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At least 73 records · Page 4

Helium bubble nucleation and growth in alloy HT9 through the use of in situ TEM: Sequential he-implantation and heavy-ion irradiation versus dual-beam irradiation

The formation of He bubbles in Ferritic/Martensitic steel HT9 is investigated through the use of in situ Transmission Electron Microscopy coupled with He implantation and heavy ion irradiation. Of particular interest is the effect of increasing He appm/dpa ratio on the formation and growth of the bubbles, as well as the effect of the sequential order of ion irradiation i.e. He-pre-implantation followed by heavy-ion irradiation versus true dual-beam irradiation. Finally, the role of He is discussed.

Duemmler, Kai↗

Synthesis of magnesiowüstite nanocrystallites embedded in an amorphous silicate matrix via low energy multiple ion implantations

The synthesis process is presented for experimentally simulating modifications in cosmic dust grains using sequential ion implantations or irradiations followed by thermal annealing. Cosmic silicate dust analogues were prepared via implantation of 20–80 keV Fe - , Mg - , and O - ions into commercially available p-type silicon (100)wafers. The as-implanted analogues are amorphous with a Mg/(Fe+Mg) ratio of 0.5 tailored to match theoretical abundances in circumstellar dusts. Before the ion implantations were performed, Monte-Carlo-based ion-solid interaction codes were used to model the dynamic redistribution of the implanted atoms in the silicon substrate. 600 keV helium ion irradiation was performed on one of the samples before thermal annealing. Two samples were thermally annealed at a temperature appropriate for an M-class stellar wind, 1000 K, for 8.3 h in a vacuum chamber with a pressure of 1 x 10 -7 torr. The elemental depth profiles were extracted utilizing Rutherford Backscattering Spectrometry (RBS) in the samples before and after thermal annealing. X-ray diffraction (XRD)analysis was employed for the identification of various phases in crystalline minerals in the annealed analogues. Transmission electron microscopy (TEM) analysis was utilized to identify specific crystal structures. RBS analysis shows redistribution of the implanted Fe, Mg, and O after thermal annealing due to incorporation into the crystal structures for each sample type. XRD patterns along with TEM analysis showed nanocrystalline Mg and Fe oxides with possible incorporation of additional silicate minerals.

79 ASTRONOMY AND ASTROPHYSICS↗

Comparative study of helium bubbles in a Ti-Ta alloy and a Ti/Ta nanocomposite

Here, we investigated the size, density, and distribution of helium (He) bubbles in a Ti-Ta single-phase alloy and a Ti/Ta dual-phase nanocomposite using transmission electron microscopy. The Ti/Ta nanocomposite was fabricated via phase separation during high-temperature annealing of the single-phase Ti-Ta alloy. He ion implantation in the Ti-Ta single-phase alloy leads to the formation of nano-scale He bubbles (~1.7 nm in size, ~2.6×10 5 /μm 3 in volumetric density). He bubbles were found to segregate to grain boundaries. Under identical implantation conditions, numerous He bubbles also formed in the Ti/Ta nanocomposite. Closer inspection revealed that He bubbles in the Ti-rich phase are smaller and of higher volumetric density (~1.2 nm, ~8.4×10 5 /μm 3 ) than those in the Tarich phase (~3 nm, ~1.8×10 5 /μm 3 ) and the single-phase alloy. He bubbles were also observed to decorate phase boundaries, but they were generally smaller than those on grain boundaries. These results suggest that Ti/Ta phase boundaries are less conducive to the growth of large He bubbles than grain boundaries in the Ti-Ta single phase alloy.

36 MATERIALS SCIENCE↗

Origin of increased helium density inside bubbles in Ni (1–$x$) Fe $x$ alloys

Due to virtually no solubility, He atoms implanted or created inside materials tend to form bubbles, which are known to damage material properties through embrittlement. Higher He density in nano-sized bub- bles was observed both experimentally and computationally in Ni (1–$x$) Fe $x$ -alloy samples compared to Ni. The bubbles in the Ni (1–$x$) Fe $x$ -alloys were observed to be faceted, whereas in elemental Ni they were more spherical. Molecular dynamics simulations showed that stacking fault structures formed around bubbles at maximum He density. Higher Fe concentrations stabilize stacking fault structures, suppress evolution of dislocation network around bubbles and suppress complete dislocation emission, leading to higher He density.

36 MATERIALS SCIENCE↗

New Directions in Focused Ion Beam Induced Deposition for the Nanoprinting of Functional 3D Heterostructures

The focused ion beam (FIB) microscope is well established as a high-resolution machining instrument capable of site-selectively removing material down to the nanoscale. Beyond subtractive processing, however, the FIB can also add material via a technique known as focused ion beam induced deposition (FIBID). Using FIBID, the FIB can thus be employed for the direct-write of complex nanostructures. This work explores new directions in three-dimensional FIBID nanoprinting, harnessing unique features of helium and neon FIBs. In particular, the superior spatial resolution of these novel FIBs is leveraged to fabricate precise multimaterial architectures, an isotope effect is used to create satellite deposits, and dose-controlled implantation of the gaseous ions is used to engineer internal voids. In the context of voids, the fabrication of hollow nanopillars by helium-FIBID due to concurrent milling (as shown previously by others) is revisited. Insight into the chemical and structural composition of the nanostructures is obtained using advanced electron microscopy, accurately revealing buried interfaces, crystallite distributions, chemical compositions, and material transformations. Next-generation devices and technologies that could be enabled by the novel heterostructures demonstrated here are discussed, setting the stage for the potential evolution of FIBID into a versatile platform for functional nanomaterials design and fabrication.

FIBID↗

An exploratory study on helium mobility in amorphous and crystallized bulk metallic glasses

In this study, Zr 52.5 Cu 17.9 Ni 14.6 Al 10 Ti 5 and Cu 60 Zr 20 Hf 10 Ti 10 amorphous and crystallized bulk metallic glasses (BMGs) were implanted at room temperature by 150 keV 3 He + ions to fluences of 2 × 10 15 cm -2 and 5 × 10 15 cm -2 , producing peak implanted He concentrations of ~1,100 and 3,500 appm, respectively. Nuclear reaction analysis (NRA) performed on post-implantation annealed samples at various temperatures between 250 and 600 °C (~0.30 to 0.75 of the absolute melting temperature T m of the BMGs) revealed no appreciable He migration. Complementary thermal desorption spectroscopy (TDS) on as-implanted samples, which involved in situ annealing, showed appreciable He release only at temperatures higher than ~700 °C (~0.76-0.90 T m ) in all the samples. Half or more of the implanted He did not desorb up to the maximum investigated TDS annealing temperature of 770 °C (~0.85-0.97 T m ). The lack of pronounced He diffusion up to 600 °C as observed from the NRA and TDS data was attributed to He trapping in free volume sites present in the BMGs, which seems to play a similar role to vacancies in crystalline materials. It was also observed that in both the amorphous and crystallized forms of the Zr BMG, the sample implanted to the lower fluence released more He as compared to the sample implanted with a higher fluence. The crystalline forms of both the Cu and Zr BMGs released more He as compared to their amorphous counterparts.

36 MATERIALS SCIENCE↗

Unraveling the Early-Stage Ordering of Krypton Solid Bubbles in Molybdenum: A Multimodal Study

Self-organization of defects such as fission gas bubbles in materials can lead to high inventory capacity for fission gas storage and help mitigate swelling caused by fission gases in nuclear fuel materials under radiation in nuclear reactors. Here, we report the physical mechanism of self-organization of krypton (Kr) gas bubbles in molybdenum (Mo) under ion implantation. The ion fluence and temperature-dependent formation of Kr solid bubble superlattice (SBS) in Mo were investigated by using both synchrotron-based small-angle X-ray scattering (SAXS) and transmission electron microscopy (TEM). Early stage self-organization of gas bubbles is observed at a fluence of 2.5 × 10 16 ions/cm 2 at temperatures of 300–400 °C. The bubble lattice constant increases with increasing implantation temperature from 300 to 400 °C. Both experiments and atomic kinetic Monte Carlo modeling indicate that the Kr solid bubbles are weakly ordered in comparison to previously studied helium (He) gas bubble superlattice (GBS) while the lattice constant are relatively smaller for Kr SBS compared to that of He GBS. The irradiation conditions suggest that spinodal decomposition, which is a form of phase separation, probably precedes gas bubble ordering in Mo. Altogether, our work sheds light on the formation mechanism of noble gas superlattice toward the development of radiation-tolerant materials which are important for the design of advanced nuclear reactors.

36 MATERIALS SCIENCE↗

Effects of elastic softening and helium accumulation kinetics on surface morphological evolution of plasma-facing tungsten

Based on a continuous-domain model, capable of accessing the spatiotemporal scales relevant to fuzz formation on the surface of plasma-facing component (PFC) tungsten, we report self-consistent simulation results that elucidate the effects of elastic softening and helium (He) accumulation kinetics on the surface morphological response of PFC tungsten. The model accounts for the softening of the elastic moduli in the near-surface region of PFC tungsten, including both thermal softening at high temperature and softening due to He accumulation upon He implantation. The dependence of the elastic moduli on the He content follows an exponential scaling relation predicted by molecular-dynamics simulations, while the He content in the near-surface region of PFC tungsten evolves according to a first-order saturation kinetics, consistent with experimental and simulation results reported in the literature. We establish that this elastic softening accelerates both nanotendril growth on the PFC surface and the onset of fuzz formation. We also explore the role of the rate of He accumulation to a saturation level in the near-surface region of irradiated tungsten in the onset of fuzz formation. For PFC tungsten surfaces such as W(110) where, under typical irradiation conditions, the characteristic time scale for stress-driven surface diffusion is comparable to the characteristic time scale for He accumulation, we find that accelerating the rate of He accumulation accelerates the growth rate of nanotendrils emanating from the surface. Additionally, we present a systematic parametric study of the PFC surface morphological response to explore its dependence on the He accumulation kinetics that is controlled by the irradiation conditions for low-energy implantation. Finally, we introduce an incubation time for nanotendril growth on the PFC surface, a concept equivalent to that of incubation fluence discussed in the literature, to predict and explain the minimum exposure time required to observe fuzz formation on PFC tungsten surfaces.

36 MATERIALS SCIENCE↗

Grain boundary softening from stress assisted helium cavity coalescence in ultrafine-grained tungsten

The formation of helium cavities in coarse-grained materials produces hardening proportional to the number density and size of the cavities and due to the interaction of dislocations with intragranular helium defects. In nanostructured metals containing a high density of interfacial sinks, preferential cavity formation in the grain boundaries instead produces softening that is often attributed to enhanced interfacial plasticity. Here, employing two grades of ultrafine-grained tungsten, we explore this effect using targeted implantation studies to map cavity evolution as a function of the irradiation conditions and quantify its impact on the mechanical response through nanoindentation. Softening is reported at implantation temperatures above the threshold for preferential grain boundary cavity formation but at a sufficiently low fluence prior to the growth of intragranular cavities. Collective changes in the mean cavity size, density, and morphology beneath a residual impression on an implanted surface indicate that cavity coalescence accompanied the reduction in hardness. Complementary atomistic simulations demonstrate that, in tungsten grain structures exhibiting softening, grain boundary bubble coalescence is driven by stress concentrations that further act to localize strain in the grain boundaries through cooperative deformation processes involving local atomic shuffling and sliding, dislocation emission, and even the nucleation of unstable twinning events.

36 MATERIALS SCIENCE↗

The effect of helium on cavity swelling in dual-ion irradiated Fe and Fe-10Cr ferritic alloys

We report Ferritic-martensitic (FM) steels for in-vessel components in proposed fusion reactors are expected to suffer from high levels of displacement damage and helium (He) generation by neutron transmutation. However, a thorough understanding of the He synergistic effects on the cavity swelling in FM steels is still not well established. To gain fundamental insights into the He effect on cavity swelling, high purity Fe and Fe-10 wt.% Cr ferritic model alloys were irradiated with 8 MeV Ni ions and co-implanted He ions at 400 to 550 °C up to 30 displacements per atom (dpa) with He implantation rates of 0.1, 10 and 50 appm He/dpa. The current study focuses on the 50 appm He/dpa, 500 °C behavior vs. 0.1 and 10 appm He/dpa. Irradiation-induced defects, including cavities, dislocation loops, and dislocation networks were characterized using transmission electron microscopy (TEM). In the grain interior, a bimodal cavity size distribution was observed in the 10 and 50 appm He/dpa samples, but not for 0.1 appm He/dpa. Cavity swelling was maximized at intermediate He implantation rates of ~10 appm He/dpa for both ion-irradiated Fe and Fe-10Cr alloys. The cavity swelling behavior as a function of He implantation rate appears to be controlled by the He/dpa-dependent variation of cavity sink strengths. Treating small bubbles as biased sinks for interstitial absorption can significantly increase the ratio of biased to unbiased sink strengths (Q) and results in maximized cavity swelling for a Q ratio close to one.

36 MATERIALS SCIENCE↗

Anomalous lattice expansion of bcc Ta in helium-loaded diamond anvil cells

Anomalous lattice expansion of bcc Ta is observed in helium-loaded diamond anvil cell (DAC) experiments near 6 GPa and above 400 K, while co-loaded W, Mo, and Au exhibit normal thermal expansion. The Ta volume expansion increases with temperature, reaching ~14% near 650 K before plateauing, and is largely retained after recovery to ambient conditions. Time-resolved measurements at 500 K reveal progressive expansion over several hours, consistent with gradual, thermally activated He incorporation. The largely retained expansion during subsequent cooling and holding at 400 K indicates that the incorporated He is predominantly kinetically trapped. The data reveal two distinct regimes: below ~550 K, modest and spatially uniform expansion consistent with interstitial He trapping at isolated, randomly distributed vacancies; above ~550 K, He-vacancy cluster growth producing dramatically larger expansion, peak broadening, and a core–shell microstructure revealed by micron-resolution X-ray diffraction mapping. These results demonstrate that He is not always a passive pressure medium in DAC experiments and reveal a previously unrecognized regime of He-mediated lattice modification in Ta, complementing conventional ion-implantation studies relevant to nuclear and fusion structural materials.

Diamond anvil cell↗

Formation of misfit dislocation arrays and helium nanochannels near copper surface assisted by high-temperature graphene deposition

Misfit dislocation arrays (MDAs) at semi-coherent heterogeneous interface have been demonstrated effectiveness to trap and then outgas helium (He) for alleviating void swelling in metals, but limited by atomic-level thin film deposition that is difficult to scale-up for industrial production. In this work, we proposed an innovative strategy that could generate semi-coherent homophase interfaces in a same grain by varying surface energy density assisted by high-temperature graphene (Gr) deposition. This strategy transforms strain energy and surface energy, two originally distinctive processes into successive processes, and demonstrates experimentally and theoretically by introducing {111} copper (Cu) in a {100} Cu grain. Subsequent He implantation and electrical resistivity measurement results suggest that high-density MDAs originated at this {111}/{100} interface could form stable He nanochannels near Cu surface with Gr assistance, manifesting by ultra-low increased ratio of the electrical resistivity (i.e. ~3800% of Cu vs. ~90% of Gr/Cu) after He implantation. Finally, the present findings may provide a new strategy for efficiently managing He and achieving surface protection of advanced metals, merely by depositing a super-rigid material on metal surface to greatly reduce surface energy density.

36 MATERIALS SCIENCE↗

Deciphering the influence of high-flux helium plasma exposure on tungsten nanostructure growth using real-time, in situ spectroscopic ellipsometry

In situ analysis of surfaces during high-flux plasma exposure represents a long-standing challenge in the study of plasma–material interactions. While post-mortem microscopy can provide a detailed picture of structural and compositional changes, in situ techniques can capture the dynamic evolution of the surface. In this study, we demonstrate how spectroscopic ellipsometry can be applied to the real-time characterization of W nanostructure (also known as “fuzz”) growth during exposure to low temperature, high-flux He plasmas. Strikingly, over a wide range of sample temperatures and helium fluences, the measured ellipsometric parameters (Ψ,Δ) collapse onto a single curve that can be directly correlated with surface morphologies characterized by ex situ helium ion microscopy. The initial variation in the (Ψ,Δ) parameters appears to be governed by small changes in surface roughness (<50 nm) produced by helium bubble nucleation and growth, followed by the emergence of 50 nm diameter W tendrils. This basic behavior appears to be reproducible over a wide parameter space, indicating that the spectroscopic ellipsometry may be of general practical use as a diagnostic to study surface morphologies produced by high-flux He implantation in refractory metals. An advantage of the methods outlined here is that they are applicable at low incident ion energies, even below the sputtering threshold. As an example of this application, we apply in situ ellipsometry to examine how W fuzz growth is affected both by varying ion energy and the temperature of the surface.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Revealing nano-scale lattice distortions in implanted material with 3D Bragg ptychography

Small ion-irradiation-induced defects can dramatically alter material properties and speed up degradation. Unfortunately, most of the defects irradiation creates are below the visibility limit of state-of-the-art microscopy. As such, our understanding of their impact is largely based on simulations with major unknowns. Here we present an x-ray crystalline microscopy approach, able to image with high sensitivity, nano-scale 3D resolution and extended field of view, the lattice strains and tilts in crystalline materials. Using this enhanced Bragg ptychography tool, we study the damage helium-ion-irradiation produces in tungsten, revealing a series of crystalline details in the 3D sample. Our results lead to the conclusions that few-atom-large ‘invisible’ defects are likely isotropic in orientation and homogeneously distributed. A partially defect-denuded region is observed close to a grain boundary. These findings open up exciting perspectives for the modelling of irradiation damage and the detailed analysis of crystalline properties in complex materials.

42 ENGINEERING↗

Suppression of Helium Bubble Nucleation in Beryllium Exposed Tungsten Surfaces.

One of the most severe obstacles to increasing the longevity of tungsten-based plasma facing components, such as divertor tiles, is the surface deterioration driven by sub-surface helium bubble formation and rupture. Supported by experimental observations at PISCES, this work uses molecular dynamics simulations to identify the microscopic mechanisms underlying suppression of helium bubble formation by the introduction of plasma-borne beryllium. Simulations of the initial surface material (crystalline W), early-time Be exposure (amorphous W-Be) and final WBe 2 intermetallic surfaces were used to highlight the effect of Be. Significant differences in He retention, depth distribution and cluster size were observed in the cases with beryllium present. Helium resided much closer to the surface in the Be cases with nearly 80% of the total helium inventory located within the first 2 nm. Moreover, coarsening of the He depth profile due to bubble formation is suppressed due to a one-hundred fold decrease in He mobility in WBe2, relative to crystalline W. This is further evidenced by the drastic reduction in He cluster sizes even when it was observed that both the amorphous W-Be and WBe 2 intermetallic phases retain nearly twice as much He during cumulative implantation studies.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

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↗

Thermal expansion of plasma-exposed tungsten

We report results from a systematic analysis of thermal expansion of plasma-exposed tungsten based on molecular-dynamics simulations using models of tungsten with distributions of helium (He) bubbles in the tungsten matrix. We distinguish between two approaches of filling the bubbles with He, where the amount of He in the bubble can or cannot vary with temperature. In the former case, the thermal expansion coefficient decreases monotonically with the porosity and He content of the tungsten matrix, while in the latter case, the thermal expansivity increases monotonically with increasing porosity and He content. The latter condition, where the He content in the bubble is determined at the implantation temperature and remains constant with varying temperature in the tungsten matrix, is consistent with He species transport in tungsten used as a plasma-facing component (PFC) in nuclear fusion reactors and implies the development of biaxial compressive thermal strains in the PFC material that contribute to accelerating the growth of a nanostructure on PFC tungsten surfaces. Furthermore our analysis advances the fundamental understanding of thermal expansion in PFC tungsten and contributes to the development of a thermophysical property database for properly incorporating effects of realistic heat loads into modeling the dynamical response of PFC tungsten under fusion reactor operating conditions.

36 MATERIALS SCIENCE↗

Influence of helium bubbles on the bulk equation of state of gold under static compression

Nuclear materials often evolve into two-phase systems comprising a bulk matrix with dispersed inert-gas bubbles. The presence of these bubbles can have consequences to the thermomechanical response of materials and is a key life-limiting factor in some nuclear fuel forms. Understanding the behavior of these two-phase, bubble-matrix systems is, thus, important to improved predictive models and frameworks for many nuclear materials applications. While temperature excursions of these two-phase systems have been characterized, fewer studies have focused on the evolution of inert-gas bubbles under pressure. Here, in this paper, we use x-ray tools to interrogate a He-implanted gold foil to determine the pressure-dependent evolution of the individual components (Au matrix + bubbles), and we compare that total pressure dependence to theoretical equation-of-state descriptions based on mixing rules.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗