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Nanoparticle Precipitation in Irradiated and Annealed Ceria Doped with Metals for Emulation of Spent Fuels
Epsilon alloy precipitates have been observed with varied compositions and sizes in spent nuclear fuels, such as UO2. Presence of the inclusions, along with other oxide precipitates, gas bubbles and irradiation-induced structural defects, can significantly degrade the physical properties of the fuel. To predict fuel performance, a fundamental study of the precipitation processes is needed. This study uses ceria (CeO2) as a surrogate for UO2. Polycrystalline CeO2 films doped with Mo, Ru, Rh, Pd and Re (surrogate for Tc) were grown at 823 K using pulsed laser deposition, irradiated at 673 K with He+ ions, and subsequently annealed at higher temperatures. A number of methods, including transmission electron microscopy and atom probe tomography, were applied to characterize the samples. The results indicate that there is a uniform distribution of the doped metals in the as-grown CeO2 film. Pd particles of ~3 nm in size appear near dislocation edges after He+ ion irradiation to ~13 dpa. Thermal annealing at 1073 K in air leads to formation of precipitates with Mo and Pd around grain boundaries. Further annealing at 1373 K produces 70 nm sized precipitates with small grains at cavities.
Through-Thickness Vertically Ordered Lamellar Block Copolymer Thin Films on Unmodified Quartz with Cold Zone Annealing
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The nontrivial effects of annealing on superconducting properties of Nb single crystals
The effect of annealing on the superconducting properties of niobium single crystals was studied using optical, magnetic, and scanning tunneling microscopy (STM) methods. Pieces of the same crystal boule were studied before and after the annealing at 800 ${^\circ}\textrm{C}$, 1400 ${^\circ}\textrm{C}$, and near the melting point of niobium (2477 ${^\circ}\textrm{C}$). The initial samples had a high hydrogen content and low-temperature imaging revealed large hydrides (hundreds of micrometers) appearing below 190 K. The formation of these large precipitates is already completely suppressed by annealing at 800 ${^\circ}\textrm{C}$. However, the overall superconducting properties of the annealed samples did not improve and, in fact, worsened. In particular, the superconducting transition temperature decreased, the upper critical field increased, and the pinning strength increased. In the STM study, the sample was annealed initially at 400 ${^\circ}\textrm{C}$, measured, annealed at 1700 ${^\circ}\textrm{C}$, and measured again. The STM revealed a ‘dirty’ superconducting gap with a significant spatial variation in tunneling conductance after annealing at 400 ${^\circ}\textrm{C}$. The clean gap was recovered after annealing at 1700 ${^\circ}\textrm{C}$. This is likely due to oxygen redistribution near the surface, which is always covered by oxide layers in as-grown crystals. Our results indicate that vacuum annealing at least up to 1400 ${^\circ}\textrm{C}$, while removing a large percentage of hydrogen, introduces additional nanosized defects, likely hydride precipitates, that act as efficient pair-breaking and pinning centers. The dimensionless scattering rate is estimated to have increased from $\Gamma = 0.2$ to about $\Gamma = 0.4$ after annealing at 1400 ${^\circ}\textrm{C}$. These results on single crystals differ drastically from those obtained in polycrystalline bulk niobium (i.e. cut from superconducting radio-frequency cavities), where annealing is known to have a significant positive effect that is attributed to the improvement of the crystalline structure masking the more subtle influence of the hydrides.
Isochronal annealing effects on local structure, crystalline fraction, and undamaged region size of radiation damage in Ga-stabilized δ-Pu
The effects on the local structure due to self-irradiation damage of Ga stabilized δ-Pu stored at cryogenic temperatures have been examined using extended x-ray absorption fine structure (EXAFS) experiments. Extensive damage, seen as a loss of local order, was evident after 72 days of storage below 15 K. The effect was observed from both the Pu and the Ga sites, although less pronounced around Ga. Isochronal annealing was performed on this sample to study the annealing processes that occur between cryogenic and room temperature storage conditions, where damage is mostly reversed. Damage fractions at various points along the annealing curve have been determined using an amplitude-ratio method, a standard EXAFS fitting, and a spherical crystallite model, and provide information complementary to the previous electrical resistivity- and susceptibility-based isochronal annealing studies. The use of a spherical crystallite model accounts for the changes in EXAFS spectra using just two parameters, namely, the crystalline fraction and the particle radius. Together, these results are discussed in terms of changes to the local structure around Ga and Pu throughout the annealing process and highlight the unusual role of Ga in the behavior of the lowest temperature anneals.
Effects of annealing parameters on microstructural evolution of a typical nickel-based superalloy during annealing treatment
Highlights: • Adopting an annealing treatment after deformation can improve the homogeneity of microstructure. • Heterogeneous grains become homogeneous firstly, and then heterogeneous with increasing annealing time. • The optimum annealing parameters are the temperature of 980 °C and the time of 10 min. - Abstract: It is usually one of important goals to obtain the homogeneous microstructure for forgings by hot working, such as hot die forging. However, there is always a large inhomogeneous deformation in die forgings during hot deformation. It often results in an inhomogeneous microstructure of forging due to the different dynamic recrystallization (DRX) fractions and grain sizes in different strain regions. In this study, a method was proposed to improve the homogeneity of deformed microstructure by annealing treatment. The microstructural evolution of a typical nickel-based superalloy during annealing treatment has been investigated. The Optical Microscope (OM), Electron Backscatter Diffraction (EBSD) and Scanning Electron Microscope (SEM) technologies were applied to observe microstructures. It is found that adopting an annealing treatment after deformation can effectively improve the homogeneity of microstructure due to the static recrystallization. There is an incubation period which is not less than 5 min for the occurrence of static recrystallization. The initial heterogeneous grains become homogeneous firstly, and then heterogeneous again when the annealing time is increased from 5 to 30 min. The deformation accelerates the dissolution of delta phase in annealing treatment. The fraction of delta phase decreases at the early stage of annealing whether the temperature exceeds the solution temperature. Based on a comprehensive consideration of all factors, the optimum annealing parameters, which are the temperature of 980 °C and the time of 10 min, have been obtained.
The Effect of Dopant Concentration and Annealing Treatments on N-Type Iodine Doped CdTe
We report properties of highly conducting n-type cadmium telluride single crystals doped with iodine (CdTe:I). These crystals were grown with dopant concentrations in the range of 10^17 cm-3 to 10^19 cm-3 by Modified Vertical Bridgman (MVB) melt growth. Post-growth dopant activation, including Cd annealing, Te annealing, and rapid thermal annealing (RTA), was applied to improve free carrier density. The structural, optical, and electrical properties were analyzed by Glow Discharge Mass Spectroscopy (GDMS), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), Photoluminescence Spectroscopy (PL), optical absorption, Hall measurements, Capacitance-Voltage (CV) measurements, and time-resolved photoluminescence (TRPL). The results indicate that Cd annealing is the most effective activation method to get 100% donor activation (n is approximately 2 x 10^18 cm-3), which is close to the room temperature solubility limit of iodine. This leads to the lowest resistivity and the highest mobility. Moreover, this data suggests a potential role of Cd vacancy-related defects on electrical self-compensation.
Near infrared laser annealing of CdTe and in-situ measurement of the evolution of structural and optical properties
The high performance of polycrystalline CdTe thin film solar cells is enabled by annealing in the presence of Cl. This process is typically carried out for tens of minutes resulting in reduction of defect states within the bandgap among other beneficial effects. In this work, we investigate laser annealing as a means of rapidly annealing CdTe using a continuous wave sub-bandgap 1064 nm laser. The partial transmission of the beam allows us to monitor the annealing process in-situ and in real time. We find that optoelectronic and structural changes occur through two distinct kinetic processes resulting in the removal of deep defects and twinned regions, respectively. A multilayer optical model including surface roughness is used to interpret both the in-situ transmission as well as ex-situ reflectivity measurements. These experiments demonstrate beneficial material changes resulting from sub-bandgap laser-driven CdCl{sub 2} treatment of CdTe in minutes, which is an important step towards accelerating the processing of the CdTe absorber layer.
Influence of annealing on the photodeposition of silver on periodically poled lithium niobate
The preferential deposition of metal nanoparticles onto periodically poled lithium niobate surfaces, whereby photogenerated electrons accumulate in accordance with local electric fields and reduce metal ions from solution, is known to depend on the intensity and wavelength of the illumination and the concentration of the solution used. Here, it is shown that for identical deposition conditions (wavelength, intensity, concentration), post-poling annealing for 10 h at 200 °C modifies the surface reactivity through the reorientation of internal defect fields. Whereas silver nanoparticles deposit preferentially on the +z domains on unannealed crystals, the deposition occurs preferentially along 180° domain walls for annealed crystals. In neither case is the deposition selective; limited deposition occurs also on the unannealed –z domain surface and on both annealed domain surfaces. The observed behavior is attributed to a relaxation of the poling-induced defect frustration mediated by Li{sup +} ion mobility during annealing, which affects the accumulation of electrons, thereby changing the surface reactivity. The evolution of the defect field with temperature is corroborated using Raman spectroscopy.
The role of Frenkel defect diffusion in dynamic annealing in ion-irradiated Si
The formation of stable radiation damage in crystalline solids often proceeds via complex dynamic annealing processes, involving migration and interaction of ballistically-generated point defects. The dominant dynamic annealing processes, however, remain unknown even for crystalline Si. Here, we use a pulsed ion beam method to study defect dynamics in Si bombarded in the temperature range from -20 to 140 °C with 500 keV Ar ions. Results reveal a defect relaxation time constant of ~10–0.2 ms, which decreases monotonically with increasing temperature. The dynamic annealing rate shows an Arrhenius dependence with two well-defined activation energies of 73 ± 5 meV and 420 ± 10 meV, below and above 60 °C, respectively. Rate theory modeling, bench-marked against this data, suggests a crucial role of both vacancy and interstitial diffusion, with the dynamic annealing rate limited by the migration and interaction of vacancies.
Structural changes and self-activated photoluminescence in reductively annealed Sr{sub 3}AlO{sub 4}F
White light emission of self-activated photoluminescence (PL) in Sr{sub 3}AlO{sub 4}F under 254 nm light is only observed after annealing in a reducing atmosphere of 5%H{sub 2}/95%Ar. High-resolution neutron powder diffraction reveals that the FSr{sub 6} octahedrons and AlO{sub 4} tetrahedrons in this anti-perovskite structure are closer packed in reduced than in air-annealed samples which show no PL. Careful analysis of temperature-dependent neutron powder diffraction data establishes smaller isotropic displacement parameters for Sr(1) and O in Sr{sub 3}AlO{sub 4}F annealed in a reducing atmosphere indicating that the denser packing of the polyhedral sub-units leads to a slightly deeper potential for the Sr(1) and O atoms. Both the air- and reductively-annealed samples have identical thermal expansion within the temperature range between 3 and 350 K. The Debye temperatures were calculated using the atomic displacement parameters and show no significant differences between the air and reductively annealed samples making the Debye temperature a bad proxy for self-activated PL. - Graphical abstract: Annealing Sr{sub 3}AlO{sub 4}F under reducing conditions results in an intense self-activated photoluminescence which is correlated with a denser packing of FSr{sub 6} and AlO{sub 4} polyhedra. - Highlights: • Sr{sub 3}AlO{sub 4}F made in air does not show self-activated photoluminescence. • Only when annealing Sr{sub 3}AlO{sub 4}F in a reducing gas is photoluminescence observed. • FSr{sub 6} and AlO{sub 4} polyhedra in reduced Sr{sub 3}AlO{sub 4}F structure are packed more efficient. • Smaller displacement parameters are found for under-bonded Sr(1) and O sites.
In situ TEM and synchrotron characterization of U–10Mo thin specimen annealed at the fast reactor temperature regime
U–Mo metallic alloys have been extensively used for the Reduced Enrichment for Research and Test Reactors (RERTR) program, which is now known as the Office of Material Management and Minimization under the Conversion Program. This fuel form has also recently been proposed as fast reactor metallic fuels in the recent DOE Ultra-high Burnup Fast Reactor project. In order to better understand the behavior of U–10Mo fuels within the fast reactor temperature regime, a series of annealing and characterization experiments have been performed. Annealing experiments were performed in situ at the Intermediate Voltage Electron Microscope (IVEM-Tandem) facility at Argonne National Laboratory (ANL). An electro-polished U–10Mo alloy fuel specimen was annealed in situ up to 700 °C. At an elevated temperature of about 540 °C, the U–10Mo specimen underwent a relatively slow microstructure transition. Nano-sized grains were observed to emerge near the surface. At the end temperature of 700 °C, the near-surface microstructure had evolved to a nano-crystalline state. In order to clarify the nature of the observed microstructure, Laue diffraction and powder diffraction experiments were carried out at beam line 34-ID of the Advanced Photon Source (APS) at ANL. Phases present in the as-annealed specimen were identified with both Laue diffraction and powder diffraction techniques. The U–10Mo was found to recrystallize due to thermally-induced recrystallization driven by a high density of pre-existing dislocations. A separate in situ annealing experiment was carried out with a Focused Ion Beam processed (FIB) specimen. A similar microstructure transition occurred at a lower temperature of about 460 °C with a much faster transition rate compared to the electro-polished specimen. - Highlights: • TEM annealing experiments were performed in situ at the IVEM facility up to fast reactor temperature. • At 540 °C, the U-10Mo specimen underwent a slow microstructure transition where nano-sized grains were observed to emerge. • UO{sub 2} phase exists at the thin area of the as-annealed specimen whereas U-10Mo γ phase dominated at the thicker part. • Bcc γ U-10Mo recrystallized to become nano-meter sized crystallites near the specimen surface. • A separateannealing experiment was conducted with a FIB processed specimen where similar transition occurred at a lower temperature of 460 °C with a faster rate.
Shock, Post-Shock Annealing, and Post-Annealing Shock in Ureilites
The thermal and shock histories of ureilites can be divided into four periods: 1) formation, 2) initial shock, 3) post-shock annealing, and 4) post-annealing shock. Period 1 occurred approx.4.55 Ga ago when ureilites formed by melting chondritic material. Impact events during period 2 caused silicate darkening, undulose to mosaic extinction in olivines, and the formation of diamond, lonsdaleite, and chaoite from indigenous carbonaceous material. Alkali-rich fine-grained silicates may have been introduced by impact injection into ureilites during this period. About 57% of the ureilites were unchanged after period 2. During period 3 events, impact-induced annealing caused previously mosaicized olivine grains to become aggregates of small unstrained crystals. Some ureilites experienced reduction as FeO at the edges of olivine grains reacted with C from the matrix. Annealing may also be responsible for coarsening of graphite in a few ureilites, forming euhedral-appearing, idioblastic crystals. Orthopyroxene in Meteorite Hills (MET) 78008 may have formed from pigeonite by annealing during this period. The Rb-Sr internal isochron age of approx.4.0 Ga for MET 78008 probably dates the annealing event. At this late date, impacts are the only viable heat source. About 36% of ureilites experienced period 3 events, but remained unchanged afterwards. During period 4, approx.7% of the ureilites were shocked again, as is evident in the polymict breccia, Elephant Moraine (EET) 83309. This rock contains annealed mosaicized olivine aggregates composed of small individual olivine crystals that exhibit undulose extinction. Ureilites may have formed by impact-melting chondritic material on a primitive body with heterogeneous O isotopes. Plagioclase was preferentially lost from the system due to its low impedance to shock compression. Brief melting and rapid burial minimized the escape of planetary-type noble gases from the ureilitic melts. Incomplete separation of metal from silicates during impact melting left ureilites with relatively high concentrations of trace siderophile elements.
Tribology and sliding electrical contact resistance of e-beam hard Au: Effects of annealing
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p-type conductivity and damage recovery in implanted GaN annealed by rapid gyrotron microwave annealing
We demonstrate p-type activation of GaN doped by Mg ion implantation, and in situ during metalorganic chemical vapor deposition through sequential short-duration gyrotron microwave heating cycles at temperatures of 1200–1350 °C. GaN is implanted with 1019 cm−3 Mg ions, capped with AlN, and annealed under 3 MPa N2 overpressure in 5 s heating cycles for less than 60 s total using a high-power gyrotron microwave heating source. Through I–V characterization, photoluminescence spectroscopy, and Raman spectroscopy, we study the evolution of electrical properties, optically active point defects, and material strain in response to implantation and annealing. For Mg-implanted samples, increasing annealing temperature is characterized by an increase in the PL substitutional Mg-related peak (UVL) relative to the shallow-donor vacancy-related peak (GL2). Through comparison of implanted and in situ doped samples, it is demonstrated that the origin of compensating VN lies primarily in implantation rather than degradation from the annealing process. Transmission line measurements and diode I–V measurements show a sheet resistance of 1083 kΩ/□ and a hole concentration of 1.23 × 1015 cm−3, respectively, in the Mg-implanted material annealed at 1350 °C. We conclude that temperature-cycled gyrotron annealing at 1350 °C decreases implant-induced compensating point defects and activates Mg to obtain selective p-type conduction.
The effects of post-growth annealing on the structural and magnetic properties of BaFe 2 As 2
Here, we investigate the effects of post-growth annealing on the structural and magnetic properties of BaFe 2 As 2 . Magnetic susceptibility measurements, which exhibit a signal corresponding to the magnetic phase transition, and high-resolution x-ray diffraction measurements, which directly probe the structural order parameter, show that annealing causes the ordering temperatures of both the phase transitions to increase, sharpen and converge. In the as grown sample, our measurements show two distinct transitions corresponding to structural and magnetic ordering, which are separated in temperature by approximately 1 K. After 46 days (d) of annealing at 700 °C, the two become concurrent in temperature. These measurements demonstrate that the structural phase transition is second-order like when the magnetic and structural phase transitions are separated in temperature, and first-order like when the two phase transition temperatures coincide. This observation indicates that annealing causes the system to cross a hitherto undiscovered tricritical point. In addition, x-ray diffraction measurements show that the c-axis lattice parameter increases with annealing up to 30 d, but remains constant for longer annealing times. Comparisons of BaFe 2 As 2 to SrFe 2 As 2 are made when possible.
IPL-Annealed Mixed-Cation Perovskites with Robust Coating Window toward Scalable Manufacturing of Commercial Perovskite Solar Cells
Perovskite solar cells (PSCs) are a promising alternative solar technology, but the technical challenges of (1) stability/durability, (2) efficiency at scale, and (3) manufacturability must be overcome to achieve widespread PSC commercialization. The challenge of balancing solution ink formulation and scalable manufacturing is often overlooked in the literature, where focus is on adopting inks from processes that will not scale. In this study, we apply a classical roll-to-roll manufacturing perspective, utilizing both compositional engineering and intense pulsed light (IPL) annealing, to develop a mixed-cation perovskite ink with a robust coating window that simultaneously solve issues of stability and manufacturability for PSCs. Our method resulted in blade-coated, flexible, mixed-cation PSCs on ITO-PET substrates with a champion power conversion efficiency (PCE) efficiency of 16.7% using IPL annealing of the absorber layer and, to our knowledge, is one of the fastest processing methods for the perovskite layer. This overall reduction in processing time with a stable ink represents an advance toward the scaled production of perovskite solar cells on flexible substrates.
Displacement cascades and defect annealing in tungsten, Part II: Object kinetic Monte Carlo simulation of tungsten cascade aging
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