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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 523 records · Page 29

Discovery, Design, Synthesis and Testing of High Performance Structural Alloys (Final Technical Report)

The overarching goal of this project is to understand the phase stability and mechanical behavior of non-stoichiometric multi-principal element alloy (MPEA) materials. In order to identify suitable alloys, we plan to use a combinatorial thin film screening approach, in collaboration with scientists at Lawrence Berkeley National Laboratory who are performing computational work as well as complementary experimental work. Specific tasks within the scope of this project include the fabrication, using thin film deposition from six sputtering targets, of combinatorial samples with multi-dimensional gradients in composition and microstructure. These samples are studied to screen MPEA systems for promising candidate alloys with specific composition(s), based on characterization of composition, structure and mechanical behavior across the thin film. We want to produce single-phase MPEAs with chemical homogeneity in a given thin film region, simple grain structures, and no intermetallic phases present. Gradient films facilitate first-pass screening for desirable characteristics and inform the next stage of work that involves fabrication of bulk MPEA specimens for (tensile) mechanical testing and characterization. To make the bulk alloys, metal (elemental) pieces are melted to form MPEAs, followed by heat treatment to homogenize the composition and microstructure. A subset of alloys is also cast, using vacuum arc melting, to yield larger samples (diameter ~1 cm and length ~5-10 cm) and these allow us to assess viability of scale-up for the alloys in structural applications. Further processing plans include rolling and heat treatment to recrystallize selected bulk MPEAs and grow grains to different extents, in order to investigate size effects in the mechanical behavior of MPEAs. Microspecimen testing will be performed (primarily in tension) to assess the mechanical behavior over a range of temperatures. The deformation microstructure of mechanically tested alloys will be characterized using transmission electron microscopy (TEM) to provide a scientific basis for understanding the structure-property relationships in MPEA mechanical behavior.

36 MATERIALS SCIENCE↗

Preparation of low strategic metal content superalloys

The properties of modified NIMONIC 115 and UDIMET 720 with reduced levels of cobalt were evaluated. Vacuum induction melted and vacuum arc remelted ingots were hot rolled to 3/4 inch diameter bar. Hot workability was evaluated in terms of the ingot rolling behavior and the hot ductility of the as-rolled bar. Variations in workability and bar ductility were correlated to variations in incipient melting temperature and gamma prime solvus, both of which varied with cobalt content. Heat treatments were defined to yield, as far as possible, similar structures from alloy to alloy. At the lowest cobalt levels N-115 workability was severely limited and the alloys could not be worked to bar. It is suggested that incipient melting in combination with heavy grain boundary carbide precipitation reduced ingot workability. Final heat treatment of modified alloys was difficult in the situation where the gamma prime solvus temperature was close to the incipient melting point, indicating that it may not be feasible to fully solution low cobalt alloys to obtain the large grain size required for optimum creep resistance.

Sczerzenie, F. E.↗

Crystallization behavior and properties of BaO-Al2O3-2SiO2 glass matrices

Glass of stoichiometric celsian composition, BaO-Al2O3-2SiO2, is a potential glass-ceramic matrix for high-temperature composites. The glass has a density of 3.39 g/cu cm, thermal expansion coefficient of 6.6 x 10(exp -6)/deg C glass transition temperature of 910 C, and dilatometric softening point of 925 C. On heat treatment, only hexacelsian crystallized out on the surface, but both celsian and hexacelsian were present in the bulk. Effects of cold isostatic pressing (CIP), sintering, and hot pressing, in the presence and absence of an additive, on the formation of the celsian phase in the glass were studied. CIP'ed samples, after appropriate heat treatments, always crystallized out as celsian whereas the presence of 5 to 10 weight percent of an additive was necessary for formation of celsian in sintered as well as hot pressed specimens. Green density increased with CIP'ing pressure but had no effect on sintered density. Hot pressing resulted in fully dense samples.

Drummond, Charles H., III↗

Diffusion of Sn donors in β-Ga 2 O 3

Diffusion of the n-type dopant Sn in β-Ga 2 O 3 is studied using secondary-ion mass spectrometry combined with hybrid functional calculations. The diffusion of Sn from a Sn-doped bulk substrate with surface orientation (001) into an epitaxial layer is observed after heat treatments in the temperature range of 1050–1250 °C. Calculated formation energies of Sn-related and intrinsic defects show that the migration of Sn is mediated by Ga vacancies ( V Ga ) through the formation and dissociation of intermittent mobile V Ga Sn Ga complexes. The evolution of the Sn concentration vs depth profiles after heat treatments can be well described by a reaction–diffusion model. Using model parameters guided by the hybrid functional calculations, we extract a V Ga Sn Ga complex migration barrier of 3.0 ± 0.4 eV with a diffusion coefficient of 2 × 10 –1 cm 2 /s. The extracted migration barrier is consistent with our theoretical predictions using the nudged elastic band method, which shows migration barriers of 3.42, 3.15, and 3.37 eV for the [100], [010], and [001] directions, respectively.

36 MATERIALS SCIENCE↗

Crystallization behavior and properties of BaO-Al2O3-2SiO2 glass matrices

Glass of stoichiometric celsian composition, BaO-Al2O3-SiO2, has a density of 3.39 g/cu cm, a thermal expansion coefficient of 6.6 x 10 to the -6th/C, a glass-transition temperature of 910 C, and a dilatometric softening point of 925 C. On heat treatment, only hexacelsian crystallized out on the surface, but both celsian and hexacelsian were present in the bulk. Effects of cold isostatic pressing (CIP), sintering, and hot-pressing, in the presence and absence of an additive, on the formation of the celsian phase in the glass have been studied. CIP'd samples, after appropriate heat treatments, always crystallized out as celsian, whereas presence of 5-10 wt pct of an additive was necessary for formation of celsian in sintered as well as hot-pressed specimens. Green density increased with CIP'ing pressure but had no effect on sintered density. Hot-pressing resulted in fully dense samples.

Drummond, Charles H., III↗

Interaction of metal layers with polycrystalline Si

Solid-phase reactions of metal films deposited on 0.5-micron-thick polycrystalline layers of Si grown by chemical vapor deposition at 640 C were investigated by MeV He-4 backscattering spectrometry, glancing angle X-ray diffraction, and SEM observations. For the metals Al, Ag, and Au, which form simple eutectics, heat treatment at temperatures below the eutectic results in erosion of the poly-Si layer and growth of Si crystallites in the metal film. Crystallite formation is observed at temperatures exceeding 550 C for Ag, at those exceeding 400 C for Al, and at those exceeding 200 C for Au films. For Pd, Ni, and Cr, heat treatment results in silicide formation. The same initial silicides (Pd2Si, Ni2Si, and CrSi2), are formed at similar temperatures on single-crystal substrates.

Nakamura, K.↗

Report on Properties and Microstructure of 3D Printed Inc-718

The report presents the microstructure and mechanical properties of 3D printed Inconel 718 to assess its potential use as a structural material for the Transformation Challenge Reactor (TCR). The structural components near the outlet of the core will experience significant neutron fluxes and outlet coolant temperatures from the hot standby temperature of 300°C to nearly 550°C at the center of the part. These components must support the core in appropriate loading conditions and require structural analysis at relevant temperatures. Strong spatial and chemical heterogeneity was found in as-built (ASB) Inconel 718. Three heat treatments were designed and conducted to simplify the microstructure and determine how each precipitating phase contributed to the overall strength. Baseline mechanical properties were measured from uniaxial tensile tests on subsize SS-J2 specimens at room temperature and at elevated temperatures of 300, 450, and 600°C. Microstructure electron microscopy was performed on ASB Inconel 718 and heat treated to correlate the observed mechanical properties with nanoscale features. Homogenization of the microstructure led to a highly ductile Inconel with lower strength compared with wrought Inconel 718. The tensile properties of additively manufactured 718 using a standard ASTMrecommended heat treatment were consistent with literature and with the ASTM for the properties of this alloy. A higher fraction of the δ phase led to shorter uniform elongation without altering other engineering properties.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Advancement of Extreme Environment Additively Manufactured Alloys for Next Generation Space Propulsion Applications

The National Aeronautics and Space Administration (NASA) has been involved in the development and maturation of metal additive manufacturing (AM) for space applications since the late 2000’s. Several efforts focused on the understanding of AM processes through material characterization and testing, standards development, component fabrication, and infusion into propulsion development and flight applications. NASA matured commonly used aerospace alloys from various alloy families (Nickel, Copper, Stainless and Steel, Aluminum, and Titanium-based) through detailed AM process and heat treatment characterization, in addition to mechanical and thermophysical testing. While these alloys are actively used in many propulsion applications, there is a need for ongoing AM optimized alloys using integrated computational materials engineering (ICME) and process development for high performance applications. The applications targeted are liquid rocket engines; advanced propulsion systems; and in-space propulsion with high heat fluxes, high pressure, and/or that use propellants that can degrade alloys (e.g., hydrogen). This paper highlights the characterization and physical properties of the more common AM alloys using laser powder bed fusion (L-PBF) and laser powder directed energy deposition (LP-DED) processes. Additionally, this paper discusses some of the ongoing novel alloy development and maturation using AM for use in these harsh environments, such as GRCop42, GRCop-84, NASA HR-1, GRX-810, and C-103. The results from these processes demonstrated that AM could enable rapid development and ongoing efforts for optimized alloys using ICME, yielding higher performances. These alloys have undergone modeling, fundamental metallurgical evaluations, heat treatment studies, detailed microstructure characterization, and mechanical testing campaigns. This, combined with direct application-specific component fabrication and hot-fire testing, enabled the increase of the Technology Readiness Level (TRL) through high duty-cycle testing. A background and overview of these novel AM-enabled alloys and AM processing developments including metallurgical and mechanical property studies is presented here. The latest advancement in the parallel component development and hot-fire testing and future developments for these alloys is also discussed.

Additive Manufacturing↗

Advancement of Extreme Environment Additively Manufactured Alloys for Next Generation Space Propulsion Applications

The National Aeronautics and Space Administration (NASA) has been involved in the development and maturation of metal additive manufacturing (AM) for space applications since the late 2000’s. Several efforts focused on the understanding of AM processes through material characterization and testing, standards development, component fabrication, and infusion into propulsion development and flight applications. NASA matured commonly used aerospace alloys from various alloy families (Nickel, Copper, Stainless and Steel, Aluminum, and Titanium-based) through detailed AM process and heat treatment characterization, in addition to mechanical and thermophysical testing. While these alloys are actively used in many propulsion applications, there is a need for ongoing AM optimized alloys using integrated computational materials engineering (ICME) and process development for high performance applications. The applications targeted are liquid rocket engines; advanced propulsion systems; and in-space propulsion with high heat fluxes, high pressure, and/or that use propellants that can degrade alloys (e.g., hydrogen). This paper highlights the characterization and physical properties of the more common AM alloys using laser powder bed fusion (L-PBF) and laser powder directed energy deposition (LP-DED) processes. Additionally, this paper discusses some of the ongoing novel alloy development and maturation using AM for use in these harsh environments, such as GRCop-42, GRCop-84, NASA HR-1, GRX-810, and C-103. The results from these processes demonstrated that AM could enable rapid development and ongoing efforts for optimized alloys using ICME, yielding higher performances. These alloys have undergone modeling, fundamental metallurgical evaluations, heat treatment studies, detailed microstructure characterization, and mechanical testing campaigns. This, combined with direct application-specific component fabrication and hot-fire testing, enabled the increase of the Technology Readiness Level (TRL) through high duty-cycle testing. A background and overview of these novel AM-enabled alloys and AM processing developments including metallurgical and mechanical property studies is presented here. The latest advancement in the parallel component development and hot-fire testing and future developments for these alloys is also discussed.

Additive Manufacturing↗

Exploring the tempering behaviour of additively manufactured high-alloy tool steel using synchrotron X-ray and neutron techniques

Post-processing heat treatment provides a critical pathway toward the commercialisation of additively manufactured (AM) S390 high-speed steel, which is a representative high-alloy tool steel employed in precision manufacturing, offering up to 1.5 times longer tool life and over 20% higher cutting speeds compared to conventional grades. In this study, the phase evolution of AM S390 steel during heat treatment, with particular emphasis on carbide precipitation behaviour, was systematically investigated using a combination of synchrotron X-ray and neutron techniques. The metastable M2C carbides were found to dissolve during austenitisation, while the stable primary carbides MC and M6C experienced coarsening with an average size increase of about 60 nm after just 2 min of tempering. Moreover, the austenite lattice parameters reduced from 3.618 to 3.608 Å within the first 10 min of tempering, suggesting carbon depletion in the steel matrix was likely associated with the formation of secondary carbides. This interpretation was substantiated by small-angle scattering results, which revealed the presence of nanoscale precipitates with a volume fraction of 3.1% after 60 min of tempering. These microstructural evolutions collectively accounted for the observed peak hardness of 921 HV. Furthermore, a comparative analysis of synchrotron and neutron small-angle scattering data highlighted the complementary strengths of each technique, offering critical insight into their suitability for characterising nanoscale features in AM high-alloy steels.

Synchrotron X-ray diffraction↗

Interplay of strain and phase evolution of laser powder bed fusion Ti–6Al–4V

While additive manufacturing (AM) provides a method of producing geometrically complex and highly detailed structures, the generation of residual strain in AM processes like laser powder bed fusion (L-PBF) can negatively impact performance-enabling properties. In applications such as orthopedic implants, specific performance windows require optimized microstructures in order to obtain desirable properties from multi-phase alloys like Ti–6Al–4V. This research aims to quantify the microscale origins of strain in L-PBF manufactured Ti–6Al–4V by understanding how strain is distributed at the grain and sub-grain scale, the interplay between phase evolution and strain, and examining post-processing strain relief strategies to control these features. Model spinal cage implants were manufactured from Ti–6Al–4V powder via L-PBF and then subjected to strain relieving heat treatment cycles above and below the Ti–6Al–4V β transus as a function of time and cooling rate. Residual strain was then studied via high resolution electron backscatter diffraction (HR-EBSD), and 2D strain maps with sub-micron resolution were generated for each post-processing state. It was found that macroscale thermal strains decreased with heat treatment time, but additional contributions from phase stabilizing residual strains retained primarily in the α' grains as lattice distortive strain remained. Additionally, the retention of β phase significantly changed the strain and dislocation distribution while reducing overall residual strain. In conclusion, these results were validated and reinforced with 3D mesoscopic micromechanical modeling of strain behavior across simulated microstructures, confirming that the local lattice dilation of α’ martensite is a primary contributor of microscale strain generation and retention in L-PBF Ti–6Al–4V.

36 MATERIALS SCIENCE↗

Microstructural Evolution of Tantalum During Deformation and Subsequent Annealing

Microstructure-aware models are necessary to predict the behavior of material based on process knowledge or to extrapolate mechanical properties of materials to environmental conditions which are not easily reproduced in the laboratory, e.g., nuclear reactor environments. Elemental Ta provides a relatively simple BCC system in which to develop a microstructural understanding of deformation processes which can then be applied to more complicated BCC alloys. In situ neutron diffraction during compressive deformation and subsequent heat treatment have been used to monitor the evolution of microstructural features in Ta throughout simulated processing steps. Crystallographic texture and dislocation density are determined as a function of first plastic strain, then temperature. Lattice strains are determined and attributed to stresses at macroscopic, grain and dislocation length scales. The increase of the dislocation density through deformation and subsequent recovery during heat treatment is monitored through the changing diffraction line profile. Also, randomization of the texture is used as a signature of recrystallization. The recovery of dislocations through annihilation is not observed to depend on the initial dislocation density in the range studied here. In contrast, recrystallization is observed to depend strongly on the initially dislocation density.

36 MATERIALS SCIENCE↗

Effect of Deposition Conditions on Phase Content and Mechanical Properties of Yttria-Stabilized Zirconia Thin Films Deposited by Sol-Gel/Dip-Coating

The effect of yttria concentration (0-33.4 mol%), extraction rates (0.17, 0.33, 0.50, and 0.67 mm s -1 ), and the number of layers (up to four) on the phase content, surface defects, thickness, hardness, adhesion strength, and wear rate of yttria-stabilized zirconia coatings produced by sol-gel/dip-coating were studied for its use on thermolabile substrates. At 700°C, a metastable tetragonal phase ($\mathcal{t''}$) was obtained even with 33.4 mol% yttria when heat treated for 24 hours; however, a fully cubic structure was attained by extending the heat treatment up to 48 hours as confirmed by Raman spectroscopy. Furthermore, it was necessary to use withdrawal speeds of at least 0.67 mm s -1 to produce defect-free coatings. Although the coatings were produced at low temperature, they showed 41% lower wear rate than steel and an adhesion strength of 30 MPa. Our work stresses the importance of the heat treatment history on the stabilization of the cubic phase in sol-gel YSZ coatings.

36 MATERIALS SCIENCE↗

Sapphire reinforced alumina matrix composites

Unidirectionally reinforced A1203 matrix composites have been fabricated by hot pressing. Approximately 30 volume % of either coated or uncoated sapphire fiber was used as reinforcement. Unstabilized ZrO2 was applied as the fiber coating. Composite mechanical behavior was analyzed both after fabrication and after additional heat treatment. The results of composite tensile tests were correlated with fiber-matrix interfacial shear strengths determined from fiber push-out tests. Substantially higher strength and greater fiber pull-out were observed for the coated fiber composites for all processing conditions studied. The coated fiber composites retained up to 95% and 87% of their as-fabricated strength when heat treated at 14000C for 8 or 24 hours, respectively. Electron microscopy analysis of the fracture surfaces revealed extensive fiber pull-out both before and after heat treatment.

Jaskowiak, Martha H.↗

On the high-temperature stability of the Al 8 Cu 3 Ce intermetallic in an additively manufactured Al-Cu-Ce-Zr alloy

High-temperature resistant eutectic Al alloys are crucial materials for lightweight and energy efficient design in the automotive and aviation industries. Additive manufacturing offers a pathway to refine eutectic microstructures and develop novel alloys with superior high-temperature strength. High-volume fraction intermetallic Al-Cu-Ce alloys have been developed to deliver high-temperature strength in combination with reduced hot-tearing susceptibility. Zr is added to provide additional strengthening via nanoscale Al 3 Zr precipitation, and to stabilize and avoid coarsening of the Al 8 Cu 3 Ce phase. However, the detailed interaction between Zr and Al 8 Cu 3 Ce remains unexplored. In this work, we show with synchrotron X-ray diffraction that laser powder bed fusion fabricated Al-Cu-Ce and Al-Cu-Ce-Zr alloys contain predominantly the Al 8 Cu 3 Ce intermetallic in the as-fabricated condition. Heat treatment of the Al-Cu-Ce alloy results in the Al 8 Cu 3 Ce → Al 8 Cu 4 Ce phase transformation. In the Al-Cu-Ce-Zr alloy, minor fractions of (Al,Cu,Si) 4 Ce and Al 2 Cu-θ are found in the as-fabricated condition, while Al 8 Cu 3 Ce remains stable during heat treatment. Atom probe microscopy quantifies intermetallic stoichiometries and reveals how Zr is enriched at the Al-matrix/Al 8 Cu 3 Ce interface acting as a diffusion barrier against solute exchange. Calibrated thermodynamic modeling underpins this as a kinetic effect. Here, a qualitative microstructural model summarizes, how Zr stabilizes Al 8 Cu 3 Ce against phase transformations and coarsening.

36 MATERIALS SCIENCE↗

Influence of interfacial shear strength on the mechanical properties of SiC fiber reinforced reaction-bonded silicon nitride matrix composites

An evaluation is made of the influence of interfacial microstructure and shear strength on the mechanical properties of a 30 vol pct uniaxially-aligned SiC fiber-reinforced reaction-bonded Si3N4-matrix composite whose interface microstructure was varied through control of fabrication conditions and by heat-treatment in an oxidizing environment. The carbon-rich coating of the as-produced SiC fibers was stable in composites fabricated at 1200 C in an N or N + 4-percent H mixture for 40 hrs. This coating was degraded in composites fabricated at 1350 C in N + 4 percent H for 40 and 72 hrs, as well as after heat-treatment in an oxidizing environment at 600 C for 100 hrs even after fabrication at 1200 C in N. This degradation occurred via carbon removal.

Bhatt, Ramakrishna T.↗

On the Prediction of Uniaxial Tensile Behavior Beyond the Yield Point of Wrought and Additively Manufactured Ti-6Al-4V

In this paper, phenomenological relationships are presented that permit the prediction of the plastic regime of stress–strain curves using a limited number of parameters. These relationships were obtained from both conventional (wrought + β annealed) and additively manufactured (i.e., “3D printed”) Ti-6Al-4V. Three different methods of additive manufacturing have been exploited to produce the materials, including large-volume electron beam additive manufacturing, large-volume laser hot wire additive manufacturing, and small-volume selective laser melting. The general fundamental expressions are independent not only of the additive manufacturing process, but also of a wide variety of post-deposition heat treatments, however the coefficients are specific to material states. Thus, this work demonstrates that it is possible to predict not only the ultimate tensile strength, but also the full true stress, true strain curves, if certain parameters of the material are known. In general, the prediction of ultimate tensile strength are within 5% of the experimentally measured values across all additive manufacturing variants and subsequent heat treatments. The absolute values of ultimate tensile strength range from ~ 910 MPa to ~ 1170 MPa for the single alloy Ti-6Al-4V. Data representing 113 explicit samples are included in this work.

36 MATERIALS SCIENCE↗

Milestone 1.2.11: H 2 Production from Surrogate Non-Native Corrosion Plumes on Aluminum 6061-T6 Fuel Cladding Surrogates

Thick, localized, “non-native” corrosion plumes have been identified on Advanced Test Reactor fuel elements, raising concern on their impact on the radiolytic formation of molecular hydrogen gas (H 2 ) from aluminum-clad spent nuclear fuel (ASNF) under proposed extended (> 50 years) dry storage conditions. Here, we report our findings on H 2 generation from the gamma irradiation (up to 52 MGy) of surrogate “non-native” corrosion plume coupons: ambient-temperature-corroded (~350 days in water) aluminum alloy 6061 (AA6061) coupons in helium gas environments with ~0% added relative humidity. Additionally, we provide a comparison of proposed ASNF drying techniques— vacuum drying only, vacuum drying + 100 °C for 4 hr, and vacuum drying + 220 °C for 4 hr—on the yield of H 2 from these surrogate systems. The presented data indicates that similar amounts of H 2 (~2 × 10–3 µmol J–1) are formed from gamma irradiated AA6061 coupons corroded under different temperature regimes, i.e., ambient/350 days vs. 90 C/30 days. These findings validate current, complimentary modelling predictions based on high-temperature-corrosion irradiation data only. Further, the application of a heat treatment procedure (100 and 220 °C), in conjunction with vacuum drying, accelerated the rate at which a steady-state H 2 yield was attained, in comparison to vacuum only, due to the removal of H 2 precursors in the form of adsorbed waters. Interestingly, within the confidence limits of our measurements, negligible difference in total H 2 yield was found between the two investigated heat treatment procedures.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗