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Amorphous TiO 2 nanotubes were irradiated in-situ in a transmission electron microscope (TEM) with Kr+ ions at energies of 46 keV, 150 keV, and 1 MeV and with 46 keV Xe+ ions, to investigate the structural and morphological evolution of the nanotubes under irradiation. At all irradiation conditions, amorphous TiO 2 nanotubes exhibited significant morphological instability, and tended to undergo volumetric swelling with increasing ion counts, often until collapse of the original nanotube structure. Molecular dynamics (MD) simulations confirmed that irradiation-induced defects can explain the observed swelling. Structurally, nanotubes remain amorphous following all Kr+ irradiation conditions, but irradiation with 46 keV Xe+ leads to the formation of anatase nanocrystallites. Importantly, through systematically varying ion energy and ion species, we try to elucidate the influence of nuclear and electronic stopping power on ion irradiation induced changes. By contextualizing these results within the existing literature, we propose that the observed changes in TiO 2 nanotube morphology and structure could be due to a competition between two mechanisms: (1) disorder-induced swelling and (2) irradiation-induced amorphous-to-crystalline transformation. [ABSTRACT FROM AUTHOR]

Understanding the stability of irradiation-induced voids in materials is important for engineering material's swelling behavior under irradiation. In-situ TEM offers a spatial and temporal resolution that is suitable for investigating the evolution of voids under irradiation. However, the in-situ videos have often been too large to be analyzed manually, leaving the valuable data underutilized. We developed a deep learning-based semantic segmentation model to consistently study the growth and shrinkage of voids in nickel under 1 MeV krypton ion irradiation at various temperatures from 525 °C to 650 °C. With a foil thickness near 100 nm and ion flux of 6.3 × 1011 ions⋅ cm−2⋅s−1, the pre-existing voids, which were created beforehand by irradiation at 600 °C to 0.5 dpa, shrank at low temperatures and grew at high temperatures under irradiation, where the transition occurred at 575 °C (∼0.5 T M). The observed stability transition provided new insight for the shrinkage mechanism of voids under irradiation. In addition, an annealing experiment on nickel, previously irradiated at 600 °C to 3 dpa, was performed sequentially at 650 °C to 720 °C to reveal the shrinkage rate of void as a function of temperature and void size. The advantage of combining computer vision and in-situ TEM to obtain comprehensive void evolution was demonstrated. [Display omitted] [ABSTRACT FROM AUTHOR]

Fe and Fe-Cr (Cr = 10–16 at.%) specimens were neutron-irradiated at 300 °C to 0.01, 0.1 and 1 dpa. The TEM observations indicated that the Cr significantly reduced the mobility of dislocation loops and suppressed vacancy clustering, leading to distinct damage microstructures between Fe and Fe-Cr. Irradiation-induced dislocation loops in Fe were heterogeneously observed in the vicinity of grown-in dislocations, whereas the loop distribution observed in Fe-Cr is much more uniform. Voids were observed in the irradiated Fe samples, but not in irradiated Fe-Cr samples. Increasing Cr content in Fe-Cr results in a higher density, and a smaller size of irradiation-induced dislocation loops. Orowan mechanism was used to correlate the observed microstructure and hardening, which showed that the hardening in Fe-Cr can be attributed to the formation of dislocation loops and α′ precipitates. [ABSTRACT FROM AUTHOR]

The microstructural evolution in ferrite and austenitic in cast austenitic stainless steel (CASS) CF8, as received or thermally aged at 400 °C for 10,000 h, was followed under TEM with in situ irradiation of 1 MeV Kr ions at 300 and 350 °C to a fluence of 1.9 × 10 15 ions/cm 2 (∼3 dpa) at the IVEM-Tandem Facility. For the unaged CF8, the irradiation-induced dislocation loops appeared at a much lower dose in the austenite than in the ferrite. At the end dose, the austenite formed a well-developed dislocation network microstructure, while the ferrite exhibited an extended dislocation structure as line segments. Compared to the unaged CF8, the aged specimen appeared to have lower rate of damage accumulation. The rate of microstructural evolution under irradiation in the ferrite was significantly lower in the aged specimen than in the unaged. This difference is attributed to the different initial microstructures in the unaged and aged specimens, which implies that thermal aging and irradiation are not independent but interconnected damage processes. [ABSTRACT FROM AUTHOR]

Thermally-aged cast austenitic stainless steels (CASS) CF8 was irradiated with 1 MeV Kr ions at 300, 350 and 400 °C to 1.88 × 10 19 ions/m 2 (∼3 dpa) at the IVEM-Tandem Facility at the Argonne National Laboratory. Before irradiation, the distribution of G-phase precipitates in the ferrite showed spatial variations, and both their size and density were affected by the ferrite–austenite phase boundary and presence of M 23 C 6 carbides. Under 300 °C irradiation, in situ TEM observation showed G-phase precipitates were relatively unchanged in the vicinity of the phase boundary M 23 C 6 carbides, while the density of G-phase precipitates increased with increasing dose within the ferrite matrix. Coarsening of G-phase precipitates was observed in the vicinity of phase boundary M 23 C 6 carbides at 350 °C and 400 °C. [ABSTRACT FROM AUTHOR]

Alloy 709 stainless steel (A709 SS) has gained an increased interest in nuclear applications due to its advanced properties at high temperatures over the widely used Type 316 SS. However, how this alloy behaves under irradiation with concurrent environmental factors, such as mechanical deformation and/or thermal annealing, has not been studied. In this work, we used in-situ ion irradiation inside a transmission electron microscope (TEM) to investigate the effects of irradiation on the microstructures of A709 SS samples with different prior processing histories, including as-received, annealed, and creep-deformed. It was found that, compared to room temperature irradiation, 600°C irradiation led to larger dislocation loop sizes and lower loop densities. With 600°C irradiation, the creep-deformed sample, which had the highest precipitate density and the highest dislocation density, had the smallest loop size and the lowest loop density compared to others. This observation has been rationalized with quantitative evaluation of the sink strength factors in each sample. This study shows that in-service deformation can significantly affect the irradiation performance in structural materials at reactor operating conditions. [ABSTRACT FROM AUTHOR]

• Two new ternary Ni(II) CPs were synthesized and characterized. • CP 1 displays a 1D zigzag chain. CP 2 possesses a 2D 3,5L27 network. • Two CPs show highly performance for photodegradation of MB. • CPs 1–2 exhibited highly selectivity and sensitive towards benzaldehyde and Fe3+. Two nickel(II) coordination polymers (CPs), [Ni(5-NIP)(L)(H 2 O)] n (1) and [Ni(1,4-PDA)(L)(H 2 O)] n (2) (L = 1,3-bis(5,6-dimethylbenzimidazol-1-yl)propane, 5-H 2NIP = 5-nitroisophthalic acid, 1,4-H 2PDA = 1,4-phenylenediacetic acid) were hydrothermally synthesized and structurally characterized. 1 displays a 1D zigzag chain alone the a -axis. 2 shows a 3,5-connected 3,5L27 framework with a point symbol of {3.4.5}{32.42.5.63.72}. Two compounds exhibit remarkable photocatalytic activities for degradation of the methylene blue under UV irradiation. 1 and 2 can serve as the dual-responsive luminescent chemosensors for the selective detection of benzaldehyde and Fe3+ in aqueous systems. Two Ni(II)-based coordination polymers(CPs) have been synthesized. CP 1 possesses a 1D [Ni(nip)] n zigzag chain while CP 2 shows a 3,5-connected framework 3,5L27 topological type with a point symbol of {3.4.5}{32.42.5.63.72}. They display high photocatalytic capacities for degrading the methylene blue (MB) solution. Meanwhile, 1 and 2 exhibit selective and sensitive detection of benzaldehyde and Fe3+ by fluorescence quenching effect. Image, graphical abstract [ABSTRACT FROM AUTHOR]

To evaluate the potential of high entropy alloys (HEAs) for nuclear applications, two HEAs, Al 0.3 CoCrFeNi and CoCrFeMnNi, and a conventional Type 316H stainless steel (SS) were irradiated with 1 MeV krypton ions at 500 °C up to 1 dpa, and examined in-situ with a transmission electron microscope (TEM). After irradiation, a high density of ordered L1 2 nanoparticles was observed in Al 0.3 CoCrFeNi. In contrast, no phase transformation was observed in CoCrFeMnNi and 316H SS. In the thin foil regions of TEM samples, stacking-fault tetrahedra were observed in the HEAs. In the thick foil regions, interstitial dislocation loops were observed for all alloys, and the areal loop density increased linearly with foil thickness. The Al 0.3 CoCrFeNi had the largest loop size (the lowest density), followed by the CoCrFeMnNi and then the 316H SS. The higher loop nucleation rate in the 316H SS was attributed to carbon content. The degree of irradiation hardening was slightly lower for the HEAs than for the 316H SS, which is a promising sign for the nuclear application of HEAs at high temperatures. Bright-field TEM micrographs of Al0.3CoCrFeNi, CoCrFeMnNi and 316H SS irradiated with 1 MeV Kr ions at 500 °C to 1 dpa. All images were taken at similar foil thickness near 110 zone axis with g = 200. The two high entropy alloys exhibited significantly larger size and smaller density of dislocation loops as compared with the 316H stainless steels. Image 1 [ABSTRACT FROM AUTHOR]

In situ irradiations with 1 MeV Kr ions at 50~613 K up to a fluence of 6.25 × 1014 ions/cm2 (~1.25 displacements per atom, dpa) have been performed on pre-aged dilute Cu-0.9%Co, Cu-0.9%Fe and Cu-0.8%Cr alloys containing uniform matrix dispersions of coherent precipitates in order to study the effects of initial precipitate sink strength, damage dose and irradiation temperature on radiation-induced coherency loss of precipitates. Coherent precipitates with different point defect sink strengths (2πNd, where N and d are the precipitate density and diameter) were used in this work to examine potential differences in atomic relaxation during absorption of point defects. In all cases, irradiation to low doses (<~1 dpa) was very effective at inducing loss of precipitate coherency. At low sink strengths (~1013 m−2), loss of precipitate coherency could be induced for doses ~0.01 dpa. This suggests there might be an efficient preferential medium-range strain-induced bias for absorption of interstitial defects due to tensile strains emanating from the undersized precipitates, which induces relatively rapid loss of coherency at low precipitate sink strengths. High precipitate sink strength (~1014 m−2) conditions were relatively resistant to the radiation-induced loss of coherency (requiring higher doses approaching ~1 dpa) and this might be due to nearly equal numbers of interstitial and vacancy defects arriving at the precipitate interface for such high sink strength conditions. The precipitate coherency loss was observed to have a weak dependence on irradiation temperature. Molecular dynamics simulations confirm a strong effect of precipitate sink strength on the probability of interstitial absorption at precipitates. [Display omitted] [ABSTRACT FROM AUTHOR]

This study characterizes the microstructural evolution of single-phase complex concentrated solid-solution alloy (CSA) compositions under heavy ion irradiation with the goal of evaluating mechanisms for CSA radiation tolerance in advanced fission systems. Three such alloys, Cr 18 Fe 27 Mn 27 Ni 28 , Cr 15 Fe 35 Mn 15 Ni 35 , and equimolar NbTaTiV, along with reference materials (pure Ni and E90 for the CrFeMnNi family and pure V for NbTaTiV) were irradiated at 50 K and 773 K with 1 MeV Kr++ ions to various levels of displacements per atom (dpa) using in-situ transmission electron microscopy. Cryogenic irradiation resulted in small defect clusters and faulted dislocation loops as large as 12 nm in face-centered cubic (FCC) CSAs. With thermal diffusion suppressed at cryogenic temperatures, defect densities were lower in all CSAs than in their less compositionally complex reference materials indicating that point defect production is reduced during the displacement cascade stage. High temperature irradiation of the two FCC CSA resulted in the formation of interstitial dislocation loops which by 2 dpa grew to an average size of 27 nm in Cr 18 Fe 27 Mn 27 Ni 28 and 10 nm in Cr 15 Fe 35 Mn 15 Ni 35. This difference in loop growth kinetics was attributed to the difference in Mn-content due to its effect on the nucleation rate by increasing vacancy mobility or reducing the stacking-fault energy. Image, graphical abstract [ABSTRACT FROM AUTHOR]

The objective of this study is to understand irradiation-induced and assisted defect evolution in binary body center cubic (bcc) Fe-based alloys. The broader class of bcc ferritic alloys are leading candidates for advanced nuclear fission and fusion applications, in part due to their exceptional void swelling resistance. However, their irradiated microstructure evolution is sensitive to solute species present, since these solutes can act as traps for irradiation-induced defects due to the surrounding tensile or compressive stress fields. Here, three alloys (Fe-9.5%Cr, Fe-4.5%P, and Fe-2.3%N) are selected for study because they systematically exhibit varying solute sizes and solute positions (i.e., substitutional or interstitial). Ex situ and in situ ion irradiations reveal that Fe-P has a considerably finer and denser population of irradiation-induced defects than Fe-Cr and Fe-N at the same irradiation conditions, which is attributed to strong defect trapping at undersized substitutional P, consequently hindering the development of extended defects. Meanwhile, oversized substitutional solutes (e.g., Cr) and interstitial solutes (e.g., N) may also suppress dislocation loop development due to weak solute-defect trapping. [ABSTRACT FROM AUTHOR]

Nanopatterned microstructures in materials can have a profound impact on materials' physical and chemical properties. While voids are typically considered as detrimental defects in irradiated materials, the patterning of nanoscale voids causes the formation of void superlattices and provides a highly efficient mechanism for gas storage. Despite the important applications of nanopatterned defect superlattices, how they degrade under irradiation remains unclear. Here we provide direct observation of the evolution of void superlattices under irradiation and elucidate the interaction of void superlattices with irradiation cascades. We reveal that the instability of void superlattices under irradiation is caused by heterogenous void shrinkage and demonstrate the imperative role of mixed 1D/3D diffusion of self-interstitial atoms and injected inert gas atoms on void shrinkage and void superlattice instability. Understanding the degradation mechanisms of nanopatterned microstructures is essential to designing damage-tolerant materials and broadening their applications in extreme environments. [Display omitted] [ABSTRACT FROM AUTHOR]

Single crystal CeO2, as a surrogate material to UO2, was irradiated with 500keV xenon ions at 800°C while being observed using in situ transmission electron microscopy (TEM). Experimental results show the formation and growth of defect clusters including dislocation loops and cavities as a function of increasing atomic displacement dose. At high dose, the dislocation loop structure evolves into an extended dislocation line structure, which appears to remain stable to the high dose levels examined in this study. A high concentration of cavities was also present in the microstructure. Despite high atomic displacement doses, the specimen remained crystalline to a cumulated dose of 5×1015 ions/cm2, which is consistent with the known stability of the fluorite structure under high dose irradiation. Kinetic Monte Carlo calculations show that oxygen mobility is substantially higher in hypo-stoichiometric UO2/CeO2 than hyper-stoichiometric systems. This result is consistent with the ability of irradiation damage to recover even at intermediate irradiation temperatures. [ABSTRACT FROM AUTHOR]

Refractory alloys consisting of reduced activity elements are attractive for nuclear applications to allow safe post-service recycling and meet fusion reactor requirements. Here, ion irradiation response was studied for a newly developed refractory high entropy alloy, HfTaTiVZr, with low activation constituent elements. Ion irradiation led to around 20% hardening for the high entropy alloy compared to 50% hardening for stainless steel under identical conditions. Superior irradiation resistance of the concentrated alloy was explained by the reduced mobility of point defects and self-healing ability. [ABSTRACT FROM AUTHOR]