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NASA NTRS2003

Microstructure and Mechanical Properties of Extruded Gamma Microstructure Met PX

A gamma TiAl alloy with a high Nb content is being assessed as a compressor blade material. The microstructure and mechanical properties of extruded Ti-45Al-X(Nb,B,C) (at.%) were evaluated in both an as-extruded condition and after a lamellar heat treatment. Tensile behavior of both as-extruded and lamellar heat treated specimens was studied in the temperature range of RT to 926 C. In general, the yield stress and ultimate tensile strength reached relatively high values at room temperature and decreased with increasing deformation temperature. The fatigue strength of both microstructures was characterized at 650 C and compared to a baseline TiAl alloy and to a Ni-base superalloy. Tensile and fatigue specimens were also exposed to 800 C for 200 h in air to evaluate the alloy's environmental resistance. A decrease in ductility was observed at room temperature due to the 800 C. exposure but the 650 C fatigue properties were unaffected. Compressive and tensile creep testing between 727 and 1027 C revealed that the creep deformation was reproducible and predictable. Creep strengths reached superalloy-like levels at fast strain rates and lower temperatures but deformation at slower strain rates and/or higher temperature indicated significant weakening for the as-extruded condition. At high temperatures and low stresses, the lamellar microstructure had improved creep properties when compared to the as-extruded material. Microstructural evolution during heat treatment, identification of various phases, and the effect of microstructure on the tensile, fatigue, and creep behaviors is discussed.

Draper, S. L.↗

NASA NTRS1994

Influence of convection on microstructure

The primary motivation for this research was to determine the cause for space processing altering the microstructure of some eutectics, especially the MnBi-Bi eutectic. Four primary hypotheses were to be tested under this current grant: (1) A fibrous microstructure is much more sensitive to convection than a lamellar microstructure, which was assumed in our prior theoretical treatment. (2) An interface with one phase projecting out into the melt is much more sensitive to convection than a planar interface, which was assumed in our prior theoretical treatment. (3) The Soret effect is much more important in the absence of convection and has a sufficiently large influence on microstructure that its action can explain the flight results. (4) The microstructure is much more sensitive to convection when the composition of the bulk melt is off eutectic. These hypotheses were tested. It was concluded that none of these can explain the Grumman flight results. Experiments also were performed on the influence of current pulses on MnBi-Bi microstructure. A thorough review was made of all experimental results on the influence of convection on the fiber spacing in rod eutectics, including results from solidification in space or at high gravity, and use of mechanical stirring or a magnetic field. Contradictory results were noted. The predictions of models for convective influences were compared with the experimental results. Vigorous mechanical stirring appears to coarsen the microstructure by altering the concentration field in front of the freezing interface. Gentle convection is believed to alter the microstructure of a fibrous eutectic only when it causes a fluctuating freezing rate with a system for which the kinetics of fiber branching differs from that for fiber termination. These fluctuations may cause the microstructure to coarsen or to become finer, depending on the relative kinetics of these processes. The microstructure of lamellar eutectics is less sensitive to freezing rate fluctuations and to gentle convection.

Wilcox, William R.↗

NASA NTRS2022

Analysis of Base Metal Microstructures and Mechanical Properties of a Single-Piece, Spin-Formed Forward Pressure Vessel Bulkhead

In 2012, a pathfinder forward pressure vessel bulkhead (FPVBH) for the Orion Multi-Purpose Crew Vehicle (MPCV) was fabricated using aluminum (Al) alloy 2219. The demonstration article was offered as a replacement for the baseline configuration, which at that time was a multi-piece welded construction using aluminum-lithium (Al-Li) alloy 2195. In 2014, the NASA Engineering and Safety Center (NESC) funded a Phase I effort to explore spin-forming as a manufacturing method to produce a complex-shaped, single-piece FPVBH for the crew module (CM) [1]. The primary focus of the NESC effort was to expand spin-forming technology to the fabrication of an Al-Li 2195 FPVBH. As a result, limited testing and analysis was performed on the original Al 2219 article. In this study, a sufficiently large plate of Al 2219 was not available for the fabrication of a FPVBH. Therefore, the forming blank comprised two plates (from different lots) butt welded together using a single friction stir weld. The welded forming blank was then spin formed into the FPVBH configuration and heat treated to the T62 temper. Mechanical property testing of the spin-formed 2219-T62 FPVBH revealed that the tensile properties were comparable to the Metallic Material Properties Development and Standardization (MMPDS) A-basis allowable for Al 2219-T6 wrought products. However, post-spin forming application of the standard heat treatment produced large, recrystallized grains in the material. The response varied within the two plates; one plate lot exhibited nearly complete recrystallization, while the other lot contained bands of recrystallization. Although no reduction in tensile properties was observed due to these microstructural variations, a more detailed investigation was recommended to better understand the effect of spin forming on the recrystallization mechanism and the impact on other material properties. The current study examined the microstructure and mechanical properties of the fully processed Al 2219-T62 FPVBH with emphasis on comparing differences between the two plates. Testing was limited to the cone region of the FPVBH. The two specific tasks in this study were: a) Characterization of the microstructure and mechanical properties in the two plates used in the FPVBH. b) Isolation of the impact of each step in the thermo-mechanical processing (TMP) sequence of the FPVBH on recrystallization and grain growth. Mechanical property testing sampled regions containing both large, recrystallized and small, unrecrystallized grains. Tensile strengths and elongations were equivalent in both regions and exceeded MMPDS A-basis allowables. Fracture toughness was equivalent in both regions and fracture morphology was typical of aluminum alloys. The fatigue precrack region of the fracture toughness specimens appeared more faceted in the recrystallized plate. This suggests that property testing that is more sensitive to grain size, such as fatigue crack growth rate and stress corrosion cracking, may be warranted. Alcoa reviewed the production records for the two plate lots and confirmed that composition of both plates was within the allowable range for Al 2219 and that plate processing steps were all performed within production limits. However, the Fe content was notably higher in the fully recrystallized plate, resulting in a greater volume fraction of large Fe-bearing inclusions and Al-Cu constituent particles. Alcoa did not provide details regarding plate processing variables for the two plate lots. It was surmised that deformation by hot rolling was the most accurate TMP simulation of commercial spin forming within a laboratory setting. Both hot rolling and spin forming comprise combinations of shear and compressive deformation. The through-thickness strain caused by hot rolling is symmetrical about the mid-plane, as the rollers contact both sides of the material. Shear strains are maximum at the inner and outer surfaces and trend toward zero at the mid-thickness. In contrast, spin forming utilizes a single roller on the outer surface, producing a gradient in shear stress through the thickness. Shear strains in spin-formed material are highest at the outer surface due to direct contact with the roller, and trend toward zero at the inner surface. Consequently, there will undoubtedly be some discrepancies in the mechanical response of hot-rolled and spin-formed products in the through-thickness direction. Interrupted TMP simulations were performed on remnant plate from the FPVBH forming blank in order to isolate the effects of a post-weld anneal, spin-forming deformation/thermal cycling, and solution heat treatment (SHT) on development of the recrystallized microstructures. Analysis confirmed that large, recrystallized grains formed exclusively during SHT and only after a certain deformation level was exceeded. Remnant plate from both lots that received thermal processing only did not exhibit recrystallization but exhibited fully recrystallized microstructures when processed by hot rolling. This indicates that (1) the level of deformation exceeded the critical level for recrystallization in both plates and (2) that the level of deformation during hot rolling was greater than that which accumulated during spin forming of the FPVBH. Comparison of the hot-rolled plate with the spin-formed material showed that the recrystallized grain size was larger in the FPVBH, providing further evidence that deformation levels were lower in the FPVBH. The most plausible explanation for the differing degrees of recrystallization in the two plates is particle stimulated nucleation (PSN) at the Fe-bearing inclusions and large Al-Cu constituent particles. In the plate with higher solute content, the greater volume fraction of these particles reduces the deformation level required to promote recrystallization. During spin forming the critical deformation level was likely exceeded for the higher Fe content plate resulting in a fully recrystallized microstructure. The lower Fe content plate developed a microstructure that exhibited bands of recrystallization due to the combination of a non-uniform distribution of particles and deformation. The critical deformation required for recrystallization was likely only exceeded during spin forming in regions of higher particle content. While there were differences in Fe content between these lots of Al 2219 plate, the composition of both was within defined alloy limits and Alcoa reported no anomalies during plate production. The observed differences in recrystallization after spin forming may reflect the inherent variability between these two lots of plate. The spin-forming vendor, Spincraft, reported that similar variations in recrystallized microstructures have been observed during examination of multiple spin-forming trials of a different 2xxx series aluminum alloy. Hence, tighter chemical specification limits on impurity levels in Al 2219 plate may help ensure uniform, predictable microstructures. Finally, the tensile and fracture toughness properties were not affected by the microstructural variations noted.

single-piece↗

NASA NTRS1999

Use of Microgravity to Control the Microstructure of Eutectics

This grant began in June of 1996. Its long term goal is to be able to control the microstructure of directionally solidified eutectic alloys, through an improved understanding of the influence of convection. The primary objective of the projects in the present grant is to test hypotheses for the reported influence of microgravity on the microstructure of eutectics. The prior experimental results on the influence of microgravity on the microstructure of eutectics have been contradictory. With lamellar eutectics, microgravity had a negligible effect on the microstructure. Microgravity experiments with fibrous eutectics sometimes showed a finer microstructure and sometimes a coarser microstructure. Most research has been done on the MnBi/Bi rod-like eutectic. Larson and Pirich obtained a two-fold finer microstructure both from microgravity and by use of a magnetic field to quench buoyancy-driven convection. Smith, on the other hand, observed no change in microgravity. Prior theoretical work at Clarkson University showed that buoyancy-driven convection in the vertical Bridgman configuration is not vigorous enough to alter the concentration field in front of a growing eutectic sufficiently to cause a measurable change in microstructure. We assumed that the bulk melt was at the eutectic composition and that freezing occurred at the extremum, i.e. with minimum total undercooling at the freezing interface. There have been four hypotheses attempting to explain the observed changes in microstructure of fibrous eutectics caused by convection: I .A fluctuating freezing rate, combined with unequal kinetics for fiber termination and branching. 2. Off-eutectic composition, either in the bulk melt due to an off-eutectic feed or at the freezing interface because of departure from the extremum condition. 3. Presence of a strong habit modifying impurity whose concentration at the freezing interface would be altered by convection. At the beginning of the present grant, we favored the first of these hypotheses and set out to test it both experimentally and theoretically. We planned the following approaches: I .Pass electric current pulses through the MnBi/Bi eutectic during directional solidification in order to produce an oscillatory freezing rate. 2. Directionally solidify the MnBi/Bi eutectic on Mir using the QUELD II gradient freeze furnace developed by Professor Smith at Queen's University. 3. Select another fibrous eutectic system for investigation using the Accelerated Crucible Rotation Technique to introduce convection. 4. Develop theoretical models for eutectic solidification with an oscillatory freezing rate. Because of the problems with Mir, we substituted ground-based experiments at Queen's University with QUELD II vertical and horizontal, with and without vibration of the furnace. The Al-Si system was chosen for the ACRT experiments. Three related approaches were used to model eutectic solidification with an oscillatory freezing rate. A sharp interface model was used to calculate composition oscillations at the freezing interface in response to imposed freezing rate oscillations.

Wilcox. William R.↗

NASA NTRS1992

Influence of convection on microstructure

The primary motivation for this research has been to determine the cause for space processing altering the microstructure of some eutectics, especially the MnBi-Bi eutectic. Prior experimental research at Grumman and here showed that the microstructure of MnBi-Bi eutectic is twice as fine when solidified in space or in a magnetic field, is uninfluenced by interfacial temperature gradient, adjusts very quickly to changes in freezing rate, and becomes coarser when spin-up/spin-down (accelerated crucible rotation technique) is used during solidification. Theoretical work at Clarkson predicted that buoyancy driven convection on earth could not account for the two fold change in fiber spacing caused by solidification in space. However, a lamellar structure with a planar interface was assumed, and the Soret effect was not included in the analysis. Experimental work at Clarkson showed that the interface is not planar, and that MnBi fibers project out in front of the Bi matrix on the order of one fiber diameter. Originally four primary hypotheses were to be tested under this current grant: (1) a fibrous microstructure is much more sensitive to convection than a lamellar microstructure, which was assumed in our prior theoretical treatment; (2) an interface with one phase projecting out into the melt is much more sensitive to convection than a planar interface, which was assumed in our prior theoretical treatment; (3) the Soret effect is much more important in the absence of convection and has a sufficiently large influence on microstructure that its action can explain the flight results; and (4) the microstructure is much more sensitive to convection when the composition of the bulk melt is off eutectic. As reported previously, we have learned that while a fibrous microstructure and a non-planar interface are more sensitive to convection than a lamellar microstructure with a planar interface, the influence of convection remains too small to explain the flight and magnetic field results. Similarly addition of the Soret effect does not explain the flight and magnetic field results.

Wilcox, William R.↗

NASA NTRS1999

Role of Dynamic Nucleation at Moving Boundaries in Phase and Microstructure Selection

Solidification microstructures that form under steady-state growth conditions (cells, dendrites, regular eutectics, etc.) are reasonably well understood in comparison to other, more complex microstructures, which form under intrinsically non-steady-state growth conditions due to the competition between the nucleation and growth of several phases. Some important practical examples in this latter class include microstructures forming in peritectic systems in highly undercooled droplets, and in strip cast stainless steels. Prediction of phase and microstructure selection in these systems has been traditionally based on (1) heterogeneous nucleation on a static interface, and (2) comparing the relative growth rate of different phase/microstructures under steady-state growth conditions. The formation of new phases, however, occurs via nucleation on, or ahead of, a moving boundary. In addition, the actual selection process is controlled by a complex interaction between the nucleation process and the growth competition between the nuclei and the pre-existing phase under non-steady-state conditions. As a result, it is often difficult to predict which microstructure will form and which phases will be selected under prescribed processing conditions. This research addresses this critical role of nucleation at moving boundaries in the selection of phases and solidification microstructures through quantitative experiments and numerical modeling in peritectic systems. In order to create a well characterized system in which to study this problem, we focus on the directional solidification of hypo- and hyper-peritectic alloys in the two-phase region, imposing a large enough ratio of temperature gradient/growth rate (G/V(sub p)) to suppress the morphological instability of both the parent (alpha) and peritectic (Beta) phases, i.e. each phase alone would grow as a planar front. Our combined experimental and theoretical results show that, already in this simplified case, the growth competition of these two phases leads to a rich variety of microstructures that depend sensitively upon the relative importance of nucleation, diffusion, and convection.

Karma, Alain↗

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.↗

NASA NTRS2002

Dual Microstructure Heat Treatment of a Nickel-Base Disk Alloy Assessed

Gas turbine engines for future subsonic aircraft will require nickel-base disk alloys that can be used at temperatures in excess of 1300 F. Smaller turbine engines, with higher rotational speeds, also require disk alloys with high strength. To address these challenges, NASA funded a series of disk programs in the 1990's. Under these initiatives, Honeywell and Allison focused their attention on Alloy 10, a high-strength, nickel-base disk alloy developed by Honeywell for application in the small turbine engines used in regional jet aircraft. Since tensile, creep, and fatigue properties are strongly influenced by alloy grain size, the effect of heat treatment on grain size and the attendant properties were studied in detail. It was observed that a fine grain microstructure offered the best tensile and fatigue properties, whereas a coarse grain microstructure offered the best creep resistance at high temperatures. Therefore, a disk with a dual microstructure, consisting of a fine-grained bore and a coarse-grained rim, should have a high potential for optimal performance. Under NASA's Ultra-Safe Propulsion Project and Ultra-Efficient Engine Technology (UEET) Program, a disk program was initiated at the NASA Glenn Research Center to assess the feasibility of using Alloy 10 to produce a dual-microstructure disk. The objectives of this program were twofold. First, existing dual-microstructure heat treatment (DMHT) technology would be applied and refined as necessary for Alloy 10 to yield the desired grain structure in full-scale forgings appropriate for use in regional gas turbine engines. Second, key mechanical properties from the bore and rim of a DMHT Alloy 10 disk would be measured and compared with conventional heat treatments to assess the benefits of DMHT technology. At Wyman Gordon and Honeywell, an active-cooling DMHT process was used to convert four full-scale Alloy 10 disks to a dual-grain microstructure. The resulting microstructures are illustrated in the photomicrographs. The fine grain size in the bore can be contrasted with the coarse grain size in the rim. Testing (at NASA Glenn) of coupons machined from these disks showed that the DMHT approach did indeed produce a high-strength, fatigue resistant bore and a creep-resistant rim. This combination of properties was previously unobtainable using conventional heat treatments, which produced disks with a uniform grain size. Future plans are in place to spin test a DMHT disk under the Ultra Safe Propulsion Project to assess the viability of this technology at the component level. This testing will include measurements of disk growth at a high temperature as well as the determination of burst speed at an intermediate temperature.

Gayda, John↗

NASA NTRS2010

Microstructure Modeling of Third Generation Disk Alloys

The objective of this program was to model, validate, and predict the precipitation microstructure evolution, using PrecipiCalc (QuesTek Innovations LLC) software, for 3rd generation Ni-based gas turbine disc superalloys during processing and service, with a set of logical and consistent experiments and characterizations. Furthermore, within this program, the originally research-oriented microstructure simulation tool was to be further improved and implemented to be a useful and user-friendly engineering tool. In this report, the key accomplishments achieved during the third year (2009) of the program are summarized. The activities of this year included: Further development of multistep precipitation simulation framework for gamma prime microstructure evolution during heat treatment; Calibration and validation of gamma prime microstructure modeling with supersolvus heat treated LSHR; Modeling of the microstructure evolution of the minor phases, particularly carbides, during isothermal aging, representing the long term microstructure stability during thermal exposure; and the implementation of software tools. During the research and development efforts to extend the precipitation microstructure modeling and prediction capability in this 3-year program, we identified a hurdle, related to slow gamma prime coarsening rate, with no satisfactory scientific explanation currently available. It is desirable to raise this issue to the Ni-based superalloys research community, with hope that in future there will be a mechanistic understanding and physics-based treatment to overcome the hurdle. In the mean time, an empirical correction factor was developed in this modeling effort to capture the experimental observations.

Jou, Herng-Jeng↗

NASA NTRSDate not supplied

Microstructure Quantification and Random Forest Regression Models for Li4Ti5O12–Ni Property Prediction

All-solid-state structural lithium-ion batteries are sought to enable all-electric propulsion in next generation aerospace concepts through improved safety and systems level weight savings. In this work, the influence of processing conditions on microstructural evolution was evaluated for anode composites of strain-free Li4Ti5O12 and metallic nickel current collector. Beyond size distributions, this study explored methods of quantifying microstructural features that describe changes in the spatial distribution and coalescence of nickel particles as a function of sample composition and sintering conditions. Processing-microstructure-property relationships were described by microstructure quantifiers including nickel particle count per area, nearest neighbor distance distribution, and edge-to-edge distance distribution. Machine learning methods were applied to compare the relative influence of processing conditions and microstructural features on electrical conductivity and mechanical strength to optimize for simultaneous energy storage and load bearing performance. Insights gained from this work inform future evaluation of alternative energy storage materials and microstructures for multifunctional performance, and generation of microstructural descriptors strengthens modeling across length scales.

anode↗

NASA NTRS1992

Solidification in immiscible systems: The influence of processing conditions on resulting microstructures

Research carried out over the past two decades in which attempts have been made to produce desirable microstructures in immiscible alloys is reviewed. Factors affecting the formation of desirable microstructures in immiscible alloys are addressed and some of the techniques that have been successful in controlling these factors in order to produce useful structures are discussed. Some of the intended applications of these alloys require a dispersion of one phase in the other, while other applications favor the use of aligned, fibrous microstructures with continuity of both phases. The microstructures obtained in immiscible alloys are often strongly influenced by processing conditions. Perhaps the most well known effect is gravity induced sedimentation of the denser immiscible phase during solidification. This difficulty with sedimentation led to low gravity processing in attempts to produce dispersed microstructures. However, experimentation under low gravity conditions soon revealed that many other factors, including wetting of the crucible walls and surface tension driven flows, often resulted in complete separation and coalescence of the two immiscible phases. The production of aligned fibrous microstructures in hypermonotectic alloys appears to be even more difficult than the formation of a dispersion. Here, in addition to sedimentation and crucible wetting, convective and interfacial instabilities must be considered as well. Calculation of the limits of stability during directional solidification were carried out but require experimental verification.

Andrews, J. Barry↗

NASA NTRS2017

Correlations Among Microstructure, Morphology, Chemistry, and Isotopic Systematics of Hibonite in CM Chondrites

Introduction: Hibonite is a primary refractory phase occurring in many CAIs, typically with spinel and perovskite. Our microstructural studies of CAIs from carbonaceous chondrites reveal a range of stacking defect densities and correlated non-stoichiometry in hibonite. We also conducted a series of annealing experiments, demonstrating that the Mg-Al substitution stabilized the formation of defect-structured hibonite. Here, we continue a detailed TEM analysis of hibonite-bearing inclusions from CM chondrites that have been well-characterized isotopically. We examine possible correlations of microstructure, morphology, mineralogy, and chemical and isotopic systematics of CM hibonites in order to better understand the formation history of hibonite in the early solar nebula. Methods: Fifteen hibonite-bearing inclusions from the Paris CM chondrite were analyzed using a JEOL 7600F SEM and a JEOL 8530F electron microprobe. In addition to three hibonite-bearing inclusions from the Murchison CM chondrite previously reported, we selected three inclusions from Paris, Pmt1-6, 1-9, and 1-10, representing a range of 26Al/27Al ratios and minor element concentrations for a detailed TEM study. We extracted TEM sections from hibonite grains using a FEI Quanta 3D field emission gun SEM/FIB. The sections were then examined using a JEOL 2500SE field-emission scanning TEM equipped with a Thermo-Noran thin window EDX spectrometer. Results and Discussion: A total of six hibonite-bearing inclusions, including two platy hibonite crystals (PLACs) and four spinel-hibonite inclusions (SHIBs), were studied. There are notable differences in chemical and isotopic compositions between the inclusions (Table 1), indicative of their different formation environment or timing. Our TEM observations show perfectly-ordered, stoichiometric hibonite crystals without stacking defects in two PLACs, 2-7-1 and 2-8-2, and in three SHIBs, Pmt1-6, 1-9, and 1-10. In contrast, SHIB 1-9-5 hibonite grains contain a low density of stacking defects linked to an increase in MgO contents, indicating complex, disordered intergrowths of stoichiometric and MgO-enriched hibonites. From the data collected to date, we find no clear correlation between the microstructures of hibonite and its morphological and mineralogical types that reflect distinct chemical and isotopic systematics [6-8,10]. Interestingly, the presence of no or few stacking defects in hibonite from the PLACs and SHIBs are in contrast to our experimental studies that produced very high densities of stacking defects in hibonite [3-5]. Unlike our experi-ments, electron microprobe data from the PLACs and SHIBs hibonite grains show a strong correlation between (Ti4++Si4+) and Mg2+ cations, suggesting that coupled substitutions of (Ti4++Mg2+) and (Si4++Mg2+) for 2Al3+ inhibit the formation of defect-structured hibonite. However, our experimental studies suggest that kinetics (e.g., cooling rate) or other thermal effects also exert a strong control on the microstructures and chemical compositions of hibonite. In Pmt1-6, elongated perovskite grains present at the hibonite grain boundaries display (121) twinning, indicative of a fast cooling (>50degC/min) after high-temperature events. Therefore, the nebular microstructural characteristics of hibonite, at least in this inclusion, would not have destroyed by subsequent high-temperature annealing. Conclusions: Our TEM observations thus far show no clear correlation in microstructures, morphological and mineralogical characteristics, and chemical and isotopic systematics of hibonites from CM chondrites. The observed variation in stacking defect densities in the hibonites may be controlled by thermal processes in the early solar nebula. A detailed TEM analysis of additional CM hibonite samples is underway to evaluate this hypothesis.

Han, J.↗

NASA NTRSDate not supplied

Zircon (U-Th)/He Impact Crater Thermochronometry and the Effects of Shock Microstructures on Helium Diffusion Kinetics

Accurate and precise age determination of impact cratering events remains challenging and often contentious; less than half of all known craters are regarded as accurately and precisely dated. Zircon (U-Th)/He (ZHe) dating of impactites can be employed to date medium to large impact structures as ZHe ages can be fully reset in minutes at T >1000°C, a plausible scenario in the central melt pool. In contrast, complete resetting of ZHe at 200-300°C, encountered near the crater margins or due to post-impact hydrothermal overprinting, may take >103-6 years. To test the reliability of ZHe impact dating, we have quantified the effects of shock-induced microstructures on helium diffusion kinetics in well-characterized variably shocked zircon. We investigated samples from two impact structures, the Chicxulub multi-ring crater and Ries complex crater, to compare diffusion kinetics from structures with different size, age, and hydrothermal system longevity. Shock microstructures were characterized by backscattered-electron imaging prior to determining the He diffusion kinetics by prograde and retrograde fractional-release experiments via light-bulb furnace with incremental step-heating (10°C) from 300°C to 600°C. Next, we examine the internal interconnectivity and sizes of the diffusion domains by EBSD. While we found that zircon with few shock microstructures exhibited no marked deviation from helium diffusion kinetics of undamaged zircon, zircon grains with planar microstructures and granular textures are characterized by a dramatic decrease in helium retentivity due to the reduction in the effective domain size and the introduction of interconnected fast diffusion pathways. A subset of grains were ZHe dated and showed that less deformed grains yielded a weighted mean age within error of the accepted impact ages, while the grains with planar microstructures or granular textures gave systematically younger ages. These new diffusion data and ZHe ages demonstrate that highly shocked grains are unsuitable for ZHe impact crater dating. Therefore, detailed characterization of impact-induced microstructures is critical for determining accurate ZHe impact ages and offers the possibility of investigating post-impact hydrothermal circulation.

Zircon↗

NASA NTRSDate not supplied

The Porous Microstructure Analysis (PuMA) software

The open-source Porous Microstructure Analysis (PuMA) software was implemented to offer an efficient framework for determining material characteristics from 3D microstructures. Its development was inspired by progress in X-ray microtomography, an imaging technology that captures the internal structure of materials in 3D, and even in a 4D temporal context. Over recent years, this method has transformed the domain of materials science due to its capability to non-destructively examine material microstructures while presenting digital data about their geometrical details. It has provided insights into materials relevant to several NASA missions, including heatshields, parachute fabrics, meteorites, and other advanced composites. PuMA, in its current version 3, delivers an array of features, spanning from basic geometric insights of a microstructure to intricate anisotropic thermo-elastic and chemical behavior. Specifically, the software evaluates morphological attributes (specific surface area, volume fractions, mean intercept lengths, orientation) and physical characteristics (conductivity, elasticity, permeability, and tortuosity). Additionally, it can model material degradation processes, such as oxidation and surface chemistry interactions. The software can generate synthetic microstructures, from straightforward geometrical designs to intricate woven and non-woven geometries. Coupling material generation and characterization enable parametric studies and sensitivity analysis to optimize the microstructural performance and inform design decisions and reliability assessment based on uncertainty quantification. A recent addition to PuMA includes the TomoSAM plugin, devised to incorporate the cutting-edge Segment Anything Model (SAM). SAM is a promptable deep learning model that can identify objects and create image masks in a zero-shot manner, based only on a few user clicks. The synergy between these tools aids in the segmentation of complex 3D datasets from tomography or other imaging techniques, which would otherwise require a laborious manual segmentation process.

Tomography↗

NASA NTRSDate not supplied

The Porous Microstructure Analysis (PuMA) software

The open-source Porous Microstructure Analysis (PuMA) software was created to offer an efficient framework for determining material properties from 3D microstructures. Its development was inspired by progress in X-ray microtomography, an imaging technology that captures the internal structure of materials in 3D, and even in a 4D temporal context. Over recent years, this method has transformed the domain of materials science due to its capability to non-destructively examine material microstructures while presenting digital data about their geometrical details. It has provided insights into materials relevant to several NASA missions, including heatshields, parachute fabrics, meteorites, and other advanced composites. PuMA, in its current version 3, delivers an array of features, spanning from basic geometric insights of a microstructure to intricate anisotropic thermo-elastic and chemical behavior. Specifically, the software evaluates morphological attributes (specific surface area, volume fractions, mean intercept lengths, orientation) and physical characteristics (conductivity, elasticity, permeability, and tortuosity). Additionally, it can model material degradation processes, such as oxidation and surface chemistry interactions. The software can generate synthetic microstructures, from straightforward geometrical designs to intricate woven and non-woven geometries. Coupling material generation and characterization enables parametric studies and sensitivity analysis to optimize the microstructural performance and inform design decisions and reliability assessment based on uncertainty quantification. A recent addition to PuMA includes the TomoSAM plugin, devised to incorporate the cutting-edge Segment Anything Model (SAM) into our image segmentation workflow. SAM is a promptable deep learning model that can identify objects and create image masks in a zero-shot manner, based only on a few user clicks. The synergy between these tools aids in the segmentation of complex 3D datasets from tomography and other imaging techniques, which would otherwise require a laborious manual segmentation process.

Tomography↗

NASA NTRS2026

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↗

NASA NTRS2020

An Algorithm for Characterization of Fiber Aggregation in Composite Microstructures

Composite structures are susceptible to localized flaws, or variability, that drive global failure. To capture this variance, a multiscale model needs to be introduced that not only accurately represents the statistical nature of the composite microstructure but is also efficient. At the microscale, fiber aggregation creates local stress concentrations, where failure is likely to occur sooner than expected. A method of rapid microstructure generation, in conjunction with cluster characterization, is examined to develop accurate reproductions of 2D composite cross-sections. Parameterization of shape and size of fiber clusters is used to characterize representative volume elements. The discrete element method is used to generate pseudo-microstructures. The clustering parameters from the pseudo- and actual microstructure arrangements (obtained from micrographs) can be compared to determine the validity of the representative volume element generated with the discrete element method. Results show a promising approach to evaluating randomness of fiber distributions and how to accurately recreate microstructures for strength analysis.

Carbon fiber↗

NASA NTRS1972

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.↗