Mechanical properties of fluorite-related oxides subjected to swift ion irradiation: Pyrochlore and zirconia

The modifications of the mechanical properties of related-fluorite oxides (cubic zirconia [c-ZrO₂] and pyrochlores [Gd₂(Ti_1−xZr_x)₂O₇ with x = 0.5 and x = 1]) induced by swift heavy ion irradiation are investigated. Polycrystalline pellets of both materials were irradiated at room temperature with 940 MeV Pb or 870 MeV Xe ions at the GANIL accelerator in Caen at fluences ranging from 2 × 10¹¹ to 10¹³ cm⁻². Residual macroscopic stresses induced by irradiation were determined using X-ray diffraction and the sin²ψ method. The microhardness and the fracture toughness of irradiated samples were studied by Vickers micro-indentation. Amorphization occurs in Gd₂TiZrO₇ and not in Gd₂Zr₂O₇ and c-ZrO₂. The mechanical behavior of materials is found to be closely related to the residual stresses induced in the surface layer by irradiation. Compressive stresses are generated in c-ZrO₂ and Gd₂TiZrO₇ (leading to an increase of fracture toughness), whereas tensile stresses (inducing a large decrease of fracture toughness) are observed in Gd₂Zr₂O₇ due to the lattice contraction related to a pyrochlore fluorite→transition.     

Tensile and fracture toughness properties of neutron-irradiated CuCrZr

Tensile and fracture toughness properties of a precipitation-hardened CuCrZr alloy were investigated in two heat treatment conditions: solutionized, water quenched and aged (CuCrZr SAA), and hot isostatic pressed, solutionized, slow-cooled and aged (CuCrZr SCA). The second heat treatment simulated the manufacturing cycle for large components, and is directly relevant for the ITER divertor components. Specimens were neutron irradiated at ∼80 °C to two fluences, 2 × 10²⁴ and 2 × 10²⁵ n/m² (E > 0.1 MeV), corresponding to displacement doses of 0.15 and 1.5 displacements per atom (dpa). Tensile and fracture toughness tests were carried out at room temperature. Significant irradiation hardening and plastic instability at yield occurred in both heat treatment conditions with a saturation dose of ∼0.1 dpa. Neutron irradiation slightly reduced fracture toughness in CuCrZr SAA and CuCrZr SCA. The fracture toughness of CuCrZr remained high up to 1.5 dpa (J_Q > 200 kJ/m²) for both heat treatment conditions.     

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.     

Relationship between radiation damage anisotropy in MgO and YSZ single crystals and the Ion/Atom ratio deposition parameter in biaxially-textured MgO and YSZ thin films fabricated by ion beam assisted deposition

To elucidate the underlying physics of ion beam assisted deposition (IBAD), irradiation damage effects in magnesia (MgO) and yttria-stabilized zirconia (YSZ) were investigated. Ion irradiations were performed on MgO and YSZ single crystals of three low-index crystallographic orientations using 100 and 150 keV Ar⁺ ions over a fluence range from 1 × 10¹⁴ to 5 × 10¹⁶ Ar/cm². Damage accumulation was analyzed using Rutherford backscattering spectrometry combined with ion channeling. Damage evolution with increasing ion fluence proceeded via several characteristic stages and the total damage exhibited a strong dependence on crystallographic orientation. For both MgO and YSZ, damage anisotropy was maximal at a stage when the damage saturated, with the (1 1 0) crystallographic orientation being the most radiation damage resistant. The Ion/Atom ratio deposition parameter reported for IBAD of MgO and YSZ films was found to correlate with the damage plateau stage described above. Finally, the role of the Ion/Atom ratio is discussed in terms of radiation damage anisotropy mechanism.     

Irradiation embrittlement characterization of the EUROFER 97 material

The paper summarizes original results of irradiation embrittlement study of EUROFER 97 material that has been proposed as one candidate of structural materials for future fusion energy systems and GEN IV.Test specimens were manufactured from base metal as well as from weld metal and tested in initial unirradiated condition and also after neutron irradiation.Irradiation embrittlement was characterized by testing of toughness properties at transition temperature region - static fracture toughness and dynamic fracture toughness properties, all in sub-size three-point bend specimens (27 × 4 × 3 mm³). Testing and evaluation was performed in accordance with ASTM and ESIS standards, fracture toughness K_JC and K_Jd data were also evaluated with the “Master curve” approach. Moreover, J-R dependencies were determined and analyzed.The paper compares unirradiated and irradiated properties as well as changes in transition temperature shifts of these material parameters. Discussion about the correlation between static and dynamic properties is also given.Results from irradiation of EUROFER 97 show that this steel - base metal as well as weld metal - is suitable as a structural material for reactor pressure vessels of innovative nuclear systems - fusion energy systems and GEN IV. Transition temperature shifts after neutron irradiation by 2.5 dpa dose show a good agreement in the case of EUROFER 97 base material for both static and dynamic fracture toughness tests. From the results it can be concluded that there is a low sensitivity of weld metal to neutron irradiation embrittlement in comparison with EUROFER 97 base metal.     

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.     

Swift heavy ion induced phase transition in CdTe films deposited by spray pyrolysis in presence of electric field

CdTe polycrystalline thin films possessing hexagonal phase regions are obtained by spray deposition in presence of a high electric field. Thin film samples are irradiated with 100 MeV Ag ions using Pelletron accelerator to study the swift heavy ion induced effects. The ion irradiation results in the transformation of the metastable hexagonal regions in the films to stable cubic phase due to the dense electronic excitations induced by beam irradiation. The phase transformation is seen from the X-ray diffraction patterns. The band gap of the CdTe film changes marginally due to ion irradiation induced phase transformation. The value changes from 1.47 eV for the as deposited sample to 1.44 eV for the sample irradiated at the fluence 1×10¹³ ions/cm². The AFM images show a gradual change in the shape of the particles from rod shape to nearly spherical ones after irradiation.     

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.     

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.     

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.     

Raman investigation of incident N-, Xe-ions induced effects in ZnO thin films

Highly c-axis orientation ZnO thin films with hundreds nanometers in thickness have been deposited on (1 0 0) Si substrate by RF magnetron sputtering. These films are implanted at room temperature by 80 keV N-ions with fluences from 5.0 × 10¹⁴ to 1.0 × 10¹⁷ ions/cm², implanted by 400 keV Xe-ions with 2.0 × 10¹⁴ to 2.0 × 10¹⁶ ions/cm², irradiated by 3.64 MeV Xe-ions with 1.0 × 10¹² to 1.0 × 10¹⁵ ions/cm², or irradiated by 308 MeV Xe-ions with 1.0 × 10¹² to 5.0 × 10¹⁴ ions/cm², respectively. Then the ZnO films are investigated using a Raman spectroscopy. The obtained Raman spectra show that a new Raman peak located at about 578 cm⁻¹ relating to simple defects or disorder phase appears in all ZnO films after ion implantation/irradiation, a new Raman peak at about 275 cm^-1 owing to N-activated zinc-like vibrations is observed in the N-implanted samples. Moreover, a new Raman peak at about 475 cm⁻¹ is only seen in the samples after 400 keV and 3.64 MeV Xe-ions bombardment. The area intensity of these peaks increases with increasing ion fluence. The effects of ion fluence, element chemical activity, atom displacements induced by nuclear collisions as well as energy deposition on the damage process of ZnO films under ion implantation/irradiation are discussed briefly.     

Grain growth and crack formation in NiO thin films by swift heavy ion irradiation

NiO thin films grown on Si(1 0 0) substrates by electron beam evaporation and sintered at 700 °C, were irradiated by 120 MeV Au⁹⁺ ions. Though irradiation is known to induce lattice disorder and suppression of crystallinity, we observe grain growth at some fluences of irradiation. Associated with the growth of grains, the films develop cracks at a fluence of 3 × 10¹² ions cm⁻². The width of the cracks increased at higher fluences. Swift heavy ion irradiation induced atomic diffusion and strain relaxation in nanoparticle thin films, which are not in thermodynamic equilibrium, seem to be responsible for the observed grain growth. This phenomenon along with the tensile stress induced surface instability lead to crack formation in the NiO thin films.     

Change in magnetic properties of MgB2 thin films after irradiation by 200 MeV Au ion beam

The SHI irradiation induced effects on magnetic properties of MgB₂ thin films are reported. The films having thickness 300-400 nm, prepared by hybrid physical chemical vapor deposition (HPCVD) were irradiated by 200 MeV Au ion beam (S_e ∼ 23 keV/nm) at the fluence 1 × 10¹² ion/cm². Interestingly, increase in the transition temperature T_c from 35.1 K to 36 K resulted after irradiation. Substantial enhancement of critical current density after irradiation was also observed because of the pinning provided by the defects created due to irradiation. The change in surface morphology due to irradiation is also studied.     

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.     

Ion-irradiation-induced athermal annealing of helium bubbles in SiC

We have compared the microstructural evolution of helium bubbles under ion irradiation and high temperature annealing. 4H-SiC was irradiated first by 140 keV He ions to a fluence of 1.0 × 10¹⁷ cm⁻² and then annealed at 1200 K for 30 min. Then, the samples were either irradiated by 2 MeV He ions to a fluence of 3.0 × 10¹⁶ cm⁻² at room temperature or annealed additionally at 1200 K for 30 min. Before and after 2 MeV He ion irradiation, significant microstructural changes were observed, similar to effects of high temperature annealing. Thus, the study provides evidence of ion-irradiation-induced athermal annealing on defect Ostwald ripening process and bubble evolution. Possible mechanisms are discussed.     

Proton irradiation study of GFR candidate ceramics

This work investigated the microstructural response of SiC, ZrC and ZrN irradiated with 2.6 MeV protons at 800 °C to a fluence of 2.75 × 10¹⁹ protons/cm², corresponding to 0.71-1.8 displacement per atom (dpa), depending on the material. The change of lattice constant evaluated using HOLZ patterns is not observed. In comparison to Kr ion irradiation at 800 °C to 10 dpa from the previous studies, the proton irradiated ZrC and ZrN at 1.8 dpa show less irradiation damage to the lattice structure. The proton irradiated ZrC exhibits faulted loops which are not observed in the Kr ion irradiated sample. ZrN shows the least microstructural change from proton irradiation. The microstructure of 6H-SiC irradiated to 0.71 dpa consists of black dot defects at high density.     

Mixing of Cr and Si atoms induced by noble gas ions irradiation of Cr/Si bilayers

Cr/Si bilayers were irradiated at room temperature with 120 keV Ar, 140 keV Kr and 350 keV Xe ions to fluences ranging from 10¹⁵ to 2 × 10¹⁶ ions/cm². The thickness of Cr layer evaporated on Si substrate was about 400 Å. Rutherford backscattering spectrometry (RBS) was used to investigate the atomic mixing induced at the Cr-Si interface as function of the incident ion mass and fluence. We observed that for the samples irradiated with Ar ions, RBS yields from both Cr layer and Si substrate are the same as before the irradiation. There is no mixing of Cr and Si atoms, even at the fluence of 2 × 10¹⁶ ions/cm². For the samples irradiated with Kr ions, a slight broadening of the Cr and Si interfacial edges was produced from the fluence of 5 × 10¹⁵ ions/cm². The broadening of the Cr and Si interfacial edges is more pronounced with Xe ions particularly to the fluence of 10¹⁶ ions/cm². The interface broadening was found to depend linearly on the ion fluence and suggests that the mixing is like a diffusion controlled process. The experimental mixing rates were determined and compared with values predicted by ballistic and thermal spike models. Our experimental data were well reproduced by the thermal spikes model.     

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.     

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.     

Study of swift heavy ion irradiation effect on indium tin oxide coated electrode for the dye-sensitized solar cell application

Our long term objective is to study the swift heavy ion (SHI) irradiation effect on photoanode of dye-sensitized solar cell (DSSC) with the aim to investigate the stability of DSSC component in space irradiations and possibility of improvement in efficiency of DSSC due to ion induced effects in oxide layer. The DSSC photoanode consists of three layers viz; transparent conducting oxide (TCO), porous oxide with wide band gap and monolayer of dye molecule on top of corning glass substrate respectively. In the present study, procured radio frequency (RF) sputtered indium tin oxide (ITO) film on corning glass substrate were irradiated by SHI using 110 MeV Ni⁸⁺ ions at different fluences ranging from 3.0 × 10¹¹ ion/cm² to 1.0 × 10¹⁴ ion/cm². After irradiation significant changes have been observed in the structural, optical and electrical properties using X-ray diffraction (XRD), UV-Vis and Four Probe measurements, respectively. Overall there is 13% increase in optical transmittance which is favorable and moderate increase in sheet resistance from 8 Ω/□ to 18 Ω/□ which is still within acceptable limits for DSSC applications.