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At least 19 records

Microstructural Evolution and Mechanical Properties of LP-DED NASA HR-1 – A Hydrogen Resistant AM Superalloy for Space Propulsion Applications

The National Aeronautics and Space Administration (NASA) has actively pursued metal additive manufacturing (AM) technologies for spaceflight applications since the late 2000s. AM offers transformative advantages in cost, schedule, part consolidation, and design flexibility. Among the various AM techniques, laser powder directed energy deposition (LP-DED) is particularly well suited for fabricating complex geometries with fine feature resolution. In propulsion systems that utilize high-pressure gaseous hydrogen—such as liquid hydrogen rocket engines—hydrogen environment embrittlement (HEE) presents a serious threat to material performance 1,2 . Mechanical property degradation under these conditions can compromise component reliability, especially under cyclic loading. To address this challenge, NASA developed NASA HR-1 (Hydrogen Resistant-1) as a solution for liquid rocket engine components operating in hydrogen-rich environments, using the LP-DED technique 3-9 . A key component in a liquid rocket engine is the exhaust nozzle, which is typically regeneratively cooled (regen) due to the high heat flux. NASA HR-1 was specifically developed for regen nozzle applications using hydrogen as a propellant, providing resistance to HEE, a critical issue for many materials. The AM version of NASA HR-1 was also formulated to achieve high ultimate tensile strength, along with high yield strength and ductility in this environment 5,6 . Low-cycle fatigue (LCF) is another important consideration in nozzle design, as components are expected to endure multiple starts and missions. Additionally, the LP-DED version of the alloy exhibits improved thermal conductivity compared to its wrought counterpart, which benefits nozzle cooling. Overall, NASA HR-1 offers an excellent balance of high strength, HEE resistance, LCF performance, thermal conductivity, and ductility to meet the demanding requirements of channel-cooled nozzles and other components used with hydrogen and other propellants. The LP-DED–processed NASA HR-1 requires several post-processing heat treatment steps to achieve the material properties desirable for its intended application 6 . These steps include stress relief, homogenization, solution annealing, and aging for precipitation hardening. The stress relief treatment mitigates residual stresses accumulated during the LP-DED process and minimizes the potential for distortion. Homogenization, a common step for AM materials, reduces elemental segregation and promotes recrystallization to develop a more equiaxed grain structure. The subsequent solution annealing treatment heats the part to a solid solution temperature to dissolve the undesirable η-phase that forms during cooling from homogenization, followed by rapid cooling to retain an η-phase–free microstructure. Finally, aging promotes precipitation of the strengthening γ′ phase in the alloy. The integration of compositional design and optimized thermal processing enables high-quality LP-DED NASA HR-1 components with excellent microstructural and mechanical stability. Improved chemical and microstructure homogeneity enhances ductility and fatigue resistance—both critical for safe and reliable operation in high-pressure hydrogen environments. NASA has successfully fabricated and hot-fire tested multiple subscale and full-scale channel wall nozzles using LP-DED NASA HR-1 5,6, 9-14 . These efforts included process refinements to support thin-wall construction and various channel geometries. Throughout development, several key observations emerged. After homogenization, the as-built columnar grain structure transforms into a fully equiaxed microstructure. However, subsequent treatments—such as solution annealing and aging—result in changes that are more difficult to track. The grain structure remains largely unchanged, and the γ′ precipitates, typically 5–10 nm in diameter, are beyond the resolution of scanning electron microscopy (SEM). While transmission electron microscopy (TEM) can resolve these fine precipitates, TEM sample preparation is time-consuming and difficult for LP-DED material. As an alternative, differential scanning calorimetry (DSC) offers a useful, qualitative approach to monitor precipitate evolution throughout different stages of heat treatment. The overall goal is to improve the understanding of how heat treatment affects the microstructure and mechanical performance of LP-DED NASA HR-1. This paper presents heat treatment design considerations, microstructural characterization, mechanical testing – including tensile and LCF testing in both air and hydrogen environments.

Superalloy

Environmental hydrogen embrittlement of an alpha-beta titanium alloy - Effect of microstructure.

Study of environmental hydrogen embrittlement of a Ti-6 Al-4 alloy as a function of test displacement rate and of variations in alpha-beta microstructure. Embrittlement in low-pressure (about 1 atm) gaseous hydrogen was inversely dependent on test displacement rate and strongly dependent on microstructure. At a given displacement rate, microstructures having a continuous alpha-phase matrix were less severely embrittled than those having a continuous beta-phase matrix. Further, brittle fracture occurred in the former microstructures by transgranular cleavage and in the latter microstructures by intergranular separation. These observations are consistent with previous studies made on slow strain-rate embrittlement of hydrogen-charged titanium alloys and are explained in terms of relative hydrogen transport rates within the alpha-phase and beta-phase titanium.

Nelson, H. G.

A microstructural lattice model for strain oriented problems: A combined Monte Carlo finite element technique

A specialized, microstructural lattice model, termed MCFET for combined Monte Carlo Finite Element Technique, was developed which simulates microstructural evolution in material systems where modulated phases occur and the directionality of the modulation is influenced by internal and external stresses. In this approach, the microstructure is discretized onto a fine lattice. Each element in the lattice is labelled in accordance with its microstructural identity. Diffusion of material at elevated temperatures is simulated by allowing exchanges of neighboring elements if the exchange lowers the total energy of the system. A Monte Carlo approach is used to select the exchange site while the change in energy associated with stress fields is computed using a finite element technique. The MCFET analysis was validated by comparing this approach with a closed form, analytical method for stress assisted, shape changes of a single particle in an infinite matrix. Sample MCFET analytical for multiparticle problems were also run and in general the resulting microstructural changes associated with the application of an external stress are similar to that observed in Ni-Al-Cr alloys at elevated temperature.

Gayda, J.

Influence of convection on microstructure

The mechanism responsible for the difference in microstructure caused by solidifying the MnBi-Bi eutectic in space is sought. The objectives for the three year period are as follows: (1) completion of the following theoretical analyses - determination of the influence of the Soret effect on the average solid composition versus distance of off-eutectic mixtures directionally solidified in the absence of convection, determination of the influence of convection on the microstructure of off-eutectic mixtures using a linear velocity profile in the adjacent melt, determination of the influence of volumetric changes during solidification on microconvection near the freezing interface and on microstructure, and determination of the influence of convection on microstructure when the MnBi fibers project out in front of the bismuth matrix; (2) search for patterns in the effect of microgravity on different eutectics (for example, eutectic composition, eutectic temperature, usual microstructure, densities of pure constituents, and density changes upon solidification); and (3) determination of the Soret coefficient and the diffusion coefficient for Mn-Bi melts near the eutectic composition, both through laboratory experiements to be performed here and from data from Shuttle experiments.

Wilcox, William R.

Revealing the microstructure of materials

The objectives are to demonstrate how the microstructure of materials may be revealed by abrasive polishing and chemical etching, and to illustrate how microstructural information is used to monitor manufacturing processes, provide in-depth inspection, and perform failure analysis. Microstructural analysis is the procedure used to reveal the internal microstructural details of a material or part by sectioning and polishing the cut surface so that it may be examined under a suitable microscope. A printed wiring board was selected as the test material because it contains both metals and nonmetals that have distinctive microstructures, and because this technique is used throughout the electronic industry as a key quality control tool. The three principle component materials in printed circuit boards are glass/epoxy laminates faced with copper foil; copper, deposited by both electroless and electrolytic plating; and tin/lead solder. Sample preparation, mounting, grinding, polishing, and examination and analysis are discussed.

Nelson, James A.

Review of the Effects of Microstructure on Fatigue in Aluminum Alloys

Literature survey was conducted to determine the effects of different microstructural features and different load histories on fatigue crack initiation and propagation of aluminum alloys. Comparison of microstructure and monotonic and cyclic properties between powder metallurgy (P/M) and ingot metallurgy (I/M) alloys is presented. The two alloys that are representative of each process on which the comparison is focused are X7091 and 7050. Included is a detailed description of the microstructure produced through the P/M and I/M proesses. The effect of each pertinent microstructural feature on monotonic and cyclic properties, such as yield strength, toughness, crack initiation and propagation is discussed. Also discussed are the proposed mechanisms for crack initiation and propagation, as well as the effects of aggressive environments on these cyclic properties. The effects of variable amplitude loadin on fatigue crack propagation and the various models proposed to predict load interaction effects are discussed.

Telesman, J.

Microstructural evolution in the HAZ of Inconel 718 and correlation with the hot ductility test

The nickel-base alloy 718 was evaluated to study the role of preweld heat treatment in reducing or eliminating heat-affected zone hot cracking. Three heat treatments were studied using the Gleeble hot ductility test. A modified hot ductility test was also used to follow the evolution of microstructure during simulated welding thermal cycles. The microstructural evolution was correlated with the hot ductility data in order to evaluate the mechanism of hot cracking in alloy 718. The correlation of hot ductility with microstructure showed that recrystallization, grain growth, and dissolution of precipitates did not in themselves cause any loss of ductility during cooling. Ductility loss during cooling was not initiated until the constitutional liquation of NbC particles was observed in the microstructure. Laves-type phases were found precipitated in the solidified grain boundaries but were not found to correlate with any ductility loss parameter. Mechanisms are reviewed which help to explain how heat treatment controls the hot crack susceptibility of alloy 718 as measured in the hot ductility test.

Thompson, R. G.

Relationships between microstructure and microfissuring in alloy 718

Microfissures which occur in the weld heat affected zone of alloy 718 can be a limiting factor in the material's weldability. Several studies have attempted to relate microfissuring susceptibility to processing conditions, microstructure, and/or heat-to-heat chemistry differences. The present investigation studies the relationships between microstructure and microfissuring by isolating a particular microstructural feature and measuring microfissuring as a function of that feature. Results to date include the identification of a microstructure-microfissure sequence, microfissuring susceptibility as a function of grain size, and microfissuring susceptibility as a function of solution annealing time.

Thompson, R. G.

Effect of convection on the microstructure of the MnBi/Bi eutectic

For the quasi-regular fibrous microstructure of MnBi formed at freezing rates of 9 mm/h and above, good agreement between experimental and theoretical results for fiber spacing, freezing rate, radial position, and ampoule rotation rate is found. For the irregular blade-like microstructure formed at lower freezing rates, convection is found to coarsen the microstructure somwhat more than predicted. The volume fraction of MnBi was also shown to depend on ampoule rotation and radial position, even in the absence of ampoule rotation. The two-fold finer microstructure observed in space-processed material could not be explained by the elimination of buoyancy-driven natural convection.

Eisa, Gaber Faheem

Thermal stability of the microstructure of an aged Nb-Zr-C alloy

The effects of thermal aging with and without an applied stress on the microstructure of a Nb-Zr-C alloy containing 0.9 wt percent Zr and 0.06 wt percent C were studied. Chemical analysis, metallographic examination, energy dispersive x-ray spectra of the bulk material, and chemical and x-ray analyses of the phase-extracted residue were used to characterize the microstructure. The samples examined were from a creep strength study involving hot and cold working, and various combinations of exposure to temperatures ranging from 1350 to 1755 K with and without applied load for times as long as 34,000 plus hours. The results showed that the initial microstructure consisted primarily of orthorombic precipitates of Nb sub 2 C which were partially or completely transformed to face-centered cubic carbides of nb and Zr, (Zr, Nb)C, upon prolonged exposure to elevated temperatures. Furthermore, it was found that the microstructure of the alloy is extremely stable owing to the very finely distributed precipitates throughout its matrix and along the grain boundaries. The lattice parameters of the cubic carbides were determed to vary from 0.458 to 0.465 nm as the Zr/Nb ratio varied from 38/62 to 75/25.

Uz, Mehmet

Property and microstructural nonuniformity in the yttrium-barium-copper-oxide superconductor determined from electrical, magnetic, and ultrasonic measurements

The purpose of this dissertation was the following: (1) to characterize the effect of pore fraction on a comprehensive set of electrical and magnetic properties for the yttrium-barium-copper-oxide (YBCO) high temperature ceramic superconductor; and (2) to determine the viability of using a room-temperature, nondestructive characterization method to aid in the prediction of superconducting (cryogenic) properties. The latter involved correlating ultrasonic velocity measurements at room temperature with property-affecting pore fraction and oxygen content variations. The use of ultrasonic velocity for estimating pore fraction in YBCO is presented, and other polycrystalline materials are reviewed, modeled, and statistically analyzed. This provides the basis for using ultrasonic velocity to interrogate microstructure. The effect of pore fraction (0.10-0.25) on superconductor properties of YBCO samples was characterized. Spatial (within-sample) variations in microstructure and superconductor properties were investigated, and the effect of oxygen content on elastic behavior was examined. Experimental methods used included a.c. susceptibility, electrical, and ultrasonic velocity measurements. Superconductor properties measured included transition temperature, magnetic transition width, transport and magnetic critical current density, magnetic shielding, a.c. loss, and sharpness of the voltage-current characteristics. An ultrasonic velocity image constructed from measurements at 1mm increments across a YBCO sample revealed microstructural variations that correlated with variations in magnetic shielding and a.c. loss behavior. Destructive examination using quantitative image analysis revealed pore fraction to be the varying microstructural feature.

Roth, Don J.

Thermal stability of the microstructure of an aged Nb-Zr-C alloy

The effects of thermal aging with and without an applied stress on the microstructure of a Nb-Zr-C alloy containing 0.9 wt percent Zr and 0.06 percent C were studied. Chemical analysis, metallographic examination, energy dispersive X-ray spectra of the bulk material, and chemical and X-ray analyses of the phase-extracted residue were used to characterize the microstructure. The samples examined were from a creep strength study involving hot and cold working, and various combinations of exposure to temperatures ranging from 1350 to 1755 K with and without applied load times as long as 34,000 plus hours. The results showed that the initial microstructure consisted primarily of orthorombic precipitates of Nb sub C which were partially or completely transformed to face-centered cubic carbides of Nb and Zr, (Zr, Nb)C, upon prolonged exposure to elevated temperatures. Furthermore, it was found that the microstructure of the alloy is extremely stable owing to the very finely distributed precipitates throughout its matrix and along the grain boundaries. The lattice parameters of the cubic carbides were determined to vary from 0.458 to 0.465 nm as the Zr/Nb ratio varied from 38/62 to 75/25.

Uz, Mehmet

Avoidance of stress corrosion susceptibility in high strength aluminum alloys by control of grain boundary and matrix microstructure

The relation of microstructure to the mechanical strength and stress corrosion resistance of highest strength and overaged tempers of BAR and 7050 aluminum alloys was investigated. Comparison is made with previously studied 7075 aluminum alloy. Optical microscopy, transmission electron microscopy, and differential scanning calorimetry were used to characterize the grain morphology, matrix microstructure, and grain boundary microstructure of these tempers. Grain boundary interparticle spacing was significant to stress corrosion crack propagation for all three alloys; increasing interparticle spacing led to increased resistance to crack propagation. In addition, the fire grain size in Bar and 7050 appears to enhance crack propagation. The highest strength temper of 7050 has a comparatively high resistance to crack initiation. Overall stress corrosion behavior is dependent on environment pH, and evaluation over a range of pH is recommended.

Adler, P.

Microstructure and mechanical properties of hip-consolidated Rene 95 powders

The effects of heat-treatments on the microstructure of P/M Rene 95 (a nickel-based powder metal), consolidated by the hot-isostatic pressing (HIP), were examined. The microstructure of as-HIP'd specimen was characterized by highly serrated grain boundaries. Mechanical tests and microstructural observations reveal that the serrated grain boundaries improved ductility at both room and elevated temperatures by retarding crack propagation along grain boundaries.

Shimanuki, Y.

Influence of cobalt, tantalum, and tungsten on the microstructure and mechanical properties of superalloy single crystals

The influence of Co, Ta, and W on the microstructure and mechanical properties of nickel base super-alloy single crystals was investigated. A matrix of alloys was based on Mar-M 247 stripped of C, B, Zr, and Hf. The microstructures of the alloys were examined using optical and electron microscopy, phase extraction, X-ray diffraction, and differential thermal analysis. Tensile and creep-rupture tests were performed at 1000 C. An increase in tensile and creep strength resulted when Co was removed from alloys containing high refractory metal contents, but Co effects were negligible for alloys with lower refractory metal levels. In the composition range studied, W was more effective than Ta in increasing the creep resistance. The mechanical properties are discussed in relation to the microstructures of the alloys.

Nathal, M. V.

Influence of the microstructure on the corrosion behavior of magnetron sputter-quenched amorphous metallic alloys

The microstructure and corrosion behavior of magnetron sputter deposited amorphous metallic films of (Mo6ORu40)82B18 under varying sputtering atmospheres have been investigated. The microstructural details and topology of the films have been studied by scanning electron microscopy and correlated with the deposition conditions. By reducing the pressure of pure argon gas, the characteristic features of rough surface and columnar growth full of vertical voids can be converted into a mirror-smooth finish with very dense deposits. Films deposited in the presence of O2 or N2 exhibit columnar structure with vertical voids. Film deposited in pure argon at low pressure show remarkably high corrosion resistance due to the formation of a uniform passive surface layer. The influence of the microstructure and surface texture on the corrosion behavior is discussed.

Thakoor, A. P.

The effect of microstructure on 650 C fatigue crack growth in P/M Astroloy

The effect of microstructure on fatigue crack propagation at 650 C has been studied in a P/M nickel-base superalloy, Astroloy. Crack propagation data were obtained in air and vacuum at 20 cpm with a modified compact tension specimen. The rate of crack growth, da/dn, was correlated with the stress intensity range. Key microstructural variables examined were grain size and the distribution and size of the strengthening gamma prime phase. A fine grain size less than 20 microns always promoted rapid, intergranular failure, while a large grain size promoted slower, transgranular failure which decreased as the size and volume fraction of aging gamma prime was manipulated so as to increase alloy strength. The rapid, intergranular mode of failure of the fine grain microstructures was suppressed in vacuum.

Gayda, J.

Microstructures and properties of rapidly solidified alloys

The microstructure and properties of rapidly solidified aluminum alloys were researched. The effects of powder and flake chemistry and morphology and alternative consolidation processing parameters are being conducted. Samples of the powders being utilized were obtained for comprehensive metallurgical characterization. Seven aluminum alloys in the form of thin foils were studied by a variety of techniques including optical metallography, scanning electron microscope, and transmission electron microscope. Details of the microstructural characteristics are presented along with a discussion of the solidification process. A better understanding of the microstructure of the rapidly solidified aluminum alloys prepared by a variety of techniques such as roller quenching, the vacuum atomized procedure, ultrasonically atomized in inert atmospheres, and atomized in flue gas was provided.

Shechtman, D.