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High Entropy Alloys (HEAs) are prospective materials for nuclear fusion reactors and were irradiated in this study at a broad range of energetic ion fluences. Different ion masses (Cu and Au ions) and energies (3 and 5 MeV) were selected to investigate dpa (displacement per atom) development, radiation defect accumulation based on prevailing collision processes (Au ions) and ionization processes (Cu ions) in various HEAs. The studied HEAs differ in terms of elemental composition, internal morphology (grain structure) and other modifiers. Dpa values of 1 to ∼66 were achieved at Cu and Au ion fluences from 4 × 1014 to 1.3 × 1016 ions.cm−2 at room temperature, which generated varying levels of lattice damage. Theoretical simulations were performed to estimate the energy stopping and dpa depth distribution using SRIM code and compared with Au-concentration depth profiles determined by Rutherford backscattering spectrometry for Au-ions with 3 MeV ion energy. The prevailing energy losses of ions via ionization processes for Cu-5 MeV ions were found to increase the damage through lattice strain and probable lattice distortion, although the main defect introduction is expected to occur via collisions during nuclear stopping. Structural modification and defect accumulation were investigated by positron annihilation spectroscopy (PAS), which revealed a broader damaged layer with defects, where HEA-Nb (NbCrFeMnNi) exhibited the least damage accumulation from chosen alloys with no strong relation to the Au-5 MeV ion implantation fluence, whereas strong defect accumulation was recorded in the Au-ion implanted Eurofer97 used for comparison and HEA-Co (CoCrFeMnNi). PAS analysis also allowed defect sizes to be determined as an additional structural characteristic. The observed trends were also confirmed by thermal property analysis, with a worsening of thermal effusivity recorded after the irradiation in HEA-Co and Eurofer97. The worsening of the thermal properties was confirmed by the layer thickness, where the layer identified by PAS was found to be broader than the SRIM theoretical predictions. Nanoindentation measurements confirmed less pronounced radiation hardening of HEA-Nb relative to that observed in HEA-Co and Eurofer97. Transmission Electron Microscopy (TEM) analysis revealed layer thicknesses in reasonable agreement with the dpa depth profiles. The thermal effusivity decreased in the surface-irradiated layer in all investigated samples, the least influenced material was HEA-Nb.

In this study, novel flexible micro-scale humidity sensors were directly fabricated in graphene oxide (GO) and polyimide (PI) using ion beam writing without any further modifications, and then successfully tested in an atmospheric chamber. Two low fluences (3.75 × 10 14 cm -2 and 5.625 × 10 14 cm -2 ) of carbon ions with an energy of 5 MeV were used, and structural changes in the irradiated materials were expected. The shape and structure of prepared micro-sensors were studied using scanning electron microscopy (SEM). The structural and compositional changes in the irradiated area were characterized using micro-Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), Rutherford back-scattering spectroscopy (RBS), energy-dispersive X-ray spectroscopy (EDS), and elastic recoil detection analysis (ERDA) spectroscopy. The sensing performance was tested at a relative humidity (RH) ranging from 5% to 60%, where the electrical conductivity of PI varied by three orders of magnitude, and the electrical capacitance of GO varied in the order of pico-farads. In addition, the PI sensor has proven long-term sensing stability in air. We demonstrated a novel method of ion micro-beam writing to prepare flexible micro-sensors that function over a wide range of humidity and have good sensitivity and great potential for widespread applications.

The structural differences in (100)-, (110)- and (111)-oriented cubic yttria-stabilised zirconia (YSZ) single crystals after implantation with 2 MeV Si + ions at the fluences of 5 × 10 15 , 1 × 10 16 and 5 × 10 16 cm -2 were studied using Rutherford backscattering spectrometry in the channelling mode (RBS-C), X-ray diffraction (XRD) and Raman spectroscopy. The RBS-C results show that the damage accumulation in the 〈110〉 direction exhibits a lower level of disorder (<0.3) than the other orientations (<0.6) and it seems that the (110) crystallographic orientation is the most resistant to radiation damage. The experimental results from the RBS measurement were compared with the results from the XRD measurements. The XRD data were analysed using the standard two-beam dynamical X-ray diffraction theory and the pure isotropic strain was deduced from the fit for the fluence of 5 × 10 15 cm -2 . It was shown that the maximum value of the isotropic strain does not depend on the surface orientation. The increase in signal intensity at ∼689 cm -1 is probably related to an increase in implantation defects such as oxygen vacancies.

Self-assembled surface nanoscale structures on various ZnO facets are excellent templates for the deposition of semiconductor quantum dots and manipulation with surface optical transparency. In this work, we have modified the surface of c -, m - and a -plane ZnO single-crystals by high-energy W-ion irradiation with an energy of 27 MeV to observe the aspects of surface morphology on the optical properties. We kept ion fluences in the range from 5 × 10 9 cm -2 to 5 × 10 11 cm -2 using the mode of single-ion implantation and the overlapping impact mode to see the effect of various regimes on surface modification. Rutherford backscattering spectroscopy in the channeling mode (RBS-C) and Raman spectroscopy have identified a slightly growing Zn-sublattice disorder in the irradiated samples with a more significant enhancement for the highest irradiation fluence. Simultaneously, the strong suppression of the main Raman modes and the propagation of the modes corresponding to polar Zn-O vibrations indicate disorder mainly in the O-sublattice in non-polar facets. The surface morphology, analysed by atomic force microscopy (AFM), shows significant changes after ion irradiation. The c - and a -plane ZnO exhibit the formation of small grains on the surface. The m -plane ZnO forms a sponge-like surface for lower fluences and grains for the highest fluence. The surface roughness itself increases with the irradiation fluence as shown by AFM measurement as well as spectroscopic ellipsometry (SE) analysis. The damage caused by high-energy irradiation leads to non-radiative processes and suppression of the near-band-edge peak as well as the deep-level emission peak in the photoluminescence spectra. Furthermore, the refraction index n and the extinction coefficient k of irradiated samples, determined by SE, have features corresponding to the particular exciton states blurred and are slightly lower in the optical bandgap region especially for the polar c -plane ZnO facet.

Three different crystallographic orientations of the wurtzite ZnO structure (labeled as c -plane, a -plane and m -plane) were implanted with Au + ions using various energies and fluences to form gold nanoparticles (GNPs). The ion implantation process was followed by annealing at 600 °C in an oxygen atmosphere to decrease the number of unwanted defects and improve luminescence properties. With regard to our previous publications, the paper provides a summary of theoretical and experimental results, i.e., both DFT and FLUX simulations, as well as experimental results from TEM, HRTEM, RBS, RBS/C, Raman spectroscopy and photoluminescence. From the results, it follows that in the ZnO structure, implanted gold atoms are located in random interstitial positions -experimentally, the amount of interstitial gold atoms increased with increasing ion implantation fluence. During ion implantation and subsequent annealing, the metal clusters and nanoparticles with sizes from 2 to 20 nm were formed. The crystal structure of the resulting gold was not cubic (confirmed by diffraction patterns), but it had a hexagonal close-packed ( hcp ) arrangement. The ion implantation of gold leads to the creation of Zn and O interstitial defects and extended defects with distinct character in various crystallographic cuts of ZnO, where significant O-sublattice disordering occurred in m -plane ZnO.

In this paper, the effect of light ion irradiation on graphene oxide foil structure and composition was studied. Due to the excellent properties of graphene based materials suitable for application in electronics, optoelectronics, micro-mechanics and space technologies, the interaction of energetic ions with graphene based structures is worth studying. From the fundamental point of view, it is also interesting to get information about graphene oxide structure modification and the possible functional properties after irradiation by energetic ions. The light ion irradiation of graphene oxide (GO) foil was performed using 2.5 MeV H + and 5.1 MeV He 2+ ions. The change in the elemental composition of the GO foils after ion irradiation was investigated using Rutherford Backscattering Spectrometry and Elastic Recoil Detection Analysis. The influence of ion irradiation was further studied by microscopy methods. The chemical composition and structural changes of the GO foil surface were characterized by spectroscopy techniques including XPS, FTIR and Raman spectroscopy. Although the results of ion beam analysis indicated no significant compositional changes in the bulk of GO foils connected to ion irradiation, XPS, ATR-FTIR and Raman spectroscopy revealed reduction and removal of oxygen functionalities on the surface of graphene oxide. This reduction leads to a surface resistivity decrease after ion irradiation dependent on the ion species, fluence and energy.

The reduction of graphite oxide is one of the most important reactions in the production of graphene in gram quantities. The mechanisms of these widely used reactions are poorly understood. The mechanism of the chemical reduction of two different graphite oxides prepared by the chlorate (Hofmann method) and permanganate methods (Hummers method) has been investigated. Three different reduction agents, lithium tetrahydridoaluminate, sodium tetrahydridoborate, and lithium tetrahydridoborate, as well as their deuterated counterparts, were used for the reduction of graphite oxide. Reduced graphite oxides were analyzed by scanning electron microscopy, energy-dispersive spectroscopy, elemental combustion analysis, Raman spectroscopy, high-resolution X-ray photoelectron spectroscopy, and simultaneous thermal analysis. The concentration of boron incorporated into graphene was measured by prompt gamma activation analysis. Rutherford back-scattering spectroscopy and elastic recoil detection analysis were used for the determination of the elemental composition, including deuterium concentration, as evidence of CH bond formation., (Copyright © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

Graphane is one of the most intensively studied derivatives of graphene. Here we demonstrate the evaluation of exact degree of graphene hydrogenation using the Clemmensen reduction reaction and deuterium labeling. The Clemmensen reduction reaction is based on application of zinc in an acid environment. It effectively reduces various functional groups (like ketones) present in graphite oxide. However, the mechanism of reduction is still unknown and elusive. Here we bring a major insight into the mechanisms of the Clemmensen reduction via deuterium labeling and the topochemical approach applied on graphite oxide. The use of deuterated reactants and the exact measurement of deuterium concentration in reduced/hydrogenated graphene by nuclear methods can be used for accurate estimation of C-H bond abundance in graphene. Various topochemical configurations of experiments showed that the reduction of a ketonic group proceeds in contact with the zinc metal by a carbenoid mechanism. Our results showed that the application of nuclear methods of isotope analysis in combination with deuterium labeling represents a very effective tool for investigation of graphene based materials. Our results demonstrate that graphene based materials can also be effectively used for the investigation of organic reaction mechanisms, because the robust structure of graphene allows the use of various spectroscopic techniques which could not be applied on small organic molecules.

For the past decade, researchers have been trying to understand the mechanism of the thermal reduction of graphite oxide. Because deuterium is widely used as a marker in various organic reactions, we wondered if deuterium-labeled graphite oxide could be the key to fully understand this mechanism. Graphite oxides were prepared by the Hofmann, Hummers, Staudenmaier, and Brodie methods, and a deuterium-labeled analogue was synthesized by the Hofmann method. All graphite oxides were analyzed not only using the traditional techniques but also by gas chromatography-mass spectrometry (GC-MS) during exfoliation in hydrogen and nitrogen atmospheres. GC-MS enabled us to compare differences between the chemical compositions of the organic exfoliation products formed during the thermal reduction of these graphite oxides. Nuclear analytical methods (Rutherford backscattering spectroscopy, elastic recoil detection analysis) were used to calculate the concentrations of light elements, including the ratio of hydrogen to deuterium. Combining all of these results we were able to determine graphite oxide's thermal reduction mechanism. Carbon dioxide, carbon monoxide, and water are formed from the thermal reduction of graphite oxide. This process is also accompanied by various radical reactions that lead to the formation of a large amount of carcinogenic volatile organic compounds, and this will have major safety implications for the mass production of graphene.