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At least 325 records · Page 18

Solidification processing of alloys using an applied electric field

A method is provided for obtaining an alloy having an ordered microstructure which comprises the steps of heating the central portion of the alloy under uniform temperature so that it enters a liquid phase while the outer portions remain solid, applying a constant electric current through the alloy during the heating step, and solidifying the liquid central portion of the alloy by subjecting it to a temperature-gradient zone so that cooling occurs in a directional manner and at a given rate of speed while maintaining the application of the constant electric current through the alloy. The method of the present invention produces an alloy having superior characteristics such as reduced segregation. After subsequent precipitation by heat-treatment, the alloys produced by the present invention will have excellent strength and high-temperature resistance.

Mckannan, Eugene C.↗

Directional solidification processing of alloys using an applied electric field

A method is provided for obtaining an alloy having an ordered microstructure which comprises the steps of heating the central portion of the alloy under uniform temperature so that it enters a liquid phase while the outer portions remain solid, applying a constant electric current through the alloy during the heating step, and solidifying the liquid central portion of the alloy by subjecting it to a temperature-gradient zone so that cooling occurs in a directional manner and at a given rate of speed while maintaining the application of the constant electric current through the alloy. The method is particularly suitable for use with nickel-based superalloys. The method of the present invention produces an alloy having superior characteristics such as reduced segregation. After subsequent precipitation by heat-treatment, the alloys produced by the present invention will have excellent strength and high-temperature resistance.

McKannan, Eugene C.↗

Shining light on nanoscale ‘vine-on-stick’ eutectic structures in the Al-Ce-Ni system

Multiphase eutectics often comprise entangled solid phases with nanoscale periodicity, making it difficult to unravel their 3D connectivity using conventional 2D techniques. Among such systems, the three-phase eutectic Al-Al 11 Ce 3 -Al 3 Ni stands out for its ultrafine (∼100 nm) interphase spacing and promising creep resistance, yet its microstructure remains relatively unexplored despite its potential for high-temperature applications. Here, we use scanning hard X-ray microscopy with an unprecedented ∼10 nm pixel size to resolve its 3D morphology. Reconstructions reveal a novel “vine-on-stick” motif, wherein Al 11 Ce 3 wraps around Al 3 Ni pillars. Analysis of phase tortuosities confirms that Al 11 Ce 3 exhibits more convoluted morphologies than Al 3 Ni. No orientation relationship was observed between the two intermetallics, suggesting that growth is controlled by local solute gradients rather than epitaxy. Fragmentation of intermetallics along their longitudinal axis suggests a Rayleigh-type breakup mechanism in solid state. The “vine-on-stick” pattern may generalize to other alloy systems with variable interfacial anisotropies and low mutual solubilities.

36 MATERIALS SCIENCE↗

Accelerated creep profiling: a high-throughput thermal- and stress-gradient approach applied to additive and wrought stainless steel

Here, this study investigates logarithmic creep behavior at temperatures near room temperature in wrought and additively manufactured (AM) 316 L austenitic stainless steel. A novel high-throughput (HiTp) methodology employed thermal gradients to obtain stress- and temperature-dependence of creep behavior. The findings, based on 104 two-week creep tests, reveal significant differences in creep response between wrought and AM materials. Compared to the wrought material, the AM material exhibited a higher activation energy and a lower activation volume. These differences were attributed to the materials’ distinct microstructural features, e.g., dislocation cell structures and precipitate distributions, which alter the susceptibility to dislocation glide creep, particularly at stresses below the yield stress. The HiTp methodology provides both an accelerated determination of low-temperature creep mechanisms, offering critical data for the design and optimization of alloys in near-ambient, high stress applications.

316 L Stainless steel↗

Microstructural and micromechanical characteristics of ultra-high performance concrete with superabsorbent polymer (SAP)

In this study, the hydration product, C-S-H density, and pore structure at different layers from the drying surface were measured. Besides, the zone affected by the released internal curing water from SAP was identified by assessing the nanoindentation modulus. The results found that the SAP affected the moisture distribution and changed the evaporation and self-desiccation rates in the inner and outer layers. Such imposed moisture gradients affected the micromechanical properties of UHPC at different layers due to the change in the hydration degree of the binder, the density of C-S-H, and the pore structure of the matrix. The addition of SAP improved the hydration dynamics and transferred the LD C-S-H into HD or UHD C-S-H. As the distance from the drying surface increased, the affected zone of SAP increased from 60 to 120 μm, showing the more effectiveness of SAP at inner layers.

36 MATERIALS SCIENCE↗

Thermophysical and Thermomechanical Properties of Thermal Barrier Coating Systems

Thermal barrier coatings have been developed for advanced gas turbine and diesel engine applications to improve engine reliability and fuel efficiency. However, the issue of coating durability under high temperature cyclic conditions is still of major concern. The coating failure is closely related to thermal stresses and oxidation in the coating systems. Coating shrinkage cracking resulting from ceramic sintering and creep at high temperatures can further accelerate the coating failure process. The purpose of this paper is to address critical issues such as ceramic sintering and creep, thermal fatigue and their relevance to coating life prediction. Novel test approaches have been established to obtain critical thermophysical and thermomechanical properties of the coating systems under near-realistic temperature and stress gradients encountered in advanced engine systems. Emphasis is placed on the dynamic changes of the coating thermal conductivity and elastic modulus, fatigue and creep interactions, and resulting failure mechanisms during the simulated engine tests. Detailed experimental and modeling results describing processes occurring in the thermal barrier coating systems provide a framework for developing strategies to manage ceramic coating architecture, microstructure and properties.

Zhu, Dongming↗

Synthesis of bulk reactive Ni–Al composites using high pressure torsion

Self-propagating exothermic reactions, for instance in the nickel-aluminum (Ni-Al) system, have been widely studied to create high performance intermetallic compounds or for in-situ welding. Their easy ignition once the phase spacing is reduced below the micron scale, makes top-down methods like high-energy ball milling, ideal to fabricate such reactive nanostructures. A major drawback of ball milling is the need of a sintering step to form bulk pieces of the reactive material. However, this is not possible, as the targeted reactions would already proceed. Therefore, we investigate the ability of high pressure torsion as an alternative process, capable to produce bulk nanocomposites from powder mixtures. Severe straining of powder mixtures with a composition of 50 wt% Ni and 50 wt% Al enables fabrication of self-reactive bulk samples with microstructures similar to those obtained from ball milling or magnetron sputtering. Additionally, samples deformed at ambient temperature are highly reactive and can be ignited significantly below the Al melting point, finally predominantly consisting of Al 3 Ni 2 and Al 3 Ni, independent of the applied strain. Although the reaction proceeds first at the edge of the disk, the strain gradient present in the disks does not prevent reaction of the whole sample.

36 MATERIALS SCIENCE↗

Less can be more: Insights on the role of electrode microstructure in redox flow batteries from two-dimensional direct numerical simulations

Understanding how to structure a porous electrode to facilitate fluid, mass, and charge transport is key to enhancing the performance of electrochemical devices, such as fuel cells, electrolyzers, and redox flow batteries (RFBs). Here, using a parallel computational framework, direct numerical simulations are carried out on idealized porous electrode microstructures for RFBs. Strategies to improve an electrode design starting from a regular lattice are explored. By introducing vacancies in the ordered arrangement, it is possible to achieve higher voltage efficiency at a given current density, thanks to improved mixing of reactive species, despite reducing the total reactive surface. Careful engineering of the location of vacancies, resulting in a density gradient, outperforms disordered configurations. Our simulation framework is a new tool to explore transport phenomena in RFBs, and our findings suggest new ways to design performant electrodes.

25 ENERGY STORAGE↗

Effect of thermal cycling in a Mach 0.3 burner rig on properties and structure of directionally solidified gamma/gamma prime-delta eutectic

An experimental study was carried out to evaluate the effect of cyclic thermal exposures on the mechanical properties of a gamma/gamma prime-delta eutectic alloy parallel to the growth direction. The alloy had a nominal composition by weight of Ni-20 Nb-6 Cr-2.5 Al and was directionally solidified at 3 cm/hr in a furnace with a thermal gradient of at least 200 C/cm. Bars of the alloy were exposed in a Mach 0.3 burner rig and cycled 300 times between 1100 and 425 C. Oxidation-erosion characteristics of the alloy were determined by weight loss measurements at 300-cycle intervals. After cyclic exposure, stress rupture and tensile tests were performed at both 760 and 1040 C. Microstructural changes from cyclic exposure were determined. Thermal cycling resulted in gamma prime coarsening and Widmanstaetten delta precipitation in the gamma phase. An unidentified precipitate, presumably gamma prime, was observed within the delta phase. These microstructural changes did not affect the mechanical properties of the eutectic. High oxidation-erosion weight loss rate was observed.

Gray, H. R.↗

Directional solidification of alloys in systems containing a liquid miscibility gap

The problem considered is the unidirectional growth of alloys close to monotectic composition and within the miscibility gap when the direction of gravity is down the temperature gradient (solidification upwards) or up the temperature gradient (solidification downwards). The systems Al-In and Al-Bi are taken as examples. With solidification upwards it is shown that bulk liquid composition adjusts to that of the monotectic while in the reverse situation, the bulk liquid gradually rises. In the former case it is possible to grow aligned fibrous structures of monotectic composition but in the latter the microstructures are irregular and globular.

Grugel, R. N.↗

USE OF TWO-PISTON SPLAT QUENCHING TO INVESTIGATE & CHARACTERIZE THE IMPACT OF COMPOSITIONAL VARIATIONS ON RAPID SOLIDIFICATION MICROSTRUCTURES & SUB-MICROSCALE FEATURES IN STAINLESS STEEL ALLOY.

The objective of this dissertation was to use two-piston splat quenching (SQ) to investigate the impact of compositional modifications on the solidification and microstructure of rapidly solidified austenitic stainless steels (SS) and to demonstrate the ability of SQ to quickly and effectively simulate rapid solidification conditions similar to those found in powder bed fusion (PBF) additive techniques. PBF techniques like laser powder bed fusion (LPBF) are being implemented across a breadth of research and industrial applications to create parts with complex geometries and performance capabilities while pushing the current limits of processing conditions and understanding of material systems. In this work, SQ was used to experimentally produce rapid solidification in 20+ unique austenitic SS compositions with systematic variations of the chrome and nickel equivalency ratio (Cr/Nieq) through targeted compositional modifications. From the targeted change of Cr, Ni, and Mo concentrations in rapidly solidified SS alloys, the ferrite solidification mode was found to be the primary solidification mode at significantly lower Cr/Nieq than previously predicted for RS. Also, decreasing concentrations of Fe at a constant Cr/Nieq ratio (i.e., different Fe isopleths), or increased Mo concentrations at a constant Cr/Nieq ratio were found to suppress the ferrite to austenite massive transformation when compared to alloys with lower concentrations at the same Cr/Nieq. Using an established empirical relationship between cell size and cooling rate, the SQ technique was estimated to produce cooling rates between 106 and 108 K/s. Thermal gradients were extracted from 2-D heat transfer simulations of the SQ solidification event and used with these cooling rates to produce solidification rate estimates for SQ which were between 0.4-1.6m/s. The primary solidification mode was observed to be the determining factor in which elements segregated to the cell boundaries during RS, for which Cr and Mo were the main elements to segregate during primary austenite solidification and Ni during primary ferrite solidification. Finally, the solidification rates and conditions produced by SQ experiments resulted in similar microstructures, features, and microsegregation to what was found in LPBF samples of the same feedstock.

Hasenbusch, Zachary↗

The metallic microstructures and thermal histories of severely reheated chondrites

The metallographic structures of eight severely reheated chondrites - Farmington, Ramsdorf, Orvinio, Wickenburg, Lubbock, Rose City, Arapahoe, and Tadjera - were studied using optical, SEM and electron microprobe techniques. The following metallographic criteria were used to estimate the post-shock residual temperature of the chondrites: melted metal-troilite appearance, presence of martensite, phosphorus enrichment of metal and averaging of central metal grain compositions. The presence of phosphides and secondary kamacite are due to slow post-shock cooling rates. Ni rim gradients indicate both extensive remelting of metal grains and relatively fast cooling.

Smith, B. A.↗

Report on the Integration of Experimental and Modeling Data for Initial Equivalence Study of Mechanical Performance in Irradiated LPBF 316 Stainless Steel

To ensure the rapid development, deployment, and use of advanced nuclear technologies, faster qualification approaches are needed. Typically, the primary pathway uses traditional data packages consistent with the American Society of Mechanical Engineers Boiler and Pressure Vessel Code, which does not consider the environmental effects the material will experience such as corrosion and radiation damage. Examining radiation effects requires a significant amount of space in US facilities at the Advanced Test Reactor and the High Flux Isotope Reactor (HFIR) and suffers from natural gradients in temperature and neutron flux profiles. Ion irradiation may enable rapid assessment of radiation-induced damage to a material and is proposed as part of an accelerated materials qualification framework through the Advanced Materials and Manufacturing Technologies program. To enhance the utility of ion irradiation as an examination tool, this report provides the initial assessment of engineering-relevant properties of microstructures produced from ion irradiation in the near-surface volume. Nanoindentation, Vickers hardness, and known tensile properties were brought together with simple mathematical models and experimental data for an initial equivalence study of the mechanical performance of irradiated laser powder bed fusion (LPBF) 316 stainless steels across length scales. Direct observation of the calculated ion irradiation yield stress and measured neutron irradiation yield stress at 2 dpa showed that both datasets exhibit the same trend with irradiation temperature and overlap within an acceptable band of stress values. Ion irradiations at 10 dpa serve as a prediction of properties to compare to postirradiation examination of HFIR-irradiated LPBF 316H further in the program. This work is a significant demonstration of the Licensing Approach with Ions and Neutrons, which uses ion irradiations to generate mechanical property information more rapidly than through neutron irradiations.

36 MATERIALS SCIENCE↗

Microstructural evaluation of thin-wall sections of 316L stainless steel produced by laser powder-bed fusion processing

The synthesis of thin wall sections that are only 0.4 mm thick is achieved with LPBF AM. Sample preparation is optimized using metallographic polishing to produce samples with only 0.3 um rms roughness for scanning electron microanalysis with EBSD and EDS. A fully austenitic 316L phase is found without evidence of secondary phases. Unlike some AM products that can readily evidence composition segregation due to solute rejection as attributable to temperature gradients within the solidification

Jankowski, Alan F. [Sandia National Laboratories (↗

Fundamental Studies of Solidification in Microgravity Using Real-Time X-Ray Microscopy

This research applies a state of the art X-ray Transmission Microscope, XTM, to image (with resolutions up to 3 micrometers) the solidification of metallic or semiconductor alloys in real-time. We have successfully imaged in real-time: interfacial morphologies, phase growth, coalescence, incorporation of phases into the growing interface, and the solute boundary layer in the liquid at the solid-liquid interface. We have also measured true local growth rates and can evaluate segregation structures in the solid; a form of in-situ metallography. During this study, the growth of secondary phase fibers and lamellae from eutectic and monotectic alloys have been imaged during solidification, in real-time, for the first time in bulk metal alloys. Current high resolution X-ray sources and high contrast X-ray detectors have advanced to allow systematic study of solidification dynamics and the resulting microstructure. We have employed a state-of-the-art sub-micron source with acceleration voltages of 10-100 kV to image solidification of metals. One useful strength of the XTM stems from the manner an image is formed. The radiographic image is a shadow formed by x-ray photons that are not absorbed as they pass through the specimen. Composition gradients within the specimen cause variations in absorption of the flux such that the final image represents a spatial integral of composition (or thickness). The ability to image these features in real-time enables more fundamental and detailed understanding of solidification dynamics than has previously been possible. Hence, application of this technique towards microgravity experiments will allow rigorous testing of critical solidification models.

Curreri, Peter A.↗

Three-Dimensional In Situ Observations of Polycrystalline Microstructure Evolution During Directional Solidification of Transparent Alloys Aboard the ISS and Quantitative Comparison with Numerical Modeling

Cellular/dendritic microstructures formed during solidification have a crucial influence on the mechanical properties of a wide range of structural alloys. By minimizing the amount of gravity-induced convection in the liquid, directional solidification experiments using transparent organic alloys conducted in the DECLIC-DSI onboard the International Space Station have provided unique 3D in situ observations of the spatiotemporal evolution of the solid-liquid interface during the formation of cellular and dendritic microstructures under purely diffusive growth conditions. Those observations have made it possible to perform benchmark quantitative comparisons with the predictions of state-of-the-art phase-field simulations of microstructure formation in 3D on experimentally relevant length and time scales. This talk will report quantitative comparisons between microgravity experiments and phase-field simulations in succinonitrile-camphor alloys of two different compositions, which shed new light on the selection of dendritic array structures, and on roles of macroscopic curvatures and subgrain boundaries between grains with a small misorientation with respect to the temperature gradient in the spatiotemporal evolution of the primary cellular spacing.

Kaihua Ji↗

Understanding Fission Gas Bubble Distribution and Zirconium Redistribution in Neutron-irradiated U-Zr Metallic Fuel Using Machine Learning

U-10wt.% Zr (U-10Zr) based metallic fuel is the leading candidate for next-generation sodium cooled fast reactor in United States. Currently, Idaho National Laboratory (INL) has been the leading national laboratory for research, development, and demonstration (RD&D) on metallic fuel. Advanced post-irradiation characterization will help to understand fuel microstructure and property change during irradiation, benefiting fuel qualification for commercial application. Characterization capabilities ranging from sub-nanometer to micrometer, such as scanning electron microscopy (SEM), focused ion beam (FIB) sampling, transmission electron microscopy (TEM) characterization, and local thermal conductivity microscopy (TCM), have been utilized recently on irradiated U-10Zr fuel samples to gain a better understanding of nuclear fuel microstructure and property evolution inside a reactor. The FIB/SEM coupled with energy dispersive X-ray spectroscopy (EDS) can capture the essential information to achieve better understanding of fuel behaviors. Inside a nuclear reactor, the phase and microstructure of U-10Zr is constantly changing under neutron bombardment. For example, the gaseous fission product atoms have a limited solubility inside fuel matrix and tend to precipitate out in bubble form, which not only contribute to fuel thermal conductivity degradation but also provide a shortcut for movement of fission products, i.e. lanthanides. The resultant deposition of lanthanides at the cladding inner surface will potentially trigger a chemical reaction/interaction between nuclear fuel and cladding at reactor operational conditions, threatening fuel integrity and safety. FIB/SEM coupled with EDS can provide the fission bubble information as well as probe into phase separation or Zr redistribution, which is fundamental to predict the fuel performance. With high velocity image data generating method, such as FIB/SEM, an automatic way to extract the microstructural information quantitively can better serve the needs from post irradiation characterization. A trained machine learning model, named Decision Tree, is employed to generate a bubble classifier and to categorize bubbles into three categories: isolated bubble, connected without lanthanides, and connected with lanthanides bubbles[3]. This work presents a showcase of this approach on six regions of a fuel cross-section along the radial temperature gradient. We obtained distributions of bubble categories and porosity rates along the six regions. Moreover, a secondary phase U-Zr2 was determined and found on regions 5 and 6. The secondary phase fraction was increasing from 15.61% in region 5 to 34.79% in region 6 based on this approach . This quantitative data offers insights into the lanthanide migration and potentially thermal conductivity degradation. This information from machine learning will be fed into fuel design code for better prediction of fuel performance.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗