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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2014

Microstructure of multistage annealed nanocrystalline SmCo 2 Fe 2 B alloy with enhanced magnetic properties

The microstructure and chemistry of SmCo 2 Fe 2 B melt-spun alloy after multistage annealing was investigated using high resolution transmission electron microscopy (HRTEM) and 3D atom probe tomography. The multistage annealing resulted in an increase in both the coercivity and magnetization. The presence of Sm(Co,Fe) 4 B (1:4:1) and Sm 2 (Co,Fe) 17 B x (2:17:x) magnetic phases were confirmed using both techniques. Fe 2 B at a scale of -5 nm was found by HRTEM precipitating within the 1:4:1 phase after the second-stage annealing. Ordering within the 2:17:x phase was directly identified both by the presence of antiphase boundaries observed by TEM and the interconnected isocomposition surface network found in 3D atom probe results in addition to radial distribution function analysis. The variations in the local chemistry after the secondary annealing were considered pivotal in improving the magnetic properties.

Environmental Molecular Sciences Laboratory↗
DOE OSTI2013

Improved zircon fission-track annealing model based on reevaluation of annealing data

The thermal recovery (annealing) of mineral structure modified by the passage of fission fragments has long been studied by the etching technique. In minerals like apatite and zircon, the annealing kinetics are fairly well constrained from the hour to the million-year timescale and have been described by empirical and semi-empirical equations. On the other hand, laboratory experiments, in which ion beams interact with minerals and synthetic ceramics, have shown that there is a threshold temperature beyond which thermal recovery impedes ion-induced amorphization. In this work, it is assumed that this behavior can be extended to the annealing of fission tracks in minerals. It is proposed that there is a threshold temperature, T0, beyond which fission tracks are erased within a time t0, which is independent of the current state of lattice deformation. This implies that iso-annealing curves should converge to a fanning point in the Arrhenius pseudo-space (ln t vs. 1/T). Based on the proposed hypothesis, and laboratory and geological data, annealing equations are reevaluated. The geological timescale estimations of a model arising from this study are discussed through the calculation of partial annealing zone and closure temperature, and comparison with geological sample constraints found in literature. It is shown that the predictions given by this model are closer to field data on closure temperature and partial annealing zone than predictions given by previous models.

annealing↗
DOE OSTI2017

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.

Jiang, Weilin↗
DOE OSTI2024

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.

43 PARTICLE ACCELERATORS↗
DOE OSTI2011

Local Resistance Profiling of Ultra Shallow Junction Annealed with Combination of Spike Lamp and Laser Annealing Processes using Scanning Spreading Resistance Microscope

Local resistance profiles of ultra shallow boron and arsenic implanted into silicon with energies of 2.0 and 4.0 keV and doses of 2.0x10{sup 15} and 1.0x10{sup 15} ions/cm{sup 2} activated by a combination of conventional spike lamp and laser annealing processes were measured by scanning spreading resistance microscope (SSRM) with a depth resolution of less than 10 nm. The lowest local resistance at the low resistance region in 2.0 keV boron implanted silicon with 1050 deg. C spike lamp annealing followed by 0.35 kW/mm{sup 2} laser annealing was half of that without laser annealing. The lowest local resistance at the low resistance region in the arsenic implanted silicon activated by 1050 deg. C spike lamp annealing followed by 0.39 kW/mm{sup 2} laser annealing was 74% lower than that followed by 0.36 kW/mm{sup 2} laser annealing. The lowest local resistances at the low resistance regions in the arsenic implanted silicon with 0.36 and 0.39 kW/mm{sup 2} laser annealing followed by 1050 deg. C spike lamp annealing were 41 and 33% lower than those with spike lamp annealing followed by laser annealing. Laser annealing followed by spike lamp annealing could suppress the diffusion of the impurities and was suitable for making the ultra shallow and low resistance regions.

36 MATERIALS SCIENCE↗
DOE OSTI2016

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.

36 MATERIALS SCIENCE↗
DOE OSTI2018

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.

36 MATERIALS SCIENCE↗
DOE OSTI2023

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.

annealing↗
DOE OSTI2016

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.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2012

Thermal annealing of laser damage precursors on fused silica surfaces

Previous studies have identified two significant precursors of laser damage on fused silica surfaces at fluences <35 J/cm2: photoactive impurities from polishing and surface fractures. We evaluate isothermal heating as a means of remediating the defect structure associated with surface fractures. Vickers indentations are applied to silica surfaces at loads between 0.5 and 10 N, creating fracture networks. The indentations are characterized before and following thermal annealing under various time and temperature conditions using confocal time-resolved photo-luminescence (CTP) imaging, and R/1 damage testing with 3-ns, 355-nm laser pulses. Improvements in the damage thresholds with reductions in CTP intensity are observed at temperatures well below the glass transition temperature (Tg). The damage threshold on 0.5-N indentations improves from <8 to >35 J/cm2 after annealing at approximately 750°C. Larger fracture networks require longer or higher temperature treatment to achieve similar results. At an annealing temperature >1100°C, optical microscopy indicates morphological changes in some of the fractures surrounding the indentations, although remnants of the original fractures are still observed. In conclusion, we demonstrate the potential of using isothermal annealing to improve the laser damage resistance of silica optics, and provide a means of further understanding the physics of optical damage and mitigation.

36 MATERIALS SCIENCE↗
DOE OSTI2016

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.

36 MATERIALS SCIENCE↗
DOE OSTI2017

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.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

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.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗