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At least 613 records · Page 34
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Materials Characterization, Prediction, and Control Project: Characterization of 316L Stainless Steel after Solid Phase Processing using Ultrasonic NDE Method

The Pacific Northwest National Laboratory undertook the Materials Characterization, Prediction, and Control Laboratory Directed Research and Development Project to advance understanding of nuclear material processing and enable multifold acceleration in the development and qualification of new material systems produced via advanced manufacturing methods, such as solid phase processing, for use in national security and advanced energy applications (Smith 2021). A motivation of the Materials Characterization, Prediction, and Control Project was to demonstrate ultrasonic testing as a nondestructive evaluation method to complement traditional destructive methods for characterizing material microstructure with emphasis on grain size determination using a method that may have future applications for real-time inline process monitoring. The objective of the work described in this report is to establish the process and an analysis method for measuring grain sizes of polycrystalline metals with ultrafine grains using ultrasonic shear wave backscattering, building on prior studies on coarser-grained material. The work involves five tasks: Measured ultrasonic backscattering experimentally for a series of 316L stainless steel specimens with various grain sizes made by friction stir processing. Calculated ultrasonic backscattering coefficients from experimental data based on a physical measurement model. Measured ground truth grain sizes of the specimens from electron backscatter diffraction grain boundary images using a generalization of the ASTM E112 (ASTM 2021) intercept method. Built a curve of ultrasonic backscattering coefficients versus the ground truth intercept-based grain sizes to determine the correlation between mean grain sizes and ultrasonic measurements. Demonstrated the ability of using the correlation curve to deduce grain sizes with measured ultrasonic backscattering coefficients for a few 316L stainless steel specimens whose grain sizes were unknown beforehand but were targeted to be an extrapolation to larger grain sizes than used to formulate the correlation curves. Experimental procedures and computational algorithms are developed and validated for these tasks. This work establishes an ultrasonic technique for characterizing material microstructure with ultrafine grains that are often resulted by solid-phase processing. The technique is nondestructive, and it has the potential to be used for real time inline process monitoring. This work successfully demonstrates the viability of an ultrasonic nondestructive evaluation method for microstructural characterization of material having ultrafine grain structure (as small as 1?mm) and produced by an advanced manufacturing method. This includes a demonstration of the method to extrapolate to other conditions. While not demonstrated here, the method is expected to be viable for in-line, or near-inline, process monitoring in advanced manufacturing applications with suitable consideration for access of instrumentation to the material being manufactured.

316 L Stainless Steel↗
NASA NTRS1991

Advanced composite applications for sub-micron biologically derived microstructures

A major thrust of advanced material development is in the area of self-assembled ultra-fine particulate based composites (micro-composites). The application of biologically derived, self-assembled microstructures to form advanced composite materials is discussed. Hollow 0.5 micron diameter cylindrical shaped microcylinders self-assemble from diacetylenic lipids. These microstructures have a multiplicity of potential applications in the material sciences. Exploratory development is proceeding in application areas such as controlled release for drug delivery, wound repair, and biofouling as well as composites for electronic and magnetic applications, and high power microwave cathodes.

Schnur, J. M.↗
DOE OSTI2020

Build Orientation Dependent Microstructure in Polymer Laser Sintering: Relationship to Part Performance and Evolution with Aging

Laser sintering (LS) is widely used to produce functional polymeric parts; however, the resulting parts are often limited by their porous structure, and performance of the part may be strongly anisotropic. Relating the structural features of parts to build process conditions or powder feedstock has been explored previously. In contrast, little is known regarding how the unique internal structures of LS parts evolve and relate to their performance later in their life cycle, for example, after use in a real-world operating environment. In this study, a tightly controlled LS build process and measurement campaign by standard X-ray computed tomography (XCT), supported by high-resolution synchrotron XCT, was used to benchmark the internal microstructure (e.g. porosity) as a function of four different build orientations in printed polyamide-12 (PA-12) parts. The initial performance of the parts after printing was characterized by tensile testing and dynamic mechanical analysis (DMA). Arrays of PA-12 parts in different build orientations were exposed to steam (under pressure) and air across multiple temperature and time points for the purposes of accelerated aging through oxidative and hydrolytic breakdown. Exposing parts to steam dramatically altered the internal microstructure and functional properties such as the glass transition temperature, tensile properties, and damping behavior. Notably, post-aging XCT revealed large microstructural changes after only 40 h of steam treatment relative to the as-printed specimens. Furthermore, pore reorganization and changes in crystallinity occurred regardless of whether the steam temperature was aggressive enough to induce a significant loss in mechanical properties. The build orientation dependence on the aging rate was minimal with the relative trend in performance persisting across most metrics among the different orientations even after aging.

36 MATERIALS SCIENCE↗
DOE OSTI2020

In-field critical current and pinning mechanisms at 4.2 K of Zr-added REBCO coated conductors

The critical current and pinning mechanisms at 4.2 K have been studied over a magnetic field range of 0–14 T for Zr-added (0, 5 and 15 mol.%) REBa 2 Cu 3 O 7-x (REBCO and RE = rare earth) coated conductors fabricated by advanced metal organic chemical vapor deposition (A-MOCVD). It is found that the (Ba + Zr)/Cu content in Zr-added (5 and 15 mol.%) REBCO affects the critical current at 77 K, 0 T as well as density, continuity and shape of BaZrO 3 (BZO) self-assembled nanocolumns and RE 2 O 3 in-plane precipitates that significantly enhance the pinning force density Fp(H) as well as isotropic pinning landscape at 4.2 K. In addition to bell-shape dependence of critical current density, J c , at 4.2 K with (Ba + Zr)/Cu content we observed an unusual Fp(H) behavior correlated to particular type of pinning centers, morphology and distribution that have been revealed by TEM microstructure analysis. By fitting the Dew–Hughes equation of the pinning force density Fp(H) at 4.2 K we extract the scaling behaviors of the Fp(H) associated with the competition of pinning mechanisms driven by vertically-aligned BZO nanorods and in-plane RE 2 O 3 pinning defects. This result sheds light on approaches towards interactive control of strong and isotropic pinning centers in Zr-added REBa 2 Cu 3 O 7-x (REBCO and RE = rare earth) coated conductors, and especially understanding the correlation between microstructural characteristics and vortex pinning mechanisms at 4.2 K in high magnetic fields.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2026

Model Parameter Development for Complex Materials: Species-Specific Diffusion Barriers in 316 Stainless Steel from Systematic DFT Calculations

Vacancy-mediated diffusion barriers in 316 stainless steel have been systematically calculated using density functional theory to provide essential parameters for mesoscale microstructure evolution models. A statistical sampling approach employing 210 nudged elastic band calculations across multiple special quasi-random structures captures the effects of local chemical environments in this concentrated alloy. The computational methodology addresses challenges specific to chemically disordered systems, including proper magnetic treatment throughout multi-step calculations and validation against experimental structural properties. The calculated activation barriers reveal clear species-dependent diffusion behavior with the hierarchy Ni >> Fe ˜ Cr >> Mo. Nickel exhibits the highest barriers (0.74–1.31 eV, mean 1.045 eV), confirming its role as the slowest-diffusing major component. Iron and chromium show similar moderate barriers averaging 0.587 eV and 0.522 eV, respectively. Remarkably, molybdenum demonstrates exceptionally low barriers (0.12–0.28 eV, mean 0.194 eV), suggesting much higher mobility than previously recognized and potentially significant implications for precipitation kinetics and microstructure evolution. The barrier ranges remain consistent across different 316 SS compositions, supporting parameter transferability for modeling applications. The overall mean barrier of 0.64 eV provides a practical approximation for phase field simulations, while species-specific values enable detailed treatments of diffusion-controlled processes. This systematic approach establishes a validated framework for generating diffusion parameters in other concentrated alloys where experimental data are limited, while providing the first systematic set of species-specific barriers for predictive modeling of 316 stainless steel microstructure evolution.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Rationalization of the tensile creep behavior of the Nb45Ta25Ti15Hf15 bcc refractory complex concentrated alloy using Rao-Suzuki screw dislocation glide model

Published experimental tensile creep data for refractory body-centered cubic alloy Nb45Ta25Ti15Hf15 (NTTH) at temperatures ranging from 850–950 °C and applied tensile stresses 50–300 MPa are analyzed using the Rao-Suzuki screw dislocation glide model of solid solution strengthening. It is shown that the experimental creep data as well as transmission electron microscopy observations of post- creep deformation dislocation microstructure are in agreement with the model results. This suggests that the creep deformation of NTTH at 850–950 °C is controlled by screw dislocation glide.

Rao, Satish I↗
NASA NTRS1981

Fracture and failure: Analyses, mechanisms and applications; Proceedings of the Symposium, Los Angeles, CA, March 17-20, 1980

Papers are presented on the application of fracture mechanics to spacecraft design, fracture control applications on the Space Shuttle reaction control thrusters, and an assessment of fatigue crack growth rate relationships for metallic airframe materials. Also considered are fracture mechanisms and microstructural relationships in Ni-base alloy systems, the use of surface deformation markings to determine crack propagation directions, case histories of metallurgical failures in the electronics industry, and a failure analysis of silica phenolic nozzle liners.

Tung, P. P.↗
NASA NTRS1999

Third and Final Shuttle Mission of the Isothermal Dendritic Growth Experiment Conducted: Highest Supercooling Ever Recorded Achieved

Dendrites describe the treelike crystal morphology commonly assumed in metals and alloys that freeze from supercooled or supersaturated melts. There remains a high level of engineering interest in dendritic solidification because the size, shape, and orientation of the dendrites determine the final microstructure of a material. It is the microstructure that then determines the physical properties of cast or welded products. Although it is well known that dendritic growth is controlled by the transport of latent heat from the moving solid-liquid interface, an accurate and predictive model has not yet been developed. The effects of gravity-induced convection on the transfer of heat from the interface have prevented adequate testing, under terrestrial conditions, of solidification models. The Isothermal Dendritic Growth Experiment (IDGE) constituted a series of three microgravity experiments flown aboard the Space Shuttle Columbia. The apparatus was used to grow and record dendrite solidification in the absence of gravity-induced convective heat transfer, thereby producing a wealth of benchmark-quality data for testing solidification models and theories.

Glicksman, Martin E.↗
NASA NTRS2006

Further Investigations of High Temperature Knitted Spring Tubes for Advanced Control Surface Seal Applications

Knitted metallic spring tubes are the structural backbones that provide resiliency in control surface seals for use on current and future reusable space launch vehicles. Control surface seals fill the space between movable control surfaces such as body flaps, rudders and elevons, and the static body structures to which they are attached. These seals must remain in continuous contact with opposing surfaces to prevent the ingestion of damaging hot gases encountered during atmospheric re-entry. The Inconel X-750 (Special Metals Corporation) spring tube utilized in the baseline control surface seal shows significant resiliency loss when compressed at temperatures as low as 1200 F. High temperature compression testing and microstructural analysis show that creep is the dominant deformation mechanism leading to permanent set and resiliency loss in tested spring tube samples. Additional evaluation using a structured design of experiments approach shows that spring tube performance, primarily high temperature resiliency, can be enhanced through material substitution of Rene 41 (Allvac) alloy (for the baseline Inconel X-750 material) when coupled with specialized thermal processing.

Taylor, Shawn C.↗
DOE OSTI2025

Deuterium trapping mechanisms in reduced activation ferritic martensitic steels and their correlation with mechanical strengthening

Development of high-strength materials often involves introduction of additional strengthening microstructures that also serve as tritium trapping sites. Such additions in fusion material development could degrade the fuel efficiency in fusion reactors and raise radiological concerns. The contribution of individual microstructure features in hydrogen trapping must be evaluated to ensure fuel efficiency and radiological safety. This study explores the mechanistic origins of deuterium trapping in reduced-activation ferritic–martensitic steels and its correlation to mechanical strengthening. A series of model alloys and engineering steels were fabricated and subjected to different heat treatments to control deuterium trapping site density. Deuterium retention was evaluated using D 2 gas charging and thermal desorption spectroscopy, focusing on the role of grain boundary, dislocation, M 23 C 6 precipitates, and TiC precipitates. Multiscale microstructure characterization and synchrotron X-ray diffraction were performed to characterize microstructure, which was correlated to the deuterium retention property. Results show that TiC precipitates exhibit the highest deuterium trapping capacity, followed by M 23 C 6 precipitates. Dislocation and grain boundary demonstrate the lowest and similar efficiencies. Furthermore, the relationship of trapping quantity and mechanical strengthening of these microstructure features was quantified, demonstrating that TiC precipitates offer highest deuterium trapping per unit of mechanical strengthening.

Retention↗
NASA NTRS2014

Robust Informatics Infrastructure Required For ICME: Combining Virtual and Experimental Data

With the increased emphasis on reducing the cost and time to market of new materials, the need for robust automated materials information management system(s) enabling sophisticated data mining tools is increasing, as evidenced by the emphasis on Integrated Computational Materials Engineering (ICME) and the recent establishment of the Materials Genome Initiative (MGI). This need is also fueled by the demands for higher efficiency in material testing; consistency, quality and traceability of data; product design; engineering analysis; as well as control of access to proprietary or sensitive information. Further, the use of increasingly sophisticated nonlinear, anisotropic and or multi-scale models requires both the processing of large volumes of test data and complex materials data necessary to establish processing-microstructure-property-performance relationships. Fortunately, material information management systems have kept pace with the growing user demands and evolved to enable: (i) the capture of both point wise data and full spectra of raw data curves, (ii) data management functions such as access, version, and quality controls;(iii) a wide range of data import, export and analysis capabilities; (iv) data pedigree traceability mechanisms; (v) data searching, reporting and viewing tools; and (vi) access to the information via a wide range of interfaces. This paper discusses key principles for the development of a robust materials information management system to enable the connections at various length scales to be made between experimental data and corresponding multiscale modeling toolsets to enable ICME. In particular, NASA Glenn's efforts towards establishing such a database for capturing constitutive modeling behavior for both monolithic and composites materials

Mutli-scale models↗
NASA NTRS1984

Changes in solidified microstructures

The properties and casting behavior of metals are significantly affected by their cast structure. This structure is optimized by producing columnar versus equiaxed grains and coarse versus fine grains by controlling solidification conditions. The transition from columnar to equiaxed grains is favored by: constitutional supercooling with effective nucleation of free dendrites; melting off and transport of dendrite tips and arms; mechanical vibration; falling down of free dendrites from a chilled top surface; and induced flow in the solidifying structure by oscillation of rotation.

Wallace, J. F.↗
NASA NTRS2012

Controlled Directional Solidification of Aluminum - 7 wt Percent Silicon Alloys: Comparison Between Samples Processed on Earth and in the Microgravity Environment Aboard the International Space Station

An overview of the international "MIcrostructure Formation in CASTing of Technical Alloys" (MICAST) program is given. Directional solidification processing of metals and alloys is described, and why experiments conducted in the microgravity environment aboard the International Space Station (ISS) are expected to promote our understanding of this commercially relevant practice. Microstructural differences observed when comparing the aluminum - 7 wt% silicon alloys directionally solidified on Earth to those aboard the ISS are presented and discussed.

Grugel, Richard N.↗
NASA NTRS2003

Minimizing Segregation during the Controlled Directional Solidification of Dendric Alloys

Gravity-driven convection induced in the liquid by density gradients of temperature or composition disrupts uniform dendritic growth during controlled directional solidification and promotes severe macrosegregation. The solute-rich region about the dendrite tip appears to play a pivotal role in channel initiation. Allen and Hunt referred to this region as an "initial transient" or dynamic region constituting steep concentration gradients. Experimental investigation also point to the role the tip region plays in developing microstructure. Hellawell and co-workers showed that flow-through dendritic channels could be effectively disrupted, and segregation minimized, during the gradient freezing of bulk castings by rotating the melt through a slight angle with respect to Earth's gravity vector. Adapting this principle to controlled directional solidification, it has been shown" that segregation in dendritic alloys can be minimized, and properties improved, by processing the sample near horizontal in conjunction with a slow axial rotation of the crucible. It is postulated that the observed microstructural uniformity arises by maintaining the developing solute field about the dendrite tip. Solute rejected during vertical directional solidification will rise or sink parallel to the primary dendrite arms during axial rotation setting the stage for accumulation, instabilities, and segregation. In contrast, during horizontal growth, the rejected solute will sink or rise perpendicular to the primary dendrite. Now, in the presence of a slight axial rotation, solute that was initially sinking (or rising) will find itself above (or below) its parent dendrite, i.e., still about the tip region. The following is intended to experimentally demonstrate the viability of this concept in coordination with a model that gives predictive insight regarding solute distribution about growing dendrites. Alloys based on the lead-tin eutectic system were used in this study. The system is well characterized, the constituent metals are available in a very pure form, and the thermophysical properties are well known. During solidification of hypoeutectic alloys, e.g., 55 wt pct Pb, the primary dendrites reject the less dense tin, and for the hypereutectic alloys, e.g., 75 wt pct Sn, the primary dendrites reject denser lead. Alloys were prepared by melting appropriate amounts of lead and tin in a glass crucible after which the homogeneous liquid was sucked directly into 5-mm i.d. glass tubes. The sample tube, containing approximately 30 cm of alloy, was then mechanically driven into the directional solidification furnace assembly and positioned such that approx. 20 cm of the sample was remelted. Subsequently, directional solidification was initiated by withdrawing the sample through a water-cooled jacket at a constant growth velocity of 2 ,microns/s. After 5 to 6 cm of growth, the sample was quickly removed from the furnace and quenched in a water bath to preserve the solid-liquid interface. Samples were directionally solidified vertically upward, nearly horizontally, and some in conjunction with an applied axial rotation of the crucible. Temperature gradients at the solid-liquid interface were measured with an in-siru K-type thermocouple. Solidified samples were cut perpendicular and parallel to the growth direction and conventionally prepared for microscopic examination.

Grugel, Richard N.↗
DOE OSTI2026

Correlation between microstructure and residual stress formation in friction stir welded armor steels characterized by neutron diffraction

Friction stir welding (FSW) is a solid-state joining process that minimizes the heat-affected zone (HAZ) compared with fusion-based arc welding, making it well suited for joining martensitic armor steels where hardness and ballistic resistance are critical. This study investigates residual stress formation in three defect-free FSW butt-joint configurations relevant to armored-vehicle fabrication: similar rolled homogeneous armor (RHA–RHA, Case 1), similar high-hardness armor (HHA–HHA, Case 2), and dissimilar HHA–RHA (Case 3) joints produced under temperature-controlled conditions (770 °C). Neutron diffraction was employed to quantify the magnitude and spatial distribution of residual stresses in the longitudinal, transverse, and normal directions and to correlate them with weld microstructure and hardness. Tensile residual stresses were concentrated in the softened HAZ, reaching approximately 300 MPa for Case 2 and 400 MPa for Case 1 (≈50–70 % of the base-metal yield strength; ∼581 MPa for RHA and ∼566 MPa for HHA), while compressive residual stresses dominated the stir zone. The spatial extent of tensile stresses scaled with the width of the softened HAZ, which was largest in the dissimilar HHA–RHA joint and smallest in the HHA–HHA joint. Full-width-at-half-maximum (FWHM) analysis revealed low microstrain in overtempered HAZ regions and high microstrain in the stir zone associated with severe plastic deformation and fresh martensite formation. This work demonstrates that residual stress evolution in FSW of martensitic armor steels is governed not primarily by peak temperature or thermal contraction, as inferred from fusion-welding analogies, but by the competition between transformation-induced volumetric expansion and tempering-induced stress relaxation. The relative dominance of these mechanisms is shown to depend on alloy hardenability and local thermal history, leading to more extensive HAZ softening and broader tensile stress regions in the lower-hardenability RHA steel. These findings establish a transferable mechanistic framework for optimizing solid-state joining strategies in high-strength steels and other transformation-hardening alloys beyond armor applications.

Friction stir welding↗
DOE OSTI2021

Role of scan strategies and heat treatment on grain structure evolution in Fe-Si soft magnetic alloys made by laser-powder bed fusion

A major goal in printing soft magnetic Fe-Si steels using additive manufacturing is to take advantage of the potential for complex geometric designs and site-specific grain control. One major step in the processing of these alloys is understanding how processing parameters might impact how the as-built microstructure responds to annealing (i.e. the annealing response). The impact of scan strategy on the annealing response for thin wall geometries is specifically explored. Two scan strategies were explored for a thin wall geometry that produced a strongly columnar grain structure and equiaxed grain structure. Additionally, samples from both scan strategies annealed at 1200 °C showed a marked difference in annealing response with the more equiaxed sample seeing full recrystallization and grain growth, while the more columnar grain structure saw little change in microstructure. After analysis through characterization techniques and thermal-mechanical simulations Differences in internal energy within the grains were ruled out because calculated GND density values were similar for both samples. The formation of secondary particles was ruled out as a contributing factor due to the type of oxide formations and their size. It was concluded that the contributing factor to the difference in the annealing response were a difference in the resulting grain size and the density of high angle grain boundaries. These two differences were largely attributed to differences in the thermal gradient conditions due to grains preferentially growing in the direction of the steepest thermal gradient.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Hybrid additive manufacturing of AISI 316L via asynchronous powder and hot-wire laser directed energy deposition

Hybrid Additive Manufacturing (AM) offers a way to leverage the advantages of different AM technologies, enabling the efficient production of sizeable parts without compromising material properties or geometric complexity capabilities. This study presents an asynchronous hybrid Directed Energy Deposition (DED) strategy employing laser powder DED and laser hot-wire DED. AISI 316L parts comprising multiple powder and wire segments were fabricated with optional machining on AISI 316L substrates to investigate how quality is impacted by (i) alternative process sequences (laser powder DED followed by laser hot-wire DED and vice versa), (ii) machined vs. as-printed interfacial conditions, and (iii) material deposition on top vs. alongside previously built segments. Optical microscopy, X-ray computed tomography, and Vickers hardness were used to characterize the morphology and microstructure of the parts, localized porosity and lack of fusion defects, bulk density, and mechanical properties. Interfacial machining was necessary for dimensional control but promoted lack of fusion voids, resulting in a 99.71 ± 0.01% dense part. As-printed interfaces resulted in a denser part (99.82 ± 0.02%) at the expense of dimensional accuracy. The hardness of the parts with as-printed and machined interfaces was 196 ± 0.37 HV and 192 ± 0.40 HV, respectively, compared to 156 ± 1.4 HV for the substrate. Depositing powder alongside or on top of wire sections resulted in interfaces with a hardness of 217 ± 2.2 HV, compared to 185 ± 3.4 HV for the wire-powder interfaces.

36 MATERIALS SCIENCE↗
DOE OSTI2021

A constitutive model for glass–ceramic materials

Glass–ceramics have received recent attention for use in glass–ceramic to metal hermetic seals. Due to their heterogeneous microstructure, these materials exhibit a number of advantageous responses over conventional glass based seals. Key amongst them is the possibility of a controllable thermal strain response and apparent coefficient of thermal expansion which may be used to minimize thermally induced residual stresses for aforementioned seals. Furthermore, these behaviors result from an inorganic glass matrix and variety of crystalline ceramic phases including silica polymorph(s) that may undergo reversible solid-to-solid transformations with associated inelastic strain. Correspondingly, these materials exhibit complex thermomechanical responses associated with multiple inelastic mechanisms (viscoelasticity and phase transformation). While modeling these behaviors is essential for developing and analyzing the corresponding applications, no such model exists. Therefore, in this work a three-dimensional continuum constitutive model for glass–ceramic materials combining these various inelastic mechanisms is developed via an internal state variable approach. A corresponding fully implicit three dimensional numerical formulation is also proposed and implemented. The model is used to simulate existing experiments and validate the proposed formalism. As an example, the simple seal problem of a glass–ceramic seal inside a concentric metal shell is explored. Finally, the impact of the cooling rates, viscoelastic shift factors, and inelastic strain on final residual stress state are all investigated and the differing contributions highlighted.

36 MATERIALS SCIENCE↗