Heteroepitaxial Er0.49Gd0.51Si1.7 layers formed by channeled ion beam synthesis

Epitaxial ternary silicide Er_0.49Gd_0.51Si_1.7 layers with a good crystalline quality (χ_min of Er and Gd is 3.7%) have been formed by 60 keV Er and Gd ion implantation into Si(1 1 1) substrates to a total dose of 1.0 × 10¹⁷/cm² at 450°C using channeled ion beam synthesis (CIBS). The composition, the structure, the strain and the thermal stability of these layers have been studied using energy dispersive spectroscopy (EDS), Rutherford backscattering (RBS)/channeling and X-ray diffraction (XRD). It is shown that the perpendicular and parallel elastic strains of the Er_0.49Gd_0.51Si_1.7 epilayer are e^⊥=−0.46% ± 0.02% and e⁶=+0.73% ± 0.19%. The layer is stable up to 900°C. Annealing at 950°C results in a phase transformation.     

Tungsten and CFC degradation under combined high cycle transient and steady state heat loads

Within the ITER divertor lifetime millions of transient events are expected during H-mode operation due to edge localized modes (type I ELMs). These will deposit their energy on plasma facing materials that are pre-heated to various surface temperatures, depending on the steady state heat load (SSHL) at the respective location, leading to synergistic effects. An electron beam facility was used to simulate ELM-like heat loads with ITER relevant power densities (≈0.5 GW/m²) and pulse duration (0.5 ms). At the same time additional SSHL was applied to obtain different base temperatures. Experiments were performed on actively cooled pure tungsten and the carbon fiber composite (CFC) NB41, applying 10³–10⁶ pulses of 0.5 ms duration with a power density of 0.14–0.55 GW/m² and 0.55–0.68 GW/m² on tungsten and CFC, respectively. Surface temperatures were about 200 °C, 400 °C and 700 °C for tungsten and about 450 °C for CFC. Crack formation in tungsten was preceded by roughening due to plastic deformation. In case of T_surf ≈ 200 °C cracks propagated comparably fast (brittle material), while slow propagation and recrystallization around the crack edges indicated fatigue damage at higher temperatures. Compared to tungsten, CFC showed a higher damage threshold.     

Hot deformation and processing maps of Inconel 690 superalloy

The hot deformation behavior of Inconel 690 has been investigated by means of hot compression tests in the temperature range of 950–1200 °C and strain rate range of 0.001–10 s^?1. The results show that the maximum stress decreases with decreasing strain rate and increasing temperature, and the activation energy is about 380.215 kJ/mol. Processing maps developed on the basis of experimental data and using the principles of the dynamic materials model exhibited two domains. The first domain occurs in the temperature range of 970–1120 °C and strain rate range of 0.03–3.3 s^?1, with a peak efficiency of power dissipation of 0.39. The second domain occurs in the temperature range of 1150–1200 °C and strain rate range of 0.003–0.1 s^?1, with a peak efficiency of power dissipation of about 0.37. Microstructural observations revealed that the full dynamic recrystallization (DRX) occurred in these two domains. In the first domain, the undissolved carbides assisted in nucleating DRX and restricted the coarsening of the full DRX grains and the refined grains were obtained. A small regime of flow instability was noticed at low temperature and high strain rate.     

Effects of hydrogen implantation into GaN

Proton implantation in GaN is found to reduce the free carrier density through two mechanisms – first, by creating electron and hole traps at around E_C − 0.8 eV and E_V + 0.9 eV that lead to compensation in both n- and p-type material, and second, by leading to formation of (AH)° complexes, where A is any acceptor (Mg, Ca, Zn, Be, Cd). The former mechanism is useful in creating high resistivity regions for device isolation, whereas the latter produces unintentional acceptor passivation that is detrimental to device performance. The strong affinity of hydrogen for acceptors leads to markedly different redistribution behavior for implanted H⁺ in n- and p-GaN due to the chemical reaction to form neutral complexes in the latter. The acceptors may be reactivated by simple annealing at ⩾600°C, or by electron injection at 25–150°C that produces debonding of the (AH)° centers. Implanted hydrogen is also strongly attracted to regions of strain in heterostructure samples during annealing, leading to pile-up at epi–epi and epi–substrate interfaces. IR spectroscopy shows that implanted hydrogen also decorates V_Ga defects in undoped and n-GaN.     

Optical contrast formation in amorphous silicon carbide with high-energy focused ion beams

Thin films (d ～ 1 μm) of hydrogenated amorphous silicon carbide (a-Si_1?xC_x:H), deposited by RF reactive magnetron sputtering with different carbon content x, have been implanted with high fluences (Φ = 1016–1017 cm^?2) of high-energy (E = 0.2–1 MeV) He⁺ ions as the implant species. The induced structural modification of the implanted material results in a considerable change of its optical properties, best manifested by a significant shift of the optical absorption edge to lower photon energies as obtained from photo-thermal-deflection spectroscopy (PDS) data. This shift is accompanied by a remarkable increase of the absorption coefficient over one order of magnitude (photo-darkening effect) in the measured photon energy range (0.6–3.8 eV), depending on the ion fluence, energy and carbon content of the films. These effects could be attributed both to additional defect introduction and increased graphitization, as confirmed by Raman spectroscopy and infra-red (IR) optical transmission measurements. The optical contrast thus obtained (between implanted and unimplanted film material) could be made use of in the area of high-density optical data storage using focused high-energy He⁺ ion beams.     

Ion beam mixing in uranium nitride thin films studied by Rutherford Backscattering Spectroscopy

Thickness, composition, concentration depth profile and ion irradiation effects on uranium nitride thin films deposited on fused silica have been investigated by Rutherford Backscattering Spectroscopy (RBS) using 2 MeV He⁺ ions. The films were prepared by reactive DC sputtering at the temperatures of ?200 °C, +25 °C and +300 °C. A perfect 1U:1N stoichiometry with a layer thickness of 660 nm was found for the film deposited at ?200 °C. An increase of the deposition temperature led to an enhancement of surface oxidation and an increase of the thickness of the mixed U–N–Si–O layers at the interface. The sample irradiation by 1 MeV Ar⁺ ion beam with ion fluence of about 1.2–1.7 × 10¹⁶ ions/cm² caused a large change in the layer composition and a large increase of the total film thickness for the films deposited at ?200 °C and at +25 °C, but almost no change in the film thickness was detected for the film deposited at +300 °C. An enhanced mixing effect for this film was obtained after further irradiation with ion fluence of 2.3 × 10¹⁶ ions/cm².     

Swelling behaviors of GMZ bentonite–sand mixtures inundated in NaCl–Na2SO4 solutions

In this study, the swelling behaviors of compacted GMZ bentonite–sand mixtures inundated in NaCl–Na₂SO₄ solutions are investigated and the influence of chemical solutions on the swelling behaviors of GMZ bentonite–sand mixtures as backfill/buffer material in China for high level radioactive waste (HLW) is investigated. The sand addition ratios of the bentonite–sand mixtures are 0%, 20%, 30% and 50%, and the total dissolved solids (TDS) of the NaCl–Na₂SO₄ (NaCl:Na₂SO₄ = 2:1 by mass) solution are 0.5, 1.0, 3.0, 6.0 and 12.0 g/L (pH 7.1). The specimens of bentonite–sand mixtures for swelling tests are prepared by static-compaction to various dry densities, ranging from 1.50 to 1.90 g/cm³.Test results indicate that liquid limit (LL) and plasticity limit (PL), swell time, maximum swelling pressure and maximum swelling strain decrease with the increase of TDS for GMZ bentonite–sand mixtures. All of the LL, PI and maximum swelling strain are decreased exponentially with TDS increase: very quickly as TDS < 3.0 g/L, slowly as TDS = 3.0–6.0 g/L and almost stabilized as TDS > 6.0 g/L. The maximum swelling pressure shows a linear reduction with the TDS increasing, but the pure bentonite indicates a high sensitivity than the bentonite–sand mixtures with 30% sand addition ratio. As NaCl–Na₂SO₄ (TDS = 0.5 g/L) solution was used according to the ground water, with initial dry density of 1.70 g/cm³, the maximum swelling pressure of specimens decrease exponentially while the maximum strain decrease linearly with the increase of sand addition. With 30% sand addition in 0.5 g/L NaCl–Na₂SO₄ solution, the maximum swelling pressure increase exponentially while the maximum strain increase linearly with the increase of initial dry density.Compared with the pure bentonite, bentonite–sand mixtures show a better tolerance withstanding the chemical attack to ground water chemistry because of the replacement of some quantity of expansive clay by quartz sand in the mixtures.     

Investigation of hydrogen concentration and hardness of ion irradiated organically modified silicate thin films

A study of the effects of ion irradiation of organically modified silicate thin films on the loss of hydrogen and increase in hardness is presented. NaOH catalyzed SiNa_wO_xC_yH_z thin films were synthesized by sol–gel processing from tetraethylorthosilicate (TEOS) and methyltriethoxysilane (MTES) precursors and spin-coated onto Si substrates. After drying at 300 °C, the films were irradiated with 125 keV H⁺ or 250 keV N²⁺ at fluences ranging from 1 × 10¹⁴ to 2.5 × 10¹⁶ ions/cm². Elastic Recoil Detection (ERD) was used to investigate resulting hydrogen concentration as a function of ion fluence and irradiating species. Nanoindentation was used to measure the hardness of the irradiated films. FT-IR spectroscopy was also used to examine resulting changes in chemical bonding. The resulting hydrogen loss and increase in hardness are compared to similarly processed acid catalyzed silicate thin films.     

The effect of neutron irradiation dose on vacancy defect accumulation and annealing in pure nickel

In order to investigate the dose dependence of vacancy defect evolution in nickel, specimens of high-purity Ni were neutron-irradiated at ～330 K in the IVV-2M reactor (Russia) to fluencies in the range of 1 × 10²¹–1 × 10²³ n/m² (E > 0.1 MeV) corresponding to displacement dose levels in the range of about 0.0001–0.01 dpa and subsequently stepwise annealed to about 900 K. Ni was characterized both in as-irradiated state as well as after post-irradiation annealing by positron annihilation spectroscopy. The formation of three-dimensional vacancy clusters (3D-VCs) in cascades was observed under neutron irradiation, the concentration of 3D-VCs increases with increasing dose level. 3D-VCs collapse into secondary-type clusters (stacking fault tetrahedra (SFTs), and vacancy loops) during stepwise annealing at 350–450 K. It is shown that the thermal stability of SFTs grow with increasing dose level, probably, it is due to growth of the average SFT size during annealing. The results of annealing experiments on electron-irradiated Ni at 300 K are indicated in the paper, for comparison. We also have briefly discussed the positron response to the SFT-like structures.     

Quantifying helium distribution in dual-ion beam irradiated SiCf/SiC composites by electron energy loss spectroscopy

In this study, we report a method to quantify the helium distribution in the SiC_f/SiC composites, which are used as the first-wall materials of fusion reactor. The helium-bubble formation in Hi-Nicalon Type-S (HNS) was observed in the irradiated SiC_f/SiC composites at a level of 100 dpa and at 800 °C and 1000 °C, respectively. We applied transmission electron microscopy and electron energy loss spectroscopy to investigate the helium-gas-bubbles-formation mechanisms. To simulate the practical first-wall environment of Deuterium–Tritium (D–T) fusion reactor, a dual-ion beam (6 MeV Si³⁺ and 1.13 MeV He⁺) was performed to irradiate the SiC_f/SiC composites. The relationship between the energy shift of He K-edge and the radius of the bubble of the SiC composites was estimated by electron energy loss spectroscopy analysis. The results show that all of the helium atoms irradiated at 1000 °C and formed the bubbles. On the other hand, at 800 °C, only 25.5% of the helium atoms form the helium bubbles. A clear thermal-dependent formation mechanism is found.     

Determination of differential cross-sections for the natK(p, p0) and 39K(p, α0) reactions in the backscattering geometry

In the present work, new, differential cross-section values are presented for the ^natK(p, p₀) reaction in the energy range E_lab = 3000–5000 keV (with an energy step of 25 keV) and for detector angles between 140° and 170° (with an angular step of 10°). A qualitative discussion of the observed cross-section variations through the influence of strong, closely spaced resonances in the p + ³⁹K system is also presented. Information has also been extracted concerning the ³⁹K(p,α₀) reaction for E_lab = 4000–5000 keV in the same angular range. As a result, more than ～500 data points will soon be available to the scientific community through IBANDL (Ion Beam Analysis Nuclear Data Library – http://www-nds.iaea.org/ibandl/) and could thus be incorporated in widely used IBA algorithms (e.g. SIMNRA, WINDF, etc.) for potassium depth profiling at relatively high proton beam energies.     

Effects of BF2+ implantation on the strain-relaxation of pseudomorphic metastable Ge0.06Si0.94 alloy layers

Metastable pseudomorphic Ge_0.06Si_0.94 alloy layers grown by molecular beam epitaxy (MBE) on Si (1 0 0) substrates were implanted at room temperature by 70 keV BF₂⁺ ions with three different doses of 3 × 10¹³, 1 × 10¹⁴, and 2.5 × 10¹⁴ cm⁻². The implanted samples were subsequently annealed at 800°C and 900°C for 30 min in a vacuum tube furnace. Observed by MeV ⁴He channeling spectrometry, the sample implanted at a dose of 2.5 × 10¹⁴ BF₂⁺ cm⁻² is amorphized from surface to a depth of about 90 nm among all as-implanted samples. Crystalline degradation and strain-relaxation of post-annealed Ge_0.06Si_0.94 samples become pronounced as the dose increases. Only the samples implanted at 3 × 10¹³ cm⁻² do not visibly degrade nor relax during anneal at 800°C . In the leakage current measurements, no serious leakage is found in most of the samples except for one which is annealed at 800°C for 30 min after implantation to a dose of 2.5 × 10¹⁴ cm⁻². It is concluded that such a low dose of 3 × 10¹³ BF₂⁺ cm⁻² can be doped by implantation to conserve intrinsic strain of the pseudomorphic GeSi, while for high dose regime to meet the strain-relaxation, annealing at high temperatures over 900°C is necessary to prevent serious leakages from occuring near relaxed GeSi/Si interfaces.     

Ion implantation into aluminum and copper by a beam of carbon nanoparticles from regenerative sooting discharges

We present a new technique to generate light carbon nanoparticles from regenerative sooting discharges and its use for ion implantation on aluminum and copper surfaces at an energy of 40 keV. Films formed at fluences up to 3 × 10¹⁵ C⁺/cm² for aluminum and 10¹⁶ C⁺/cm² for copper are studied using Raman spectroscopy, X-ray diffraction and atomic force microscopy. Raman spectroscopy reveals the existence of graphite and diamond like structures in all samples. Precipitates of Al₄C₃ of rhombohedral and hexagonal types were found in the nanometer ranges from the X-ray diffraction pattern for aluminum samples and the probable formation of body-centered cubic diamond and hexagonal carbon in copper samples. The average grain sizes of Al₄C₃ were calculated ～40 nm for Al and ～35 nm for Cu. Mass spectra from a graphite hollow cathode duoplasmatron ion source are also presented. Atomic force microscopy images of a Cu sample also support the existence of 46 nm structures. Light carbon nanoparticles are readily available from the ion source in which a special carbonaceous environment creates regenerative soot. Support gas Ar produces more C₃ than Ne.     

Study of modifications in Lexan polycarbonate induced by swift O6+ ion irradiation

Swift Heavy Ion (SHI) irradiation of the polymeric materials modifies their physico-chemical properties. Lexan polycarbonate films were irradiated with 95 MeV oxygen ions to the fluences of 10¹⁰, 10¹¹, 10¹², 10¹³ and 2 × 10¹³ ions/cm². Characterization of optical, chemical, electrical and structural modifications were carried out by UV–Vis spectroscopy, FTIR spectroscopy, Dielectric measurements and X-ray Diffraction. A shift in the optical absorption edge towards the red end of the spectrum was observed with the increase in ion fluence. The optical band gap (E_g), calculated from the absorption edge of the UV–Vis spectra of these films in 200–800 nm region varied from 4.12 eV to 2.34 eV for virgin and irradiated samples. The cluster size varied in a range of 69–215 carbon atoms per cluster. In FTIR spectra, appreciable modification in terms of breaking of the cleavaged C–O bond of carbonate and formation of phenolic O–H bond was observed on irradiation. A rapidly decreasing trend in dielectric constant is observed at lower frequencies. The dielectric constant increases with fluence. It is observed that the loss factor increases moderately with fluence and it may be due to scissoring of polymer chains, resulting in an increase in free radicals. A sharp increase in A.C. conductivity in pristine as well as in irradiated samples is observed with frequency and is attributed to scissoring of polymer chains. XRD analyses show significant change in crystallinity with fluence. A decrease of ～9.02% in crystallite size of irradiated sample at the fluence of 2 × 10¹³ ions/cm² is observed.     

Annealing of ion implanted 4H–SiC in the temperature range of 100–800 °C analysed by ion beam techniques

Ion implantation induced damage formation and subsequent annealing in 4H–SiC in the temperature range of 100–800 °C has been investigated. Silicon Carbide was implanted at room temperature with 200 keV ⁴⁰Ar ions with two implantation fluences of 4 × 10¹⁴ and 2 × 10¹⁵ ions/cm². The samples were characterized by Rutherford backscattering and nuclear reaction analysis techniques in channeling mode using 2.00 and 4.30 MeV ⁴He ion beams for damage buildup and recovery in the Si and C sublattices, respectively. At low ion fluence, the restoration of the Si sublattice is evident already at 200 °C and a considerable annealing step occurs between 300 and 400 °C. Similar results have been obtained for the C sublattice using the nuclear resonance reaction for carbon, ¹²C(α,α)¹²C at 4.26 MeV. For samples implanted with the higher ion fluence, no significant recovery is observed at these temperatures.     

Ion beam synthesis of SiC by C implantation into SIMOX(1 1 1)

We report the conversion of a 65 nm Si(1 1 1) overlayer of a SIMOX(1 1 1) into 30–45 nm SiC by 40 keV carbon implantation into it. High temperature implantation (600 °C) through a SiO₂ cap, 1250 °C post-implantation annealing under Ar ambient (with 1% of O₂), and etching are the base for the present synthesis. Sequential C implantations (fluence steps of about 5 × 10¹⁶ cm^?2), followed by 1250 °C annealing, has allowed to estimate the minimum C fluence to reach the stoichiometric composition as ～2.3 ×  10¹⁷ cm^?2. Rutherford Backscattering Spectrometry was employed to measure layer composition evolution. A two-sublayers structure is observed in the synthesized SiC, being the superficial one richer in Si. Transmission electron microscopy has shown that a single-step implantation up to the same minimum fluence results in better structural quality. For a much higher C fluence (4 × 10¹⁷ cm^?2), a whole stoichiometric layer is obtained, with reduction of structural quality.     

Swift heavy ion induced modifications of optical and microstructural properties of silver–fullerene C60 nanocomposite

In this paper, we study the optical and microstructural properties of silver–fullerene C₆₀ nanocomposite and their modifications induced by swift heavy ion irradiation. Silver nanoparticles embedded in fullerene C₆₀ matrix were synthesized by co-deposition of silver and fullerene C₆₀ by thermal evaporation. The nanocomposite thin films were irradiated by 120 MeV Ag ions at different fluences ranging from 1 × 10¹² to 3 × 10¹³ ions/cm². Optical absorption studies revealed that the surface plasmon resonance of Ag nanoparticles showed a blue shift of ～49 nm with increasing ion fluence up to 3 × 10¹³ ions/cm². Transmission electron microscopy and Rutherford backscattering spectroscopy were used to quantify particle size and metal atomic fraction in the nanocomposite film. Growth of Ag nanoparticles was observed with increasing ion fluence. Raman spectroscopy was used to understand the effect of heavy ion irradiation on fullerene matrix. The blue shift in plasmonic wavelength is explained by the transformation of fullerene C₆₀ matrix into amorphous carbon.     

Preparation and investigation of aluminized coating and subsequent heat treatment on 9Cr–1Mo Grade 91 steel

Iron aluminide inner coating with alumina top layer is being considered as a potential solution for tritium permeation barrier and mitigating MHD pressure drop for liquid metal blanket concepts in the fusion reactor systems. Hot-dip aluminizing with subsequent heat treatment seems to offer a good possibility to produce aluminized coating with alumina top layer. 9Cr–1Mo Grade 91 steel samples were hot dipped in Al melt containing 2.25 wt% of Si at 750 °C for 3 min. Heat treatment was performed at 650, 750 and 950 °C for 5 h; samples were either air cooled or furnace cooled. Coatings have been evaluated by SEM, EDX, X-ray diffraction, microhardness, scratch adhesion and Raman spectroscopy. The thickness of the layers and phases formed were influenced by the heat treatment adopted. Fe₂Al₅ was the major phase present in the samples heat treated at 650/750 °C, whereas FeAl and α-Fe(Al) primarily made up the outer and inner layers respectively in the samples heat treated at 950 °C. Cooling method deployed affected the hardness. Air cooled samples had comparatively higher hardness than furnace cooled samples. The scratch test showed the adhesion for the samples heat treated at 950 °C was much better as compared to the samples heat treated at 650/750 °C. Raman spectroscopy analysis showed the presence of both α-Al₂O₃ and γ-Al₂O₃ on the surface of the samples heat treated at 950 °C, while Fe₃O₄ was present in the furnace cooled sample only.     

Effect of fluence on the lattice site of implanted Er and implantation induced strain in GaN

A GaN thin film was implanted with 5 × 10¹⁴ cm^?2 of 60 keV stable ¹⁶⁶Er, followed by the implantation of 2 × 10¹³ cm^?2 radioactive ¹⁶⁷Tm (t_1/2 = 9.3 d) and an annealing sequence up to 900 °C. The emission channeling (EC) technique was applied to assess the lattice location of Er following the Tm decay from the conversion electrons emitted by ^167mEr, which showed that more than 50% of ^167mEr occupies substitutional Ga sites. The results are briefly compared to a ^167mEr lattice location experiment in a GaN sample not pre-implanted with ¹⁶⁶Er. In addition, high-resolution X-ray diffraction (HRXRD) was used to characterize the perpendicular strain in the high-fluence implanted film. The HRXRD experiments showed that the Er implantation resulted in an increase of the c-axis lattice constant of the GaN film around 0.5–0.7%. The presence of significant disorder within the implanted region was corroborated by the fact that the EC patterns for off-normal directions exhibit a pronounced angular broadening of the order of magnitude of 0.5°.     

Mechanical and fatigue properties of martensitic Fe-13Cr steel in contact with lead and lead-bismuth melts

The influence of stagnant liquid-metal environments (Pb and Pb-Bi) on mechanical (strength and plasticity) and fatigue properties (low cycle fatigue) of martensitic Fe-13Cr steel in temperature interval of 250–600 °С have been investigated. Heavy liquid metals facilitate decreasing in ultimate strength by 10–20% against that in vacuum. The increase of temperature enhances this effect. Fe-13Cr steel is susceptible to liquid-metal embrittlement in the temperature interval of 350–450 °С, which manifests itself more substantially in lead-bismuth eutectic. The decrease of plasticity in Pb is 11% at 450 °С and in Pb-Bi is 30% in temperature interval 350–400 °С. Liquid metal environments significantly reduce fatigue life of Fe-13Cr steel. Pb-Bi has a more negative impact. In particular, with increasing total strain amplitude (up to 1.0%), the decrease in the cycle number to fracture by more than two orders of magnitude occurs.