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At least 343 records · Page 19

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NASA NTRS1987

High frequency ultrasonic characterization of sintered SiC

High frequency (60 to 160 MHz) ultrasonic nondestructive evaluation was used to characterize variations in density and microstructural constituents of sintered SiC bars. Ultrasonic characterization methods included longitudinal velocity, reflection coefficient, and precise attenuation measurements. The SiC bars were tailored to provide bulk densities ranging from 90 to 98 percent of theoretical, average grain sizes ranging from 3.0 to 12.0 microns, and average pore sizes ranging from 1.5 to 4.0 microns. Velocity correlated with specimen bulk density irrespective of specimen average grain size, average pore size, and average pore orientation. Attenuation coefficient was found to be sensitive to both density and average pore size variations, but was not affected by large differences in average grain size.

Baaklini, George Y.↗

NASA NTRS1989

High-frequency ultrasonic characterization of sintered silicon carbide

High-frequency 60- to 160-MHz ultrasonic nondestructive evaluation was used to characterize variations in density and microstructural constituents of sintered SiC bars. Ultrasonic characterization methods included longitudinal velocity, reflection coefficient, and precise attenuation measurements. The SiC bars were tailored to provide bulk densities ranging from 90 to 98 percent of theoretical, average grain sizes ranging from 3.0 to 12.0 microns, and average pore sizes ranging from 1.5 to 4.0 microns. Velocity correlated with specimen bulk density irrespective of specimen average grain size, average pore size, and average pore orientation. The attenuation coefficient was found to be sensitive to both density and average pore size variations, but was not affected by large differences in average grain size.

Baaklini, George Y.↗

NASA NTRS1989

Advanced single crystal for SSME turbopumps

The objective of this program was to evaluate the influence of high thermal gradient casting, hot isostatic pressing (HIP) and alternate heat treatments on the microstructure and mechanical properties of a single crystal nickel base superalloy. The alloy chosen for the study was PWA 1480, a well characterized, commercial alloy which had previously been chosen as a candidate for the Space Shuttle Main Engine high pressure turbopump turbine blades. Microstructural characterization evaluated the influence of casting thermal gradient on dendrite arm spacing, casting porosity distribution and alloy homogeneity. Hot isostatic pressing was evaluated as a means of eliminating porosity as a preferred fatigue crack initiation site. The alternate heat treatment was chosen to improve hydrogen environment embrittlement resistance and for potential fatigue life improvement. Mechanical property evaluation was aimed primarily at determining improvements in low cycle and high cycle fatigue life due to the advanced processing methods. Statistically significant numbers of tests were conducted to quantitatively demonstrate life differences. High thermal gradient casting improves as-cast homogeneity, which facilitates solution heat treatment of PWA 1480 and provides a decrease in internal pore size, leading to increases in low cycle and high cycle fatigue lives.

Fritzemeier, L. G.↗

NASA NTRS2008

Thermal Stir Welding Development at Marshall Space Flight Center

Solid state welding processes have become the focus of welding process development at NASA's Marshall Space Flight Center. Unlike fusion weld processes such as tungsten inert gas (TIG), variable polarity plasma arc (VPPA), electron beam (EB), etc., solid state welding processes do not melt the material during welding. The resultant microstructure can be characterized as a dynamically recrystallized morphology much different than the casted, dentritic structure typical of fusion weld processes. The primary benefits of solid state processes over fusion weld processes include superior mechanic properties and the elimination of thermal distortion and residual stresses. These solid state processes attributes have profoundly influenced the direction of advanced welding research and development within the NASA agency. Thermal Stir Welding (TSW) is a new solid state welding process being developed at the Marshall Space Flight Center. Unlike friction stir welding, the heating, stirring and forging elements of the weld process can be decoupled for independent control. An induction coil induces energy into a workpiece to attain a desired plastic temperature. An independently controlled stir rod, captured within non-rotating containment plates, then stirs the plasticized material followed by forging plates/rollers that work the stirred weld joint. The independent control (decoupling) of heating, stirring and forging allows, theoretically, for the precision control of microstructure morphology. The TSW process is being used to evaluate the solid state joining of Haynes 230 for ARES J-2X applications. It is also being developed for 500-in (12.5 mm) thick commercially pure grade 2 titanium for navy applications. Other interests include Inconel 718 and stainless steel. This presentation will provide metallurgical and mechanical property data for these high melting temperature alloys.

Ding, Robert J.↗

NASA NTRS2003

Superalloy Lattice Block Developed for Use in Lightweight, High-Temperature Structures

Successful development of advanced gas turbine engines for aircraft will require lightweight, high-temperature components. Currently titanium-aluminum- (TiAl) based alloys are envisioned for such applications because of their lower density (~4 g/cm3) in comparison to superalloys (~8.5 g/cm3), which have been utilized for hot turbine engine parts for over 50 years. However, a recently developed concept (lattice block) by JAMCORP, Inc., of Willmington, Massachusetts, would allow lightweight, high-temperature structures to be directly fabricated from superalloys and, thus, take advantage of their well-known, characterized properties. In its simplest state, lattice block is composed of thin ligaments arranged in a three dimensional triangulated trusslike configuration that forms a structurally rigid panel. Because lattice block can be fabricated by casting, correctly sized hardware is produced with little or no machining; thus very low cost manufacturing is possible. Together, the NASA Glenn Research Center and JAMCORP have extended their lattice block methodology for lower melting materials, such as Al alloys, to demonstrate that investment casting of superalloy lattice block is possible. This effort required advances in lattice block pattern design and assembly, higher temperature mold materials and mold fabrication technology, and foundry practice suitable for superalloys (ref. 1). Lattice block panels have been cast from two different Ni-base superalloys: IN 718, which is the most commonly utilized superalloy and retains its strength up to 650 C; and MAR M247, which possesses excellent mechanical properties to at least 1100 C. In addition to the open-cell lattice block geometry, same-sized lattice block panels containing a thin (~1-mm-thick) solid face on one side have also been cast from both superalloys. The elevated-temperature mechanical properties of the open cell and face-sheeted superalloy lattice block panels are currently being examined, and the microstructure is being characterized in terms of casting defects. In addition, a small study (ref. 3) is being undertaken with GE Aircraft Engines to determine the suitability of superalloy lattice block for engine components.

Hebsur, Mohan G.↗

DOE OSTI2025

A critical analysis of U-Pu-Zr phase transitions using calorimetric, microstructural, and phase equilibria data

Metallic fuels consisting primarily of uranium, plutonium, and zirconium (U-Pu-Zr) are a leading material candidate for fast-spectrum nuclear reactors. Early demonstration programs proved the principle of safe and efficient fast reactor operation, however there is still considerable uncertainty regarding the phase equilibria and microstructural evolution across the ternary composition space. Quantitative phase formation and identification measurements are scarce and often incomplete, with studies reporting either phase transition temperatures or phase identification data, but not both from the same specimens. In this study, we critically compared experimental and calculated phase transition data and correlated with the microstructure and phase characterization data of as-cast and annealed U-Pu-Zr alloys. Differential scanning calorimetry (DSC) was used to measure phase transitions in the subsolidus regions (723−948 K) of three ternary U-Pu-Zr alloys with similar plutonium concentrations but various U/Zr ratios. Due to sluggish kinetics and narrow ranges of phase stability, complex peaks required the use of a Frazier-Suzuki peak fitting algorithm to deconvolute and calculate transition peak temperatures and enthalpies. We also identified trends of phase transition behavior by critically comparing our DSC data with previous phase transition measurements as well as historical and calculated phase equilibrium diagrams. In conclusion, this provides a critical approach for benchmarking and assessing the quality of new U-Pu-Zr phase equilibria data prior to its incorporation into nuclear material databases.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS2001

Microstructure, Mechanical Properties, Hot-Die Forming, and Joining of 47XD Gamma TiAl Rolled Sheets

The microstructure and mechanical properties, along with the hot-die forming and joining of Ti-47Al-2Nb-2Mn-0.8 vol% TiB, sheets (known as 47XD), produced by a low-cost rolling process, were evaluated. A near-gamma microstructure was obtained in the as-rolled condition. The microstructures of heat-treated sheets ranged from a recrystallized equiaxed near-gamma microstructure at 1,200 to 1,310 C, to a duplex microstructure at 1,350 C, to a fully lamellar microstructure at 1,376 C. Tensile behavior was determined for unidirectionally rolled and cross-rolled sheets for room temperature (RT) to 816 C. Yield stress decreased gradually with increasing deformation temperature up to 704 C; above 704 C, it declined rapidly. Ultimate tensile strength exhibited a gradual decrease up to 537 C before peaking at 704 C, followed by a rapid decline at 816 C. The modulus showed a gradual decrease with temperature, reaching approximately 72% of the RT value at 816 C. Strain to failure increased slowly from RT to 537 C; between 537 C and 704 C it exhibited a phenomenal increase, suggesting that the ductile-brittle transition temperature was below 704 C. Fracture mode changed from transgranular fracture at low temperature, to a mixture of transgranular and intergranular fracture at intermediate temperature, to ductile fracture at 816 C, coupled with dynamic recrystallization at large strains. Creep rupture response was evaluated between 649 and 816 C over the stress range of 69 to 276 MPa. Deformation parameters for steady-state creep rate and time-to-rupture were similar: activation energies of approximately 350 kJ/mol and stress exponents of approximately 4.5. Hot-die forming of sheets into corrugations was done at elevated temperatures in vacuum. The process parameters to join sheets by diffusion bonding and brazing with TiCuNi 70 filler alloy were optimized for test coupons and successfully used to fabricate large truss-core and honeycomb structures. Nondestructive evaluation methods, e.g., ultrasonic C-scans and thermography along with metallography, were used to characterize bond quality. Microstructural evaluation during heat treatment, identification of phases at the braze/matrix interface, determination of shear strengths of brazed joints, and deformation mechanisms during tensile and creep processes will be discussed.

Das, G.↗

DOE OSTI2026

Microstructural evolution, defect mitigation, and precipitation behavior in AA6061 via laser powder bed fusion with high-temperature substrate heating

Defects, particularly solidification cracking, remain persistent challenges in the laser powder bed fusion (LPBF) processing of AA6061 aluminum alloy. This study systematically investigates defect mitigation, microstructural evolution, and mechanical properties associated with high-temperature substrate preheating at 500 °C. Comprehensive microstructural analyses, including characterization of defects, grain structures, and precipitation behavior, were performed on samples in both as-built and T6 heat-treated states. Elevated preheating substantially reduced solidification cracking across a wide processing window, while demonstrating decreased crack sensitivity to laser parameters. Columnar cracks along the build direction were observed despite substrate preheating. Lack-of-fusion and keyhole porosity were effectively eliminated, though gas-induced microporosity persisted at higher powers. In-depth characterization of two distinct laser power and speed conditions confirmed the formation of micron-sized, non-coherent Mg 2 Si precipitates under heated substrate conditions, alongside α-AlFeCrMnSi intermetallic phases indicative of in-situ thermal effects during fabrication. Subsequent T6 heat treatment revealed the formation of fine, coherent needle-shaped β″ strengthening precipitates. Despite substantial differences in processing parameters, comparable mechanical properties were measured in the as-built samples (∼52 MPa yield strength, ∼130 MPa tensile strength), primarily due to reduced strain hardening effects and consistent precipitation characteristics. Meanwhile, the T6 heat treatment led to significant improvement in properties, enhancing yield strength by over 400%, aligning closely with the performance of conventional wrought AA6061-T6. These findings underscore that high-temperature substrate preheating offers an effective means to suppress cracks, control precipitation, and enhance mechanical performance in LPBF-processed AA6061.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Mitigate Stress Corrosion Cracking (SCC) in High-strength Al Castings (CRADA 508)

Development of high strength, corrosion resistant, aluminum alloys is important to a number of industries, including automotive, aerospace, power, etc. Understanding how processing methods such as casting, chemistry, additives and recycle content affect an alloy’s microstructure and performance in real world environments is crucial to their implementation. One major concern is how the repeated exposure to saline solutions can be detrimental to the structural integrity of aluminum alloy components. This study was undertaken as a collaboration between Eck Industries and PNNL to investigate the stress corrosion cracking (SCC) and corrosion behavior of aluminum alloys. This work examines the SCC response of three different materials set. First is cast A206 Al alloy produced by three different casting techniques (i.e., permanent mold, and sand casting with and without chill) and with or without nano forming additives as potential grain refiners. The second materials set comprises Al alloy tubes extruded by PNNL’s ShAPE process and produced using raw material with three different ratios of twitch and pre-consumer Al 6061 scrap. Finally, the third materials set comprises two Al-Si-Mg-Fe alloys with controlled Si% and Fe% to mimic recycle grade Al alloys. The corrosion behavior of these materials was characterized using SCC testing and scanning electrochemical cell microscopy (SECCM) technique; mechanical behavior was characterized using tensile testing, and microstructure was characterized using optical and electron microscopy techniques. Of the A206 Al alloys, the samples with nano forming additives performed poorly compared to those without. The best SCC performance (i.e. least degradation in mechanical properties) was demonstrated by A206 alloy sand cast with chill while the permanent mold sample showed the worst SCC performance. The SECCM was performed on A206 alloy sand cast with chill to understand the effect of microstructure and determine the location-dependent corrosion properties on grain boundaries (GB) and inside grains (IG) on the sample. The corrosion potential and current measured on GB and IG at various points on the sample established that the GB locations are more cathodic and corrosive than the IG locations. Further work needs to be conducted to investigate the mechanisms behind the observed dependence of SCC on casting technique and nano forming additives. Among the ShAPE extruded tubes, SECCM data suggests the decreasing order of tendency to corrode as follows: 100% twitch > 75% twitch > 50% twitch. Finally, both variants of the Al-Si-Mg-Fe alloys showed a large volume fraction of Fe- and Si-containing intermetallics and additional work is needed to discern differences in their respective corrosion responses. In summary, correlating local electrochemical behavior (e.g. via SECCM) with micro/nanostructure, in conjunction with bulk mechanical behavior, can help identify the right fabrication method and alloy chemistry to minimize SCC issues in Al alloys.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Influence of porous aluminosilicate grain size materials in experimental and modelling Cs + adsorption kinetics and wastewater column process

This paper focuses on the influence of the grain size of a geopolymer based adsorbent on its Cs + adsorption performances both in batch and fixed-bed process. The geopolymer phase was used as a binder to support NaY zeolite particle in a 20 wt% charged porous composite with 160 m 2 .g –1 of porous surface area. These samples were shaped with three grain sizes (50 /100/500 µm) to remove 80–90 mg/g of Cs + in batch and column operations. After their microstructural and porous characterizations, their efficiency and adsorption characteristics were investigated through adsorption isotherms and kinetic in the two processes. While the grain size has no influence on the maximal extraction capacity of the adsorbent, it strongly affects the sorption kinetic. By coupling experimental data and a modelling approach, the complex sorption mechanism was highlighted, suggesting a new insight of the contaminant sorption kinetic. Then, comparison of batch and column adsorption experiments illustrates the detailed explanation of various process parameters for column study. The results show challenges for fixed-bed column utilization by the choice of the appropriate grain size as a compromise between the material sorption kinetic and hydrodynamic considerations. Furthermore, this is of high importance to more accurately optimize the design of column adsorption to assess the transport of Cs+ in multi-porous tailored grain size materials.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Hydrogen influences thermal activation parameters for dislocation glide during low cycle fatigue of 316L stainless steel

Measurements of activation areas are used to investigate the effect of hydrogen on the kinetics of dislocation glide during cyclic deformation in cold-worked 316L stainless steel. Non-charged and hydrogen-precharged (H-precharged) specimens were tested in low cycle fatigue (LCF) under plastic strain control. A series of plastic strain rate changes was performed periodically at the peak true plastic strain from the first cycle to half-life, and at various plastic strain values around stable hysteresis loops near half-life to determine the operational activation area, Δ a ∗. Both material conditions demonstrate a rapid increase in Δ a ∗ during the initial rapid softening followed by a region of approximately constant values coinciding with a reduced rate of softening. Near half-life, hydrogen reduces Δ a ∗ at a given true stress due to its effect on the activation distance and obstacle spacing. The magnitudes of Δ a ∗ reveal that bypassing solutes, cutting forest dislocations, and initiating cross slip are important mechanisms of thermally activated dislocation glide at all amplitudes, except hydrogen suppresses cross slip at the lowest plastic strain amplitudes. These results are supported by electron microscopy characterization of deformed microstructures. A Haasen plot analysis indicates that forest dislocations control the kinetics of deformation in both material conditions. It also reveals the presence of athermal obstacles in both non-charged and H-precharged conditions, likely dense dislocation tangles and cell walls. Additionally, the effect of hydrogen on microstructure evolution (by reducing the propensity for cross slip) leads to a dependence of athermal stress on plastic strain amplitude.

Activation area↗

DOE OSTI2024

Metal Scrap Upcycling with Shear Assisted Processing and Extrusion (ShAPE)

The overarching objective of this project is to convert metal scraps, such as aluminum, titanium, and other alloys provided by the industry, into extruded tubing, wires, and rods. Upcycling of scrap will be accomplished using Shear Assisted Processing and Extrusion (ShAPE). This approach is a new solution for recycling. The specific aims of this project are as follows: 1. Receive metal scrap under a Material Transfer Agreement (MTA), in the form of billets, from select industry partners that meet the following requirements: outer diameter of 1.245 inches (+/-0.003 inches), inner diameter drilled with a 0.404-inch drill bit, and a length of 4.0 inches (+/-0.01 inches). The billet must be cast or compacted to greater than 98% density. If the industry partner does not have the capabilities to prepare the billets, PNNL can make introductions to third-party entities as needed. Industry partners will also provide a composition analysis as weight percent. 2. Extrude metal scrap via the ShAPE process at PNNL. 3. Evaluate and benchmark the extrudate material properties per the ASTM B557-15 – Testing Tubulars Standard or similar wire and rod standards. 4. Characterize the extrudate microstructure for any of the following: grain size, second phase composition, and texture. Additional testing may include corrosion per the ASTM B117 standard and electro-potential. 5. Deliver specimens to industry partners under an MTA for additional third-party evaluations. Industry partners will, in return, provide a non-proprietary report on any testing, including testing per the ASTM B557-15, ASTM B117, and other industry standards. 6. PNNL will develop data and insights to support intellectual property capture, a published non-proprietary technical report, research collaborations, and commercialization opportunities.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Screening and qualification methodology for SiC end plug processing methods

Deployment of SiC-ceramic-based fuel cladding for light water reactors requires a hermetic end plug–to–cladding joint that can withstand neutron irradiation during normal operation and maintain integrity during design-basis accidents. Reactor experiments have shown that some SiC composite tubes with SiC end plugs can retain hermeticity after irradiation. However, achieving consistent joint performance under irradiation remains a key challenge. Resolving this issue is essential to enable integral irradiation testing and to demonstrate fuel integrity under commercial-reactor irradiation conditions. This report aims to: (1) provide guidance for designing radiation-tolerant end plug joints for SiC cladding; (2) demonstrate experimental methods to detect processing defects that are unstable under neutron irradiation at light-water-reactor-relevant temperatures and doses; and (3) outline a step-by-step approach for designing and conducting reactor experiments to screen joining methods. The resulting data will be used to improve joint processing and to define critical defect types and sizes that must be detected and eliminated through non-destructive evaluation for quality assurance. Based on prior irradiation experiments at the High Flux Isotope Reactor, differential swelling among the cladding, bonding layer, and end plug was identified as an underlying mechanism for irradiation-induced joint degradation. Accordingly, this effect must be considered in the design of radiation-tolerant joining techniques. In this work, miniature SiC end plug joint specimens irradiated during the previous project were analyzed using X-ray computed tomography to characterize the joint microstructure. Digital volume correlation of the tomography data quantified radiation-induced microstructural changes and enabled evaluation of defect-related risks. Finally, ongoing neutron irradiation efforts using larger specimen volumes are presented. These efforts aim to statistically assess joint performance and to build a microstructure–performance (e.g., leak-tightness) dataset to inform processing improvements and quality control.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

NASA NTRS1981

The growth of metastable peritectic compounds

The influence of gravitationally driven thermosolutal convection on the directional solidification of peritectic alloys is considered as well as the relationships between the solidification processing conditions, and the microstructure, chemistry, and magnetic properties of such alloys. Analysis of directionally solidified Pb-Bi peritectic samples indicates that appreciable macrosegregation occurs due to thermosolutal convection and/or Soret diffusion. A peritectic solidification model which accounts for partial mixing in the liquid ahead of the planar solidification interface and describes macrosegregation has been developed. Two-phase dendritic and banded microstructures were grown in the Pb-Bi peritectic system, refined two-phase microstructures have were observed, and candidate formation mechanisms proposed. Material handling, containment, casting, microstructural and magnetic characterization techniques were developed for the Sm-Co system. Alloys produced with these procedures are homogeneous.

Larson, D. J., Jr.↗

NASA NTRS1984

Overview of zirconia with respect to gas turbine applications

Phase relationships and the mechanical properties of zirconia are examined as well as the thermal conductivity, deformation, diffusion, and chemical reactivity of this refractory material. Observations from the literature particular to plasma-sprayed material and implications for gas turbine engine applications are discussed. The literature review indicates that Mg-PSZ (partially stabilized zirconia) and Ca-PSZ are unsuitable for advanced gas turbine applications; a thorough characterization of the microstructure of plasma-sprayed zirconia is needed. Transformation-toughened zirconia may be suitable for use in monolithic components.

Cawley, J. D.↗

NASA NTRS1985

Impurities in silicon solar cells

Metallic impurities, both singly and in combinations, affect the performance of silicon solar cells. Czochralski silicon web crystals were grown with controlled additions of secondary impurities. The primary electrical dopants were boron and phosphorus. The silicon test ingots were grown under controlled and carefully monitored conditions from high-purity charge and dopant material to minimize unintentional contamination. Following growth, each crystal was characterized by chemical, microstructural, electrical, and solar cell tests to provide a detailed and internally consistent description of the relationships between silicon impurity concentration and solar cell performance. Deep-level spectroscopy measurements were used to measure impurity concentrations at levels below the detectability of other techniques and to study thermally-induced changes in impurity activity. For the majority of contaminants, impurity-induced performance loss is due to a reduction of the base diffusion length. From these observations, a semi-empirical model which predicts cell performance as a function of metal impurity concentration was formulated. The model was then used successfully to predict the behavior of solar cells bearing as many as 11 different impurities.

Hopkins, R. H.↗

NASA NTRS1986

Ultrasonic characterization of structural ceramics

Ultrasonic velocity and attenuation measurements were used to characterize density and microstructure in monolithic silicon nitride and silicon carbide. Research samples of these structural ceramics exhibited a wide range of density and microstructural variations. It was shown that bulk density variations correlate with and can be estimated by velocity measurements. Variations in microstructural features such as grain size or shape and pore morphology had a minor effect on velocity. However, these features had a pronounced effect on ultrasonic attenuation. The ultrasonic results are supplemented by low-energy radiography and scanning laser acoustic microscopy.

Klima, S. J.↗

NASA NTRS1986

Nondestructive characterization of structural ceramics

Klima, S. J.↗