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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 OSTI2025

Characterization of Recrystallized Grains During Static Recrystallization of Hot-Compressed Mg–Zn–Ca Alloys Using In Situ Far-Field High-Energy Diffraction Microscopy

In this study, we explored the effect of Zn content on the static recrystallization of three 80 pct hot-compressed alloys, Mg–0.5Zn–0.1Ca wt pct (ZX050), Mg–1Zn–0.1Ca wt pct (ZX10), and Mg–3.2Zn–0.1Ca wt pct (ZX30), using far-field high-energy microscopy (ff-HEDM). Individual recrystallized grains were tracked and their 3D centroid, relative volume, and grain-averaged crystallographic orientation were measured during annealing. These measurements were used to compare the recrystallization kinetics and texture evolution of recrystallized grains in ZX alloys as a function of the Zn content. Fully recrystallized microstructures were observed for the ZX30 and the ZX10 alloys after annealing at 230 °C and 330 °C, respectively. In contrast, only a partially recrystallized microstructure for the ZX050 alloy was observed after > 1 hour of annealing at 430 °C. The resistance to recrystallization with decreasing Zn content was also confirmed by detecting faster growth rates of recrystallized grains in the ZX10 and ZX30 alloys, and slower growth rates in the ZX050 alloy. The significant recrystallization texture weakening of the ZX10 and ZX30 alloys and the development of a basal texture in the ZX05 alloy were described based on the orientation dependency of nucleation and growth of recrystallized grains. The analysis demonstrated that texture weakening was associated with increasing Zn content in Mg–Zn–Ca alloys.

Roumina, Reza [Univ. of Michigan, Ann Arbor, MI (U↗
DOE OSTI2025

Effects of Grain Size and Interstitial Content on Recrystallization in Nb after Cold Rolling

A fully recrystallized microstructure with a fine grain size can improve the performance of superconducting radio-frequency (SRF) cavities produced from high-purity Nb (ASTM B393–18 Type 5 Nb) while providing mechanical strength. Recrystallization depends on impurity content, initial microstructure, deformation state, and annealing conditions. To better understand how fine-grained, fully recrystallized microstructures may be produced, the recrystallization behaviors of Type 5 and Type 2 Nb materials were studied. Type 5 Nb specimens were produced with both fine and coarse initial grain sizes. All were cold rolled and then annealed under vacuum for one hour to determine the rolling reductions and temperatures required for recrystallization. The recrystallized fraction exceeded 95% in fine-grained Type 5 Nb rolled to a 30% or greater thickness reduction and then annealed at 800 °C or higher. The coarse grained Type 5 Nb required greater rolling reductions to produce any recrystallized grains at 800 °C. The higher interstitial content of the Type 2 Nb required a temperature of 1000 °C or higher to reach a recrystallized fraction greater than 95% in specimens rolled to a 60% reduction. Recrystallization is more easily achieved during annealing at a given temperature for a set time by increasing rolling reduction, decreasing interstitial content, and decreasing initial grain size prior to cold rolling. In conclusion, to avoid grain growth following recrystallization, which increases grain size, the minimum time and temperature necessary for complete recrystallization should be applied.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2026

CHARACTERIZING AND CONTROLLING RECOVERY AND RECRYSTALLIZATION IN NIOBIUM FOR IMPROVED SRF CAVITY PERFORMANCE

Crystal defects, such as dislocations and low-angle boundaries, provide sources of magnetic flux trapping in the Nb materials used for superconducting radio frequency (SRF) resonating cavities. Improving the performance of SRF cavities, as measured through the quality factor, requires reducing these defects. SRF cavity production involves deformation processing, such as rolling and forming, and strategic annealing heat treatments. The resulting microstructures can be recovered, recrystallized, or both. Because recovery leaves many defects that can trap flux, recrystallization should improve cavity performance. Thus, processing schedules that produce complete recrystallization without excessive grain growth need to be designed. Solutions to this problem require understanding physical metallurgy and differentiating between recovered and recrystallized regions of microstructure. Backscattered electron microscopy techniques are applied to this end. We demonstrate that the conditions required to produce fully recrystallized microstructures depend on Nb impurity content, suggesting that processing schedules may need to be adjusted by material heat or lot. We also demonstrate that processing can be used to control growth of recrystallized grains to maintain mechanical strength in fully recrystallized materials. Forming cavities from cold-rolled Nb sheet material may provide strategic new routes to obtain microstructures that improve SRF cavity performance.

Taleff, E. [The University of Texas at Austin]↗
DOE OSTI2023

An Integrated Simulation of Multiple-Pass U-10Mo Alloy Hot Rolling and Static Recrystallization

To achieve a desired microstructure and minimize the thickness variation in rolled foils, researchers must understand the effects of foil fabrication process variables on microstructure evolution. We developed an integrated simulation of deformation and recrystallization that employs the finite element method (FEM) and the kinetic Monte Carlo (KMC) Potts model, respectively, to investigate microstructure evolution during multiple-pass hot rolling and heat treatment in polycrystalline U-10Mo fuel. Scanning electron microscopy and electron backscatter diffraction images of microstructures were directly used as input in FEM calculation of deformation, and the calculated strains were used to determine the driving force of nucleation and growth of recrystallized grains in the Potts model. Grain structures predicted by the Potts model were used to update the grain structure and material properties for FEM. Simulation alternated between FEM and the Potts model to simulate grain structure evolution during multiple rolling and heat treatments. The initial model parameters were determined by benchmarking the recrystallization kinetics against experimental data. Then, the model was applied to predict the grain structure evolution. Results showed that our model can capture the coupling between deformation and recrystallization and can quantitatively reproduce the observed U-10Mo recrystallization and grain growth kinetics. The simulation results demonstrated that the developed model can predict U-10Mo grain structures as a function of initial microstructure and foil fabrication parameters.

36 MATERIALS SCIENCE↗
NASA NTRS1981

Recrystallization of polycrystalline silicon

Optical metallography is used to investigate the recrystallization properties of polycrystalline semiconductor-grade silicon. It is found that polycrystalline silicon recrystallizes at 1380 C in relatively short times, provided that the prior deformation is greater than 30%. For a prior deformation of about 40%, the recrystallization process is essentially complete in about 30 minutes. Silicon recrystallizes at a substantially slower rate than metals at equivalent homologous temperatures. The recrystallized grain size is insensitive to the amount of prestrain for strains in the range of 10-50%.

Lall, C.↗
DOE OSTI2026

Influence of rolling reduction and annealing on recrystallization and grain structure in Ta-2.5W alloys

The microstructural evolution of wrought Tantalum - 2.5 wt% Tungsten (Ta-2.5W) alloys during thermomechanical processing is critical for optimizing their mechanical reliability in demanding applications such as aerospace, chemical processing, and nuclear technology. Despite the widespread use of Ta-W alloys, a comprehensive understanding of how rolling reduction, annealing temperature, and elemental inhomogeneity interact to determine recrystallization behavior and grain refinement remains incomplete. Here, in this study, we systematically investigate the effects of cold rolling and subsequent annealing on the microstructure of Ta-2.5W, with particular attention to grain orientation, stored energy, and elemental banding. Our results demonstrate that higher rolling reduction rates lower the onset and completion temperatures for recrystallization, resulting in finer and more homogeneous grain structures. Electron backscatter diffraction (EBSD) analysis reveals that grains with a 〈111〉 parallel to the plate normal possess higher stored energy and nucleate recrystallization more readily than grains with a 〈001〉 parallel to the plate normal. Elemental mapping shows that tungsten inhomogeneity leads to localized bands of accelerated recrystallization and hardness variation. These findings provide new insights into the mechanisms of microstructure refinement in Ta-2.5W alloys, offering guidance for tailoring processing routes to achieve superior performance in demanding engineering environments.

Annealing↗
DOE OSTI2025

Meshfree simulation and prediction of recrystallized grain size in friction stir processed 316L stainless steel

Friction stir processing (FSP) is a promising solid-phase microstructural modification technique that can repair and enhance damaged stainless steel surfaces exposed to harsh environments. The quality of the repaired material is closely correlated to the recrystallized grain size in the stir zone (SZ), which is influenced by the thermomechanical conditions dictated by FSP process parameters. Thus, establishing a reliable relationship between these parameters and recrystallized grain size in the SZ is crucial for optimizing repair quality. However, existing experimental approaches often rely on indirect temperatures measured far from the SZ, along with rough strain rate estimations, which are imprecise and time-consuming. Meanwhile, existing mesh-based modeling methods usually face numerical challenges when dealing with the large material deformations inherent in FSP. Here, to address these issues, this study introduces a meshfree process model for FSP based on the smoothed particle hydrodynamics (SPH) method, aimed at predicting process conditions under different parameters. The model is validated using experimental data from 11 combinations of tool traverse and rotation speeds on 316 L stainless steel. Correlations between process parameters, material flow, temperature, strain, strain rate, and recrystallized grain size are revealed through SPH simulations and electron backscatter diffraction (EBSD) imaging. The results show that in situ SZ temperatures range from 1071 to 1322°C, which exceed the tool temperature by over 300°C. Furthermore, SZ temperature, strain rate, and grain size increase monotonically with higher tool temperature and faster traverse speed. A relationship is then established between the model-predicted Zener-Hollomon parameter and the recrystallized grain size based on EBSD data, expressed as ln(d) = -0.364 ln(Z) + 14.673. Finally, this relationship exhibits satisfactory accuracy with errors of less than 26.9% in predicting grain sizes at various SZ locations, which offers valuable insights for optimizing FSP repair processes for 316 L stainless steel.

316L stainless steel↗
NASA NTRS1953

Effect of Prestraining of Recrystallization Temperature and Mechanical Properties of Commercial, Sintered, Wrought Molybdenum

Given three presumably identical lots of commercial, sintered, wrought molybdenum, the 1-hour recrystallization temperature of one lot remained above 2900 F by limiting the amount of effective restraining to 35 percent or less. Different recrystallization temperatures were obtained in various atmospheres, the highest in argon and the lowest in hydrogen. Metal thus fabricated and then stress-relieved possessed an ultimate tensile strength at room temperature within 10 percent of metal swaged 99 percent and also possessed equivalent ductility. At 1800 F, equivalent strength and ductility was obtained irrespective of the amount of swaging over the range of 10 to 99 percent. The amount of swaging greatly influenced the recrystallized grain size but the difference in grain size is not the major controlling factor which determines whether recrystallized molybdenum is ductile or brittle at room temperature.

MATERIALS, PROPERTIES - TENSILE↗
NASA NTRS1996

Recrystallized Impact Glasses of the Onaping Formation and the Sudbury Igneous Complex, Sudbury Structure, Ontario, Canada

The origin of the Sudbury Structure and of the associated heterolithic breccias of the Onaping Formation and the Sudbury Igneous Complex have been controversial. While an impact origin of the structure has gained wide acceptance over the last 15 years, the origin of the recrystallized Onaping Formation glasses and of the igneous complex is still being debated. Recently the interpretation of the breccias of the Onaping Formation as suevitic fall-back impact breccias has been challenged. The igneous complex is interpreted either as a differentiated impact melt sheet or as a combination of an upper impact melt represented by the granophyre, and a lower, impact-triggered magmatic body consisting of the norite-sublayer formations. The Onaping Formation contains glasses as fluidal and nonfluidal fragments of various shapes and sizes. They are recrystallized, and our research indicates that they are petrographically heterogeneous and span a wide range of chemical compositions. These characteristics are not known from glasses of volcanic deposits. This suggests an origin by shock vitrification, an interpretation consistent with their association with numerous and varied country rock clasts that exhibit microscopic shock metamorphic features. The recrystallized glass fragments represent individual solid-state and liquid-state vitrified rocks or relatively small melt pods. The basal member lies beneath the Gray and Black members of the Onaping Formation and, where not metamorphic, has an igneous matrix. Igneous-textured melt bodies occur in the upper two members and above the Basal Member. A comparison of the chemical compositions of recrystallized glasses and of the matrices of the Basal Member and the melt bodies with the components and the bulk composition of the igneous complex is inconclusive as to the origin of the igneous complex. Basal Member matrix and Melt Bodies, on average, are chemically similar to the granophyre of the Sudbury Igneous Complex, suggesting that they are genetically related. Our chemical results allow interpretation of the entire igneous complex as a differentiated impact melt. However, they are also consistent with the granophyre alone being the impact melt and the nofite and quartz gabbro beneath it representing an impact-triggered magmatic body. This interpretation is preferred, as it is consistent with a number of field observations. A re-evaluation and extension of structural field studies and of geochemical data, as well as a systematic study of the contact relationships of the various igneous phases of the igneous complex, are needed to establish a Sudbury impact model consistent with all data and observations

Dressler, B. O.↗
DOE OSTI2023

Incorporating dynamic recrystallization into a crystal plasticity model for high-temperature deformation of Ti-6Al-4V

During hot deformation of (α + β) titanium alloys, the simultaneous action of strain and temperature in the (α + β) regime facilitates dynamic recovery, dynamic recrystallization (DRX), and phase transformations via non-equilibrium paths. DRX is manifested in the form of fine recrystallized α or β grains. Here, in the present study, a two-phase crystal plasticity finite element framework (CP-DRX) has been developed which incorporates DRX kinetics into the crystal plasticity (CP) model to predict the flow characteristics of Ti-6Al-4V alloys during thermo-mechanical processing. The CP slip system parameters, as well as elastic properties from both α and β phases of Ti, are calibrated for different strain rate conditions. An EBSD-informed two-phase microstructure representation has been utilized in the CP-DRX framework to explore the time-dependent evolution of DRX microstructure and crystal orientation for different strain rate conditions. The proposed CP-DRX can capture the evolution of crystal orientation and plastic flow stress–strain response of polycrystalline Ti-6Al-4V during the deformation process. Furthermore, the proposed model is able to capture the softening behavior, observed in average stress–strain response from experiments performed using a Gleeble thermomechanical simulator and predict the recrystallization texture.

(α+ β)-Titanium (Ti) Alloys↗
DOE OSTI2026

Influence of the as-built microstructure on the recrystallization of an additively manufactured Inconel939 Ni-based superalloy

This study investigates the influence of the as-built microstructure on the recrystallization (RX) behavior and mechanical properties of the Ni-based superalloy Inconel 939 produced by laser powder bed fusion (PBF-LB/M). Two distinct as-built microstructures were obtained by varying the hatch distance (h d ): a columnar, strongly textured condition (h d =50, termed h d 50) and an equiaxed, weakly textured condition (h d =70, termed h d 70)). Both were subjected to nine solution treatments combining three temperatures (1100, 1150, and 1200 °C) and three holding times (1, 4, and 8 h). Comprehensive microstructural characterization was conducted to assess grain morphology, texture, grain boundary character, dislocation density, and precipitate distribution. Recrystallization was found to be significantly slower than in cast counterparts, requiring higher temperatures and longer times for completion. The initial microstructure plays a decisive role: full RX was achieved only in hd70 specimens after treatment at 1200 °C for 8 h, whereas hd50 samples exhibited delayed and incomplete RX under identical conditions. This behavior is attributed to the finer grain size and higher fraction of high-angle grain boundaries in hd70, which promote recrystallization. Mechanical testing revealed that hd70 samples subjected to a 1200 °C/8 h treatment followed by standard double ageing show higher yield and tensile strengths across the investigated temperature range than both printed and cast Inconel939 processed under conventional conditions, albeit with slightly reduced ductility. The enhanced mechanical performance is attributed to the larger grain size, which limits grain boundary sliding. These results demonstrate the critical importance of controlling the as-built microstructure and tailoring post-processing strategies to optimize high-temperature performance of PBF-LB/M Inconel939.

Inconel939↗
DOE OSTI2023

Role of geometric dynamic recrystallization in nanocrystalline alloys

Nanocrystalline and near-nano-grained metals are plagued with an overall lack of ductility and formability. This is in part due to their inability to support the dislocation mechanisms or undergo the same types of transformations that conventional coarse-grained metals access in order to increase their workability. Therefore, despite their advanced properties such as high strength, the manufacturing of such fine-grained metals, which exposes them to multi-axial states of stress in operations such as rolling, drawing, extrusion, forging, and bending, has not been possible. In this work, we address this limitation and highlight an important aspect of geometric dynamic recrystallization (GDRX) in nanocrystalline materials as a way to improve manufacturability. In particular, using two different alloy compositions and two different processing techniques, this study points to the fact that if nanocrystalline or near nano metals can be truly stabilized, they can repeatedly undergo the same types of processes that conventional coarse-grained metals endure, increasing both their formability and hence manufacturability. The results reveal that due to a large number of initial high-angle grain boundaries and large applied compressive strains, GDRX is activated in the absence of any discontinuous dynamic recrystallization (DDRX) or continuous dynamic recrystallization (CDRX). This is a unique aspect of stabilized nanocrystalline materials, as traditionally fine-grained metals are not microstructurally stable enough to accommodate such an event.

36 MATERIALS SCIENCE↗
DOE OSTI2023

3D mapping of residual stresses in growing grains of partially recrystallized Gum Metal

The crystallographic orientations and residual stresses within recrystallizing grains in partially recrystallized beta titanium-Gum Metal-were examined non-destructively in 3D using synchrotron Differential Aperture X-ray Microscopy. Contrary to common assumptions, significant local stresses and stress variations are observed within the recrystallizing grains. The results reveal that the development of these local residual stresses depends on the plastic deformation mode and material's elastic constants, rather than grain properties such as size and orientation, or even the material's yield stress. This work provides insights valuable for the design of advanced materials with heterogeneous microstructures.

36 MATERIALS SCIENCE↗
DOE OSTI2025

High-pressure high-temperature melting and recrystallization of nanolamellar high-entropy alloys

Additively manufactured (AM) High Entropy Alloys (HEAs) are notable for their exceptional high-yield strength and large tensile ductility. The nanolamellar Eutectic HEA (EHEA) AlCoCrFeNi 2.1 was fabricated by laser powder bed fusion (L-PBF) in the as-printed form (EHEA1) and subsequently annealed at 1000oC (EHEA2) and 600oC (EHEA3) to achieve a broad range of mechanical properties. EHEA2 and EHEA3 samples were studied using Scanning transmission electron microscopy (STEM), energy dispersive X-ray diffraction (EDXRD) at high-pressures and high temperatures, nanoindentation hardness and modulus measurements. According to EDXRD EHEA2 and EHEA3 are composed of B2 and L1 2 phases. High-pressure high-temperature EDXRD studies show melting for EHEA2 at 1698 ± 25 K at a pressure of 6.5 GPa and melting for EHEA3 at 1598 ± 25 K at a pressure of 5.8 GPa. Post-melt and recrystallized samples were recovered at ambient conditions, and XRD analysis showed retention of B2 and L1 2 phases, although a new σ phase appeared for both EHEA2 and EHEA3 samples due to high-pressure and high-temperature melting and recrystallization experiment. SEM analysis also demonstrated the preservation of the nanolamellar morphology. Nanoindentation studies revealed that recrystallized EHEAs retain their original mechanical property hierarchy, with EHEA3 being 47% harder than EHEA2, largely related to higher content of B2-phase and retention of nanolamellar morphology. We also present Pressure-Volume-Temperature (P-V-T) data for 3-D printed and annealed eutectic high entropy alloys and extract mechanical and thermal properties data.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Depth-dependent recovery of thermal conductivity after recrystallization of amorphous silicon

The depth-dependent recovery of silicon thermal conductivity was achieved after the recrystallization of silicon that had been partially amorphized due to ion implantation. Transmission electron microscopy revealed nanoscale amorphous pockets throughout a structurally distorted band of crystalline material. The minimum thermal conductivity of as-implanted composite material was 2.46 W m −1 K −1 and was found to be uniform through the partially amorphized region. X-ray diffraction measurements reveal 60% strain recovery of the crystalline regions after annealing at 450 °C for 30 min and almost full strain recovery and complete recrystallization after annealing at 700 °C for 30 min. In addition to strain recovery, the amorphous band thickness reduced from 240 to 180 nm after the 450 °C step with nanoscale recrystallization within the amorphous band. A novel depth-dependent thermal conductivity measurement technique correlated thermal conductivity with the structural changes, where, upon annealing, the low thermal conductivity region decreases with the distorted layer thickness reduction and the transformed material shows bulk-like thermal conductivity. Full recovery of bulk-like thermal conductivity in silicon was achieved after annealing at 700 °C for 30 min. After the 700 °C anneal, extended defects remain at the implant projected range, but not elsewhere in the layer. Previous results showed that high point-defect density led to reduced thermal conductivity, but here, we show that point defects can either reform into the lattice or evolve into extended defects, such as dislocation loops, and these very localized, low-density defects do not have a significant deleterious impact on thermal conductivity in silicon.

Huynh, Kenny↗
DOE OSTI2024

Effect of Processing Parameters on Recrystallization During Hot Isostatic Pressing of Stellite-6 Fabricated Using Laser Powder Bed Fusion Technique

Crack-free Stellite-6 alloy was fabricated using the laser powder bed fusion technique equipped with a heating module as the first attempt. Single tracks were printed with a build plate heated to 400 °C to identify the processing window. Based on the melt pool dimensions, two combinations (sample A: 300 W/750 mm/s and sample B: 275 W/1000 mm/s) were identified to print the cubes. The as-printed microstructure comprised FCC-Co dendrites with M7C3 in the interdendritic region. W-rich M6C particles were found in the overlapping regions between the melt pools, matching the Scheil simulations. However, gas pores were observed due to the higher nitrogen and oxygen content of the feedstock requiring hot isostatic pressing (HIP) at 1250 °C and 150 MPa for 2 h. Sample A was partially recrystallized with slightly coarsened M7C3, while sample B underwent complete recrystallization followed by grain growth along with higher coarsening of the M7C3 after HIP. The varying recrystallization behavior can be attributed to the difference in residual stresses and grain aspect ratio in the as-built condition dictated by laser power and scanning speed. The microhardness after HIP was slightly higher than its wrought counterpart, indicating no severe impact of post-processing on the properties of Stellite-6 alloy.

Sridar, Soumya (ORCID:0000000306775408)↗
NASA NTRS1975

A study of the oxide dispersion and recrystallization in NiCrAl prepared from preoxidized powder

The sintered aluminum powder (SAP) technique of dispersion strengthening (formation of an oxide dispersion by preoxidation of metal powders) was applied to atomized powder of a nickel alloy containing, by weight, 17% Cr, 5% Al, and 0.2% Y. The SAP-NiCrAl alloy (without the ytterbium removed by oxdation) was worked by extrusion and rod rolling at 1205 C and by swaging at 760 C. Annealing treatments were applied after working to determine the recrystallization response. The NiCrAlY alloy, similarly prepared from atomized powder, but without a preoxidation treatment, was examined for comparison. The SAP-NiCrAl alloy exhibited oxide particle size and spacing much larger than that usually observed in oxide dispersion strengthened alloys; nonetheless, it was possible to achieve abnormal (secondary) recrystallization in the SAP-NiCrAl alloy as has been reported for other oxide dispersion strengthened alloys. In contrast, the unoxidized NiCrAlY alloy exhibited only primary recrystallization.

Glasgow, T. K.↗
NASA NTRS1975

A study of the oxide dispersion and recrystallization in NiCrAl prepared from preoxidized powder

The SAP technique of dispersion strengthening (formation of an oxide dispersion by preoxidation of metal powders) was applied to atomized powder of the alloy Ni-17Cr-5Al-0.2 Y. SAP-NiCrAl was worked by extrusion and rod rolling at 1205 C and by swaging at 760 C. A variety of annealing treatments were applied after working to determine the recrystallization response. NiCrAlY, similarly prepared from atomized powder, but without a preoxidation treatment, was examined for comparison. The SAP-NiCrAl of this study exhibited oxide particle size and spacing much larger than that usually observed in oxide dispersion strengthened alloys; nonetheless, it was possible to achieve abnormal (secondary) recrystallization in the SAP-NiCrAl as has been reported for other oxide dispersion strengthened alloys. In contrast, unoxidized NiCrAlY exhibited only primary recrystallization.

Glasgow, T. K.↗