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At least 1,603 records · Page 89

Effect of a novel load-bearing trabecular Nitinol scaffold on rabbit radius bone regeneration

The research aim was to evaluate the bone regeneration capability of novel load-bearing NiTi alloy (Nitinol) scaffolds in a critical-size defect (CSD) model. High strength “trabecular Nitinol” scaffolds were prepared by PIRAC (Powder Immersion Reaction Assisted Coating) annealing of the highly porous Ni foam in Ti powder at 900°C. This was followed by PIRAC nitriding to mitigate the release of potentially toxic Ni ions. Scaffolds phase composition and microstructure were characterized by X-ray diffraction and scanning electron microscopy (SEM/EDS), and their mechanical properties were tested in compression. New Zealand white rabbits received bone defect in right radius and were divided in four groups randomly. In the control group, nothing was placed in the defect. In other groups, NiTi scaffolds were implanted in the defect: (i) as produced, (ii) loaded with bone marrow aspirate (BMA), and (iii) biomimetically CaP-coated. The animals were sacrificed after 12 weeks. The forelimbs with scaffolds were resected, fixed, sectioned and examined in SEM. New bone formation inside the scaffold was studied by EDS analysis and by the processing of backscattered electron images. Bone ingrowth into the scaffold was observed in all implant groups, mostly next to the ulna. New bone formation was strongly enhanced by BMA loading and biomimeatic CaP coating, the bone penetrating as much as 1–1.5 mm into the scaffold. The results of this preliminary study demonstrate that the newly developed high strength trabecular Nitinol scaffolds can be successfully used for bone regeneration in critical size defects.

36 MATERIALS SCIENCE↗

A review of helium–hydrogen synergistic effects in radiation damage observed in fusion energy steels and an interaction model to guide future understanding

Here, under fusion reactor conditions, large quantities of irradiation defects and transmutation gases are produced per unit time by neutrons, resulting in accelerated degradation of structural candidate ferritic (F) and ferritic/martensitic (F/M) steels. Due to the lack of a suitable fusion neutron testing facility, we must rely on high-dose-rate ion-beam experiments and present-day crude modeling estimates. Of particular interest is the possibility of synergistic (positive feedback) effects on materials properties due to the simultaneous action of He, H, and displacement damage (dpa) during operation. In this paper we discuss the state-of-the-art in terms of the experimental understanding of synergistic effects and carry out simulations of triple-species irradiation under ion-beam conditions using first-of-its-kind modeling techniques. Although, state-of-the-art modeling and simulation is not sufficiently well developed to shed light on the experimental uncertainties, we are able to conclude that it is not clear whether synergistic effects, the evidence of which is still not conclusive, will ultimately play a critical role in material performance under fusion energy conditions. We review here some of the evidence for the synergistic effects of hydrogen in the presence of helium and displacement damage, and also include some recent data from our research. While the experimental results to date suggest possible mechanisms for the observed synergistic effects, it is only with more advanced modeling that we can hope to understand the details underlying the experimental observations. By employing modeling and simulation we propose an interaction model that is qualitatively consistent with experimental observations of dpa/He/H irradiation behavior. Our modeling, the results of which should be helpful to researchers going forward, points to gaps and voids in the current understanding of triple ion-beam irradiation effects (displacement damage produced simultaneously with helium and hydrogen implantation) and the synergistic effects of hydrogen.

36 MATERIALS SCIENCE↗

Effects of temperature on helium bubble behaviour in Fe–9Cr alloy

In the present study, Fe–9Cr model alloys were irradiated by 275 keV He + ions at 500 to 800 °C to a peak damage level and implanted helium content of 0.5 dpa and 0.75 at% He, respectively. Effects of temperature on He bubble behaviour were studied by transmission electron microscopy (TEM) to reveal the temperature effects. The bubble spatial distribution changes from homogenous at 500 and 600 °C to heterogeneous at 700 and 800 °C, due to preferential bubble precipitation on dislocations and grain boundaries at high temperature. Faceted bubbles with low energy faces along the {001} planes were present at all four temperatures and are attributed to surface energy minimization. Bubble precipitation on the GBs became more pronounced with increasing temperature. Meanwhile, the cavity swelling increased with increasing temperature, from 0.59% at 500 °C to 8.21% at 800 °C with a sharp increase above 700 °C. By analysing the temperature dependence of bubble size and density, a transition temperature between low and high temperature regimes was obtained in terms of different activation energies which are related to different bubble nucleation and formation mechanisms.

36 MATERIALS SCIENCE↗

Identification of a new isomeric state in 76 Zn following the β decay of 76 Cu

Background: The evolution of nuclear shell structure far from stability can be explored by identifying and measuring the properties of isomers. Neutron-rich nuclei between the Z = 28 and Z = 50 closed shells have been the subject of recent studies which have identified a number of 0.1 - 10 µs isomers and measured detailed spectroscopic properties. Purpose: The purpose of this analysis was to identify and measure the properties of short-lived isomeric states populated following β decay in Z ≈ 30, N ≈ 50 nuclei near the doubly magic nucleus 78 Ni. Methods: Here, radioactive ions produced by beam fragmentation at the National Superconducting Cyclotron Laboratory were implanted into a CeBr 3 scintillator coupled to a pixelated photomultiplier tube. Ancillary arrays of HPGe clover and LaBr 3 detectors were positioned around the implantation detector to measure β-delayed γ rays. Results: The previously observed 2634-keV level in 76 Zn, populated following the β decay of 76 Cu, was identified as isomeric with a half-life of 25.4(4) ns. A combination of timing and γ-ray spectroscopy was used to confirm this assignment. Shell-model calculations were performed and indicate that this state may be a high-spin negativeparity state formed by the occupation of the ν0g 9/2 orbital. Conclusions: A new isomeric state in 76 Zn has been identified and its half-life was measured. Ambiguity about the structure of this state could be resolved with further experiments.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Lithium Nucleation of Anode-Free Solid-State Batteries with a Dry Compressible Interlayer

Anode-free lithium batteries offer promising advantages, including increased energy density and the ability to address common mechanistic failures within the cell, thus increasing safety. One way that can make this possible is to control lithium nucleation. This could be achieved by reducing the overpotential required and implanting lithophilic nucleation sites in an anodic interlayer to aid in lithium ion transport and plating. The concept has been utilized in solid-state battery systems where electrolytes are solids with further improved safety and structural longevity. In this presentation, we discuss the use of a silver-holey graphene-based anodic interlayer that can be fabricated via direct dry compression without the use of solvent or binder. The addition of silver to the holey graphene matrix creates a route to lithium plating via a lower-energy intermediate. This idea is supported by the presence of a lithium-silver alloy that forms during the activation step. It is understood that the embedded silver acts as a nucleation site for lithium ions, thereby assisting in even plating. This control, combined with the added cushion of the holey graphene itself, can help reduce dendrite formation, ultimately increasing the safety and lifetime of the solid-state batteries.

Solid state batteries↗

Site-controlled fabrication of Ga nanodroplets by focused ion beam

Ga droplets are created by focused ion beam irradiation of GaAs surface. We report that ordered Ga droplets can be formed on the GaAs surface without any implantation damage. The droplets are characterized with bigger sizes than those droplets formed on damaged area. These aligned Ga droplets are formed via the migration of Ga atoms from ion irradiation area to the edge of undamaged GaAs surface and further nucleation into droplets. The morphological evolution and size distribution of these nanodroplets are investigated systematically with different beam irradiation time and incident angles. Based on this method, well positioned Ga nanodroplets, such as chains, are achieved by using focus ion beam patterning. The controllable assembly of droplets on undamaged semiconductor surface can be used to fabricate templates, to fabricate quantum structures and quantum devices by droplet epitaxy technique.

36 MATERIALS SCIENCE↗

Characterizing the lipid and metabolite changes associated with placental function and pregnancy complications using ion mobility spectrometry-mass spectrometry and mass spectrometry imaging

Successful pregnancy is dependent upon discrete biological events, which include embryo implantation, decidualization, and placentation. Problems associated with each of these events can cause infertility or conditions such as preeclampsia. A greater understanding of the molecular changes associated with these complex processes is necessary to aid in identifying treatments for each condition. Previous nuclear magnetic resonance spectroscopy and mass spectrometry studies have been used to identify metabolites and lipids associated with pregnancy-related complications. However, due to limitations associated with conventional implementations of both techniques, novel technology developments are needed to more fully understand the initiation and development of pregnancy related problems at the molecular level. In this perspective, we describe current analytical techniques for metabolomic and lipidomic characterization of pregnancy complications and discuss the potential for new technologies such as ion mobility spectrometry-mass spectrometry and mass spectrometry imaging to contribute to a better understanding of the molecular changes that affect the placenta and pregnancy outcomes.

Environmental Molecular Sciences Laboratory↗

Oxidation State of 229 Th Recoils Implanted into MgF 2 Crystals

A solid-state nuclear clock based on the low-lying isomeric state in 229 Th has attracted growing interest. One potential problem for the solid-state nuclear clock approach is the suitability of the doped environment for photon emission of the nuclear isomeric state. Specifically, Th n+ n < 4 ions could open non-radiative decay routes for deexcitation, hindering the photon emission. Here we have used time-resolved photoluminescence (TRPL) and density functional theory (DFT) calculations to characterize MgF 2 crystals that have been implanted with 229 Th recoils via a-decay from a 233 U source with the goal of determining the charge state of the implanted thorium atoms. The DFT calculations predicted Th4+ to be the lowest energy oxidation state with Th3+ the next lowest in the MgF2 crystal environment. The DFT calculations also show Th4+:MgF 2 system has a band gap large enough so that the internal electron conversion decay channel is suppressed. Experimentally, we found no evidence for thorium in oxidations state other than +4 using TRPL spectroscopy that has a detection limit for Thn+ n < 4 ions several orders of magnitude smaller than the number of implanted 229Th recoils. This work shows that the solid-state approach is a viable option for a nuclear clock.

229Th Isomeric State↗

High-Resolution Mapping of Lunar Crustal Magnetic Fields: Correlations with Albedo Markings of the Reiner Gamma Class

During the last eight months of the Lunar Prospector mission (December 1999-July 1999), the spacecraft was placed in a relatively low-altitude (15-30-km perapsis), near-polar orbit that allowed high-resolution mapping of crustal magnetic fields. We report here initial studies of the correlation of locally strong magnetic anomalies with unusual, swirl-like albedo markings of the Reiner Gamma class. Based on this correlation, which is known from earlier studies of Apollo subsatellite magnetometer data, it has been proposed that the swirls represent regions whose higher albedos have been preserved via deflection of the solar-wind ion bombardment by strong crustal fields. This model in turn depends on the hypothesis that solar-wind implanted H is at least one component of the process that optically matures exposed silicate surfaces in the inner solar system . Specifically, it is hypothesized that implanted H acts as an effective reducing agent to enhance the rate of production of nanophase metallic Fe particles from preexisting silicates during micrometeoroid impacts. According to the model, the curvilinear shapes of these albedo markings are caused, at least in part, by the geometry of ion deflections in a magnetic field. The improved resolution and coverage of the Prospector data allow more detailed mapping of the fields, especially on the lunar farside. This permits a more quantitative test of whether all albedo markings of this class are associated with strong local magnetic fields.Only if the latter condition is met can the solar-wind deflection hypothesis he valid. The basic procedure for mapping crustal magnetic fields using Lunar Prospector magnetometer data follows that developed for analysis of Apollo subsatellite magnetometer data. The specific mapping steps are (1) selection of mission time intervals suitable for mapping crustal fields; these are limited essentially either to times when the Moon is in a lobe of the geomagnetic tail or to times when the Moon is in the solar wind but the spacecraft is in the lunar wake; the data are transformed to a radial, east, and north coordinate system with measurements given as a function of spacecraft latitude, longitude, and altitude; (2) visual editing of individual orbit segments selected for minimal external field disturbances; (3) minimization of remaining low-frequency external fields for individual orbit data segments by quadratic detrending; and (4) two-dimensional filtering of individual orbit segments to produce a vector field map along the slightly curved surface defined by the spacecraft altitude; maps of the three field components (radial, east, and north), the field magnitude, and the spacecraft altitude are constructed. For data obtained at low to middle latitudes, the horizontal resolution of the field maps is limited by the orbit-track separation (about 30 km at the equator). Maps of the field magnitude have been constructed within limited selenographic regions based mainly on data acquired in March, April, and May of 1999. This was a time period when the orbit plane was nearly aligned with the Sun-Moon line so that field mapping was possible at times when the Moon was in the solar wind as well as when the Moon was in the geomagnetic tail. Most of the coverage is across the lunar farside. However, a shows an example of a field map produced from solar-wind wake data for a region including Reiner Gamm on western Oceanus Procellarum (location: 58.5W, 7.5N). The contour interval is 3 nT and the mean spacecraft altitude is 18 km to within the accuracy allowed by the resolution of the map (30 km or about 1 deg.); strong magnetic anomalies correlate closely with swirl locations. Individual orbit profiles (whose resolution along the orbit track is comparable to the spacecraft altitude of 18 km) also demonstrate a good correlation of field magnitude with surface albedo. In order to investigate the correlation of magnetic fields with the location of swirl features, we have reexamined available lunar imagery (Lunar Orbiter, Apollo, and Clementine) to identify and map swirl locations within regions where swirls have previously been mapped. In these images, swirls were distinguished from other high-albedo features such as crater rays by their curvilinear shapes and increased visibility in forward-scattered light. Digital maps of swirls identified by all available imagery were then superposed on maps of the field magnitude at the spacecraft altitude. Based upon analysis of these composite magnetic/geologic maps, we draw the preliminary conclusion that swirl features are associated with magnetic anomalies revealed by Lunar Prospector. Detailed maps of these swirl features are currently being constructed for the magnetically strong regions antipodal to the Imbrium, Serenitatis, and Crisium Basins. Additional information contained in the original,

Hood, L. L.↗

Oxidation of silicon with a 5 eV O(-) beam

A silicon wafer has been oxidized at room temperature in vacuum using a pure, ground-state beam of O(-) ions. The beam was of sufficiently low energy that no displacement damage or implantation was energetically possible. The resulting SiO2 films were analyzed with X-ray photoelectron spectroscopy. A logarithmic dependence of oxide thickness on dose was observed, with an extrapolated oxidation efficiency of unity for the clean silicon surface. A distinct initial oxidation phase was observed, with an anomalously high level of silicon suboxides. In addition, the valence-band offset between the silicon and the oxide was unusually small, suggesting a large interfacial dipole.

Hecht, M. H.↗

Damage evolution in Au-implanted Ho2Ti2O7 titanate pyrochlore

Damage evolution at room temperature in Ho2Ti2O7 single crystals is studied under 1 MeV Au2+ ion irradiation by Rutherford backscattering spectroscopy along the <001> direction. For a better determination of ion-induced disorder profile, an iterative procedure and a Monte Carlo code (McChasy) were used to analyze ion channeling spectra. A disorder accumulation model, with contributions from the amorphous fraction and the crystalline disorder, is fit to the Ho damage accumulation data. The damage evolution behavior indicates that the relative disorder on the Ho sublattice follows a nonlinear dependence on dose and that defect-stimulated amorphization is the primary amorphization mechanism. Similar irradiation behavior previously was observed in Sm2Ti2O7. A slower damage accumulation rate for Ho2Ti2O7, as compared with damage evolution in Sm2Ti2O7, is mainly attributed to a lower effective cross section for defect-simulated amorphization.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Industrial ion source technology

Plasma probe surveys were conducted in a 30-cm source to verify that the uniformity in the ion beam is the result of a corresponding uniformity in the discharge-chamber plasma. A 15 cm permanent magnet multipole ion source was designed, fabricated, and demonstrated. Procedures were investigated for texturing a variety of seed and surface materials for controlling secondary electron emission, increasing electron absorption of light, and improved attachment of biological tissue for medical implants using argon and tetrafluoromethane as the working gases. The cross section for argon-argon elastic collisions in the ion-beam energy range was calculated from interaction potentials and permits calculation of beam interaction effects that can determine system pumping requirements. The data also indicate that different optimizations of ion-beam machines will be advantageous for long and short runs, with 1 mA-hr/cm being the rough dividing line for run length. The capacity to simultaneously optimize components in an ion-beam machine for a single application, a capacity that is not evident in competitive approaches such as diode sputtering is emphasized.

Kaufman, H. R.↗

Solar Ion Processing of Itokawa Grains: Constraints on Surface Exposure Times

Analytical TEM observations obtained to date reveal that a significant sub-population of grains returned from the surface of asteroid Itokawa have had their outer 30-100 nm processed by space weathering effects. Although the effects include some surface deposition of condensed impact vapor and isolated impact melt splashes, much of the width of the space weathered outer margins or "rims" on grains is derived from solar wind processing of the original host grain. Similar to what has long been reported for some lunar grains, the ion-processed rims on Itokawa grains exhibit varing degrees and depths of penetration of atomic-displacement ion damage, resulting in complete amorphization for some rims (particularly in plagioclase), or formation of highly defective but still crystalline structures in others (particularly in pyroxene and olivine). Possibly different from lunar grains, however, is the presence of isolated internal cavities or voids in Itokawa grain rims, which may be implantation "bubbles" due to accumulating implanted solar wind H and/or He. For a given mineral exposed at a particular set of long term solar wind conditions, the level of ion damage in a given grain rim, the depth of damage penetration represented by the rim width, and the formation or lack of formation of implantation bubbles can all be linked to the time spent by the grain in an uncovered state on the topmost, space-exposed, regolith surface. For the lunar case, we have previously shown that with reasonable assumptions about solar wind characteristics over time, a model can be developed to estimate this exposure time based on the width of amorphous rims on lunar grains. Here we report on an expansion of the model to cover exposure time information contained in the array of solar ion-induced features in Itokawa grains.

Christoffersen, R.↗

A macro-scale ruck and tuck mechanism for deformation in ion-irradiated polycrystalline graphite

A vein structure, which becomes more pronounced with increasing ion dose, was found on the surface of polycrystalline HOPG (highly oriented pyrolytic graphite) implanted by ex situ C + (up to 1.8 × 10 17 ions/cm 2 ), and in situ Ar + in a transmission electron microscope (TEM). These veins are found to be independent of the crystallographic orientations and are associated with the formation of pores. Underneath the veins, a triangular-shaped core was formed with the graphite platelet inside the core displaced up towards the surface. A macro-scale ‘ruck&tuck’ geometry was thus generated at these triangle structure boundaries. Progressive movement of dislocations along basal planes during irradiation was observed, and a mechanistic model was proposed on this basis to explain the vein formation. A small increase of c-spacing was observed with irradiation but it is believed that macro-scale vein formation plays a more vital role in the dimensional and property changes in polycrystalline graphite, especially when a stress gradient is present. Here, the model proposed also explains the change of thermal expansion in HOPG with irradiation. Together with Heggie’s ‘ruck&tuck’ and Barsoum’s ‘ripplocations’ models, the present model is considered to have provided an additional experimentally proven mechanism responsible for irradiation behaviour in graphite materials.

36 MATERIALS SCIENCE↗

Evaluation of neon focused ion beam milling for TEM sample preparation

Summary Gallium‐based focused ion beams generated from liquid–metal sources are widely used in micromachining and sample preparation for transmission electron microscopy, with well‐known drawbacks such as sample damage and contamination. In this work, an alternative (neon) focused ion beam generated by a gas field‐ionization source is evaluated for the preparation of electron‐transparent specimens. To do so, electron‐transparent sections of Si and an Al alloy are prepared with both Ga and Ne ion beams for direct comparison. Diffraction‐contrast imaging and energy dispersive x‐ray spectroscopy are used to evaluate the relative damage induced by the two beams, and cross‐sections of milled trenches are examined to compare the implantation depth with theoretical predictions from Monte Carlo simulations. Our results show that for the beam voltages and materials systems investigated, Ne ion beam milling does not significantly reduce the focused ion beam induced artefacts. However, the Ne ion beam does enable more precise milling and may be of interest in cases where Ga contamination cannot be tolerated.

PEKIN, T. C.↗

Deuterium retention and blistering in tungsten foils

To investigate deuterium retention and the onset of blistering, deuterium was implanted in cold rolled tungsten foils at fluences ranging from 3x1020 to 3x1022 D/m2. Ion energies were 300 eV and 2000 eV in order to be below and above the tungsten theoretical damage energy threshold. While there were energy dependent phenomena, blistering occurs regardless of ion energy. Both plastically and elastically deformed blisters were observed, as manifest in before and after micrographs. The fraction of plastically deformed blisters did not saturate at the fluences used in these studies. However, the size of the largest blister that relaxes during TDS does saturate at ~7 µm. A simple conceptual model is presented that identifies that deuterium released from elastically deformed blisters appears at ~600 K in the thermal desorption spectra, which is consistent with large vacancy clusters.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Measurement of Damage Profiles from Solar Wind Implantation

NASA's Genesis Mission launched from Cape Canaveral in August of 2001 with the goal of collecting solar wind in ultra-pure materials. The samples were returned to Earth more than three years later for subsequent analysis. Although the solar wind is comprised primarily of protons, it also contains ionized species representing the entire periodic table. The Genesis mission took advantage of the natural momentum of these ionized species to implant themselves in specialized collectors including single crystal Si and SiC. The collectors trapped the solar wind species of interest and sustained significant damage to the surface crystal structure as a result of the ion bombardment. In this work, spectroscopic ellipsometry has been used to evaluate the extent of this damage in Si and SiC samples. These results and models are compared for artificially implanted samples and pristine non-flight material. In addition, the flown samples had accumulated a thin film of molecular contamination as a result of outgassing in flight, and we demonstrate that this layer can be differentiated from the material damage. In addition to collecting bulk solar wind samples (continuous exposure), the Genesis mission actually returned silicon exposed to four different solar wind regimes: bulk, high speed, low speed, and coronal mass ejections. Each of these solar wind regimes varies in energy, but may vary in composition as well. While determining the composition is a primary goal of the mission, we are also interested in the variation in depth and extent of the damage layer as a function of solar wind regime. Here, we examine flight Si from the bulk solar wind regime and compare the results to both pristine and artificially implanted Si. Finally, there were four samples which were mounted in an electrostatic "concentrator" designed to reject a large fraction (>85%) of incoming protons while enhancing the concentration of ions mass 4-28 amu by a factor of at least 20. Two of these samples were single crystal 6H silicon carbide. (The others were polycrystalline CVD diamond and amorphous carbon that were not examined in the work.) The ion damaged SiC samples from the concentrator were studied in comparison to the flight Si from the bulk array to understand differences in the extent of the damage.

McNamara, K. M.↗

Tungsten diffusion in silicon

Two doses (10{sup 13} and 10{sup 15} cm{sup −2}) of tungsten (W) atoms were implanted in different Si(001) wafers in order to study W diffusion in Si. The samples were annealed or oxidized at temperatures between 776 and 960 °C. The diffusion profiles were measured by secondary ion mass spectrometry, and defect formation was studied by transmission electron microscopy and atom probe tomography. W is shown to reduce Si recrystallization after implantation and to exhibit, in the temperature range investigated, a solubility limit close to 0.15%–0.2%, which is higher than the solubility limit of usual metallic impurities in Si. W diffusion exhibits unusual linear diffusion profiles with a maximum concentration always located at the Si surface, slower kinetics than other metals in Si, and promotes vacancy accumulation close to the Si surface, with the formation of hollow cavities in the case of the higher W dose. In addition, Si self-interstitial injection during oxidation is shown to promote W-Si clustering. Taking into account these observations, a diffusion model based on the simultaneous diffusion of interstitial W atoms and W-Si atomic pairs is proposed since usual models used to model diffusion of metallic impurities and dopants in Si cannot reproduce experimental observations.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗