Publikationen - Ionenstrahlbeschleuniger
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The absence of metamictisation in natural monazite
Nasdala, L.; Akhmadaliev, S.; Burakov, B. E.; Chanmuang N, C.; Škoda, R.
The actinide-containing mineral monazite–(Ce) is a common accessory rock component that bears petrogenetic information, is widely used in geochronology and thermochronology, and is considered as potential host material for immobilisation of radioactive waste. Natural samples of this mineral show merely moderate degrees of radiation damage, despite having sustained high self-irradiation induced by the decay of Th and U (for the sample studied herein 8.9 ± 0.3 × 1019 α/g). This is assigned to low damage-annealing temperature of monazite–(Ce) and “alpha-particle-assisted reconstitution”.
Here we show that the response of monazite–(Ce) to alpha radiation changes dramatically, depending on the damage state. Only in radiation-damaged monazite–(Ce), 4He ions cause gradual structural restoration. In contrast, its high-temperature annealed (i.e. well crystalline) analogue and synthetic CePO4 experience He-irradiation damage. Alpha-assisted annealing contributes to preventing irradiation-induced amorphisation (“metamictisation”) of monazite–(Ce); however, this process is only significant above a certain damage level.
Scientific Reports 10(2020), 14676
Heavy ion irradiation damage in Zr3(Al0.9Si0.1)C2 MAX phase
Qarra, H. H.; Knowles, K. M.; Vickers, M. E.; Zapata-Solvas, E.; Akhmadaliev, S.
A Zr3(Al0.9Si0.1)C2 MAX phase-based ceramic with 22 wt.% ZrC and 10 wt.% Zr5Si3 has been irradiated with 52 MeV I9+ ions at room temperature, achieving a maximum dose of 8 displacements per atom (dpa). The response of this MAX phase-rich material to irradiation has been studied using scanning electron microscopy, transmission electron microscopy and X-ray diffraction techniques. Post-irradiation examination of the material revealed a number of crystalline changes to the MAX phase. At low doses, Zr3(Al0.9Si0.1)C2 maintained a high degree of crystallinity, while at the highest doses, its degree of crystallinity was reduced significantly. A number of radiation-induced phase transformations were observed, including the decomposition of Zr3(Al0.9Si0.1)C2 into ZrC and other phases, and the formation of β-Zr3(Al,Si)C2, a MAX phase with a rearranged stacking sequence. Microstructural examination revealed that the majority of the extended defects in Zr3(Al0.9Si0.1)C2 lie in the (0001) basal planes. Analysis of X-ray diffraction profiles after heat treating the 8 dpa-irradiated material for 1 h at 300 °C and at 600 °C showed that there were only subtle changes to the profiles relative to that of the 8 dpa-irradiated material which had not been heat treated. Overall, the experimental results of this study show that the Zr3(Al0.9Si0.1)C2 MAX phase responds less well to irradiation relative to other MAX phases irradiated with high energy heavy ions at room temperature.
Journal of Nuclear Materials 540(2020), 152360
Hybrid graphene-based material promising target in laser matter interaction
Cutroneo, M.; Torrisi, L.; Badziak, J.; Rosinski, M.; Torrisi, A.; Fazio, M.; Sofer, Z. E.; Böttger, R.; Akhmadaliev, S.
Graphene oxide foils implanted with copper ions at low energy and high dose, have been proposed as hybrid graphene-based materials suitable to be laser irradiated in vacuum to produce hot plasmas. The special lattice structure of the graphene oxide foil can improve the propagation of the laser accelerated electrons inside the foil and to enhance the electron density emerging from the rear foil surface. In such conditions the electric field developed in the non-equilibrium plasma increases and consequently in the forward ion acceleration. The foils have been optimized in thickness and they were irradiated with optimized laser parameters in order to produce high energy and quasi-monoenergetic proton beams by the femtosecond laser at the Institute of Plasma Physics and Laser Microfusion in Warsaw, Poland. Gaf chromic film and silicon carbide detectors were used to monitor the plasma properties and to measure the velocity of the emitted protons and carbon ions from plasma.
Keywords: Data analysis; Lasers
Journal of Instrumentation 15(2020)1, C01021
Radiation damage tolerance of a novel metastable refractory high entropy alloy V2.5Cr1.2WMoCo0.04
Patel, D.; Richardson, M. D.; Jim, B.; Akhmadaliev, Sh.; Goodall, R.; Gandy, A. S.
A novel multicomponent alloy, V2.5Cr1.2WMoCo0.04, produced from elements expected to favour a BCC crystal structure, and to be suitable for high temperature environments, was fabricated by arc melting and found to exhibit a multiphase dendritic microstructure with W-rich dendrites and V-Cr segregated to the inter-dendritic cores. The as-cast alloy displayed an apparent single-phase XRD pattern. Following heat treatment at 1187 °C for 500 h the alloy transformed into three different distinct phases - BCC, orthorhombic, and tetragonal in crystal structure. This attests to the BCC crystal structure observed in the as-cast state being metastable. The radiation damage response was investigated through room temperature 5 MeV Au+ ion irradiation studies. Metastable as-cast V2.5Cr1.2WMoCo0.04 shows good resistance to radiation induced damage up to 40 displacements per atom (dpa). 96 wt% of the as-cast single-phase BCC crystal structure remained intact, as exhibited by grazing incidence X-ray diffraction (GI-XRD) patterns, whilst the remainder of the alloy transformed into an additional BCC crystal structure with a similar lattice parameter. The exceptional phase stability seen here is attributed to a combination of self-healing processes and the BCC structure, rather than a high configurational entropy, as has been suggested for some of these multicomponent "High Entropy Alloy" types. The importance of the stability of metastable high entropy alloy phases for behaviour under irradiation is for the first time highlighted and the findings thus challenge the current understanding of phase stability after irradiation of systems like the HEAs.
Keywords: High entropy alloy (HEA); Structural materials; Ion implantation; Radiation damage; Metastability
Journal of Nuclear Materials 531(2020), 152005
Diamond-blade diced trapezoidal ridge waveguides in YCOB crystal for second harmonic generation
Chen, C.; Lu, Q.; Akhmadaliev, S.; Zhou, S.
Trapezoidal ridge waveguides have been fabricated in YCOB nonlinear optical crystals by carbon ion irradiation and precise diamond-blade dicing. The diced ridges with smooth side-walls allow for near-infrared (1064 nm) light guiding with propagation losses around 1 dB/cm. Refractive index profile of a waveguide has been reconstructed in a reasonable manner. Green second harmonic light have been generated at room temperature via type I birefringent phase matching. Under the pump of continuous and pulsed lasers, conversion efficiencies for guided-wave frequency doubling can be up to ~1.10% Wsup-1 and ~6.22%, respectively.
Keywords: Trapezoidal ridge waveguides; YCOB crystal; SHG
Optics and Laser Technology 126(2020), 106128
Tuning Tailored Single-Walled Carbon Nanotubes by Highly Energetic Heavy Ions
Carbon-based nanomaterials have attracted a lot of interest lately due to their highly promising applications. Here, we report on the modifications of single-walled carbon nanotubes (SWCNTs) induced by swift (highly energetic) heavy ions. Using scanning force microscopy and Raman spec- troscopy, we observed a dramatic change in the structure of the irradiated SWCNTs, accompanied by an increase of the adhesion force as a function of ion fluence and electronic energy loss. With increasing ion fluence the SWCNTs exhibit a partial transformation from metallic to more semicon- ducting. Moreover, at high fluence they break into segments of 10–20 nm length.
Keywords: Swift Heavy Ion; Ion Irradiation; Carbon Nanotubes
Physical Review Applied 13(2020)4, 044073
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Commercial applications of research institute Tandem accelerators: the Rossendorf example
The Ion Beam Center (IBC) at the Helmholtz-Zentrum Dresden-Rossendorf (HZDR) is a unique user facility with decades of experience applying ion beams for materials analysis and modification. The IBC provides ion beams of nearly all stable elements in an unique energy range from some tens of eV up to 60 MeV using tandem accelerators and electrostatic ion implanters, focused ion beam systems, a helium ion microscope, highly-charged ions systems, as well as an accelerator mass spectrometer (AMS) and a secondary ion spectrometer combined with a tandem accelerator. Annually, the IBC offers more than 16.000 hours of beam time for research and industrial purposes to users across the globe. Continuous access to the IBC is permitted via an online proposal procedure [1, 2]. In addition to the beam time, the IBC provides numerous add-on services including sample preparation, clean-room processing, surface and thin film metrology, optical and electron-beam lithography, thermal processing, thin-film deposition, optical and electrical characterization, electron microscopy and spectroscopy, X-ray investigations, as well as simulation of ion-related processes and data evaluation.
Since 2011, the spin-off HZDR Innovation GmbH  shares the IBC equipment and offers fast and direct access to the IBC for commercial services. The activity of the spin-off is focused on the high-energy ion implantation mostly for doping and defect engineering of semiconductors. Up to 8 inch wafers are handled (semi-)automatically at accelerators of IBC under clean room conditions. Many leading international microelectronic companies are customers of HZDR Innovation GmbH. HZDR Innovation GmbH provides an important contribution to the development and production of novel techniques for micro and power electronics, making semiconductor devices more effective and climate-friendly.
Eingeladener Vortrag (Konferenzbeitrag)
NUSPRASEN Workshop on Nuclear Science Applications, 25.-27.11.2019, Helsinki, Finland
Distinct defect appearance in Gd implanted polar and nonpolar ZnO surfaces in connection to ion channeling effect
Jagerová, A.; Malinský, P.; Mikšová, R.; Nekvindová, P.; Cajzl, J.; Akhmadaliev, S.; Holý, V.; Macková, A.
(0001) c-plane, (11-20) a-plane, and m-plane (10-10) ZnO bulk crystals were implanted with 400-keV Gd+ ions using fluences of 5 × 1014, 1 × 1015, 2.5 × 1015, and 5 × 1015 cm-2. Structural changes during the implantation and subsequent annealing were characterized by Rutherford backscattering spectrometry in channeling mode (RBS-C); the angular dependence of the backscattered ions (angular scans) in c-, a-, and m-plane ZnO was realized to get insight into structural modification and dopant position in various crystallographic orientations. X-ray diffraction (XRD) with mapping in reciprocal space was also used for introduced defect identification. Defect-accumulation depth profiles exhibited differences for c-, a-, and m-plane ZnO, with the a-plane showing significantly lower accumulated disorder in the deeper layer in Zn-sublattice, accompanied by the preservation of ion channeling phenomena in a-plane ZnO. Enlargement of the main lattice parameter was evidenced, after the implantation, in all orientations. The highest was evidenced in a-plane ZnO. The local compressive deformation was seen with XRD analysis in polar (c-plane) ZnO, and the tensile deformation was observed in nonpolar ZnO (a-plane and m-plane orientations) being in agreement with RBS-C results. Raman spectroscopy showed distinct structural modification in various ZnO orientations simultaneously with identification of the disordered structure in O-sublattice. Nonpolar ZnO showed a significant increase in disorder in O-sublattice exhibited by E2(high) disappearance and enhancement of A1(LO) and E1(LO) phonons connected partially to oxygen vibrational modes. The lowering of the E2(low) phonon mode and shift to the lower wavenumbers was observed in c-plane ZnO connected to Zn-sublattice disordering. Such observations are in agreement with He ion channeling, showing channeling effect preservation with only slight Gd dopant position modification in a-plane ZnO and the more progressive diminishing of channels with subsequent Gd movement to random position with the growing ion fluence and after the annealing in c-plane and m-plane ZnO.
Keywords: doped c-, a- plane and m-plane ZnO; damage accumulation asymmetry; rare-earth ion implantation; RBS channelling; damage-depth profiling
Journal of Vacuum Science & Technology A 37(2019), 061406
Au incorporation into various ZnO crystallographic cuts realised by ion implantation – ZnO damage characterization
Mackova, A.; Malinsky, P.; Jagerova, A.; Miksova, R.; Nekvindova, P.; Cajzl, J.; Böttger, R.; Akhmadaliev, S.
Non-polar surfaces, such as a-plane (11–20) and m-plane (10-10), for ZnO have become more attractive as numerous efforts have recently been made to grow non-polar ZnO facets for applications in nanoscale photonic devices. Noble-metal incorporation into transparent semiconductors such as ZnO has been investigated because of the non-linear optical response of such structures. This paper presents a study of defect evolution in various ZnO crystallographic cuts caused by Au implantation. The investigation has focused on ZnO structure characterisation, Au distribution and the interior morphology of the a-, m- and c-planes ZnO single crystals implanted with 400 keV Au+ ions at the ion fluences of 5 × 1014 and 1 × 1015 cm−2 and subsequently annealed at 600 °C in O2. The structure modification was studied using Rutherford backscattering spectrometry (RBS) in the channelling mode (RBS/C) and Raman spectroscopy. After the ion-implantation process, low surface damage was observed in all ZnO orientations unlike deep structural damage. Deep structural damage grew with increased Au-ion fluence and Au did not exhibit strong out-diffusion from the depth to the surface during the post-implantation annealing. Small but noticeable differences were observed between different ZnO orientations. RBS measurements during ion implantation revealed more progressive deep-damage formation in the c- and m-planes than in the a-plane ZnO. Simultaneously, the smallest Zn sub-lattice disorder deduced from RBS/C measurements was observed in the a-plane ZnO. During post-implantation annealing, a slight structure recovery (about 4%) was observed in all orientations. Raman spectroscopy confirmed the increasing structure disorder with the enhanced ion fluence for all as-implanted ZnO orientations and a partial reconstruction of the ZnO structure during annealing, when the intensity of E2 phonons was increased and that of longitudinal optical (LO) phonons was suppressed because of the disorder recovery. E2 (high) and E1(LO) Raman phonon modes connected with oxygen sub-lattice ordering/disordering have been investigated in detail – they show a significant modification mainly in the m-plane. The cause of the different behaviour of ZnO planes as well as the differences in the incorporation and movement of Au and Er atoms in the ZnO structure are discussed in the work.
Vacuum 169(2019), 108892
High Temperature and Ion Implantation-Induced Phase Transformations in Novel Reduced Activation Si-Fe-V-Cr (-Mo) High Entropy Alloys
Gandy, A. S.; Jim, B.; Coe, G.; Patel, D.; Hardwick, L.; Akhmadaliev, S.; Reeves-Mclaren, N.; Goodall, R.
For fusion to be realized as a safe, sustainable source of power, new structural materials need to be developed which can withstand high temperatures and the unique fusion radiation environment. An attractive aspect of fusion is that no long-lived radioactive wastes will be produced, but to achieve this structural materials must comprise reduced activation elements. Compositionally complex alloys (CCAs) (also called high entropy alloys, HEAs) are promising candidates for use in extreme environments, including fusion, but few reported to date have low activation. To address these material challenges, we have produced novel, reduced activation, HEAs by arc-melting, and investigated their thermal stability, and radiation damage resistance using 5 MeV Au2+ ion implantation. Whilst the alloys were designed to form single phase BCC, using room temperature and non-ambient in situ X-ray diffraction we have revealed the thermodynamically stable structure of these alloys is in fact a sigma phase. We propose that a BCC phase is formed in these alloys, but at high temperatures (>1000°C). A BCC phase was also formed during heavy ion implantation, which we propose to be due to the rapid heating and cooling that occurs during the thermal spike, effectively freezing in the BCC phase produced by an implantation induced phase transformation. The BCC phase was found to have high hardness and a degree of ductility, making these new alloys attractive in the development of reduced activation HEAs for nuclear applications.
Keywords: high entropy alloy (HEA); reduced activation; phase transformation; ion implantation; thermal stability; nuclear; radiation damage
Frontiers in Materials 6(2019), 146
Heavy ion irradiation damage in Zr2AlC MAX phase
Qarra, H. H.; Knowles, K. M.; Vickers, M. E.; Akhmadaliev, S.; Lambrinou, K.
Zr2AlC MAX phase-based ceramic material with 33 wt% ZrC has been irradiated with 22 MeV Au7+ ions between room temperature and 600 °C, achieving a maximum nominal midrange dose of 3.5 displacements per atom. The response of the material to irradiation has been studied using scanning electron microscopy, transmission electron microscopy and X-ray diffraction. Under room temperature irradiation, the ions caused a partial amorphisation of the MAX phase. At high temperatures, irradiated Zr2AlC remained crystalline, but developed an increased density of dislocations and stacking faults in the (0001) basal planes. The irradiated material also exhibited a temperature-dependent microcracking phenomenon similar to that previously reported in other MAX phase materials.
Journal of Nuclear Materials 523(2019), 1-9
4He irradiation of zircon, ZrSiO4, using a micro-patterned, Si-based energy filter
Nasdala, L.; Akhmadaliev, S.; Chanmuang N., C.; Zowalla, A.; Csato, C.; Rüb, M.
The quantitative evaluation of alpha-particle damage in the mineral zircon, ZrSiO4, using 4He irradiation experiments is difficult because the vast majority of atomic knock-ons in the target are concentrated in a narrow depth range near the ends of the He-ion trajectories. Here we present a new concept to overcome this problem, namely, tailoring the depth profile of damage by means of a micromechanically fabricated “energy filter”. Lamellae of 1.5 μm thickness, prepared from ZrSiO4 using the focused-ion-beam technique, were subjected to irradiation with 8.8 MeV 4He ions. Five irradiations with ion fluences in the range 2.5 × 1015–1 × 1017 cm-2 have resulted in mild to severe damage, as monitored by the broadening and downshift of SiO4-stretching Raman bands. Our results may provide a means for quantifying the contribution of alpha particles to the total self-irradiation damage in zircon.
Keywords: Radiation damage; Helium irradiation; Energy filter; Focused ion beam; Raman spectroscopy
Nuclear Instruments and Methods in Physics Research B 443(2019), 38-42
Tuning of electrocatalytic properties of MoS2 by chalcogenide ion implantation
Luxa, J.; Mazánek, V.; Mackova, A.; Malinsky, P.; Akhmadaliev, S.; Sofer, Z.
MoS2 is one of the most explored and promising material for electrocatalytic water splitting by hydrogen evolution reaction (HER). However, in its bulk form, MoS2 possesses only poor activity towards HER. Therefore, appropriate treatment has to be employed to tune its catalytic properties. In this study, we report the influence of ion bombardment (S, Se and Te ions) with medium ion energy (400 keV) and various ion fluences (1 × 1014–1 × 1016 ions/cm2) on the electrocatalytic properties of bulk MoS2 crystals. Our results showed that upon irradiation, sulfur vacancies were created. Upon exposure to ambient atmosphere, sulfur vacancies were partially replaced by oxygen, which led to surface oxidation. Nevertheless, samples irradiated using the higher range of ion fluences have generally showed enhanced catalytic HER performance in comparison with untreated MoS2 crystals. Furthermore, we have also demonstrated that ion irradiation/implantation can serve as a tool for doping of MoS2 crystals with Se and Te which can also influence the HER performance. The reported results demonstrate that ion beam irradiation can be used for doping as well as creation of sulfur vacancies in bulk MoS2 crystals which is fundamental for the HER performance.
Keywords: Electrocatalysis; Hydrogen evolution reaction; Ion implantation; MoS2
Applied Materials Today 14(2019), 216-223
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Damage formation and Er structural incorporation in m-plane and a-plane ZnO
Macková, A.; Malinský, P.; Jagerová, A.; Mikšová, R.; Nekvindová, P.; Cajzl, J.; Rinkevičiūtė, E.; Akhmadaliev, S.
The various crystallographic orientations in semiconductors as ZnO exhibit different resistivity under the ion beam irradiation/implantation. Study of the various crystallographic orientations is mandatory for nano-structured semiconductor system development. This paper reports on the implantation damage build-up, structural modification and Er dopant position in a-plane and m-plane ZnO implanted with Er+ 400 keV ions at the ion fluences 5 × 1014, 2.5 × 1015, 5 × 1015 cm-2 and subsequently annealed at 600 °C in O2 atmosphere using Rutherford Back-Scattering spectrometry (RBS) in channelling mode as well as using Raman spectroscopy. Strongly suppressed surface damage formation was observed in both crystallographic orientations compared to the deep damage growth with the increased ion implantation fluence. More progressive damage accumulation appeared in m-plane ZnO compared to a-plane ZnO. Simultaneously, the strong Er out-diffusion depth profile in m-plane ZnO accompanied by the damage accumulation at the surface was observed after the annealing. Contrary, the surface recovery accompanied by Er concentration depth profiles keeping a normal distribution with a small maximum shift to the surface was observed in a-plane ZnO. Different structure recovery and Er behaviour was evidenced in a-plane and m-plane ZnO by RBS-C, moreover Raman spectroscopy proved a lower damage at higher ion fluences introduced in a-plane ZnO compared to m-plane. The structure modifications were discussed in connection with a damage accumulation and Er concentration depth profile shape in various ZnO crystallographic orientations in as-implanted and as-annealed samples.
Keywords: a-Plane and m-plane ZnO doped; Damage accumulation asymmetry; Er ion implantation in ZnO; RBS channelling; Damage depth profiling
Nuclear Instruments and Methods in Physics Research B 460(2019), 38-46
Irradiation effects in monazite-(Ce) and zircon: Raman and photoluminescence study of Au-irradiated FIB foils
Nasdala, L.; Akhmadaliev, S.; Artac, A.; Chanmuang, N. C.; Habler, G.; Lenz, C.
Lamellae of 1.5 µm thickness, prepared from well-crystallised monazite-(Ce) and zircon samples using the focused-ion-beam technique, were subjected to triple irradiation with 1 MeV Au+ ions (15.6% of the respective total fluence), 4 MeV Au2+ ions (21.9%) and 10 MeV Au3+ ions (62.5%). Total irradiation fluences were varied in the range 4.5E12 -1.2E14 ions/cm2. The highest fluence resulted in amorphisation of both minerals; all other irradiations (i.e. up to 4.5E13 ions/cm2) resulted in moderate to severe damage. Lamellae were subjected to Raman and laser-induced photoluminescence analysis, in order to provide a means of quantifying irradiation effects using these two micro-spectroscopy techniques. Based on extensive Monte Carlo calculations and subsequent defect-density estimates, irradiation-induced spectroscopic changes are compared with those of naturally self-irradiated samples. The finding that ion irradiation of monazite-(Ce) may cause severe damage or even amorphisation, is in apparent contrast to the general observation that naturally self-irradiated monazite-(Ce) does not become metamict (i.e. irradiation-amorphised), in spite of high self-irradiation doses. This is predominantly assigned to the continuous low-temperature damage annealing undergone by this mineral; other possible causes are discussed. According to cautious estimates, monazite-(Ce) samples of Mesoproterozoic to Cretaceous ages have stored only about 1% of the total damage experienced. In contrast, damage in ion-irradiated and naturally self-irradiated zircon is on the same order; reasons for the observed slight differences are discussed. We may assess that in zircon, alpha decays create significantly less than 1000 Frenkel-type defect pairs per event, which is much lower than previous estimates. Amorphisation occurs at defect densities of about 0.10 dpa (displacements per lattice atom).
Keywords: Radiation damage; Heavy-ion irradiation; Focused ion beam; Raman spectroscopy; Photoluminescence
Physics and Chemistry of Minerals 45(2018), 855-871
Superconductivity with broken time-reversal symmetry in ion irradiated Ba0.27K0.73Fe2As2 single crystals
Grinenko, V.; Materne, P.; Sarkar, R.; Luetkens, H.; Kihou, K.; Lee, C. H.; Akhmadaliev, S.; Efremov, D. V.; Drechsler, S.-L.; Klauss, H.-H.
Over the last years a lot of theoretical and experimental efforts have been made to find states with broken time reversal symmetry (BTRS) in multi-band superconductors. In particular, it was theoretically proposed that in the Ba1−xKxFe2As2 system either an s + is or an s + id BTRS state may exist at high doping levels in a narrow region of the phase diagram. Here we report the observation of an enhanced zero field muon spin relaxation rate below the superconducting transition temperature for a high quality crystalline sample with x ≈ 0.73. This indicates that indeed the time reversal symmetry is broken in superconducting Ba1−xKxFe2As2 at this doping level.
Physical Review B 95(2017), 214511