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At least 73 records · Page 4

Response of GaN-Based Semiconductor Devices to Ion and Gamma Irradiation

GaN has electronic properties that make it an excellent material for the next generation of power electronics; however, its radiation hardening still needs further understanding before it is used in radiation environments. In this work we explored the response of commercial InGaN LEDs to two different radiation environments: ion and gamma irradiations. For ion irradiations we performed two types of irradiations at the Ion Beam Lab (IBL) at Sandia National Laboratories (SNL): high energy and end of range (EOR) irradiations. For gamma irradiations we fielded devices at the gamma irradiation facility (GIF) at SNL. The response of the LEDs to radiation was investigated by IV, light output and light output vs frequency measurements. We found that dose levels up to 500 krads do not degrade the electrical properties of the devices and that devices exposed to ion irradiations exhibit a linear and non- linear dependence with fluence for two different ranges of fluence levels. We also performed current injection annealing studies to explore the annealing properties of InGaN LEDs.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Structural Changes in YBa 2 Cu 3 O 7 Thin Films Modified with He + -Focused Ion Beam for High-Temperature Superconductive Nanoelectronics

Irradiation of high-temperature superconductor YBa 2 Cu 3 O 7 (YBCO) with high-energy He + ions is known to cause structural changes in the YBCO film, decreasing the critical temperature T C and finally leading to a superconductor-to-insulator transition. Here, this allows one to pattern narrow insulating regions with a focused ion beam (FIB) and thus fabricate nanoscale Josephson junctions on YBCO films. Moreover, such ion irradiation is known to cause structural changes in the YBCO film. However, details of how these structural changes occur in nanoscale devices produced by FIB remain unknown. Using nanofocus X-ray diffraction, we study the changes in the YBCO crystal lattice and investigate how the nature of these changes depends on the size of the irradiated regions. These data provide an important understanding of how oxide superconductors can be tailored at the nanometer scale for various applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Rethinking radiation effects in materials science using the plasma-focused ion beam

This work demonstrates the viability of using a plasma-focused ion beam (PFIB) as a new platform to carry out radiation effects studies in solids. While materials subjected to irradiation in either nuclear reactors or energetic particle accelerators experience limitations with respect to inaccuracies in both flux measurements and lack of precise control of irradiation areas, we demonstrate a new irradiation technique that allows the exposure of a single specimen in multiple areas, at multiple doses, and in site-specific dependencies - all with flux variations on the order of only 1%. This versatile technique also allows materials to be exposed to significantly higher irradiation dose rates than conventional accelerators. To validate the new methodology, we selected the classical example of ion-beam-induced amorphization of pure single-crystal Si. By pioneering the use of the PFIB for radiation effects studies in materials science, we were able to exploit, in both micro- and nanometer-sized detail, the differences in electron image contrast arising from crystalline versus amorphous solid-state phases in classical semiconductors subjected to irradiation, thus providing new insights on amorphization mechanisms. This methodology opens new research frontiers at the fringe of materials science with promising applications beyond the scope of materials at extremes such as in nanopatterning, nanodevices and nanoarchitectonics.

36 MATERIALS SCIENCE↗

Measurement and Simulation of Vacancy Formation in 2-MeV Self-irradiated Pure Fe

Positron annihilation spectroscopy is a powerful tool to quantify the amount of vacancies and vacancy clusters in materials. The technique has been utilized to study the induced defects in materials after ion beam and neutron irradiations. Here we make the case for how the technique can and should be utilized to quantify the defects created by irradiation in situ during irradiation to foster a more thorough understanding of the surviving defects after initial collision cascades. This paper outlines a future experimental approach and its meaning for the nuclear materials community, being able to benchmark commonly used rate theory models of damage evolution.

36 MATERIALS SCIENCE↗

Determining the Effects of Neutron Irradiation on the Structural Integrity of Additively Manufactured Heat Exchangers for Very Small Modular Reactor Applications, DOE Final Report (Project # 19-16980)

Auburn University (AU) teamed with the University of Missouri Research Reactor (MURR) and Kansas State University (KSU) to determine how to best use laser-powder bed fusion (L-PBF) additive manufacturing (AM) methods for generating radiation resistant nickel-based superalloys, Inconel alloy 625 and 718, for special purpose reactor (SPR) or very small modular reactor (vSMR) heat-exchangers (HeXs). Compact, conformal, and durable HeXs that are tolerant of extreme environments are needed for supporting the technical maturity of next-generation, portable compact reactors. AM is an enabler for realizing this new wave of HeXs – providing a means to make customizable hot and cold stream architectures with novel flow path geometries (e.g., tortuous channels with non-uniform, asymmetric cross-sections) and reduced layer-to-layer contact resistance (i.e., no separate bonding procedure required). AM further enables a more time/cost efficient means for fabricating SPRs by reducing the number of suppliers required for HeX assembly and allowing for on-site HeX fabrication. The project aim has been to better understand how neutron irradiation affects the microstructure and properties of additively manufactured nickel-based superalloys, to accelerate their safe, reliable use in the modular reactor industry. The major objective was to qualify/quantify the microstructure and microhardness of nickel-based superalloys (including Inconel 718 and 625) additively manufactured via the L-PBF process in the neutron-dosed (irradiated) and non-irradiated states over a course of 3 years. Effects of build orientation during L-PBF and post-AM heat treatments on neutron resistance, microstructure and mechanical properties were also investigated. Neutron damage mechanisms via hardening were characterized. This project combined subject-matter experts in AM, mechanical/microstructure metallic part characterization, and neutron irradiation, as well as unique assets and capabilities at AU and MURR at MU, to ensure project results translated to effectively addressing known gaps in nuclear science and engineering. Parts were fabricated using L-PBF systems readily available at AU. Specimens were then irradiated using MURR facilities; a manipulator equipped hot cell was also used to measure material hardness after dosing. MURR, a 10 MW, light-water nuclear reactor, is the largest, highest powered, highest-flux university owned research reactor in the U.S. The major findings in this project provide evidence that AM can serve as an alternative way to build structural components for future advanced small modular reactors using advanced materials like Inconel 625 (IN625) or Inconel 718 (IN718). After full spectrum neutron irradiation, vertically as-built AM IN625 samples were observed to display better resistance towards radiation-induced-hardening defects relative to traditionally machined metals. A Vickers microhardness tester, using settings of 1 kgf and dwell time of 15 seconds per indentation, was used to measure hardness in this study. The as-built, vertically printed samples experienced 1.2% of radiation hardening vs. 5.25% radiation hardening observed in wrought IN625. Another set of IN625 and IN718 samples were exposed to fast neutron irradiation. It was observed that IN718 showed more resistance towards radiation hardening compared to IN625 samples indicating IN718 had a better performance. Results showed that the IN718 samples experienced less change (-2.5 to 3.24 %) in microhardness. On the other hand, IN625 samples underwent more (0.9 to 7.21%) change in microhardness after fast neutron irradiation. AM IN625 samples were irradiated using an ion (proton) beam in cyclotron. The mechanical properties of AM samples post irradiation were compared with wrought samples. The irradiated region on the samples were tested using nano-hardness indention. It was observed that the beam current and time used in this study generated an annealing effect and thus reduced the hardness of the samples. The sum of the project results provide precious insight into how one may minimize radiation hardening in AM materials while maintaining material property constraints. Results should assist engineers in selecting an appropriate heat treatment for AM nickel-based superalloys for increased radiation resistance. Results should increase confidence levels for adopting AM for building nuclear reactor components which perform the same or better than conventionally manufactured components. Fast neutron irradiation testing provided an accelerated means of obtaining radiation effects without making materials radioactive and difficult to handle.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Experiments with a prototype titanium hot cavity surface ionization source intended for electromagnetic separation of radioactive samarium and other lanthanide elements

This paper reports experimental results of a prototype titanium surface ionization source. For the first time, a lanthanide ion beam has been produced with a surface ionizer composed completely of titanium metal. Titanium does not readily activate with neutron irradiation. This offers the potential for inserting an ion source made of titanium directly into a reactor with a pre-loaded non-radioactive lanthanide target. This seamlessly integrates target irradiation with isotope separation, eliminating post irradiation sample manipulation. Samarium ion beam currents up to 960 nA have been produced in an off-line test bench equipped with rudimentary beam optics. This is a crucial step toward the development of an ionization source adopted for the electromagnetic isotope separator (EMIS) facility, which has been designed for high throughput separations of radioactive 153 Sm and other lanthanides of interest in the field of nuclear medicine. The ion current and important factors affecting the performance of the ion source, such as the ionizer temperature and thermal gradient, are discussed. Lastly, the experimental results are presented together with a discussion of future modifications to optimize the overall surface ionization source performance.

07 ISOTOPE AND RADIATION SOURCES↗

Helium causing disappearance of a/2<111> dislocation loops in binary Fe-Cr ferritic alloys

In this work, single and dual-beam self-ion irradiations were performed at 500°C on ultra-high purity Fe14%Cr alloy to ~0.33 displacements-per-atom (dpa), and 0 or 3030 atomic-parts-per-million (appm) helium/dpa, respectively. Using transmission electron microscopy, we reveal that helium can drastically modify the dislocation loop Burgers vector in Fe-Cr alloys. Helium co-implantation caused complete disappearance of a/2<111> type dislocation loops, and the microstructure consisted of only a<100> loops. Conversely, a/2<111> type loops were predominant without He co-implantation. The total loop density remained largely unaffected. The results strikingly contrast literature asserting that helium stabilizes a/2<111> type loops in bcc Fe alloys, based on low temperature irradiations. Collectively analyzing the results with literature suggest that the small positive interaction between helium and self-interstitial atoms (SIA) in Fe predicted by atomistic simulations maybe insufficient to holistically explain the dislocation loop microstructure development in presence of helium. Helium-SIA positive binding inadvertently implies elevated a/2<111> loop fraction and higher loop densities that the present results contradict. Helium induced high cavity density causing a preferential loss of highly glissile <111> clusters, leaving the matrix saturated with <100> type clusters is proposed as a potential mechanism. Further, the in-situ irradiations combined with Burgers vector analysis strengthened the evidence of Cr-induced dislocation loop mobility reduction that appears to stabilize the a/2<111> type loops and causes higher loop densities in Fe-Cr alloys.

36 MATERIALS SCIENCE↗

Electronic and optical characterization of bulk single crystals of cubic boron nitride (cBN)

Cubic boron nitride (cBN) is a relatively less studied wide bandgap semiconductor despite its many promising mechanical, thermal, and electronic properties. We report on the electronic, structural, and optical characterization of commercial cBN crystal platelets. Temperature dependent transport measurements revealed the charge limited diode behavior of the cBN crystals. The equilibrium Fermi level was determined to be 0.47 eV below the conduction band, and the electron conduction was identified as n-type. Unirradiated dark and amber colored cBN crystals displayed broad photoluminescence emission peaks centered around different wavelengths. RC series zero phonon line defect emission peaks were observed at room temperature from the electron beam irradiated and oxygen ion implanted cBN crystals, making this material a promising candidate for high power microwave devices, next generation power electronics, and future quantum sensing applications.

36 MATERIALS SCIENCE↗

Nanomechanical testing of freestanding polymer films: in situ tensile testing and Tg measurement

Abstract A method for small-scale testing and imaging of freestanding, microtomed polymer films using a push-to-pull device is presented. Central to this method was the development of a sample preparation technique which utilized solvents at cryogenic temperatures to transfer and deposit delicate thin films onto the microfabricated push-to-pull devices. The preparation of focused ion beam (FIB)-milled tensile specimens enabled quantitative in situ TEM tensile testing, but artifacts associated with ion and electron beam irradiation motivated the development of a FIB-free specimen preparation method. The FIB-free method was enabled by the design and fabrication of oversized strain-locking push-to-pull devices. An adaptation for push-to-pull devices to be compatible with an instrumented nanoindenter expanded the testing capabilities to include in situ heating. These innovations provided quantitative mechanical testing, postmortem TEM imaging, and the ability to measure the glass transition temperature, via dynamic mechanical analysis, of freestanding polymer films. Results for each of these mentioned characterization methods are presented and discussed in terms of polymer nanomechanics. Graphic Abstract

36 MATERIALS SCIENCE↗

ToF-SIMS spectral analysis of pristine and neutron irradiated single crystal tungsten

Time-of-flight secondary ion mass spectrometry (ToF-SIMS) has many promising features in studying materials including high spatial resolution and high mass accuracy of elements, molecules, and isotopes. Its ability to resolve isotopes is especially attractive in studying transmutation products of single crystal tungsten (SCW) post neutron irradiation. Tungsten (W) is a contender of plasma facing materials (PFMs) due to its high thermal and radiological stability. PFMs to be used in the construction of fusion vessels are subject to high temperature and neutron irradiation, resulting in changes to materials including transmutation, which ultimately impact material mechanical and thermal properties. We used IONTOF TOF.SIMS V instrument equipped with a 30 keV Bi 3 + primary ion beam to study pristine SCW and irradiated SCW speciemens. Scanning electron microscope coupled with focused ion beam (SEM-FIB) was used to reduce the dosage of neutron irradiated tungsten and prepare for specimens for SIMS analysis. Static ToF-SIMS spectra were obtained, and transmutation product peak identification was presented in this work. Identified molecules and molecular fragments were compared against isotope theoretical mass to charge ratios of tungsten, rhenium, osmium, and other relevant products. Our results show that ToF-SIMS provides a viable means to study transmutation products of W post neutron irradiation. Such applications are suitable to investigate transmutation effects on materials that are being considered and developed for fusion pilot plants.

36 MATERIALS SCIENCE↗

Ytterbium Ion Collection on Graphite Plates

Surface characterization and analysis of the graphite collection and strike plates was conducted in this report. These plates were from an electromagnetic isotope separation collector that had been irradiated with an ytterbium ion beam. The results of this study are reported along with analysis and discussion of the potential growth mechanism of the ytterbium layer on graphite. It is proposed that directional deposition of ytterbium ions occurs first in the defect regions of the graphite plate. As deposition continues, it leads to the eventual formation of directional globs that elongate and grow into plates, then stacks, and finally into sheets of ytterbium. The ytterbium layer appears to have a definite phase boundary with the graphite layer. It was also determined that during irradiation with the ytterbium ion beam, the sputtered carbon becomes interpolated in the ytterbium surface layer on the graphite plate and has an amorphous microstructure.

36 MATERIALS SCIENCE↗

FLASH Dose Rate Helium Ion Beams: First In Vitro Investigations

To establish and investigate the effects of dose, linear energy transfer (LET), and O{sub 2} concentration on biologic response to ultrahigh dose rate (uHDR; FLASH) helium ion beams compared with standard dose rate (SDR) irradiation.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

Finite element analysis of the impact of beam heating mode in molten salt corrosion experiments employing simultaneous ion irradiation

Finite element analysis was used to investigate the temperature and stress profiles that develop in 316L stainless steel membranes being irradiated using different proton beam conditions in contact with a molten salt environment. It was shown that in addition to a nonuniform irradiation profile, a focused 2 MeV proton beam leads to very strong temperature and stress gradients in the membrane, introducing highly localized driving forces that complicate and even compromise the integrity and reliability of the experimental results of corrosion studies. Here, the use of a focused beam in corrosion studies can create experimental artifacts that may misrepresent the true corrosion behavior. In contrast, the use of a rastered beam is shown to distribute the protons and resulting radiation damage uniformly across the membrane face, and more importantly, results in temperature and stress profiles that are not only very uniform but are of much lower magnitude. The use of a rastered beam during molten salt corrosion experiments is therefore recommended to achieve uniform damage rates, thereby reducing both gradients and magnitudes of the temperature and stress distributions.

43 - PARTICLE ACCELERATORS↗

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↗

Actinide targets for the synthesis of superheavy nuclei

The use of heavy actinide targets, including 243 Am, 240,242,244 Pu, 245,248 Cm, 249 Bk, and 249 Cf, irradiated by intense heavy ion beams of 48 Ca has resulted in a significant expansion of the periodic table since 2000, including the discovery of five new heaviest elements and more than 50 new isotopes. These actinide materials can only be produced by intense neutron irradiation in very high flux reactors followed by chemical processing and purification in specialized hot cell facilities available in only a few locations worldwide. This paper reviews the reactor production of heavy actinides, the recovery and chemical separation of actinide materials, and the preparation of actinide targets for superheavy element experiments. The focus is on 248 Cm, 249 Bk, mixed 249–251 Cf, and 254 Es, including current availabilities and new production processes. The impacts of new facilities, including the Superheavy Element Factory at Dubna, accelerator and separator upgrades at RIKEN, and proposed upgrades to the High Flux Isotope Reactor at Oak Ridge are also described. Examples of recent superheavy element research are discussed as well as future opportunities for superheavy research using actinide targets.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Experimental and Computational Studies of Stress Corrosion Cracking of Alloys 308/309 and 82/182 Weldments in Corrosive and Radiation Environment

The goal of the project was to determine factors that influence SCC and IASCC in weldments found in LWR nuclear power plants. We focused on a SA508-304L SS weldment fabricated by EPRI using gas tungsten arc welding and used an aggressive BWR normal water chemistry (NWC) immersion environment. This weldment used 309L butter and 308L groove filler material. The microstructure of the 309L butter was non-uniform, exhibiting a 20–30μm thick martensitic layer closest to the SA508 interface, a 1–4 mm thick single γ austenite phase dilution zone, and a γ–δ duplex region extending to the 308L groove filler. The 308L groove filler had an entirely γ–δ duplex microstructure. Two approximately 1-inch thick 304L and SA508 plates approximately 12 by 6 square inches were joined using standard nuclear grade welding techniques. This included a post weld heat treatment of the 309L butter after application, a 0.32 cm fit-up root opening, and 57 bead lines of 308L groove filler applied in 18 layers. A 60 degree weld bevel angle was used and the 309L butter was 1.5 cm thick. Displacement cascade damage was induced using proton irradiation at the Michigan Ion Beam Laboratory. The incident proton energy was 2 MeV, the sample temperature was 360 ºC, and the calculated dpa value at 10 μm (60% of the Bragg peak depth of ~18 μm) was 5 dpa using the quick Kinchin-Pease model. Proton irradiation to this damage level required approximately 125 hours of beam time. Two types of samples were irradiated, tensile specimens and TEM bars. Samples were selected from all regions of the weldment, including the SA508-309L butter interface, the 309L-308L interface, and 308L-304L interface. The stainless steel alloys (304L, 308L, and 309L) within the heat affected zone are characterized by a duplex skeletal morphology of δ-ferrite and γ-austenite resulting from the recrystallization associated with weld fabrication. Approximately 7 to 8 mm of length along the specimen was irradiated. The gauge volume surfaces were mechanically polished and then electro-polished to remove mechanical damage from the mechanical polishing step prior to irradiation. Immersion tests were performed in a recirculating autoclave under BWR NWC conditions (2000 ppb wt. dissolved oxygen, neutral pH, 288 ºC, 10 MPa, and inlet water conductivity <100 nS/cm) to accelerate corrosion. Constant strain rate tests were performed either to failure or to approximately 5% strain. Strain rates of 10 -7 to 10 -6 mm/mm/s were used and typical immersion testing required four to six weeks to achieve failure or strains near 5%. Analysis primarily used advanced electron microscopy techniques of FIB lift out specimens.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Atom Probe characterization of neutron irradiated commercial ZIRLO® and AXIOM X2® alloys

As part of the Mechanistic Understanding of ZIrconium Corrosion (MUZIC) program, this team has been instrumental to obtain EPRI and Westinghouse sponsorships to prepare the neutron irradiated ZIRLO® and X2® from Vogtle nuclear power plant and ship them from Studsvik’s (Sweden) hot cells to Idaho National Laboratory (INL) to be part of the NSUF library. The uniqueness of these sets of neutron irradiated alloys is that they are at the same two extremes of the fuel cycles, allowing us to study the microchemistry evolution as a function of irradiation doses, exposure time and solute content. Advanced commercial Zirconium-Niobium (Zr-Nb) alloys, such as ZIRLO® and AXIOM®, have been developed by Westinghouse to enhance the corrosion resistance of fuel cladding material for longer service time. This study specifically aims at investigating the neutron irradiation induced Nb redistribution in AXIOM® X2® to understand the effect of neutron irradiation induced microchemistry changes and the irradiation enhanced corrosion resistance observed in ZrNb alloys. The detailed sample information on chemical composition and irradiation is given in shown in Table 1a and 1b respectively. To study the neutron IIP/nanoclusters and Nb concentration in the solid solution, atom probe tomography (APT) is the primary tool to obtain reliable chemical information. APT specimens were prepared in shielded focused ion beam (FIB) at the Irradiated Materials Characterization Laboratory (IMCL) at INL followed by APT analysis at CAES facility using LEAP 4000XR

36 MATERIALS SCIENCE↗