam irradiation should, thus, be a promising modification technique for tissue engineering scaffolds.     

Effect of swift heavy ion irradiation on nanocrystalline CaS:Bi phosphors: Structural, optical and luminescence studies

Luminescence studies of CaS:Bi nanocrystalline phosphors synthesized by wet chemical co-precipitation method and irradiated with swift heavy ions (i.e. O⁷⁺-ion with 100 MeV and Ag¹⁵⁺-ion with 200 MeV) have been carried out. The samples have been irradiated at different ion fluences in the range 1 × 10¹²-1 × 10¹³ ions/cm². The average grain size of the samples before irradiation was estimated as 35 nm using line broadening of XRD (X-ray diffraction) peaks and TEM (transmission electron microscope) studies. Our results suggest a good structural stability of CaS:Bi against swift heavy ion irradiation. The blue emission band of CaS:Bi³⁺ nanophosphor at 401 nm is from the transition ³P₁ → ¹S₀ of the Bi³⁺. We have observed a decrease in lattice constant (a) and increase of optical energy band gap after ion irradiation. We presume this change due to grain fragmentation by dense electronic excitation induced by swift heavy ion. We have studied the optical and luminescent behavior of the samples by changing the ion energy and also by changing dopant concentration from 0.01 mol% to 0.10 mol%. It has been examined that ion irradiation enhanced the luminescence of the samples.     

Color center formation in silica glass induced by high energy Fe and Xe ions

Silica glass samples were implanted with 1.157 GeV ⁵⁶Fe and 1.755 GeV ¹³⁶Xe ions to fluences range from 1 × 10¹¹ to 3.8 × 10¹² ions/cm². Virgin and irradiated samples were investigated by ultraviolet (UV) absorption from 3 to 6.4 eV and photoluminescence (PL) spectroscopy. The UV absorption investigation reveals the presence of various color centers (E′ center, non-bridging oxygen hole center (NBOHC) and ODC(II)) appearing in the irradiated samples. It is found that the concentration of all color centers increase with the increase of fluence and tend to saturation at high fluence. Furthermore the concentration of E′ center and that of NBOHC is approximately equal and both scale better with the energy deposition through processes of electronic stopping, indicating that E′ center and NBOHC are mainly produced simultaneously from the scission of strained Si-O-Si bond by electronic excitation effects in heavy ion irradiated silica glass. The PL measurement shows three emissions peaked at about 4.28 eV (α band), 3.2 eV (β band) and 2.67 eV (γ band) when excited at 5 eV. The intensities of α and γ bands increase with the increase of fluence and tend to saturation at high fluence. The intensity of β band is at its maximum in virgin silica glass and it is reduced on increasing the ions fluence. It is further confirmed that nuclear energy loss processes determine the production of α and γ bands and electronic energy loss processes determine the bleaching of β band in heavy ion irradiated silica glass.     

Radiation tolerance of Cu/W multilayered nanocomposites

Magnetron sputtered Cu/W multilayer samples with individual layer thicknesses from 2.5 to 50 nm were irradiated by 50 keV He⁺ ions at ion fluences from 7 × 10²⁰ to 6 × 10²¹ m⁻² at room temperature. Evolution of the interfacial structure during irradiation is monitored by X-ray diffraction and cross-sectional transmission electron microscopy. Moreover, radiation responses on the individual layer thickness and He⁺ ion irradiation fluence are revealed. The highly morphological stability of the multilayered structure suggests that the interfacial structure and grain boundary can serve as sinks for radiation-induced defects.     

Study of 200 MeV Ag ion induced amorphisation in nickel ferrite thin films

Thin films of nickel ferrite of thickness ∼100 and 150 nm were deposited by pulsed laser deposition. The films were irradiated with a 200 MeV Ag¹⁵⁺ beam of three fluences 1 × 10¹², 2 × 10¹² and 4 × 10¹² ions/cm². X-ray diffraction showed a decrease in the intensity of peaks indicating progressive amorphisation with increased irradiation fluence. Fourier transform infra-red and Raman spectra of pristine and irradiated films were also recorded which showed a degradation of the crystallinity of the samples after irradiation. The damage cross section of the infra-red bands was determined. It was found that the two bands at 557 and 614 cm⁻¹ did not show similar behaviour with fluence.     

Ion irradiation damage effects in δ-phase Y6W1O12

Polycrystalline Y₆W₁O₁₂ samples were irradiated with 280 keV Kr²⁺ ions to fluences up to 2 × 10²⁰ ions/m² at cryogenic temperature (100 K). Ion irradiation damage effects in these samples were examined using grazing incidence X-ray diffraction (GIXRD) and cross-sectional transmission electron microscopy (TEM). The pristine Y₆W₁O₁₂ possesses rhombohedral symmetry (structure known as the δ-phase), which is closely related to cubic fluorite structure. GIXRD and TEM observations revealed that the irradiated Y₆W₁O₁₂ experiences an ordered rhombohedral to disordered cubic fluorite transformation by a displacement damage dose of ∼12 displacements per atom (dpa). At the highest experimental dose of ∼50 dpa, the uppermost irradiated region was found to be partially amorphous while the buried damage region was found to contain the same fluorite structure as observed at lower dose.     

Effect of swift heavy ion irradiation in W/Co multilayer structures

Present study reports effect of swift heavy ion irradiation on structural and magnetic properties of sputtered W/Co multilayer structures (MLS) having bilayer compositions of [W(10 Å)/Co(20 Å)]_5BL and [W(20 Å)/Co(20 Å)]_5BL. These MLS are irradiated by 120 MeV Au⁹⁺ ions up to fluence of 1 × 10¹³ ions/cm². X-ray reflectivity (XRR), wide-angle X-ray diffraction (WAXD), cross-sectional transmission electron microscopy (X-TEM) and magneto optical Kerr effect (MOKE) techniques are used for structural and magnetic characterization of pristine and irradiated MLS. Analysis of XRR data using Parratt’s formalism shows a significant increase in W/Co interface roughness. WAXD and X-TEM studies reveals that intra-layer microstructure of Co-layers in MLS becomes nano-crystalline on irradiation. MOKE study shows slight increase in coercivity at higher fluence, which may be due to increase in surface and interface roughness after recrystallization of Co-layers.     

Light ion irradiation-induced phase transformation in the monoclinic polymorph of zirconia

Ion irradiation damage experiments were performed at ∼80 K on polycrystalline samples of monoclinic, slightly sub-stoichiometric zirconia (ZrO_1.98). Following irradiation with 150 keV Ne⁺ ions, the monoclinic phase was gradually replaced by a new phase. Transmission electron microscopy (TEM) observations in cross-sectional geometry and electron microdiffraction (μD) measurements revealed that the irradiated layer in a sample irradiated to a fluence of 5 × 10²⁰ Ne/m² is partially transformed to a higher symmetry phase of high crystallinity. This phase transformation is accompanied by reduction of the initial micron-sized, highly-twinned grain distribution, to a nano-phased grain structure. Grazing incidence X-ray diffraction (GIXRD) measurements revealed that the radiation-induced phase is a tetragonal polymorph of zirconia. This was verified by the existence of strong (1 0 1) diffraction maxima and weak (1 0 2) reflections (body-centered cell). Raman spectroscopy (RS) measurements were also performed in an attempt to corroborate GIXRD results obtained from the irradiated material. RS measurements in the confocal geometry agreed with GIXRD measurements, although RS was not as definitive as GIXRD. In addition to RS showing the existence of a band corresponding to a tetragonal structure at 262 cm⁻¹, a new mystery band appeared at 702 cm⁻¹ that increased in intensity as a function of irradiation fluence.     

X-ray photoelectron and Raman spectroscopic studies of MeV proton irradiated graphite

Poly-crystalline graphite samples were irradiated using 2.25 MeV H⁺ ions with a fluence of 2 × 10¹⁷ ions/cm². Magnetic ordering in highly oriented pyrolytic graphite samples have been reported earlier under the similar irradiation conditions [Esquinazi et al., Phys. Rev. Lett. 91 (2003) 227201]. In that study, the authors attribute the observed irradiation induced magnetic ordering to the formation of a mixed sp²-sp³ hybridized carbon atoms. In the present study, we report the X-ray photoelectron and Raman spectroscopic studies on pristine and irradiated samples. Irradiated samples are found to show an increased number of sp³ hybridized carbon atoms. However, the Raman spectrum, specially the second order data, do indicate that the nature of the graphene lattice structure has been preserved in the irradiated samples. The mechanisms for the irradiation induced enhancement in sp³ hybridization are discussed.