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At least 19 records

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↗

Multiscale in-situ characterization of static recrystallization using dark-field X-ray microscopy and high-resolution X-ray diffraction

Abstract Dark-field X-ray microscopy (DFXM) is a high-resolution, X-ray-based diffraction microstructure imaging technique that uses an objective lens aligned with the diffracted beam to magnify a single Bragg reflection. DFXM can be used to spatially resolve local variations in elastic strain and orientation inside embedded crystals with high spatial (~ 60 nm) and angular (~ 0.001°) resolution. However, as with many high-resolution imaging techniques, there is a trade-off between resolution and field of view, and it is often desirable to enrich DFXM observations by combining it with a larger field-of-view technique. Here, we combine DFXM with high-resolution X-ray diffraction (HR-XRD) applied to an in-situ investigation of static recrystallization in an 80% hot-compressed Mg–3.2Zn–0.1Ca wt.% (ZX30) alloy. Using HR-XRD, we track the relative grain volume of > 8000 sub-surface grains during annealing in situ. Then, at several points during the annealing process, we “zoom in” to individual grains using DFXM. This combination of HR-XRD and DFXM enables multiscale characterization, used here to study why particular grains grow to consume a large volume fraction of the annealed microstructure. This technique pairing is particularly useful for small and/or highly deformed grains that are often difficult to resolve using more standard diffraction microstructure imaging techniques.

36 MATERIALS SCIENCE↗

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↗

Method of producing superplastic alloys and superplastic alloys produced by the method

A method for producing new superplastic alloys by inducing in an alloy the formation of precipitates having a sufficient size and homogeneous distribution that a sufficiently refined grain structure to produce superplasticity is obtained after subsequent PSN processing. An age-hardenable alloy having at least one dispersoid phase is selected for processing. The alloy is solution heat-treated and cooled to form a supersaturated solid solution. The alloy is plastically deformed sufficiently to form a high-energy defect structure useful for the subsequent heterogeneous nucleation of precipitates. The alloy is then aged, preferably by a multi-stage low and high temperature process, and precipitates are formed at the defect sites. The alloy then is subjected to a PSN process comprising plastically deforming the alloy to provide sufficient strain energy in the alloy to ensure recrystallization, and statically recrystallizing the alloy. A grain structure exhibiting new, fine, equiaxed and uniform grains is produced in the alloy. An exemplary 6xxx alloy of the type capable of being produced by the present invention, and which is useful for aerospace, automotive and other applications, is disclosed and claimed. The process is also suitable for processing any age-hardenable aluminum or other alloy.

Troeger, Lillianne P.↗

Multimodal Analysis of Spatially Heterogeneous Microstructural Refinement and Softening Mechanisms in Three-Pass Friction Stir Processed Al4Si Alloy

Multiple thermally and thermomechanically induced microstructural refinement mechanisms can be activated in metallic alloys when subjected to solid phase processing methods such as friction stir processing (FSP). In this work, we provide detailed descriptions of the relationship between region-specific microstructural refinement mechanisms and the variation in microhardness, through a systematic and multimodal microstructural characterization of an FSP-processed 75% cold-rolled Al-4 at.% Si model binary alloy. Spatially resolved high-energy synchrotron X-ray diffraction, electron backscattered diffraction, and scanning transmission electron microscopy were used to understand the spatially heterogeneous microstructural evolution due to FSP. Results provide insights into how mechanisms such as static recovery, static recrystallization, dynamic recovery and recrystallization, geometric and continuous dynamic recrystallization, and particle-stimulated static or dynamic grain nucleation may occur heterogeneously in the microstructure as a function of the distance from the stir zone in processed alloys, directly influencing the degree of softening. The systematic analysis of microstructures and hardness in the FSP-processed model binary alloy given in this work highlights the rich microstructural domains that can be uniquely harnessed through solid phase processing of metallic alloys.

Al4Si, Friction Stir Processing, Geometric Dynamic↗

Prediction of softening kinetics and recrystallization texture in non-isothermally annealed bulged tubes using CPFEM and CA models

A hierarchically coupled cellular automata (CA) model, crystal plasticity finite element method (CPFEM), and thermal finite element (FE) model is developed to predict the softening kinetics of the bulged steel tube during non-isothermal annealing. Through the developed model, the kinetics of softening mechanisms including static recovery (SRV) and static recrystallization (SRX), as well as the recrystallization texture are predicted. Later, the Johnson-Mehl-Avrami-Kohnogorov (JMAK) model based on the predicted SRX data is developed to interpret the recrystallization behavior of the material. To perform this study, diverse experimental tests including tube hydroforming (THF), annealing, uniaxial tensile test, hardness test, as well as microstructure observations through optical microscopy and Electron Backscatter Diffraction (EBSD) tests on steel tube are performed. The obtained experimental data are utilized to calibrate and verify the implemented CPFEM model for simulation of THF process, thermal FE model for prediction of the local temperature over annealing time, and CA algorithm for modeling of the softening kinetics and texture evolution throughout the annealing process. The study shows that the predicted deformation characteristics, softening kinetics, recrystallization texture and temperature profile during non-isothermal annealing are in good agreement with experimental data. During the annealing process, a total of four stages for the kinetics of softening mechanisms is observed: No softening; SRV only; SRV dominant; and SRX dominant. During the progress of SRX, the behavior of recrystallization is abruptly changed, confirming that two different mechanisms are controlling the kinetics of transformation.

36 MATERIALS SCIENCE↗

Coupling Thermomechanical Processing and Alloy Design to Improve Textures in Mg-Zn-Ca Sheet Alloys

Abstract The effect of Ca and Zn additions on the microstructure and texture evolution during thermomechanical processing of Mg-Zn-Ca sheet alloys was systematically investigated and quantified. Plane strain compression testing in a Gleeble thermomechanical simulator was used to physically simulate a 10-pass rolling schedule, while allowing for careful control and monitoring of the processing parameters. Textures in the as-deformed ternary alloy samples demonstrate a weak maximum basal intensity and spreading in the transverse direction. Increasing the Zn content to 3.2 wt.% in the ternary alloys resulted in samples that exhibited weak textures in the as-deformed state. Importantly, static recrystallization (SRX) during post-deformation annealing of these alloys promoted a desirable annular texture, with the c -axis tipped from the normal direction and a lower basal texture intensity. The evolution in texture during SRX is associated with as-deformed microstructures with broad grain orientation spreads and a low degree of recrystallization.

36 MATERIALS SCIENCE↗

The 650 °C Tensile Deformation of Graded IN718-René41 Superalloy Fabricated by Laser Blown-Powder Directed Energy Deposition

The microstructure and 650 °C tensile properties of a compositionally graded IN718-René41 (718-R41) superalloy fabricated by laser blown-powder directed energy deposition (DED-LB/M) are investigated to understand structure–property relationships and baseline tensile properties. Digital Image Correlation (DIC), in situ neutron diffraction, and conventional characterization techniques are performed to study the as-built and heat-treated states. The applied heat treatment generates static recrystallization and equiaxed grains in 718-rich compositions, while R41-rich compositions remain partially or un-recrystallized possibly influenced by a higher MC carbide fraction (>0.5%). The yield strengths of the 718 and R41 sections in the heat-treated state are comparable to wrought forms but the graded compositions show weakness due to unoptimized heat treatment. Diffraction elastic constants first decrease and then increase along the 718-R41 composition gradient, while a small difference is observed between the as-built and heat-treated states and γ, γ′ phases. Overall, the compositionally graded region shows a smooth transition in the elastic properties. Grain-level load transfer from the (220) to (200) grains shows compositional dependence, and qualitatively agrees with DIC-measured macroscopic yield strength. Within the (200) grains, the γ/γ′ phases deform elastically until the γ phase yields and afterwards, the γ′ phase takes load from the γ phase.

Huang, Shenyan (ORCID:0000000196528114)↗

Tensile Deformation of DED Graded IN718-René41 Superalloy at 650°C by in-situ Neutron Diffraction and Digital Image Correlation

A compositionally graded material comprised IN718 (718, γ'/γ" strengthened superalloy) and René41 (R41, a medium γ' strengthened superalloy) was fabricated using laser blown-powder directed energy deposition (DED/LB-M). Hot gas path components that require high and low temperature capabilities at different locations may benefit from such graded superalloy, potentially eliminating the use of welded or mechanically joined components and reducing cost. In the present work, microstructure and 650°C tensile behavior of 718-R41 graded superalloy in as-built and heat-treated states are investigated by Digital Image Correlation (DIC), in-situ neutron diffraction, coupled with conventional characterization techniques. The applied heat treatment generates static recrystallization and equiaxed grains in 718 rich compositions, while R41 rich compositions remain partially or un-recrystallized. Yield strengths of 718 and R41 sections in heat-treated state are comparable to wrought forms but the graded compositions show weakness. From neutron experiment, diffraction elastic constants and single crystal elastic constants are calculated, which show small difference between the as-built and heat-treated states and between the γ and γ' phases. Grain-level load transfer from the (220) grains to (200) grains is found to be composition dependent, and qualitatively agrees with DIC measured macroscopic yield strength. Within the (200) grains, the γ/γ' phases deform elastically until the γ phase yields and afterwards the γ' phase takes load from γ phase.

digital image correlation↗

Continuous recrystallization during thermomechanical processing of a superplastic Al-10Mg-0.1Zr alloy

Microstructural evolution via static continuous recrystallization during thermomechanical processing of an Al-Mg-Zr alloy is addressed. Mechanical property data demonstrated that as-rolled material was capable of superplastic response without further treatment. Further, superplastic ductility at 300 C was enhanced by a factor of five by increasing the reheating time between rolling passes during processing also at 300 C. This enhanced ductility was associated with a Cu-texture and a microstructure consisting of predominantly high-angle boundaries. Processing to minimize recovery resulted in a strong Brass-texture component, a predominantly low-angle boundary microstructure and poorer ductility.

Hales, S. J.↗

AP reclamation and reuse in RSRM propellant

A solid propellant ingredient reclamation pilot plant has been evaluated at the Strategic Operations of Thiokol Corporation, located in Brigham City, Utah. The plant produces AP wet cake (95 percent AP, 5 percent water) for recycling at AP vendors. AP has been obtained from two standard propellant binder systems (PBAN and HTPB). Analytical work conducted at Thiokol indicates that the vendor-recrystallized AP meets Space Shuttle propellant specification requirements. Thiokol has processed 1-, 5-, and 600-gallon propellant mixes with the recrystallized AP. Processing, cast, cure, ballistic, mechanical, and safety properties have been evaluated. Phillips Laboratory static-test-fired 70-pound and 800-pound BATES motors. The data indicate that propellant processed with reclaimed AP has nominal properties.

Miks, Kathryn F.↗

Measuring residual stress in Ti-6Al-4V with HR-EBSD, using reference patterns from annealed material

In this study, elastic strain and residual stress values in an engineering material were determined by high-resolution EBSD (HR-EBSD) using reference patterns from annealed, recrystallized material. Specifically, rolled Ti-6Al-4V sheet was analyzed using HR EBSD in both an as-annealed and a strained state, the latter established via a static two-point bend fixture. The commercial software CrossCourt4 (CC4) was used to evaluate the relative intragranular strain tensor components of the alpha grains mapped by HR-EBSD. The intragranular reference patterns identified in each grain by the software were then replaced with similarly-oriented patterns from scans of the as-annealed, recrystallized material. The CC4 analysis was then repeated to provide calibrated strain and residual stress values. Elastic strains on the order of 10–3 were detected, with corresponding residual stress values on the order of 1 GPa. Subsequent analyses using high energy synchrotron x-ray diffraction showed good correlation with the elastic strains measured by HR-EBSD using the annealed reference patterns. Additionally, the maximum macroscopic stress analytically predicted for two-point bending was in agreement with the residual stress observed. Good repeatability of the methodology and insight into the state of individual grains were also observed. The findings provide encouraging evidence that accurate intragranular and long-range residual stress measurements of engineering significance can be made with HR-EBSD using a physical reference pattern library.

36 MATERIALS SCIENCE↗

Creep Deformation and Dynamic Grain Growth in an Interstitial-Free Steel

Dynamic grain growth is demonstrated to be much faster than static grain growth in a body-centered-cubic, interstitial-free steel sheet material at 850°C. Dynamic grain growth occurs during concurrent plastic deformation at elevated temperature, whereas static grain growth occurs during static annealing. Grain growth during steady-state plastic flow in tension at 850°C to a true strain of 0.2 at a true-strain rate of 10 -4 s -1 doubled grain size, while static annealing for the same time produced no increase in grain size. This is described as dynamic normal grain growth (DNGG) because no abnormally large grains were observed. The recrystallized microstructure of the steel demonstrated a log-normal distribution of grain sizes. DNGG produced bimodal grain size distributions that deviate from the theoretical expectation of a simple shift to larger sizes during normal growth. The bimodal distributions contained a remnant of small grains that were not consumed during grain growth. DNGG produced a crystallographic texture that is unique from both the recrystallized material and that produced by lattice rotation alone. DNGG strengthened the {111}⟨110⟩ and {111}⟨112⟩ components of the strong γ-fiber component in the original recrystallization texture. Lattice rotation from tensile deformation, by contrast, strengthened the α-fiber components that intersect the original γ-fiber.

36 MATERIALS SCIENCE↗

Low-Temperature Friction-Stir Welding of 2024 Aluminum

Solid state friction-stir welding (FSW) has been demonstrated to involve dynamic recrystallization producing ultra-fine, equiaxed grain structures to facilitate superplastic deformation as the welding or joining mechanism. However, the average residual, equiaxed, grain size in the weld zone has ranged from roughly 0.5 micron to slightly more than 10 micron, and the larger weld zone grain sizes have been characterized as residual or static grain growth as a consequence of the temperatures in the weld zone (where center-line temperatures in the FSW of 6061 Al have been shown to be as high as 480C or -0.8 T(sub M) where T(sub M) is the absolute melting temperature)). In addition, the average residual weld zone grain size has been observed to increase near the top of the weld, and to decrease with distance on either side of the weld-zone centerline, an d this corresponds roughly to temperature variations within the weld zone. The residual grain size also generally decreases with decreasing FSW tool rotation speed. These observations are consistent with the general rules for recrystallization where the recrystallized grain size decreases with increasing strain (or deformation) at constant strain rate, or with increasing strain-rate, or with increasing strain rate at constant strain; especially at lower ambient temperatures, (or annealing temperatures). Since the recrystallization temperature also decreases with increasing strain rate, the FSW process is somewhat complicated because the ambient temperature, the frictional heating fraction, and the adiabatic heating fraction )proportional to the product of strain and strain-rate) will all influence both the recrystallization and growth within the FSW zone. Significantly reducing the ambient temperature of the base metal or work pieces to be welded would be expected to reduce the residual weld-zone grain size. The practical consequences of this temperature reduction would be the achievement of low temperature welding. This study compares the residual grain sizes and microstructures in 2024 Al friction-stir welded at room temperature (about 30C and low temperature (-30C).

Benavides, S.↗

Oxidation and the Effects of High Temperature Exposures on Notched Fatigue Life of an Advanced Powder Metallurgy Disk Superalloy

Oxidation and the effects of high temperature exposures on notched fatigue life were considered for a powder metallurgy processed supersolvus heat-treated ME3 disk superalloy. The isothermal static oxidation response at 704 C, 760 C, and 815 C was consistent with other chromia forming nickel-based superalloys: a TiO2-Cr2O3 external oxide formed with a branched Al2O3 internal subscale that extended into a recrystallized - dissolution layer. These surface changes can potentially impact disk durability, making layer growth rates important. Growth of the external scales and dissolution layers followed a cubic rate law, while Al2O3 subscales followed a parabolic rate law. Cr- rich M23C6 carbides at the grain boundaries dissolved to help sustain Cr2O3 growth to depths about 12 times thicker than the scale. The effect of prior exposures was examined through notched low cycle fatigue tests performed to failure in air at 704 C. Prior exposures led to pronounced debits of up to 99 % in fatigue life, where fatigue life decreased inversely with exposure time. Exposures that produced roughly equivalent 1 m thick external scales at the various isotherms showed statistically equivalent fatigue lives, establishing that surface damage drives fatigue debit, not exposure temperature. Fractographic evaluation indicated the failure mode for the pre-exposed specimens involved surface crack initiations that shifted with exposure from predominately single intergranular initiations with transgranular propagation to multi-initiations from the cracked external oxide with intergranular propagation. Weakened grain boundaries at the surface resulting from the M23C6 carbide dissolution are partially responsible for the intergranular cracking. Removing the scale and subscale while leaving a layer where M23C6 carbides were dissolved did not lead to a significant fatigue life improvement, however, also removing the M23C6 carbide dissolution layer led to nearly full recovery of life, with a transgranular initiation typical to that observed in unexposed specimens.

Sudbrack, Chantal K.↗

Static compression of Ca(OH)2 at room temperature - Observations of amorphization and equation of state measurements to 10.7 GPa

X-ray diffraction measurements are reported for Ca(OH)2 portlandite as it is compressed to 37.6 GPa in the diamond cell at room temperature. Between 10.7 and 15.4 GPa crystalline Ca(OH)2 transforms to a glass, and on decompression the glass recrystallizes between 3.6 and 5.1 GPa. Below pressures of 10.7 GPa the elastic compression of crystalline Ca(OH)2 was measured. A finite strain analysis of these data shows that the isothermal bulk modulus and its pressure derivative are 37.8 + or - 1.8 GPa and 5.2 + or - 0.7 at zero pressure. The change in the unit cell dimensions indicates that the linear incompressibilities of Ca(OH)2 differ by a factor of three.

Meade, Charles↗

Solute effects upon dislocation motion and recovery in Mg alloys (Final Report)

The objective the research was to develop a firmer understanding of the interactions between substitutional solute atoms and dislocations within Mg alloys. These interactions govern the absolute and relative mobilities of various types of dislocations in Mg (e.g., basal < a>, non-basal < a>, and pyramidal < c+a>). Furthermore, they have an impact on dislocation recovery processes (e.g., cross-glide, climb, rearrangement, and annihilation). Ultimately, solute-dislocation interactions strongly impact a) strain hardening, b) strain rate sensitivity, c) plastic anisotropy of textured polycrystals, d) texture evolution, e) dislocation substructures evolution, and even f) recrystallization behavior. It is broadly known that Mg alloys exhibit poor low temperature formability. Since formability is largely governed by properties (a) – (c) in this list, it is critical to develop a better understanding of solute-dislocation interactions, if one hopes to improve the situation. While the theory of static solute strengthening is well developed, especially for alloys with face centered cubic (FCC) crystal structures, there are outstanding questions related to applications to hexagonal close packed (HCP) crystal structures and dynamic strain aging (DSA) in materials of various structures. DSA has far-reaching implications for metal formability and, in the case of Mg alloys, appears to correlate with the so-called rare-earth (RE) texture which has been shown to benefit formability. The Portevin-Le Chatelier (PLC) effect, and associated negative strain rate sensitivity, occur at higher temperatures (>100℃) in Mg alloys as compared with similar Al alloys, even though they have similar melting points and solute diffusivities. Our preliminary research has shown that modern, physics-based models of DSA can be tuned to describe the behavior of Mg alloys if a rather higher activation enthalpy is assumed for cross-core diffusivity. While this partially explains the delay in DSA to higher temperatures, it is also hypothesized that this delay is due in part to the intrinsically more thermally activated (rate sensitive) nature of non-basal < a> dislocation motion which is required for macroscopic flow of Mg alloys, whereas octahedral slip in many FCC metals like aluminum is essentially athermal at room temperature. It was originally proposed to employ a combination of in-situ diffraction-based experimental characterization to validate existing theory. It was envisioned to perform in-situ transmission electron microscopy (TEM) to assess individual dislocation behavior and in-situ high-energy X-ray diffraction (HEXRD) techniques which were showing great promise for elucidating collective dislocation behavior, 2 including recovery, especially if the contributions to various forms of diffraction peak broadening (𝜂𝜂,𝜔𝜔,and 2𝜃𝜃) can be effectively integrated. Finally, it was envisioned to perform discrete dislocation dynamics (DDD) modeling approaches to aide in the interpretation of both TEM and HEXRD experiments. In the end, mechanical tests were performed on more complex Mg alloys which exhibited evidence of dynamic strain aging, and this led to the establishment of another project. Mechanical test data obtained at McMaster University served as the basis of an assessment of the applicability of Bazinski’s “stress equivalence” theory of solute strengthening to polycrystalline alloys of Mg. Although we did not succeed in applying the approach to Mg alloys, we did develop expertise with the HEXRD approach using a BCC, β-Ti alloy and demonstrated numerous new capabilities that may be applied to any polycrystalline material in collaboration with researchers at CHESS and around the world: (1) assessment of details of the elastoplastic transition (yielding) using a combination of HEXRD and full-field polycrystal plasticity modeling, (2) the first-ever experimental observation of strong stress rotation within the individual grains of a polycrystalline material, and (3) a comprehensive analysis of the grain-level dislocation density evolution based upon diffraction peak broadening along 𝜂𝜂,𝜔𝜔,and 2𝜃𝜃 directions. This final aspect allowed us to confirm that dislocations were gliding on multiple plane types and not restricted to {110} type planes, and it also provided clues as to why some grains were unloading during straining, with surprising implications for our understanding of the effects of geometrically necessary dislocations (GNDs). Finally, graduate student, Mohammed Shabana, developed a MATLAB code which confirmed the conclusions of Prof. Catalin Picu (Rensallear Polytechnic Institute, RPI) regarding the effect of solute-trapped, forest dislocations on the breaking stress of Lomer lock junctions in FCC metal alloys. He applied the same anisotropic line-tension model to a variety of dislocation junction configurations and found an inconsistency in the widely cited results of Dupuy and Fivel regarding the Hirth Lock, and he outlined an approach to extend these finding to HCP Mg alloys that we are still pursuing with discretionary fundings at UVA.

36 MATERIALS SCIENCE↗