Ion Irradiated Samples Research Articles

Microstructure Evolution of the Interface in SiCf/TiC-Ti3SiC2 Composite under Sequential Xe-He-H Ion Irradiation and Annealing Process.

A new type of SiCf/TiC-Ti3SiC2 composite was prepared by the Spark Plasma Sintering (SPS) method in this work. The phase transformation and interface cracking of this composite under ion irradiation (single Xe, Xe + He, and Xe + He + H ions) and subsequent annealing were analyzed using transmission electron microscopy (TEM), mainly focusing on the interface regions. Xe ion irradiation resulted in the formation of high-density stacking faults in the TiC coatings and the complete amorphization of SiC fibers. The implanted H ions exacerbated interface coarsening. After annealing at 900 °C for 2 h, the interface in the Xe + He + H ion-irradiated samples was seriously damaged, resulting in the formation of large bubbles and cracks. This damage occurred because the H atoms reduced the surface free energy, thereby promoting the nucleation and growth of bubbles. Due to the absorption effect of the SiCf/TiC interface on defects, the SiC fiber areas near the interface recovered back to the initial nano-polycrystalline structure after annealing.

Fractal formalism in crystallized-Ge via Al induced crystallization under ion irradiation

The fractal characterization of polycrystalline-Ge formed via Al induced crystallization under ion irradiation is presented. The polycrystalline (p-) Al (50 nm)/amorphous (a-) Ge (50 nm) is irradiated using 1000 keV Xe+ ions with fluences of 7 × 1014 ions/cm2, 3 × 1015 ions/cm2 and 1 × 1016 ions/cm2 followed by post-thermal annealing at 200 °C. The pristine (i.e., as-prepared) sample is also thermally annealed for comparison purposes. The X-ray diffraction measurement confirms the crystallization of Ge after thermal annealing in both pristine and ion irradiated samples whereas only ion irradiation does not show any crystallization of Ge. The optical micrograph and field emission scanning electron microscopy (FE-SEM) images show dotted like structures on the surface of the film which are found to increase with increasing ion fluence. The Rutherford backscattering spectrometry and energy dispersive X-ray spectroscopy confirm the layer exchange phenomena at the interface in the p-Al/a-Ge bilayer system with Ge crystallization. The fractal analyses have been carried out on FE-SEM images which confirms the Ge fractals formation due to crystallization of Ge followed by layer exchange. The fractal dimension and hurst exponent are calculated and found that the surface roughness decreases with increasing ion fluence up to the fluence of 3 × 1015 ions/cm2 and then increases at higher fluence.

An improved approach to decouple the indentation size effect from nanoindentation hardness of ion-irradiated samples

An improved approach to decouple the indentation size effect from nanoindentation hardness of ion-irradiated samples

Infrared spectroscopic study on Nb-ion-irradiated MgB2 thin films

Magnesium diboride (MgB2) is a two-band superconductor with a high superconducting critical temperature (Tc) of approximately 39 K. Owing to the lack of vortex pinning centers, MgB2 exhibits an abrupt decline in the critical current density (Jc) in an applied magnetic field. Here, we prepared 1 MeV Nb ion-irradiated MgB2 thin-film samples with doses of 3×1013, 7×1013, and 9×1013 ions/cm2. Temperature-dependent magnetization and x-ray diffraction (XRD) measurements were performed to determine the Tc and c-axis lattice constant of each sample. Furthermore, a Fourier transform infrared (FTIR) spectroscopy was performed to obtain the infrared properties of the Nb-ion-irradiated MgB2 thin-film samples. The optical conductivity of each sample in the low-energy region was fitted with two (narrow and broad) Drude modes. We found that the spectral weight redistribution from the low-to high-frequency regions and the broadening of the narrow Drude mode caused by irradiation are closely related to the reduction in Tc.

Extending damage accumulation of commercial reactor irradiated 316 stainless steel with ion irradiation

Austenitic 316 stainless steel flux thimble tubes (FTTs) removed from a commercial pressurized water reactor (PWR) were re-irradiated using nickel ions to evolve the irradiated microstructure to higher damage levels than those achieved in reactor. The microstructures of the neutron-plus-ion irradiated samples were compared with those of neutron irradiated only samples at the same doses to evaluate the effectiveness of ion irradiation to extend the damage range and match that created in reactor. Ion irradiations effectively captured, both qualitatively and semi-quantitatively, the evolution of dislocation loops, nanocavities, nanocluster size and density, and radiation-induced segregation (RIS) with dose. Only Ni-Si clusters were observed in ion irradiated FTT samples while Ni-Si-Mn clusters that were frequently observed in reactor irradiated samples above ∼41 dpa were absent in ion irradiated samples probably due to ballistic mixing at the high ion irradiation damage rate. Two samples were ion irradiated to ∼160 dpa to predict the irradiated microstructure that may develop due to an increase of the damage accumulation by extending a PWR life from 40 years to 60 years. The extended ion irradiation results indicated that significant microstructure changes were unlikely to occur even to very high doses near common PWR relevant temperature conditions. Overall, the microstructure resulting from ion irradiation following neutron irradiation matched that of neutron to the same dose reasonably well in most cases.

Real-Time Observation of Nanoscale Kink Band Mediated Plasticity in Ion-Irradiated Graphite: An In Situ TEM Study.

Graphite IG-110 is a synthetic polycrystalline material used as a neutron moderator in reactors. Graphite is inherently brittle and is known to exhibit a further increase in brittleness due to radiation damage at room temperature. To understand the irradiation effects on pre-existing defects and their overall influence on external load, micropillar compression tests were performed using in situ nanoindentation in the Transmission Electron Microscopy (TEM) for both pristine and ion-irradiated samples. While pristine specimens showed brittle and subsequent catastrophic failure, the 2.8 MeV Au2+ ion (fluence of 4.378 × 1014 cm-2) irradiated specimens sustained extensive plasticity at room temperature without failure. In situ TEM characterization showed nucleation of nanoscale kink band structures at numerous sites, where the localized plasticity appeared to close the defects and cracks while allowing large average strain. We propose that compressive mechanical stress due to dimensional change during ion irradiation transforms buckled basal layers in graphite into kink bands. The externally applied load during the micropillar tests proliferates the nucleation and motion of kink bands to accommodate the large plastic strain. The inherent non-uniformity of graphite microstructure promotes such strain localization, making kink bands the predominant mechanism behind unprecedented toughness in an otherwise brittle material.

Unraveling the effect of 600 keV carbon ion irradiation on the structural and magnetic properties of ZnO thin film

600 keV 12C+ carbon ions have been irradiated upon 800 nm thin ZnO film. The thin ZnO films have been grown by pulsed laser deposition technique upon SiO2/Si substrate. The glancing incidence X-ray diffraction study exhibits the hexagonal wurtzite crystal structure of ZnO, having space group P63mc. Systematic X-ray diffraction analysis of both unirradiated and irradiated samples, reveals that the strain decreases in the sample post irradiation. Room temperature magnetization studies have been performed using SQUID-VSM. As the 600 keV carbon ion fluence is varied, an onset of ferromagnetic ordering in the ZnO thin film is observed. The maximum average magnetic moment induced by each carbon ion is found to be about 6.71 μB. X-ray photoelectron spectroscopy has been utilized to analyze the oxidation state of the C/O/Zn, which also rules out the presence of any transition metal elements in carbon ions irradiated ZnO thin film samples. The chemical and structural analysis of the samples have been examined by Raman spectroscopy. It reveals a red shift in A1 (LO) mode, which confirms the presence of tensile strain in the sample post irradiation. These experimental results, clearly indicate that oxygen vacancies and strain in the film trigger the onset of ferromagnetism in the ZnO thin film system.

Effects of Ion Irradiation and Temperature on Mechanical Properties of GaN Single Crystals under Nanoindentation.

Understanding the impact of irradiation and temperature on the mechanical properties of GaN single crystals holds significant relevance for rational designs and applications of GaN-based transistors, lasers, and sensors. This study systematically investigates the influence of C-ion irradiation and temperature on pop-in events, hardness, Young's modulus, and fracture behavior of GaN single crystals through nanoindentation experiments. In comparison with unirradiated GaN samples, the pop-in phenomenon for ion-irradiated GaN samples is associated with a larger critical indentation load, which decreases with increasing temperature. Both unirradiated and ion-irradiated GaN samples exhibit a decline in hardness with increasing indentation depth, while Young's moduli do not exhibit a clear size effect. In addition, intrinsic hardness displays an inverse relationship with temperature, and ion-irradiated GaN single crystals exhibit greater intrinsic hardness than their unirradiated counterparts. Our analysis further underscores the significance of Peierls stress during indentation, with this stress decreasing as temperature rises. Examinations of optical micrographs of indentation-induced fractures demonstrate an irradiation embrittlement effect. This work provides valuable insights into the mechanical behavior of GaN single crystals under varying irradiation and temperature conditions.

Micro/nano mechanical properties differences of shallow irradiation damage layer revealed by a combined experimental and MD study

Micropillar compression and nanoindentation techniques are both adopted to measure the mechanical properties in multi-energy He ion-irradiated Ni-based samples to study their relationship, and a distinct variation is observed. TEM characterization of the microstructure evolution and calculations based on the DBH model indicate that irradiation defects are not responsible for the observed variation. Subsequently, a comparative analysis of these two methods is simulated and their mechanisms are investigated using MD. Several factors, including activation of various slip systems, plastic area, and surface absorption, account for the differences observed in indentation and pillar compression tests, leading to the distinct evolution of internal initial dislocation lines, which significantly contribute to additional hardening in indentation tests.

Readdressing nanocavity diffusion in tungsten

In nuclear fusion (ITER and the future DEMO), those components that face the plasma are exposed to high temperature and irradiation which, in the long term, modifies their thermal and mechanical properties and tritium retention. Tungsten is a candidate material and is the subject of many studies of microstructure evolution under various irradiation and temperature conditions. One milestone is the characterization of its defect properties. We here readdress the diffusion of nanocavities on broad ranges of size and temperature and compare it with dissociation, a competing process during nanocavity growth. First, at the atomic scale, we used molecular dynamics to explore the variety of elementary events involved in the nanocavity diffusion. Second, an experimental study of ion-irradiated samples, annealed at different temperatures up to 1,773 K, revealed the creation and growth of nanocavities on transmission electron microscopy images. Third, we performed multi-objective optimization of the nanocavity diffusion input of our object kinetic Monte Carlo model to reproduce the experimental results. Finally, we applied a sensitivity analysis of the main inputs of our model developed for these particular conditions—the source term which combines two cascade databases and the impurities whose interaction with the defects is characterised with a supplemented database of density functional theory calculations. Three domains of nanocavity size were observed. The first is the small vacancy clusters, for which atomistic calculations are possible and dissociation is negligible. The second is the small nanocavities, for which we provide new diffusion data and where a competition with the dissociation can take place. The third domain is the large nanocavities, for which, in any case, the dissociation prevents their existence above 1,500 K in the absence of a stabilizing interface.

Microstructural Characterization of Reactor Pressure Vessel Steels

Ion irradiation is a promising tool to emulate neutron-irradiation effects on reactor pressure vessel (RPV) steels, especially in the situation of limited availability of suitable neutron-irradiated material. This approach requires the consideration of ion-neutron transferability issues, which are addressed in the present study by comparing the effect of ions with neutron-irradiation effects reported for the same materials. The first part of the study covers a comprehensive characterization, based on dedicated electron microscopy techniques, of the selected unirradiated RPV materials, namely a base metal and a weld. The results obtained for the grain size, dislocation density, and precipitates are put in context in terms of hardening contributions and sink strength. The second part is focused on the depth-dependent characterization of the dislocation loops formed in ion-irradiated samples. This work is based on scanning transmission electron microscopy applied to cross-sectional samples prepared by the focused ion beam technique. A band-like arrangement of loops is observed in the depth range close to the peak of injected interstitials. Two levels of displacement damage, 0.1 and 1 dpa (displacements per atom), as well as post-irradiation annealed conditions, are included for both RPV materials. Compared with neutron irradiation, ion irradiation creates a similar average size but a higher number density of loops presumably due to the higher dose rate during ion irradiation.

Change in the gas sensing mechanism and improved sensing response on ion-irradiated palladium-graphene oxide nanocomposite

In this study, we synthesized Pd-graphene oxide (Pd-GO) nanocomposite layers on SiO2/Si substrates using chemical method. Pd-GO layers were treated with swift heavy ion irradiation (100 MeV Ag ions, 1013 ions/cm2). The structural properties of the pristine as well as the ion irradiated samples were investigated using synchrotron grazing incidence x-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) techniques. XRD shows peaks corresponding to Pd (FCC, space group-Fd-3m), GO and synthetic graphite. The relative graphite peak intensities increased after ion irradiation, indicating reduction of GO. The sensor responses of nanocomposite layers towards exposure of 35 ppm H2 at 100 °C, were measured for several cycles. Ion-irradiated Pd-GO samples show enhancement in the sensing response of H2 gas by about 24% and with lower recovery times (25%), as compared to pristine Pd-GO nanocomposite samples. The change in type of conductivity from p-type gas sensing layer in pristine nanocomposite to n-type conductivity, along with an increase in conductivity (about 500 times) in ion irradiated samples were observed. The change in type of conductivity on ion-irradiation is attributed to the reduction of GO layer and the changes in conductivity on hydrogen exposure is explained due to hydrogen spill-over effect in the two-component system. The improvement in sensitivity upon ion-irradiation was due to the increase in concentration of structural defects due to electronic energy loss, as studied by SRIM simulation. This study points towards using ion induced electronic energy loss as a new tool for varying the gas sensing properties of GO based sensors.

Effect of low energy cesium ion irradiation on vanadium oxide: Structural and spectroscopic study

Vanadium di-oxide (VO2) and vanadium tetra oxide (V2O4) powders are exposed to cesium (Cs) ion irradiation using Pelletron accelerator. The energy of the Cs ions ranges from 0.2 keV to 5 keV. Mass spectroscopic data from the accelerator is plotted for various energy ranges. Un-irradiated samples and Cs ion irradiated samples are characterized by using x-ray diffraction (XRD), scanning electron microscope (SEM), Raman spectroscopy and four-point probe method. XRD analysis showed improved VO2 crystallinity after ion irradiation. The V2O4 sample shows amorphous behavior after ion irradiation. Dislocation density and tolerance are calculated to explore structure distortion after ion irradiation. Raman spectroscopy reveals vibrational and rotational modes of bonding with oxygen and vanadium. SEM results explain the reduction in agglomeration after Cs ion irradiation. The resistivity of un-irradiated and irradiated (VO2 and V2O4) samples is calculated by four-point probe method. The resistivity of vanadium oxide is decreased after Cs ion irradiation to make it a potential candidate for optoelectrical applications.

Formation of vacancy-type defects and hydride introduced by irradiation in pure titanium

The effect of hydrogen ion irradiation on the formation of hydride and vacancy-type defects in pure titanium was investigated by X-ray diffraction (XRD), Doppler broadening spectrum (DBS), and coincidence Doppler broadening spectrum (CDB) based on slow positron beam. The XRD results showed that γ-TiH was observed in single hydrogen ion-irradiated and hydrogen + deuterium (H + D) sequentially irradiated specimens but not in the single deuterium plasma-implanted sample. This finding indicates that the vacancy-type defects caused by H ion irradiation greatly promoted the formation of γ-TiH. The DBS results showed that for the single D plasma-implanted sample, the damage peak was closer to the surface region and lower compared to the other two samples containing γ-TiH, indicating that vacancy generated by lattice distortion didn't diffuse to the depth of the matrix, and the concentration of that was smaller, which was not conducive to the deuteride formation. For the H + D sequentially irradiated sample, the number of hydrogen-vacancy complexes (HmVn) further increased compared with the single H ion-irradiated sample. Thus, the effective volume of vacancy defects was reduced, which led to the decrease in the S parameter.

Paramagnetic Defects and Thermoluminescence in Irradiated Nanostructured Monoclinic Zirconium Dioxide.

The ESR spectra of nanostructured samples of monoclinic ZrO2 irradiated by electrons with energies of 130 keV, 10 MeV, and by a beam of Xe ions (220 MeV) have been studied. It has been established that irradiation of samples with electrons (10 MeV) and ions leads to the formation of radiation-induced F+ centers in them. Thermal destruction of these centers is observed in the temperature range of 375-550 K for electron-irradiated and 500-700 K for ion-irradiated samples. It is shown that the decrease in the concentration of F+ centers is associated with the emptying of traps responsible for thermoluminescence (TL) peaks in the specified temperature range. In the samples irradiated with an ion beam, previously unidentified paramagnetic centers with g = 1.963 and 1.986 were found, the formation of which is likely to involve Zr3+ ions and oxygen vacancies. Thermal destruction of these centers occurs in the temperature range from 500 to 873 K.

Nanoindentation applied to ion-irradiated and neutron-irradiated Fe-9Cr and Fe-9Cr-NiSiP model alloys

Nanoindentation of ion-irradiated materials has attracted much interest as a tool envisaged to derive the dose dependence of bulk-equivalent hardness from small samples. A major challenge arises from the steep damage gradient in the thin ion-irradiated layer and its unavoidable interplay with the indentation size effect. The present study relies on a number of choices aimed at simplifying the interpretation of the results and strengthening the conclusions. The studied alloys are two ferritic Fe-9Cr model alloys differing in controlled amounts of Ni, Si, and P known to enhance irradiation hardening. Both ion-irradiated (5 MeV Fe2+ ions) and neutron-irradiated samples along with the unirradiated references were investigated using Berkovich tips. According to the collaborative nature of the study, tests were conducted in two different laboratories using different equipment. A generalized Nix–Gao approach was applied to derive the bulk-equivalent hardness and characteristic length scale parameters for the homogeneous unirradiated and neutron-irradiated samples. Comparison with Vickers hardness indicates a 6% overestimation of the bulk-equivalent hardness as compared to the ideal correlation. For the case of ion irradiation, a first model assumes a homogeneous irradiated layer on a homogeneous substrate, while a second model explicitly takes into account the damage gradient. The first model was combined with both the original and the generalized Nix–Gao relation. We have found that the results revealed for Fe-9Cr vs Fe-9Cr-NiSiP are compatible with expectations based upon known irradiation-induced microstructures. The bulk-equivalent hardness derived for ion-irradiated samples reasonably agrees with the observation for neutron-irradiated samples.

Linearly Modulated OSL in K\(_{3}\)Na(SO\(_{4}\))\(_{2}\):Eu\(^{3+}\) Phosphor Irradiated With 48 MeV Li\(^{3+}\) and 85 MeV C\(^{6+}\) Swift Heavy Ions Beam

K\({}_{3}\)Na(SO\({}_{4}\))\({}_{2}\):Eu\({}^{3+}\) shows OSL when irradiated with swift heavy ion beams of Li\({}^{3+}\) and C\({}^{6+}\) at different fluences. The micro sample is prepared through solid state diffusion method along with its counter parts of ball milled (7 days) nanophosphor and co-precipitated nanophosphor samples. The material was characterized by XRD to confirm its formation in a single phase. Comparison of the experimental data with that of the data available in the literature (JCPDS data file \#74 0398) shows formation of a single hexagonal phase, with the space group P3 m1. Study on the particle size effect shows that particle size in the 75--106 \(\mu\)m rangeis more suitable for the linearly modulated-optically stimulated luminescence (LM-OSL) dosimetry in micro form. Dosimetric properties of the phosphor material using LM-OSL technique for blue light stimulation (\(\lambda=470\) nm and \(t=120$\) seconds) show that it is highly sensitive in the linear dose range. Here in this paper, we tried to find a relationship between detrapping probabilities and photoionization cross section using curve fitting (deconvolution) method. We also calculated and converted the fluence into doses using SRIM software. Data are presented indicating that the LM-OSL peak is composed of three overlapping components originating from populated traps with optical cross sections of 10\({}^{-17}\)-10\({}^{-18}\) cm\({}^{2}\). It was found that micro and ball milled nanophosphor Carbon ion beam irradiated samples dominates the photoionization cross section as compared with lithium ion irradiated samples, but co-precipitated sample is dominant in lithium irradiated samples. Which infers about the different trapping level formation and also recombination processes involved during the preparation and in readouts of samples.

Solubility enhancement and Au-Ni bimetallic alloy formation in immiscible Au/Ni multilayers by ion irradiation

In the present work, we investigated ion beam mixing and grain growth induced in [Au/Ni] × 5 /Si multilayer by 500 keV Xe ion irradiation at different fluence values, using Field Emission Scanning Electron Microscopy (FESEM), X-ray Diffraction (XRD) and Rutherford Backscattering (RBS). Ion-induced grain growth has been evidenced using FESEM analysis and successfully compared to previous experiments and theoretical models. RBS showed total mixing and significant surface sputtering. XRD measurements offered an excellent way to bring light on ion beam mixing kinematics and new phases formation. Thermal spike model calculations combined with the available experimental results in literature of mixing rates enabled us to estimate the diffusivity and examine the validity of inter-diffusion in liquid state. For present work, the atomic diffusivity was estimated to 1.86 × 10-3 cm2/s. The thermal spike model predicted no intermixing for 100 MeV swift heavy Au ion irradiated samples, in good agreement with experimental results.

Behavior of helium cavities in ion-irradiated W-Ni-Fe ductile-phase toughened tungsten

This study reports on the distribution of helium (He) cavities in a hot-rolled W-Ni-Fe ductile-phase toughened tungsten (DPT W) composite irradiated to a dose and a helium concentration that are comparable to those in the material after 5-year irradiation in a conceptual fusion power plant. The DPT W sample consists of W particles embedded in a ductile-phase NiFeW matrix with a nominal composition of 90W-7Ni-3Fe by weight. It was hot-rolled to a thickness reduction by 87% (87R DPT W). Sequential and individual irradiations of the material with 1.2 MeV Ni+ ions to a fluence of 2.15 × 1016 Ni+/cm2 and 90 keV He+ ions to 6.5 × 1015 He+/cm2 was performed at 973 K. Larger He cavities with a lower number density are observed in NiFeW than W. Helium cavities are aggregated preferentially along the NiFeW/W interphase boundary. This behavior is not observed along the W/W grain boundary under the same irradiation conditions. The average corrected cavity diameter or volume appears to be smaller in the sequentially irradiated sample than He+ ion irradiated sample. There is no evidence for formation of visible voids or Ni precipitates in W phase irradiated with Ni+ ions only. Diffusion, clustering and trapping of vacancies and He atoms during He+ ion irradiation at 973 K may be responsible for the formation of the He cavities.

Change in nanoindentation hardness of polycrystalline tungsten irradiated with Fe ions or electrons by hydrogen gas charging

The effects of hydrogen atoms on the hardnesses of unirradiated, ion-irradiated, and electron-irradiated polycrystalline tungsten samples were investigated using nanoindentation tests. The bulk equivalent hardnesses of the unirradiated and electron-irradiated tungsten samples did not change upon hydrogen charging. The bulk equivalent hardness of the ion-irradiated tungsten increased upon the hydrogen charging. The number of hydrogen atoms trapped at dislocation loops was very small. We estimated that the hydrogen occupancy in vacancy clusters was 0.24−0.45 (in the case of tri-vacancies, the number of hydrogen atoms trapped per vacancy (H/V) is 1.04−1.95). Because of the irradiation temperature of 573 K, the density and size of irradiation-induced defects did not change during hydrogen charging at 543 K. Therefore, the hardening was mainly caused by an increase of approximately 8 − 11% in the obstacle strength α of vacancy clusters containing hydrogen atoms. The ion-irradiated area hardened upon the hydrogen charging and changed the configuration of the pile-up. Observation of the dislocation structure is required to clarify the mechanism of hardening caused by hydrogen charging.