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All sourcesNASA NTRSDOE OSTI
NASA NTRSDate not supplied

Quick and Correlative TOF-SIMS Analysis of Dispersoid Content in Powder Feedstock and Printed Oxide Dispersion Strengthened Alloys

Oxide dispersion strengthening (ODS) of metal alloys, when combined with additive manufacturing (AM), can be used to solve high-temperature material application problems. The performance of ODS materials is dependent on nano-scale oxide being distributed uniformly throughout the metal matrix; a homogenous distribution is critical to the creep and yield strength. Therefore, quantifying and analyzing these oxide nanoparticles is essential for ODS alloy development. Assessing the chemistry and morphology of dispersoids in a material can be conducted using a variety of X-ray and electron-based methods. Time of Flight Secondary Ion Mass Spectrometry (TOF-SIMS), which assesses chemical concentrations from ion masses, provides the necessary spatial resolution and avoids potential spectral overlap of all elements present. In this work, preparing ODS powder feedstock and Laser Powder Bed Fusion AM was conducted with a NiCoCr alloy and yttria dispersoid, mixed with a Resodyn resonance mixer and printed on an EOS M100 3D printer at NASA Glenn. TOF-SIMS was performed on a Physical Electronics NanoTOF TRIFT V TOF-SIMS at Case Western Reserve University. The TOF-SIMS results collected on the feedstock powder samples correspond to the qualitative interpretation of the homogeneity of the oxide coating on the metal powder from SEM images. This provides quantitative support to the qualitative microscopy images collected earlier in the process design phase. The variance in the yttrium distribution on the powder feedstock samples also correlated with the variance of the yttrium distribution detected in the printed samples. This correlation supported the hypothesis that an even coating of yttria on the metal powders contributes to an even distribution of yttria in the printed material.

Laura G. Wilson↗
NASA NTRS1977

Creep degradation in oxide-dispersion-strengthened alloys

Oxide dispersion strengthened Ni-base alloys in wrought bar form are studied for creep degradation effects similar to those found in thin gage sheet. The bar products evaluated included ODS-Ni, ODS-NiCr, and three types of advanced ODS-NiCrAl alloys. Tensile test specimens were exposed to creep at various stress levels at 1365 K and then tensile tested at room temperature. Low residual tensile properties, change in fracture mode, the appearance of dispersoid-free bands, grain boundary cavitation, and internal oxidation in the microstructure were interpreted as creep degradation effects. This work showed that many ODS alloys are subject to creep damage. Degradation of tensile properties occurred after very small amounts of creep strain, ductility being the most sensitive property. All the ODS alloys which were creep damaged possessed a large grain size. Creep damage appears to have been due to diffusional creep which produced dispersoid-free bands around boundaries acting as vacancy sources. Low angle and possibly twin boundaries acted as vacancy sources.

Whittenberger, J. D.↗
NASA NTRS1982

Long-term high-velocity oxidation and hot corrosion testing of several NiCrAl and FeCrAl base oxide dispersion strengthened alloys

Several oxide dispersion strengthened (ODS) alloys have been tested for cyclic, long-term, high gas-velocity resistance to oxidation at 1100 C and hot corrosion at 900 C. Both nominally Ni-16Cr-4Al and Fe-20Cr-4.5Al ODS alloys were subjected up to about 2500 cycles, where each cycle consisted of 1 hr in a hot, Mach 0.3 combusted gas stream followed by a 3-min quench in an ambient temperature, Mach 0.3 air blast. For comparison to existing technology, a coated superalloy was simultaneously tested. The ODS iron alloy exhibited clearly superior behavior, surviving 3800 oxidation and 2300 hot corrosion cycles essentially unscathed. While the ODS nickel alloys exhibited adequate oxidation resistance, the long-term hot corrosion resistance could be marginal, since the best life for such alloys under these conditions was only about 1100 cycles. However, the hot corrosion resistance of the ODS Ni-base alloys is excellent in comparison to that of traditional superalloys.

Lowell, C. E.↗
NASA NTRS1978

Longitudinal shear behavior of several oxide dispersion strengthened alloys

Two commercial oxide dispersion strengthened (ODS) alloys, MA-753 and MA-754, and three experimental ODS alloys, MA-757E, MA-755E, and MA-6000E, were tested in shear at 760 C. Comparisons were made with other turbine blade and vane alloys. All of the ODS alloys exhibited less shear strength than directionally solidified Mar-M 200 = Hf or then conventionally cast B-1900. The strongest ODS alloy tested, MA-755E, was comparable in both shear and tensile strength to the lamellar directionally solidified eutectic alloy gamma/gamma prime - delta. Substantial improvements in shear resistance were found for all alloys tested when the geometry of the specimen was changed from one generating a transverse tensile stress in the shear area to one generating a transverse compressive stress. Finally, 760 C shear strength as a fraction of tensile strength was found to increase linearly with the log of the transverse tensile ductility.

Glasgow, T. K.↗
NASA NTRS1977

Longitudinal shear behavior of several oxide dispersion strengthened alloys

Two commercial oxide dispersion strengthened (ODS) alloys, MA-753 and MA-754, and three experimental ODS alloys, MA-757E, MA-755E, and MA-6000E, were tested in shear at 760 C. Comparisons were made with other turbine-blade and vane alloys. All of the ODS alloys exhibited less shear strength than directionally solidified Mar-M 200 + Hf or than conventionally cast B-1900. The strongest ODS alloy tested, MA-755E, was comparable in both shear and tensile strength to the lamellar directionally solidified eutectic alloy gamma/gamma-prime - delta. Substantial improvements in shear resistance were found for all alloys tested when the geometry of the specimen was changed from one generating a transverse tensile stress in the shear area to one generating a transverse compressive stress. Finally, 760-C shear strength as a fraction of tensile strength was found to increase linearly with the log of the transverse tensile ductility.

Glasgow, T. K.↗
NASA NTRS1977

Manufacture and engine test of advanced oxide dispersion strengthened alloy turbine vanes

Oxide-Dispersion-strengthened (ODS) Ni-Cr-Al alloy systems were exploited for turbine engine vanes which would be used for the space shuttle thermal protection system. Available commercial and developmental advanced ODS alloys were evaluated, and three were selected based on established vane property goals and manufacturing criteria. The selected alloys were evaluated in an engine test. Candidate alloys were screened by strength, thermal fatigue resistance, oxidation and sulfidation resistance. The Ni-16Cr (3 to 5)Al-ThO2 system was identified as having attractive high temperature oxidation resistance. Subsequent work also indicated exceptional sulfidation resistance for these alloys.

Bailey, P. G.↗
NASA NTRS1975

Preliminary study of oxide-dispersion-strengthened B-1900 prepared by mechanical alloys

An experimental oxide dispersion strengthened (ODS) alloy based on the B-1900 composition was produced by the mechanical alloying process. Without optimization of the processing for the alloy or the alloy for the processing, recrystallization of the extruded product to large elongated grains was achieved. Materials having grain length-width ratios of 3 and 5.5 were tested in tension and stress-rupture. The ODS B-1900 exhibited tensile strength similar to that of cast B-1900. Its stress-rupture life was lower than that of cast B-1900 at 760 C. At 1095 C the ODS B-1900 with the higher grain length-width ratio (5.5) had stress-rupture life superior to that of cast B-1900. It was concluded that, with optimization, oxide dispersion strengthening of B-1900 and other complex cast nickel-base alloys has potential for improving high temperature properties over those of the cast alloy counterparts.

Glasgow, T. K.↗
DOE OSTI2026

Electric-field-assisted-sintering of rare-earth oxide dispersion strengthened Fe-Cr-Mo alloys

Oxide dispersion-strengthened (ODS) alloys are widely recognized for their exceptional high-temperature strength, creep resistance, and radiation tolerance, making them indispensable for advanced nuclear reactors, aerospace, and energy systems. Achieving a fine and stable dispersion of oxide nanoparticles is critical, as these particles act as strong barriers to dislocation motion and effective sinks for irradiation-induced defects, ensuring structural integrity under extreme conditions. Here, in this study, Fe–Cr–Mo-based ODS alloys were fabricated via mechanical alloying and consolidated using electric-field-assisted sintering (EFAS) with additions of Y 2 O 3 , La 2 O 3 , and CeO 2 . EFAS processing produced ultrafine-grained microstructures (average grain size <1 μm) with uniformly distributed oxide clusters (2–4 nm). Atom probe tomography revealed that La 2 O 3 -containing alloys exhibited the highest nanoparticle number density, resulting in superior tensile strength compared to yttria- and ceria-bearing counterparts. The combined effect of grain refinement and rare-earth oxide dispersion significantly enhanced mechanical performance, demonstrating the potential of EFAS for developing high-strength ferritic alloys for demanding environments such as nuclear systems.

36 - MATERIALS SCIENCE↗
NASA NTRS1981

Comparative thermal fatigue resistance of several oxide dispersion strengthened alloys

The thermal fatigue resistance of several oxide dispersion strengthened (ODS) alloys has been evaluated through cyclic exposure in fluidized beds. The ODS nickel-base alloy MA 754 and ODS iron-base alloy MA 956 as well as four experimental ODS Ni-16Cr-4.5Al base alloys with and without Ta additions were examined. Both bare and coated alloys were subjected to up to 6000 cycles where each cycle consisted of a 3 minute immersion in a fluidized bed at 1130 C followed by a 3 minute immersion in a bed at 357 C. Testing revealed that the thermal fatigue resistance of the ODS nickel-base alloys was excellent and about equal to that of directionally solidified superalloys. However, the thermal fatigue resistance of MA 956 was found to be poor. Metallographic examination of tested specimens revealed that, in general, the post-test microstructures can be rationalized on the basis of previous diffusion, mechanical property, and oxidation studies.

Whittenberger, J. D.↗
NASA NTRS1980

Recrystallization characteristics of oxide dispersion strengthened nickel-base alloys

Electron microscopy was employed to study the process of recrystallization in two oxide dispersion strengthened (ODS) mechanically alloyed nickel-base alloys, MA 754 and MA 6000E. MA 754 contained both fine, uniformly dispersed particles and coarser oxides aligned along the working direction. Hot rolled MA 754 had a grain size of 0.5 microns and high dislocation densities. After partial primary recrystallization, the fine grains transformed to large elongated grains via secondary (or abnormal) grain growth. Extruded and rolled MA 6000E contained equiaxed grains of 0.2 micron diameter. Primary recrystallization occurring during working eliminated virtually all dislocations. Conversion from fine to coarse grains was triggered by gamma prime dissolution; this was also a process of secondary or abnormal grain growth. Comparisons were made to conventional and oxide dispersion strengthened nickel-base alloys.

Hotzler, R. K.↗
NASA NTRS2023

Additive Manufacturing of Oxide Dispersion Strengthened Multi Principle Element Alloys for Future Aerospace Applications

Oxide Dispersion Strengthened (ODS) materials have long been of interest for their high temperature applications, and additive manufacturing enables their manufacturing viability. The ODS multi-principle element alloy NiCoCr was prepared using powder metallurgy techniques, additively manufactured, and evaluated for its processingmicrostructure-property relationships. The high temperature foundations of nickel-base superalloys and ODS materials were combined with the manufacturing advantages of 3D printing and the chemical simplicity of NiCoCr to inspire this work, which was divided into powder and printed material assessments. The project was achieved through multiple iterative project loops to assess the processing parameters’ impact on the microstructure and mechanical properties of the feedstock powder and printed material. The powder investigations (Chapter 3) focused on understanding the oxide coating that formed on the metal powder following acoustic mixing. Time of Flight Secondary Ion Mass Spectrometry was used to semi-quantitatively assess the amount of yttrium on the surface of the mixed powders, and indicated that a combination of higher mixing condition energy and moderate mixing time resulted in the most oxide coating on the NiCoCr powder. The results were supported by a qualitative assessment of scanning electron images of coated powder particles. Following mixing, the ODS NiCoCr was consolidated by Laser Powder Bed Fusion. The evaluations of the printed material (Chapter 4) frst considered screening experiments including Archimedes’ density, porosity, and grain size and number metrics from electron backscatter diffraction data. After the ideal additive manufacturing parameters were identifed, both the oxide homogeneity and yield strength were discussed for the idealized printed material. Overall, the project suggests that the combined use of qualitative or semi-quantitative powder surface analysis with Archimedes’ density analyses can be a valid high-throughput technique which can lead to process optimization of Laser Powder Bed Fusion additively manufactured ODS material.

Laura G Wilson↗
NASA NTRS1988

MATE (Materials for Advanced Turbine Engines) Program, Project 3. Volume 2: Design, fabrication and evaluation of an oxide dispersion strengthened sheet alloy combustor liner

The suitability of wrought oxide dispersion strengthened (ODS) superalloy sheet for gas turbine engine combustor applications was evaluated. Two yttria (Y2O3) dispersion strengthened alloys were evaluated; Incoloy MA956 and Haynes Development Alloy (HDA) 8077 (NiCrAl base). Preliminary tests showed both alloys to be potentially viable combustor materials, with neither alloy exhibiting a significant advantage over the other. MA956 was selected as the final alloy based on manufacturing reproducibility for evaluation as a burner liner. A hybrid PW2037 inner burner liner containing MA956 and Hastelloy X components and using a louvered configuration was designed and constructed. The louvered configuration was chosen because of field experience and compatibility with the bill of material PW2037 design. The simulated flight cycle for the ground based engine tests consisted of 4.5 min idle, 1.5 min takeoff and intermediate conditions in a PW2037 engine with average uncorrected combustor exit temperature of 1527 C. Post test evaluation consisting of visual observations and fluorescent penetrant inspections was conducted after 500 cycles of testing. No loss of integrity in the burner liner was shown.

Bose, S.↗
NASA NTRS2019

Additive Manufacturing of Oxide Dispersion Strengthened (ODS) Nickel-Based Superalloys

Additive manufacturing of oxide dispersion strengthened (ODS) Ni-based superalloys, via powder bed techniques, could enable near-net-shape manufacturing of intricately shaped components for aerospace applications. This has the potential to transform the design and manufacturing of hot sections of engines which face demands for ever-rising operating temperatures. The goal of this project is to lay the scientific foundation for additive manufacturing of ODS alloys. The objective of this poster is to present work to date as well as proposed future work.

Wilson, Laura G.↗
NASA NTRS1980

Creep and stress rupture of oxide dispersion strengthened mechanically alloyed Inconel alloy MA 754

The creep and stress rupture behavior of the mechanically alloyed oxide dispersion strengthened nickel-base alloy MA 754 was studied at 760, 982 and 1093 C. Tensile specimens with a fine, highly elongated grain structure, oriented parallel and perpendicular to the longitudinal grain direction were tested at various stresses in air under constant load. It was found that the apparent stress dependence was large, with power law exponents ranging from 19 to 33 over the temperature range studied. The creep activation energy, after correction for the temperature dependence of the elastic modulus, was close to but slightly larger than the activation energy for self diffusion. Rupture was intergranular and the rupture ductility as measured by percentage elongation was generally low, with values ranging from 0.5 to 16 pct. The creep properties are rationalized by describing the creep rates in terms of an effective stress which is the applied stress minus a resisting stress consistent with the alloy microstructure. Values of the resisting stress obtained through a curve fitting procedure are found to be close to the values of the particle by-pass stress for this oxide dispersion strengthened alloy, as calculated from the measured oxide particle distribution.

Howson, T. E.↗
NASA NTRS1981

Oxidation and hot corrosion of coated and bare oxide dispersion strengthened superalloy MA-755E

Cyclic hot corrosion and oxidation of an experimental oxide dispersion strengthened (ODS) superalloy MA-755E were conducted in a hot gas stream at Mach 0.3. The response of the ODS alloy, bare or with protective coatings, was similar to that of a conventional cast alloy, IN-792, in hot corrosion at 900 C. However, during oxidation at 1100 and 1150 C the ODS alloy differed from the cast alloy by developing a greater amount of subsurface porosity. Compared with a diffused aluminide coating, an electron beam vapor deposited NiCrAlY coating offered superior oxidation protection and decreased porosity formation. In additional testing, the tendency to form porosity was associated with the large grains of recrystallized powder metallurgy alloys but was independent of the presence of an oxide dispersion.

Glasgow, T. K.↗
NASA NTRS1976

Oxide dispersion strengthened nickel produced by nonreactive milling

It is shown that oxide dispersion strengthened alloys can be produced by a postulated nonreactive milling mechanism whereby the dispersoid is trapped at the interface between welding metal powder particles. This interparticle welding is possible because, without a suitable and sufficiently vigorous chemical reaction between the metal powder particles and the milling fluid, no protective, weld-preventing reaction coating is formed on these particles. Using water as the nonreactive milling fluid, Ni - 1.8-vol % thoria and Ni - 1.8-vol % yttria alloys with 1093 C tensile strengths ranging from 122.3 to 141.5 MN/sq m (17,900 to 20,500 psi) were produced by nonreactive milling.

Arias, A.↗