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At least 1,495 records · Page 83

A Transmission Electron Microscopy Study of the Effect of Interfaces on Bubble Formation in He-Implanted Cu-Nb Multilayers

Magnetron sputtered thin films of Cu, Nb, and Cu-Nb multilayers with 2.5 and 5 nm nominal layer thickness were deposited on Si and implanted with 4He+ and 3He+ ions. Secondary ion mass spectroscopy and nuclear reaction analysis, respectively, were used to measure the 4He+ and 3He+ concentration profile with depth inside the films. Cross-sectional transmission electron microscopy was used to characterize the helium bubbles. Analysis of the contrast from helium bubbles in defocused transmission electron microscope images showed a minimum bubble diameter of 1.25 nm. While pure Cu and Nb films showed bubble contrast over the entire range of helium implantation, the multilayers exhibited bubbles only above a critical He concentration that increased almost linearly with decreasing layer thickness. The work shows that large amounts of helium can be trapped at incoherent interfaces in the form of stable, nanometer-size bubbles.

36 MATERIALS SCIENCE↗

Characterising Ion-Irradiated FeCr: Hardness, Thermal Diffusivity and Lattice Strain

Ion-irradiated FeCr alloys are useful for understanding and predicting neutron damage in the structural steels of future nuclear reactors. Previous studies have largely focused on the structure of irradiation induced defects, probed by transmission electron microscopy (TEM), as well as changes in mechanical properties. Across these studies, a wide range of irradiation conditions has been employed on samples with different processing histories, which complicates the analysis of the relationship between defect structures and material properties. Furthermore, key properties, such as irradiation-induced changes in thermal transport and lattice strain, are little explored. Here we present a systematic study of Fe3Cr, Fe5Cr and Fe10Cr binary alloys implanted with 20 MeV Fe3+ ions to nominal doses of 0.01 dpa and 0.1 dpa at room temperature. Nanoindentation, transient grating spectroscopy (TGS) and X-ray micro-beam Laue diffraction were used to study the changes in hardness, thermal diffusivity and strain in the material as a function of damage and Cr content. Our results suggest that Cr leads to an increased retention of irradiation-induced defects, causing substantial changes in hardness and lattice strain. However, thermal diffusivity varies little with increasing damage and instead degrades significantly with increasing Cr content in the material. We find significant lattice strains even in samples exposed to a nominal displacement damage of 0.01 dpa. The defect density predicted from the lattice strain measurements is significantly higher than that observed in previous TEM studies, suggesting that TEM may not fully capture the irradiation-induced defect population. (C) 2020 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

FeCr alloys↗

Kelvin probe characterization of buried graphitic microchannels in single-crystal diamond

In this work, we present an investigation by Kelvin Probe Microscopy (KPM) of buried graphitic microchannels fabricated in single-crystal diamond by direct MeV ion microbeam writing. Metal deposition of variable-thickness masks was adopted to implant channels with emerging endpoints and high temperature annealing was performed in order to induce the graphitization of the highly-damaged buried region. When an electrical current was flowing through the biased buried channel, the structure was clearly evidenced by KPM maps of the electrical potential of the surface region overlying the channel at increasing distances from the grounded electrode. The KPM profiling shows regions of opposite contrast located at different distances from the endpoints of the channel. This effect is attributed to the different electrical conduction properties of the surface and of the buried graphitic layer. The model adopted to interpret these KPM maps and profiles proved to be suitable for the electronic characterization of buried conductive channels, providing a non-invasive method to measure the local resistivity with a micrometer resolution. The results demonstrate the potential of the technique as a powerful diagnostic tool to monitor the functionality of all-carbon graphite/diamond devices to be fabricated by MeV ion beam lithography.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Effects of 3d electron configurations on helium bubble formation and void swelling in concentrated solid-solution alloys

Currently, elemental specific chemical complexity is known to play a vital role in microstructure development in single-phase concentrated solid-solution alloys (SP-CSAs), including both He bubble formation and irradiation-induced void swelling. While cavity formation and evolution under ion irradiation at elevated temperature are complex nonequilibrium processes, chemical effects are revealed at the level of electrons and atoms herein in a simplified picture, using Ni and a special set of Ni-based SP-CSAs composed of 3d transition metals as model alloys. Based on Ni and the model alloys with minimized variables (e.g., atomic mass, size, and lattice structure), we report on the effects of chemically-biased energy dissipation, defect energetics, sluggish diffusion, and atomic transport on cavity formation and evolution under both self-ion Ni irradiation and He implantation. The observed difference in microstructure evolution is attributed to the effects of d electron interactions in their integrated ability to dissipate radiation energy. The exhibited impact of alloying 3d transition metals with larger differences in the outermost electron counts suggests a simple design strategy for tuning defect properties to improve radiation tolerance in structural alloys.

36 MATERIALS SCIENCE↗

Laser Desorption/Ionization Mass Spectrometric Imaging of Endogenous Lipids from Rat Brain Tissue Implanted with Silver Nanoparticles

Mass spectrometry imaging (MSI) of tissue implanted with silver nanoparticulate (AgNP) matrix generates reproducible imaging of lipids in rodent models of disease and injury. Gas-phase production and acceleration of size-selected 8 nm AgNP is followed by controlled ion beam rastering and soft landing implantation of 500 eV AgNP into tissue. Focused 337 nm laser desorption produces high quality images for most lipid classes in rat brain tissue (in positive mode: galactoceramides, diacylglycerols, ceramides, phosphatidylcholines, cholesteryl ester, and cholesterol, and in negative ion mode: phosphatidylethanolamides, sulfatides, phosphatidylinositol, and sphingomyelins). Image reproducibility in serial sections of brain tissue is achieved within <10% tolerance by selecting argentated instead of alkali cationized ions. The imaging of brain tissues spotted with pure standards was used to demonstrate that Ag cationized ceramide and diacylglycerol ions are from intact, endogenous species. In contrast, almost all Ag cationized fatty acid ions are a result of fragmentations of numerous lipid types having the fatty acid as a subunit. Almost no argentated intact fatty acid ions come from the pure fatty acid standard on tissue. .

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Latent ion tracks in amorphous silicon

We present experimental evidence for the formation of ion tracks in amorphous Si induced by swift heavy ion irradiation. An underlying core-shell structure consistent with remnants of a high density liquid structure was revealed by small-angle x-ray scattering and molecular dynamics simulations. Ion track dimensions dier for as-implanted and relaxed Si as attributed to dierent microstructures and melting temperatures. The identication and characterisation of ion tracks in amorphous Si yields new insight into mechanisms of damage formation due to swift heavy ion irradiation in amorphous semiconductors.

Amorphous Silicon↗

Potential benefit of amorphization in the retention of gaseous species in irradiated pyrochlores

Understanding the structure-property relationship for materials destined for irradiation extremes is a key step in developing materials with reliable, long-term performance. One crucial relationship is the ability of a material to withstand or accommodate amorphization, as this dictates its potential use as a nuclear waste form. Pyrochlores are one such class of materials for consideration as waste forms and there has been significant work examining how both the crystal structure and chemistry impacts amorphization resistance, leading to the important conclusion that the amorphization resistance of pyrochlores (A 2 B 2 O 7 ) is very sensitive to the nature of the B cations. For example, pyrochlores with B=Ti amorphize much more readily than B=Zr compounds. However, there are still questions regarding how these types of materials respond to prolonged or high-dose irradiation conditions. Gd 2 Ti 2 O 7 (GTO) and Gd 2 Zr 2 O 7 (GZO) pyrochlores were implanted with 400 keV Kr++ ions at room temperature to calculated peak damages of 119 and 135 displacements per atom (dpa), respectively. As expected, GTO amorphized completely under irradiation. However, discrete bubbles of Kr coalesced within the amorphous matrix without micro-cracking or spallation. In contrast, GZO transforms to a disordered fluorite structure under irradiation with no indications of localized amorphization. But, the accumulation of Kr within the host material leads to sub-grain structures, extended defects, and the development of micro-cracks. Thus, while GTO readily amorphizes even under low dose irradiations, the resistance of the amorphous GTO matrix to micro cracking and gas release, even in the presence of large bubble formation, suggests an enhanced propensity to retain gaseous species. Finally, consideration of long-term dose accumulation effects in nuclear waste forms would suggest reconsideration of amorphization processes in pyrochlores and related materials as a potential beneficial effect for immobilization and long-term storage of actinide materials.

36 MATERIALS SCIENCE↗

Phase decomposition and bubble evolution in Xe implanted U 3 Si 2 at 450°C

We report on the microstructure investigations of a U 3 Si 2 specimen implanted by 84 MeV Xe ions at 450°C. In the region that corresponds to the highest irradiation dose, U 3 Si 2 was found to decompose into a Si-enriched nanocrystalline USi matrix phase and a U-enriched amorphous inclusion phase. Density functional theory (DFT) calculations were used to help understand the decomposition mechanism. Xe bubbles of different morphologies were observed in USi nano-grains, on USi grain boundaries, and phase boundaries. Original U 3 Si 2 micro-grains were preserved on both sides of the irradiation damage peak region within the sample, implying a radiation dose threshold for decomposition of approximately 150 dpa at 450°C. In the preserved U 3 Si 2 region beneath the irradiation damage peak, where critical amount of Xe ions were deposited, a monomodal size distribution of intragranular Xe bubbles with an average size of 2.68 nm formed. In both decomposed and preserved U 3 Si 2 , the size of Xe bubbles was found to be lower than 50 nm. Based on this observation, the fission gas behavior of U 3 Si 2 is controllable and free of run-away swelling despite the occurrence of decomposition at this irradiation temperature. (C) 2019 Elsevier B.V. All rights reserved.

36 MATERIALS SCIENCE↗

Interpreting experimental measurements of helium bubbles using stochastic cluster dynamics models of heterogeneous nucleation and growth in irradiated ferritic alloys

Among a number of other advantageous features, ferritic/martensitic steels are being considered as fusion reactor structural materials due to their low intrinsic swelling under irradiation. However, under high-energy neutron irradiation, He produced through (n, α) reactions stabilizes vacancy clusters, which then act as seeds for bubble formation and growth, negating the intrinsic swelling resistance of these alloys. Standard models of irradiation damage accumulation and microstructural evolution consider homogeneous nucleation as the basis for bubble formation and growth. However, this generally does not explain the large bubble densities and sizes observed experimentally under a number of different conditions. Here, we propose a more realistic physical model of bubble nucleation, formation, and growth designed to capture recent experimental measurements of He-bubble formation and evolution during co-implantation of He and Fe ions in model ferritic alloys. We find that experimental results are explained only when the following three features are considered simultaneously: (i) heterogeneous nucleation of He-vacancy bubbles at defect sinks (e.g., dislocations, grain boundaries, and second-phase precipitates), (ii) nucleation and growth of bubbles via the ‘trap mutation’ mechanism (i.e., spontaneous production of Frenkel pairs due to absorption of He atoms), and (iii) transition from a growth-limited, He-stabilized bubble regime to a ‘runaway’ void-type growth scenario. The model is implemented into a stochastic cluster dynamics framework that takes advantage of cluster size grouping methods to accelerate the simulations, allowing us to reach 10 dpa of simulated irradiated dose, and to capture cluster sizes in excess of 20 nm. Further, a careful extrapolation exercise conducted assuming classical nucleation theory leads to excellent agreement with the experimental measurements at 50 dpa of irradiation.

36 MATERIALS SCIENCE↗

Commissioning of the BRIKEN detector for the measurement of very exotic β -delayed neutron emitters

A new detection system has been installed at the RIKEN Nishina Center (Japan) to investigate decay properties of very neutron-rich nuclei. The setup consists of three main parts: a moderated neutron counter, a detection system sensitive to the implantation and decay of radioactive ions, and -ray detectors. We describe here the setup, the commissioning experiment and some selected results demonstrating its performance for the measurement of half-lives and β-delayed neutron emission probabilities. Here, the methodology followed in the analysis of the data is described in detail. Particular emphasis is placed on the correction of the accidental neutron background.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Mitigating Measurement Artifacts in TOF-SIMS Analysis of Perovskite Solar Cells

Time-of-flight secondary ion mass spectrometry (TOF-SIMS) is one of the few techniques that can specifically distinguish between organic cations such as methylammonium and formamidinium. Distinguishing between these two species can lead to specific insight into the origins and evolution of compositional inhomogeneity and chemical gradients in halide perovskite solar cells, which appears to be a key to advancing the technology. TOF-SIMS can obtain chemical information from hybrid organic-inorganic perovskite solar cells (PSCs) in up to three dimensions, while not simply splitting the organic components into their molecular constituents (C, H, and N for both methylammonium and formamidinium), unlike other characterization methods. Here, we report on the apparently ubiquitous A-site organic cation gradient measured when doing TOF-SIMS depth-profiling of PSC films. Using thermomechanical methods to cleave perovskite samples at the buried glass/transparent conducting oxide interface enables depth profiling in a reverse direction from normal depth profiling (backside depth profiling). When comparing the backside depth profiles to the traditional front side profiled devices, an identical slight gradient in the A-site organic cation signal is observed in each case. This indicates that the apparent A-site cation gradient is a measurement artifact due to beam damage from the primary ion beam causing a continually decreasing ion yield for secondary ions of methylammonium and formamidinium. This is due to subsurface implantation and bond breaking from the 30 keV bismuth primary ion beam impact when profiling with too high of a data density. Here, we show that the beam-generated artifact associated with this damage can mostly be mitigated by altering the measurement conditions. We also report on a new method of depth profiling applied to PSC films that enables enhanced sensitivity to halide ions in positive measurement polarity, which can eliminate the need for a second measurement in negative polarity in most cases.

14 SOLAR ENERGY↗

Shape coexistence in Ni 68

The internal-conversion and internal-pair-production decays of the first excited 0 + state in 68 Ni are studied following the β decay of 68 Co. A novel experimental technique, in which the ions of 68 Co were implanted into a planar germanium double-sided strip detector and which required digital pulse processing, is developed. The values for the energy of the first excited 0 + state and the electric monopole transition strength from the first excited 0 + state to the ground state in 68 Ni are determined to be 1605(3) keV and 7.6 (4) × 10 -3 , respectively. Comparisons of the experimental results to Monte Carlo shell-model calculations suggest the coexistence between a spherical ground state and an oblate first excited 0 + state in 68 Ni.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Influence of measurement temperature on the luminescence properties of (113) defects in oxygen-implanted silicon

Influence of the measurement temperature in the range 5–130 K on the photoluminescence spectra of (113) defects in Si implanted with 350-keV oxygen ions at doses of 3.7 × 10{sup 14} cm{sup –2} and annealed at a temperature of 700°C for 1 h in a chlorine-containing atmosphere is studied. The temperature dependence of the line intensity is characterized by portions of intensity increase with an activation energy of 23.1 meV and intensity quenching with activation energies of 41.9 and 178.3 meV. With increasing temperature, the lines are shifted to longer wavelengths and their FWHM increases.

36 MATERIALS SCIENCE↗

Measurements of reflectance spectra of ion-bombarded ice and application to surfaces in the outer solar system

The first results of laboratory measurements of the wavelength dependence of the alternation of the visible reflectance of H2O ice irradiated by keV ions are presented. When the implanted species is chemically neutral, absorption is slightly enhanced below 0.55 micron. For an incident species containing sulfur, a strong absorption feature is produced at 0.4 micron, probably corresponding to S3. This occurs at too large a wavelength to account for the absorption feature observed at Europa by Voyager and therefore casts doubt on the recent interpretation of the reflectance data of Europa.

O'Shaughnessy, D. J.↗

Transmission Electron Microscopy Investigation of Krypton Bubbles in Polycrystalline CeO2

To gain an understanding of gas bubble transport in oxide nuclear fuel, this paper uses polycrystalline CeO2, composed of both nanograins and micrograins, as a surrogate material for UO2. The CeO2 was implanted with 150-keV Kr ions up to a dose of 1 x 1016 ions/cm2 at 600 degrees C. Transmission electron microscopy characterizations of small Kr bubbles in nanograin and micrograin regions were compared. The grain boundary acted as an efficient defect sink, as evidenced by smaller bubbles and a lower bubble density in the nanograin region as compared to the micrograin region.

99 GENERAL AND MISCELLANEOUS↗