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At least 289 records · Page 16

Measurement bias in self-heating x-ray free electron laser experiments from diffraction studies of phase transformation in titanium

X-ray self-heating is a common by-product of X-ray Free Electron Laser (XFEL) techniques that can affect targets, optics, and other irradiated materials. Diagnosis of heating and induced changes in samples may be performed using the x-ray beam itself as a probe. However, the relationship between conditions created by and inferred from x-ray irradiation is unclear and may be highly dependent on the material system under consideration. Here, we report on a simple case study of a titanium foil irradiated, heated, and probed by a MHz XFEL pulse train at 18.1 keV delivered by the European XFEL using measured x-ray diffraction to determine temperature and finite element analysis to interpret the experimental data. We find a complex relationship between apparent temperatures and sample temperature distributions that must be accounted for to adequately interpret the data, including beam averaging effects, multivalued temperatures due to sample phase transitions, and jumps and gaps in the observable temperature near phase transformations. The results have implications for studies employing x-ray probing of systems with large temperature gradients, particularly where these gradients are produced by the beam itself. Finally, this study shows the potential complexity of studying nonlinear sample behavior, such as phase transformations, where biasing effects of temperature gradients can become paramount, precluding clear observation of true transformation conditions.

Crystallography↗

Dynamic Deformation in Nuclear Graphite and Underlying Mechanisms

Time-dependent deformation in nuclear graphite is influenced by the creation and migration of radiation-induced defects in the reactor environment. This study investigates the role of pre-existing defects such as point defect clusters and Mrozowski cracks in nuclear graphite IG-110. Separate specimens were irradiated with a 2.8 MeV Au 2+ beam with a fluence of 4.38 × 10 14 cm −2 and an 8 MeV C 2+ beam with a fluence of 1.24 × 10 16 cm −2 . Microscopic specimens were either mechanically loaded inside a transmission electron microscope (TEM) or subjected to ex situ indentation-based creep loading. In situ TEM tests showed significant plasticity in regions highly localized around the Mrozowski cracks, resembling slip or ripplocation bands. Slip bands were also seen near regions without pre-existing defects but at very high stresses. Ex situ self-ion irradiation embrittled the specimens and decreased the creep displacement and rate, while heavy ion irradiation resulted in the opposite behavior. We hypothesize that the large-sized gold ions (compared to the carbon atoms) induced interplanar swelling as well as cross-plane channels for increased defect mobility. These findings illustrate the role of pre-existing defects in the dynamic relaxation of stresses during irradiation and the need for more studies into the radiation environment’s impact on the mechanical response of nuclear graphite.

creep deformation↗

Nanoscale imaging of He-ion irradiation effects on amorphous TaO x toward electroforming-free neuromorphic functions

Resistive switching in thin films has been widely studied in a broad range of materials. Yet, the mechanisms behind electroresistive switching have been persistently difficult to decipher and control, in part due to their non-equilibrium nature. Here, we demonstrate new experimental approaches that can probe resistive switching phenomena, utilizing amorphous TaO x as a model material system. Specifically, we applied scanning microwave impedance microscopy and cathodoluminescence (CL) microscopy as direct probes of conductance and electronic structure, respectively. These methods provide direct evidence of the electronic state of TaO x despite its amorphous nature. For example, CL identifies characteristic impurity levels in TaO x , in agreement with first principles calculations. We applied these methods to investigate He-ion-beam irradiation as a path to activate conductivity of materials and enable electroforming-free control over resistive switching. However, we find that even though He-ions begin to modify the nature of bonds even at the lowest doses, the films' conductive properties exhibit remarkable stability with large displacement damage and they are driven to metallic states only at the limit of structural decomposition. Finally, we show that electroforming in a nanoscale junction can be carried out with a dissipated power of <20 nW, a much smaller value compared to earlier studies and one that minimizes irreversible structural modifications of the films. Importantly, the multimodal approach described here provides a new framework toward the theory/experiment guided design and optimization of electroresistive materials.

36 MATERIALS SCIENCE↗

Synergies between H, He and radiation damage in dual and triple ion irradiation of candidate fusion blanket materials

Three ferritic/martensitic alloys were studied to understand the synergistic effect between single ion beam (Fe 2+ ), dual ion beam (Fe 2+ +He 2+ and Fe 2+ +H + ), and triple ion beam (Fe 2+ +He 2+ +H + ) irradiations on cavity evolution. A commercial alloy, F82H, a castable nanostructured alloy, CNA3, and a high purity model alloy, Fe8Cr2W, were irradiated at 400°C to 600°C to a damage level of 50 dpa at a damage rate of 1 × 10 –3 dpa/s with He and H injection rates of 10 and 40 appm/dpa, respectively. Post-irradiation characterization via bright field transmission electron microscopy and high-angle annular dark-field scanning transmission electron microscopy was performed on all irradiated conditions to characterize the cavity size distribution and determine the effects of H/He injection on cavity microstructure. In all three alloys, hydrogen co-injection with helium resulted in an increased cavity number density and maximum cavity size, producing an increase in swelling over that from helium injection alone. Swelling in F82H appears to peak between 450°C and 500°C. At 600°C, swelling was minimal and cavities of high density and small size were confined to grain boundaries and dislocations while at 400°C, swelling is also low with a nearly homogeneous, high density, distribution of very small cavities throughout. Swelling was least in the commercial alloy F82H due to the high sink strength. The CNA3 alloy underwent dissolution of precipitates that lowered the sink strength and resulted in higher swelling than F82H, but less than the model alloy. Electron energy loss spectroscopy (EELS) elemental mapping revealed hydrogen forming a halo-like structure about the periphery of the cavities and helium residing within the cavities themselves. Finally, this observation suggests that hydrogen reduces the surface energy of helium-filled cavities which results in both increased cavity number density and cavity size in triple beam irradiation over dual beam irradiation.

36 MATERIALS SCIENCE↗

Tensile behavior of dual-phase titanium alloys under high-intensity proton beam exposure: radiation-induced omega phase transformation in Ti-6Al-4V

A high-intensity proton beam exposure with 181 MeV energy has been conducted at Brookhaven Linac Isotope Producer facility on various material specimens for accelerator targetry applications, including titanium alloys as a beam window material. The radiation damage level of the analyzed capsule was 0.25 dpa at the beam center region with an irradiation temperature around 120 oC. Tensile tests showed increased hardness and a large decrease in ductility for the dual a+ß-phase Ti-6Al-4V Grade-5 and Grade-23 extra low interstitial alloys, with the near a-phase Ti-3Al-2.5V Grade-9 alloy still exhibiting uniform elongation of a few % after irradiation. Transmission Electron Microscope analyses on Ti-6Al-4V indicated clear evidence of a high-density of defect clusters with size less than 2 nm in each a-phase grain. The ß-phase grains did not contain any visible defects such as loops or black dots, while the diffraction patterns clearly indicated ?-phase precipitation in an advanced formation stage. The radiation-induced ?-phase transformation in the ß-phase could lead to greater loss of ductility in Ti-6Al-4V alloys in comparison with Ti-3Al-2.5V alloy with less ß-phase.google scho

Tensile Test, titanium, acclerator, proton beam↗

Irradiation-enhanced Interactions at UO 2 /Al 2 O 3 /Al Interfaces

Combustion synthesis is used to prepare thin UO 2 films on aluminum alloy substrates. This simple preparation method involves electrospraying uranyl nitrate + acetylacetone + 2-methoxyethanol solution on the substrate, followed by a short annealing at 350 or 550 °C. The irradiation of films with a 40 Ar 2+ ion beam (energy of 1.7 MeV and fluences of 7.7 × 10 16 and 1.3 × 10 17 ions/cm 2 ) is conducted to investigate irradiation-induced restructuring processes. High-resolution transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS) investigations show that the annealing temperature significantly influences the crystallinity and stability of materials during irradiation. A small amount of Mg in the alloy substrate diffuses into the amorphous Al 2 O 3 interfacial layer between the film and the substrate. Local thermal spikes from the incoming ions facilitate the irradiation-induced mixing of immiscible Al 2 O 3 and UO 2 for the materials prepared at 350 °C. This mass diffusion produces relatively large cavities at the interface. Selective diffusion of a more significant amount of Mg for the materials prepared at 550 °C suppresses the mixing of the Al 2 O 3 interlayer with the film but forms Mg y U 1–y O 2±x solid solutions during irradiation. Local thermal heating triggers the precipitation of a discontinuous crystalline MgO layer close to the film surface. As a result, the enhanced and selective diffusion of Mg into the film makes the materials prepared at 550 °C more robust and mechanically stable than those prepared at 350 °C.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Thermomechanical response of thickly tamped targets and diamond anvil cells under pulsed hard x-ray irradiation

In the laboratory study of extreme conditions of temperature and density, the exposure of matter to high intensity radiation sources has been of central importance. Here, we interrogate the performance of multi-layered targets in experiments involving high intensity, hard x-ray irradiation, motivated by the advent of extremely high brightness hard x-ray sources, such as free electron lasers and 4th-generation synchrotron facilities. Intense hard x-ray beams can deliver significant energy in targets having thick x-ray transparent layers (tampers) around samples of interest for the study of novel states of matter and materials’ dynamics. Heated-state lifetimes in such targets can approach the microsecond level, regardless of radiation pulse duration, enabling the exploration of conditions of local thermal and thermodynamic equilibrium at extreme temperature in solid density matter. The thermal and mechanical responses of such thick layered targets following x-ray heating, including hydrodynamic relaxation and heat flow on picosecond to millisecond timescales, are modeled using radiation hydrocode simulation, finite element analysis, and thermodynamic calculations. Assessing the potential for target survival over one or more exposures and resistance to damage arising from heating and resulting mechanical stresses, this study doubles as an investigation into the performance of diamond anvil high pressure cells under high x-ray fluences. Long used in conjunction with synchrotron x-ray radiation and high power optical lasers, the strong confinement afforded by such cells suggests novel applications at emerging high intensity x-ray facilities and new routes to studying thermodynamic equilibrium states of warm, very dense matter.

Meza-Galvez, J. (ORCID:000000032699849X)↗

Multi-Scale Characterization of Porosity and Cracks in Silicon Carbide Cladding after Transient Reactor Test Facility Irradiation

Silicon carbide (SiC) ceramic matrix composite (CMC) cladding is currently being pursued as one of the leading candidates for accident-tolerant fuel (ATF) cladding for light water reactor applications. The morphology of fabrication defects, including the size and shape of voids, is one of the key challenges that impacts cladding performance and guarantees reactor safety. Therefore, quantification of defects’ size, location, distribution, and leak paths is critical to determining SiC CMC in-core performance. This research aims to provide quantitative insight into the defect’s distribution under multi-scale characterization at different length scales before and after different Transient Reactor Test Facility (TREAT) irradiation tests. A non-destructive multi-scale evaluation of irradiated SiC will help to assess critical microstructural defects from production and/or experimental testing to better understand and predict overall cladding performance. X-ray computed tomography (XCT), a non-destructive, data-rich characterization technique, is combined with lower length scale electronic microscopic characterization, which provides microscale morphology and structural characterization. This paper discusses a fully automatic workflow to detect and analyze SiC-SiC defects using image processing techniques on 3D X-ray images. Following the XCT data analysis, advanced characterizations from focused ion beam (FIB) and transmission electron microscopy (TEM) were conducted to verify the findings from the XCT data, especially quantitative results from local nano-scale TEM 3D tomography data, which were utilized to complement the 3D XCT results. In this work, three SiC samples (two irradiated and one unirradiated) provided by General Atomics are investigated. The irradiated samples were irradiated in a way that was expected to induce cracking, and indeed, the automated workflow developed in this work was able to successfully identify and characterize the defects formation in the irradiated samples while detecting no observed cracking in the unirradiated sample. These results demonstrate the value of automated XCT tools to better understand the damage and damage propagation in SiC-SiC structures for nuclear applications.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Electron spectroscopy analysis

The Surface Science Laboratories at the University of Alabama in Huntsville (UAH) are equipped with x-ray photoelectron spectroscopy (XPS or ESCA) and Auger electron spectroscopy (AES) facilities. These techniques provide information from the uppermost atomic layers of a sample, and are thus truly surface sensitive. XPS provides both elemental and chemical state information without restriction on the type of material that can be analyzed. The sample is placed into an ultra high vacuum (UHV) chamber and irradiated with x-rays which cause the ejection of photoelectrons from the sample surface. Since x-rays do not normally cause charging problems or beam damage, XPS is applicable to a wide range of samples including metals, polymers, catalysts, and fibers. AES uses a beam of high energy electrons as a surface probe. Following electronic rearrangements within excited atoms by this probe, Auger electrons characteristic of each element present are emitted from the sample. The main advantage of electron induced AES is that the electron beam can be focused down to a small diameter and localized analysis can be carried out. On the rastering of this beam synchronously with a video display using established scanning electron microscopy techniques, physical images and chemical distribution maps of the surface can be produced. Thus very small features, such as electronic circuit elements or corrosion pits in metals, can be investigated. Facilities are available on both XPS and AES instruments for depth-profiling of materials, using a beam of argon ions to sputter away consecutive layers of material to reveal sub-surface (and even semi-bulk) analyses.

Gregory, John C.↗

Light-Matter Interaction near the Schwinger Limit Using Tightly Focused Doppler-Boosted Lasers

Strong-field quantum electrodynamics (SF QED) is a burgeoning research topic dealing with electromagnetic fields comparable to the Schwinger field (≈1.32×10 18 V/m). While most past and proposed experiments rely on reaching this field in the rest frame of relativistic particles, the Schwinger limit could also be approached in the laboratory frame by focusing to its diffraction limit the light reflected by a plasma mirror irradiated by a multipetawatt laser. Here, we explore the interaction between such intense light and matter with particle-in-cell simulations. We find that the collision with a relativistic electron beam would enable the study of the nonperturbative regime of SF QED, while the interaction with a solid target leads to a profusion of SF QED effects that retroact on the interaction. In both cases, relativistic attosecond pair jets with high densities are formed.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

SEM analysis of ionizing radiation effects in linear integrated circuits

A successful diagnostic technique was developed using a scanning electron microscope (SEM) as a precision tool to determine ionization effects in integrated circuits. Previous SEM methods radiated the entire semiconductor chip or major areas. The large area exposure methods do not reveal the exact components which are sensitive to radiation. To locate these sensitive components a new method was developed, which consisted in successively irradiating selected components on the device chip with equal doses of electrons /10 to the 6th rad (Si)/, while the whole device was subjected to representative bias conditions. A suitable device parameter was measured in situ after each successive irradiation with the beam off.

Stanley, A. G.↗

MX precipitate behavior in an irradiated advanced Fe-9Cr steel: Helium sequestration and cavity swelling performance

This work is the third and final part in an initial series on addressing the behavior of MX precipitate stability in an advanced Fe-9Cr reduced activation ferritic/martensitic (RAFM) alloy under fusion-relevant ion irradiation conditions. Here, the helium trapping properties of MX precipitates are investigated across varying damage levels (15–100 dpa), temperatures (400–600 °C), and helium doses (10–25 appm He/dpa) using sophisticated dual ion beam experiments and electron microscopy. Results indicate that individual MX precipitates efficiently sequester helium in the form of nanoscale bubbles at the precipitate-matrix interfaces near the peak swelling temperature (∼5 bubbles/precipitate at 500 °C). Swelling was primarily due to matrix cavities. The Fe-9Cr alloy reached 2% swelling by 100 dpa, suggesting a shift to steady-state swelling around 50 dpa at 500 °C. Furthermore, MX precipitate dissolution beginning at 15 dpa did not coincide with this onset of steady-state swelling.

Dual ion irradiation↗

Modulating Oxide‐Based Quantum Materials by Ion Implantation

Ion implantation has emerged as a powerful tool for manipulating and investigating oxide quantum materials, where strong electron correlations give rise to exotic phases and functionalities. This Review examines how controlled ion bombardment enables targeted modulation of structural, electronic, and magnetic properties in complex oxides. Recent advances in ion beam techniques is analyzed that provide unprecedented control over defect profiles, from point defects to extended damage cascades. In application, ion irradiation has demonstrated the ability to tune quantum phenomena including metal‐insulator transitions, magnetism, and superconductivity through selective doping, defect creation, and lattice strain. The ability to write quantum states with nanoscale precision using focused ion beams is opening new paths for quantum device fabrication. Challenges in understanding radiation damage mechanisms in strongly correlated systems is discussed, and identify opportunities for designing quantum functionality through defect‐engineering approaches. The technique's demonstrated capability to write quantum states with nanoscale precision, combined with its compatibility with existing semiconductor processing infrastructure, suggests a clear pathway for translating fundamental discoveries in quantum materials into practical technological applications.

defect engineering↗

Laboratory Astrophysics Using a Microcalorimeter and Bragg Crystal Spectrometer on an Electron Beam Ion Trap

We completed modifications to the new microcalorimeter system dedicated for use on the EBIT at NIST, which included: 1) a redesign of the x-ray calibration source from a direct electron impact source to one that irradiates the microcalorimeter with fluorescent x-rays. The resulting calibration lines are free of bremsstrahlung background; 2) the microcalorimeter electronic circuit was significantly improved to ensure long-term stability for lengthy experimental runs

Brinton, John↗

Behavior and properties of helium cavities in ductile-phase-toughened tungsten irradiated with He + ions at an elevated temperature

Ductile-phase toughened tungsten (DPT W) composites have demonstrated a great potential for plasma-facing components in fusion power systems. These materials can retain the outstanding thermomechanical properties of W while significantly enhancing the fracture toughness. The DPT W composite in this study consists of W particles (88 wt.%) embedded in a ductile NiFeW (12 wt.%) solution matrix. Irradiation of the composite was performed with 90 keV He + ions to 1.0 × 10 17 He + /cm 2 at 973 K. The He cavities formed in both W and NiFeW phases are examined using convergent-beam scanning transmission electron microscopy (CB-STEM) at an atomic-level resolution. Full-range depth profiles of the He cavity diameters and number densities are analyzed. The results show that the average cavity diameter in NiFeW is ~2.7 times that in W, while the number density is an order of magnitude lower. A quantitative analysis of the He density and pressure in the cavities is also achieved using STEM electron energy loss spectroscopy (STEM-EELS) mapping. The He atoms in the cavities in NiFeW are found to be under-pressurized, while those in similar-sized cavities in W are not detectable. Further, the He energy-loss shift exhibits a linear relationship with the He density in cavities in NiFeW, with the slope comparable to that for martensitic steel.

36 MATERIALS SCIENCE↗

Layer dissolution in accumulative roll bonded bulk Zr/Nb multilayers under heavy-ion irradiation

In this work, the heavy-ion irradiation behavior of bulk zirconium-niobium multilayered composites was investigated up to large doses. Multilayers with an average individual layer thicknesses ranging between 15 and 80 nm were synthesized by accumulative roll bonding technique. The irradiation was performed with a defocused 7 MeV Zr 2+ ion beam at 500 °C. The maximum dose achieved was ~145 dpa at the depth of ~1.5 μm from the irradiated surface. Sub-surface microstructural damage and the chemical redistribution were characterized by transmission electron microscopy and energy dispersive spectroscopy, respectively. Irrespective of the layer thicknesses, the irradiation condition caused layer instability and the extent of damage varied with the dose levels. Doses lesser than ~60 dpa caused layer fragmentation and greater than ~60 dpa resulted in layer dissolution. The chemical mixing of layers occur to a depth of ~1 μm, consuming multiple bi-layer periods. Despite the elevated irradiation temperature (500 °C) and a slightly positive heat of mixing (+6 kJ/mol), no phase separation was observed and single-phase was retained in the mixed region. The results demonstrate that chemical mixing was facilitated by the liquid phase miscibility of Zr and Nb, which propelled the interdiffusion within the thermal spikes towards mixing.

36 MATERIALS SCIENCE↗

Science on the Space Shuttle

On the Space Shuttle's third flight, scientific instruments will study the electromagnetic environment with charging and electron beams. Beam plasma discharge will be studied. The plasma diagnostics package contains electromagnetic and particle sensors to study the ionosphere. An attempt will be made to establish a more accurate base of solar UV irradiance measurements with an absolute error of 10 percent or less over the wavelength region 120-400 nm. The solar flare X-ray polarimeter will observe flare X-rays emitted between 5 and 30 keV and measure their polarization as a function of time and photon energy. A photopolarimeter will help study zodiacal light, and interplanetary dust will be sampled by a section of thick aluminum foil. Plant seedlings will be grown to research the effect of near-zero gravity on lignification. A thermal canister experiment will help determine whether instruments can be maintained at a fixed temperature under varying thermal loads.

Neupert, W. M.↗

Evaluation of the minority carrier diffusion length and surface-recombination velocity in GaAs p/n solar cells

The minority carrier diffusion length (Lp) and the surface recombination velocity (Vs) were measured as a function of distance (x) from the p-n junction in GaAs p/n concentrator solar cells. The measured Vs values were used in a theoretical expression for the normalized electron-beam-induced current. A fitting procedure was then used to fit this expression with experimental values to obtain Lp. The results show that both Vs and Lp vary with x. Lp measured in irradiated cells showed a marked reduction. These values were compared to those measured previously which did not account for Vs.

Hakimzadeh, Roshanak↗