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NASA NTRS1977

The effect of microstructure and strength on the fracture toughness of an 18 Ni, 300 grade maraging steel

Fractography and metallographic sectioning were used to investigate the influence of microstructure and strength on the fracture toughness (KIc) and fracture mechanism of an 18 Ni, 300 grade maraging steel. Increased yield strength from 1442 to 2070 MN/m squared through precipitation hardening results in a KIc loss from 143 to 55 MN/m superscript 3/2. Ti (C,N) Ti2S, and TiC inclusions in sizes from 1 to 8, 1 to 15, and 0.1 to 2 microns respectively serve as sites for void nucleation and lead to fracture by the dimpled rupture process in all strength levels considered. TiC nucleated dimples occupy more than half the fracture in all conditions. Void nucleation rate and resultant number of dimples per unit area of fracture increase with increasing yield strength. Average dimple size decreases with increasing strength and/or overaging which follows from the decreasing amount of stable void growth measured by sectioning tensile specimens. Void growth is assisted by crack branching along a path of TiC inclusions. Coalescence occurs in the highest strength materials by a combination of TiC void nucleation and premature separation at strengthening precipitates.

Psioda, J. A.↗

NASA NTRS2003

Ultra-high Temperature Ceramic Composites for Leading Edges

Ultra-high temperature ceramics (UHTC) have performed unreliably due to material flaws and attachment design. These deficiencies are brought to the fore by the low fracture toughness and thermal shock resistance of UHTC. If these deficiencies are overcome, we are still faced with poor oxidation resistance as a limitation on UHT applicability to reusable launch vehicles. We have been addressing the deficiencies of UHTC for the past two years via a small task at GRC that is in the Airframe part of the Next Generation Launch Technology Program. Our focus is on composite constructions and functional grading to address the mechanical issues and on composition modification to address the oxidation issue. The progress on approaches to improving oxidation resistance by alloying and functional grading will be reported. In particular, initial tests of tantalum additions have shown potential for major improvement. Less promising results of additional tests at higher temperatures will be presented. Two fabrication approaches are being pursued to produce carbon fiber reinforced UHTC composites: prepregging and rigid perform infiltration. Fabrication procedures and microstructures for composites will be reported.

Levine, Stanley R.↗

NASA NTRSDate not supplied

Recent Advances in Structural Carbon Nanotube Composites

Carbon nanotubes (CNT) have been a subject of investigation for more than two decades. Part of the interest in CNTs was driven by CNT tensile mechanical properties at the nanoscale that suggest their potential to outperform state-of-the-art (SOA) lightweight structural materials. Early work on the development of CNT nanocomposites involved the dispersion of CNT powder into polymer matrices. Although low levels of CNT doping resulted in meaningful increases in electrical conductivity to enable applications such as electrostatic charge dissipation, the highest concentrations of CNTs in these lightly doped nanocomposites did not yield mechanical properties that could compete with SOA carbon fiber composites. The maximum concentration of CNTs in lightly doped nanocomposites was limited to about 5% due to increases in viscosity that prevent the fabrication of good quality nanocomposites. At the lower concentrations, properties of the resulting nanocomposites were analogous to those of composites made with very short, chopped carbon fibers. About ten years ago, CNTs became available in continuous fiber form, allowing the investigation of processing methods to incorporate much higher CNT content into composites. Recent developments in CNT composite fabrication have yielded improved mechanical properties and indicate that while some standard carbon fiber composite processing methods can be used, CNTs have unique microstructural features that require techniques tailored to access the hierarchical features of CNTs. This presentation will discuss the evolution of structural CNT mechanical property advancements and collaboration mechanisms for research across federal labs, academia, and industry that accelerated the maturation of structural CNTs.

Carbon Nanotubes↗

NASA NTRS2006

Evaluation of Open Cell Foam Heat Transfer Enhancement for Liquid Rocket Engine

As NASA pursues the exploration mission, advanced propulsion for the next generation of spacecraft will be needed. These new propulsion systems will require higher performance and increased durability, despite current limitations on materials. A break-through technology is needed in the thrust chamber. In this paper the idea of using a porous metallic foam is examined for its potential cooling enhancement capabilities. The goal is to increase the chamber wall cooling without creating an additional pressure drop penalty. A feasibility study based on experiments at laboratory-scale conditions was performed and analysis at rocket conditions is underway. In the experiment, heat transfer and pressure drop data were collected using air as the coolant in a copper or nickel foam filled annular channel. The foam-channel performance was evaluated based on comparison with conventional microchannel cooling passages under equal pressure drop conditions. The heat transfer enhancement of the foam channel over the microchannel ranges from 130% to 172%. The enhancement is relatively independent of the pressure drop and increases with decreasing pore size. A direct numerical simulation model of the foam heat exchange has been built. The model is based on the actual metal foam microstructure of thin ligaments (0.2- 0.3 mm in diameter) that form a network of interconnected open-cells. The cell dimension is around 2 mm. The numerical model was built using the FLUENT CFD code. Comparison of the pressure drop results predicted by the current model with those experimental data of Leong and Jin [8] shows favorable comparisons. Pressure drop predictions have been made using hydrogen as a coolant at typical rocket conditions. Conjugate heat transfer analysis using the foam filled channel is planned for the future.

Chung, J. N.↗

NASA NTRS2021

Nanostructure and compositional segregation of soft magnetic FeNi-based nanocomposites with multiple nanocrystalline phases

Soft magnetic metal amorphous nanocomposite alloys are produced through rapid solidification and thermal annealing yielding nanocrystals embedded within an amorphous precursor. Similar free energies in Co-rich and FeNi-based alloy systems result in multiple nanocrystalline phases being formed during devitrification. Studies of multi-phase crystallization processes have been reported for Co-rich alloys but relatively few have investigated FeNi-based systems. A detailed characterization of compositional partitioning and microstructure of an optimally annealed FeNi-based MANC (Fe70Ni30)80Nb4Si2B14 alloy is presented through complementary high-resolution transmission electron microscopy (HRTEM) and atom probe tomography (APT). HRTEM demonstrates orientation relationships between FCC and BCC nanocrystals, suggesting heterogeneous nucleation of nanocrystals in the amorphous matrix or a cooperative mechanism of nucleation between BCC and FCC nanocrystallites. APT results show evidence for (i) the segregation of Fe and Ni between nanocrystals of different phases, (ii) B partitioning to the amorphous phase, and (iii) an Nb-enriched shell surrounding nanocrystals.

soft magnetic materials↗

NASA NTRS2024

A Diversity of Temperature and Pressure Conditions Recorded by Zircon within Suevite from Ries Crater, Germany

The temperature and pressure conditions experienced by rocks during an impact event can be constrained using petrologic and microstructural analysis and is crucial to providing ground truth to the impact cratering process. Suevite is a polymict, impact melt-bearing breccia, specific to Ries crater in Germany. There are competing models for suevite formation and emplacement, such as clastic flows pushed out of the crater rim or ejecta plume fallback. Knowledge of the temperature and pressure pathways recorded by grains within the suevite can help distinguish between these and other models. The accessory phase zircon (ZrSiO4) and its high-pressure polymorph reidite are particularly useful in such circumstances as they are highly refractory minerals that can record the high-temperature and/or high-pressure conditions of an impact event. Here we present evidence for a wide array of temperature and pressure conditions recorded in zircon grains within a single thin section of suevite. Zircons in this study range from unshocked to highly shocked (>53 GPa), and record temperatures more than 1673 °C. These findings confirm previous studies concluding that suevites contain material exposed to very diverse pressure and temperature conditions during initial shock compression and excavation but do not, as a whole, experience extreme temperatures (>1673 °C) or pressures (>30 GPa).

mineralogy↗

NASA NTRSDate not supplied

Advancement of Novel Additively Manufactured Alloys for Space Applications

NASA has been involved in the development and maturation of metal additive manufacturing (AM) for space applications since the late 2000’s. Several efforts have focused on the understanding of AM processes through material characterization and testing, standards development, component fabrication, and infusion into development and flight applications. While many common aerospace alloys have been and continue to be a focus of ongoing development, the need for custom-alloy developments for high performance applications enabled by AM processes has been realized. The applications being targeted are liquid rocket engines with high heat fluxes, high pressure, and that utilize propellants such as hydrogen, which can degrade the alloy. NASA has recently focused on the development and advancement of novel alloy advancement using AM for use in these harsh environments, such as GRCop-42, GRCop-84, NASA HR-1, and JBK-75. These alloys have been evaluated using the laser powder bed fusion (L-PBF) and laser powder directed energy deposition (LP-DED) processes. The results from these processes have demonstrated that AM can enable rapid development of new alloy systems that can yield higher performances. These alloys have undergone the fundamental metallurgical evaluations, heat treatment study, and microstructure characterization and mechanical testing campaign. This, combined with direct application-specific component fabrication and hot-fire testing, enabled the increase of the Technology Readiness Level (TRL). This presentation will provide a background and overview of these AM-enabled novel alloys, AM processing development including metallurgical and mechanical property studies. It will also cover the latest advancement in the parallel component development and testing and future developments. The goal of these alloy development is to allow for technology infusion into NASA and commercial spaceflight missions as well as to establish and sustain the needed commercial AM supply chain.

Additive Manufacturing↗

NASA NTRSDate not supplied

Advancement of Metal Additive Manufacturing Processes and Alloys for Rocket Propulsion Applications

NASA has been involved in the development and maturation of metal additive manufacturing (AM) for space applications since the 2000’s. Several efforts have focused on the understanding of AM processes through material characterization and testing, standards development, component fabrication, and infusion into development and flight applications. While many common aerospace alloys have been and continue to be a focus of ongoing development, the need for custom-alloy developments for high performance applications enabled by various AM processes has been realized. The applications being targeted are liquid rocket engines with high heat fluxes, high pressure, and that utilize propellants such as hydrogen, which can degrade the alloy. NASA has recently focused on the development and advancement of novel alloy advancement using AM for use in these harsh environments, such as GRCop-42, GRCop-84, NASA HR-1, and JBK-75. These alloys have been evaluated using powder bed fusion (PBF), directed energy deposition (DED), and solid-state AM processes. The results from these processes have demonstrated that AM can enable rapid development of new alloy systems that can yield higher performances across various metal AM processes. These alloys have undergone the fundamental metallurgical evaluations, heat treatment study, and microstructure characterization and mechanical testing campaign. This, combined with direct application-specific component fabrication and hot-fire testing, enabled the increase of the Technology Readiness Level (TRL). This presentation will provide a background and overview of various AM-enabled novel alloys, a comparison across the AM processes, and development including metallurgical and mechanical property studies. It will also cover the latest advancement in the parallel component development and testing and future developments. The goal of these alloy development and use of various AM processes is to allow for technology infusion into NASA and commercial spaceflight missions as well as to establish and sustain the needed commercial AM supply chain.

Additive Manufacturing↗

NASA NTRSDate not supplied

Metal Additive Manufacturing Developments for Propulsion Applications

Additive Manufacturing↗

NASA NTRS2024

Search for Presolar Materials and Isotopically Anomalous Diffuse Insoluble Organic Matter in Samples From Asteroid 101955 Bennu

Carbonaceous asteroids allow us to study the original materials that formed the planets in the protoplanetary disk. They contain organic matter and (sub-)micrometer-size dust grains, called presolar grains, that condensed in the circumstellar envelopes of evolved stars and the ejecta of stellar explosions, such as novae and supernovae, before the formation of our Solar System. The isotopically anomalous organics are thought to have formed in the interstellar medium and the early Solar System. Whereas presolar grains provide insight into the building blocks of our Solar System, studying organics can help us understand the origin of life on Earth. These organics might have contributed to ingredients that helped life emerge. The return of samples from asteroid 101955 Bennu by NASA’s Origins, Spectral Interpretation, Resource Identification, and Security–Regolith Explorer (OSIRIS-REx) mission gives us a new opportunity to elucidate the formation mechanism(s) and evolution of organics, as well as the abundance and distribution presolar grains in carbonaceous asteroids. Here, we report on our ongoing work to characterize the isotopic and chemical compositions, microstructure, distribution, and abundance of insoluble organic matter (IOM) and presolar grains in Bennu samples. This work supports hypotheses 2 and 3 of the OSIRIS-REx Sample Analysis Plan.

P. Haenecour↗

NASA NTRS2003

Ultra-High Temperature Ceramic Composites for Leading Edges

Ultra-high temperature ceramics (UHTC) have performed unreliably due to material flaws and attachment design. These deficiencies are brought to the fore by the low fracture toughness and thermal shock resistance of UHTC. If these deficiencies are overcome, we are still faced with poor oxidation resistance as a limitation on UHTC applicability to reusable launch vehicles. We have been addressing the deficiencies of UHTC for the past two years via a small task at GRC that is in the Airframe part of the Next Generation Launch Technology Program. Our focus is on composite constructions and functional grading to address the mechanical issues and on composition modification to address the oxidation issue. The progress on approaches to improving oxidation resistance by alloying and functional grading will be reported. In particular, initial tests of tantalum additions have shown potential for major improvement. Results for additional tests at higher temperatures will be presented. These oxidation improvements are being incorporated in the composites approaches. Two fabrication approaches are being persued to produce carbon fiber reinforced UHTC composites: prepregging and rigid perform infiltration. Fabrication procedures, microstructures, and initial mechanical property and oxidation results for composites will be reported.

Levine, Stanley R.↗

NASA NTRS2000

Assessment and Assurance of Microelectronics Packaging Technology of Microelectromechanical Systems (MEMS)

Microelectromechanical systems (MEMS) have shown a significant promise in the last decade for a variety of applications such as air-bag, pressure sensors, accelerometer, microgyro, etc. Standard semiconductor microelectronics packaging needs the integrated circuits to be protected from the harsh environment, and provide electrical communication with the other parts of the circuit, facilitate thermal dissipation efficiently, and impart mechanical strength to the silicon die. Microelectronics packaging involves wafer dicing, bonding, lead attachment, encapsulation to protect from the environment, electrical integrity, and package leak tests to assure the packaging technology. In the case of MEMS the microstructures (active elements) often interfaces with the hostile environment where packaging leak tests and testing of such devices using chemical and mechanical parameters will be very difficult and expensive. Packaging of MEMS is significantly complex as they serve to protect from the environment and microstructures interact with the same environment to measure or affect the desired physical or chemical parameters. The most of the silicon circuitry is sensitive to temperature, moisture, magnetic field, light, and electromagnetic interference. The package must then protect the on-board silicon circuitry while simultaneously exposing the microsensor to the effect it 'measures to assure the MEMS technology by lowering the risk to zero. MEMS technology has a major application in developing a microspacecraft for space systems provided assurance of MEMS technology is sufficiently addressed nondestructively. This technology would eventually miniaturize many of the components of the spacecraft to reach the NASA's safety and mission assurance goal by building faster, cheaper, better, smaller spacecraft to explore the space more effectively by teaming-up with the other NASA centers using the limited resources available. This paper discusses the latest developments in the MEMS technology and challenging issues in the packaging of hermetically sealed and non-hermetically sealed MEMS sensor devices based on silicon, poly-silicon, and other materials for microspacecraft applications considering the space environment and reliability assurance qualification guidelines in perspective. Acknowledgments: The above research work is supported by the NASA Electronics Parts and Packaging Program (NEPP) and performed by the Jet Propulsion Laboratory, California Institute of Technology, Pasadena, CA under a contract with the NASA - Code Q for the Office of Safety and Mission Assurance Program 323-79.

Ramesham, Rajeshuni↗

NASA NTRS1996

Microstructure, Chemistry, and Origin of Grain Rims on ilmenite from the Lunar Soil Finest Fraction

Analytical transmission electron microscope (TEM) observations reveal that ilmenite grains sampled from the sub-10 micron size fraction of Apollo 11 (10084) and Apollo 16 (61221, 67701) soils have rims 10-300 nm thick that are chemically and microstructurally distinct from the host ilmenite. The rims have a thin outer sublayer 10-50 nm thick that contains the ilmenite-incompatible elements Si, Al, Ca and S. This overlies a relatively thicker (50-250 nm) inner sublayer of nanocrystalline Ti-oxide precipitates in a matrix of single-crystal ilmenite that is structurally continuous with the underlying host grain. Microstructural information, as well as data from x-ray spectrometry (EDS) and electron energy loss spectrometry (EELS) analysis of the inner sublayer, suggest that both the inner and outer sublayer assemblages are reduced and that the inner layer is depleted in Fe relative to the underlying ilmenite. The chemistry of the outer sublayer suggests that it is a surface deposit of sputtered or impact-vaporized components from the bulk lunar soil. The inner sublayer is part of the original host grain that has been physically and chemically processed, but not amorphized, by solar ion irradiation and possibly some subsolidus heating. The fact that the deposited outer sublayer is consistently much thinner than the radiation-altered inner sublayer indicates that only a minor fraction of the total rim volume is a product of vapor or sputter deposition. This finding is in contrast to recent descriptions of thick deposited layers on one-third of regolith silicate grains and indicates that ilmenite and silicate rims as a group are different in the fraction of deposited material that they contain.

Christoffersen, Roy↗

NASA NTRS2005

Fatigue Behavior and Deformation Mechanisms in Inconel 718 Superalloy Investigated

The nickel-base superalloy Inconel 718 (IN 718) is used as a structural material for a variety of components in the space shuttle main engine (SSME) and accounts for more than half of the total weight of this engine. IN 718 is the bill-of-material for the pressure vessels of nickel-hydrogen batteries for the space station. In the case of the space shuttle main engine, structural components are typically subjected to startup and shutdown load transients and occasional overloads in addition to high-frequency vibratory loads from routine operation. The nickel-hydrogen battery cells are prooftested before service and are subjected to fluctuating pressure loads during operation. In both of these applications, the structural material is subjected to a monotonic load initially, which is subsequently followed by fatigue. To assess the life of these structural components, it is necessary to determine the influence of a prior monotonic load on the subsequent fatigue life of the superalloy. An insight into the underlying deformation and damage mechanisms is also required to properly account for the interaction between the prior monotonic load and the subsequent fatigue loading. An experimental investigation was conducted to establish the effect of prior monotonic straining on the subsequent fatigue behavior of wrought, double-aged, IN 718 at room temperature. First, monotonic strain tests and fully-reversed, strain-controlled fatigue tests were conducted on uniform-gage-section IN 718 specimens. Next, fully reversed fatigue tests were conducted under strain control on specimens that were monotonically strained in tension. Results from this investigation indicated that prior monotonic straining reduced the fatigue resistance of the superalloy particularly at the lowest strain range. Some of the tested specimens were sectioned and examined by transmission electron microscopy to reveal typical microstructures as well as the active deformation and damage mechanisms under each of the loading conditions. In monotonically strained specimens, deformation during the subsequent fatigue loading was mainly confined to the deformation bands initiated during the prior monotonic straining. This can cause dislocations to move more readily along the previously activated deformation bands and to pile up near grain boundaries, eventually making the grain boundaries susceptible to fatigue crack initiation. The mechanisms inferred from the microstructural investigation were extremely valuable in interpreting the influence of prior monotonic straining on the subsequent fatigue life of Inconel 718 superalloy.

Source record↗

NASA NTRS2014

Fabrication of Turbine Disk Materials by Additive Manufacturing

Precipitation-strengthened, nickel-based superalloys are widely used in the aerospace and energy industries due to their excellent environmental resistance and outstanding mechanical properties under extreme conditions. Powder-bed additive manufacturing (AM) technologies offer the potential to revolutionize the processing of superalloy turbine components by eliminating the need for extensive inventory or expensive legacy tooling. Like selective laser melting (SLM), electron beam melting (EBM) constructs three-dimensional dense components layer-by-layer by melting and solidification of atomized, pre-alloyed powder feedstock within 50-200 micron layers. While SLM has been more widely used for AM of nickel alloys like 718, EBM offers several distinct advantages, such as less retained residual stress, lower risk of contamination, and faster build rates with multiple-electron-beam configurations. These advantages are particularly attractive for turbine disks, for which excessive residual stress and contamination can shorten disk life during high-temperature operation. In this presentation, we will discuss the feasibility of fabricating disk superalloy components using EBM AM. Originally developed using powder metallurgy forging processing, disk superalloys contain a higher refractory content and precipitate volume fraction than alloy 718, thus making them more prone to thermal cracking during AM. This and other challenges to produce homogeneous builds with desired properties will be presented. In particular, the quality of lab-scale samples fabricated via a design of experiments, in which the beam current, build temperature, and beam velocity were varied, will be summarized. The relationship between processing parameters, microstructure, grain orientation, and mechanical response will be discussed.

oxidation↗

NASA NTRS1997

Creep and Rupture Strength of an Advanced CVD SiC Fiber

In the as-produced condition the room temperature strength (approx. 6 GPa) of Textron Specialty Materials' 50 microns CVD SiC fiber represents the highest value thus far obtained for commercially produced polycrystalline SiC fibers. To understand whether this strength can be maintained after composite processing conditions, high temperature studies were performed on the effects of time, stress, and environment on 1400 deg. C tensile creep strain and stress rupture on as-produced, chemically vapor deposited SiC fibers. Creep strain results were consistent, allowing an evaluation of time and stress effects. Test environment had no influence on creep strain but I hour annealing at 1600 deg. C in argon gas significantly reduced the total creep strain and increased the stress dependence. This is attributed to changes in the free carbon morphology and its distribution within the CVD SiC fiber. For the as-produced and annealed fibers, strength at 1400 deg. C was found to decrease from a fast fracture value of 2 GPa to a 100-hr rupture strength value of 0. 8 GPa. In addition a loss of fast fracture strength from 6 GPa is attributed to thermally induced changes in the outer carbon coating and microstructure. Scatter in rupture times made a definitive analysis of environmental and annealing effects on creep strength difficult.

Goldsby, J. C.↗

NASA NTRS2002

Initial Assessment of the Effects of Nonmetallic Inclusions on Fatigue Life of Powder-Metallurgy-Processed Udimet(TM) 720

The fatigue lives of modern powder metallurgy (PM) disk alloys are influenced by variabilities in alloy microstructure and mechanical properties. These properties can vary due to the different steps of materials/component processing and machining. One of these variables, the presence of nonmetallic inclusions, has been shown to significantly degrade low-cycle fatigue (LCF) life. Nonmetallic inclusions are inherent defects in powder alloys that are a by-product of powder-processing techniques. Contamination of the powder can occur in the melt, during powder atomization, or during any of the various handling processes through consolidation. In modern nickel disk powder processing facilities, the levels of inclusion contamination have been reduced to less than 1 part per million by weight. Despite the efforts of manufacturers to ensure the cleanliness of their powder production processes, the presence of inclusions remains a source of great concern for the designer. the objective of this study was to investigate the effects on fatigue life of these inclusions. Since natural inclusions occur so infrequently, elevated levels of inclusions were carefully introduced in a nickel-based disk superalloy, Udimet 720 (registered trademark of Special Metals Corporation), produced using PM processing. Multiple strain-controlled fatigue tests were then performed on this material at 650 C. Analyses were performed to compare the LCF lives and failure initiation sites as functions of inclusion content and fatigue conditions. A large majority of the failures in specimens with introduced inclusions occurred at cracks initiating from inclusions at the specimen surface. The inclusions could reduce fatigue life by up to 100 times. These effects were found to be dependent on strain range and strain ratio. Tests at lower strain ranges and higher strain ratios produced larger effects of inclusions on life.

Gabb, T. P.↗

NASA NTRS2024

Microgravity Effects on Nonequilibrium Melt Processing of Neodymium Titanate: Thermophysical Properties, Atomic Structure, Glass Formation and Crystallization

The relationships between materials processing and structure can vary between terrestrial and reduced gravity environments. As one case study, we compare the nonequilibrium melt processing of a rare-earth titanate, nominally 83TiO 2 -17Nd 2 O 3 , and the structure of its glassy and crystalline products. Density and thermal expansion for the liquid, supercooled liquid, and glass are measured over 300–1850 °C using the Electrostatic Levitation Furnace (ELF) in microgravity, and two replicate density measurements were reproducible to within 0.4%. Cooling rates in ELF are 40–110 °C s −1 lower than those in a terrestrial aerodynamic levitator due to the absence of forced convection. X-ray/neutron total scattering and Raman spectroscopy indicate that glasses processed on Earth and in microgravity exhibit similar atomic structures, with only subtle differences that are consistent with compositional variations of ~2 mol. % Nd 2 O 3 . The glass atomic network contains a mixture of corner- and edge-sharing Ti-O polyhedra, and the fraction of edge-sharing arrangements decreases with increasing Nd 2 O 3 content. X-ray tomography and electron microscopy of crystalline products reveal substantial differences in microstructure, grain size, and crystalline phases, which arise from differences in the melt processes.

thermophysical properties↗