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NASA NTRS1992

Fracture toughness of an Al-Li-Cu-In alloy

The crack initiation and growth fracture toughness of select AL-Li-Cu alloy variants are characterized and elucidated. Conventionally processed plates form large DC cast ingots are investigated to eliminate the variation in microstructure associated with laboratory scale and SPF-processed material. Fracture resistance is characterized using the J-integral method to establish crack initiation and growth behavior at 25 and -185 C. It is shown that state-of-the-art 2090-T81 has superior toughness compared to 2090 + In-T6 at both test temperatures, with the low toughness of 2090 + In-T6 associated with intersubgranular fracture attributed to a high density of subboundary precipitates.

Wagner, John A.↗

NASA NTRS2010

Microstructure Modeling of 3rd Generation Disk Alloys

The objective of this program is 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 will be further improved and implemented to be a useful and user-friendly engineering tool. In this report, the key accomplishment achieved during the second year (2008) of the program is summarized. The activities of this year include final selection of multicomponent thermodynamics and mobility databases, precipitate surface energy determination from nucleation experiment, multiscale comparison of predicted versus measured intragrain precipitation microstructure in quench samples showing good agreement, isothermal coarsening experiment and interaction of grain boundary and intergrain precipitates, primary microstructure of subsolvus treatment, and finally the software implementation plan for the third year of the project. In the following year, the calibrated models and simulation tools will be validated against an independently developed experimental data set, with actual disc heat treatment process conditions. Furthermore, software integration and implementation will be developed to provide material engineers valuable information in order to optimize the processing of the 3rd generation gas turbine disc alloys.

Jou, Herng-Jeng↗

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 NTRS1980

Characterization of deliberately nickel-doped silicon wafers and solar cells

Microstructural and electrical evaluation tests were performed on nickel-doped p-type silicon wafers before and after solar cell fabrication. The concentration levels of nickel in silicon were 5 x 10 to the 14th power, 4 x 10 to the 15th power, and 8 x 10 to the 15th power atoms/cu cm. It was found that nickel precipitated out during the growth process in all three ingots. Clumps of precipitates, some of which exhibited star shape, were present at different depths. If the clumps are distributed at depths approximately 20 micron apart and if they are larger than 10 micron in diameter, degradation occurs in solar cell electrical properties and cell conversion efficiency. The larger the size of the precipitate clump, the greater the degradation in solar cell efficiency. A large grain boundary around the cell effective area acted as a gettering center for the precipitates and impurities and caused improvement in solar cell efficiency. Details of the evaluation test results are given.

Salama, A. M.↗

NASA NTRS1992

Characterization of low thermal conductivity PAN-based carbon fibers

The microstructure and surface chemistry of eight low thermal conductivity (LTC) PAN-based carbon fibers were determined and compared with PAN-based fibers heat treated to higher temperatures. Based on wide-angle x ray diffraction, the LTC PAN fibers all appear to have a similar turbostratic structure with large 002 d-spacings, small crystallite sizes, and moderate preferred orientation. Limited small-angle x ray scattering (SAXS) results indicate that, with the exception of LTC fibers made by BASF, the LTC fibers do not have well developed pores. Transmission electron microscopy shows that the texture of the two LTC PAN-based fibers studied (Amoco T350/23X and /25X) consists of multiple sets of parallel, wavy, bent layers that interweave with each other forming a complex three dimensional network oriented randomly around the fiber axis. X ray photoelectron spectroscopy (XPS) analysis finds correlations between heat treated temperatures and the surface composition chemistry of the carbon fiber samples.

Katzman, Howard A.↗

NASA NTRS1989

Mechanical alloying, characterization and consolidation of Ti-Al-Ni alloys

Mechanical alloying is being investigated as a processing route for the production of aluminide intermetallics. This program involves powder production and characterization, consolidation and thermal treatments and determination of microstructure-property relationships. An attritor mill is being used to produce powder in lots up to 1000 grams and the processing parameters are being systematically varied to establish the optimum milling conditions. The mill is being instrumented to generate data related to the processing to provide a basis for theoretical modeling. Powder is being characterized using thermal analysis, optical and electron microscopy and X-ray diffraction. Particle size distributions and powder density are being determined. Consolidation of the powder is being approached in several different ways including, cold isostatic pressing, sintering, extrusion and hot pressing. The results of the program so far will be presented and future directions discussed.

Nash, P.↗

NASA NTRS1972

Mechanisms of oxidation in the Co-Cr system.

Oxidation has been studied both as a function of temperature in the range from 900 to 1300 C and of the partial pressure of oxygen in the range from 0.05 to 760 torr. In addition, microstructures of oxide scales have been studied and characterized in more detail utilizing metallographic and X-ray techniques combined with electron microprobe analysis. The parabolic rate constants in 1100 C and at 100 and 10 torr oxygen are presented in a graph as a function of chromium content. Three main different mechanisms of oxidation in the Co-Cr system have been identified. In two of these, the rate determining process controlling the oxidation is the solid state diffusion of cobalt through the oxide CoO. The rate controlling process governing the oxidation for the third mechanism is chromium diffusion in dichromium trioxide.

Kofstad, P. K.↗

NASA NTRS1985

A ceramic matrix composite based on polymerization and pyrolysis of ethynylated aromatics

A number of ethynylated aromatic monomers recently have been synthesized which thermally homopolymerize and copolymerize to produce rigid, highly cross-linked polymers with high thermal stability (Tg of about 450 C). On pyrolysis, these polymers lose few volatiles (more than 85 percent char yield) to yield carbon bodies of relatively low porosity. These properties render the ethynylated aromatics of significant interest as matrices for high temperature composites. Incorporation of a SiC particle filler in the matrix improves the rheology of the system and minimizes shrinkage during pyrolysis. Several unidirectional composites have been fabricated combining a graphite or boria-alumina-silica continuous reinforcement with an ethynylated aromatic polymer matrix and SiC filler. Thermogravimetric analysis of composite pyrolysis behavior was used to determine reaction kinetics and to establish a composite fabrication cycle. Composites retained 95 percent of their green weight on pyrolysis. Microstructure of the green and pyrolyzed composites is characterized for materials pyrolyzed at 600 C in vacuum and argon as well as for laminates heated at 1200 C in argon following pyrolysis.

Hurwitz, F. I.↗

NASA NTRS1987

Structure-property relationships in directionally solidified single crystal NiAl

The ordered intermetallic alloy NiAl is being considered as a potential high temperature structural material, but lack of ductility at ambient temperatures, especially in polycrystalline form, is presently a major obstacle in achieving this goal. Even general agreement of the intrinsic ductility that can be achieved in monocrystals is in dispute. In order to understand this problem, two directionally solidified ingots of NiAl which displayed known differences in ductility were characterized in sufficient detail to identify the corresponding microstructural differences. It was found that the type and size of casting defects, i.e., porosity, present in the material were the major factors in controlling ductility of NiAl single crystals and could explain the order of magnitude variance in fracture strains reported in the literature.

Noebe, R. D.↗

NASA NTRS1994

Characterization of Damage Progression in SCS-6/timetal 21S (0)4 Under Thermomechanical Fatigue Loadings

A detailed experimental investigation was performed at a single maximum cyclic stress (sigma max) level to physically characterize the progression of thermomechanical fatigue (lW) damage in continuously reinforced (0 deg) SCS-6/Timetal 21S, a titanium matrix composite. In-phase (IP) and out of-phase (OP) loadings were investigated at sigma max = 1000 MPa with a temperature cycle from 150 to 6500 C. Damage progression, in terms of macroscopic property degradation, was experimentally quantified through an advanced TMF test methodology which incorporates explicit measurements of the isothermal static moduli at the TMF temperature extremes and the coefficient of thermal expansion (CTE) as functions of the TMF cycles. Detailed characterization of the physical damage progression at the microstructural level was performed by interrupting multiple TMF tests at various stages of mechanical property degradation and analyzing the microstructure through extensive destructive metallography. Further, the extent of damage was also quantified through residual static strength measurements. Results indicated that damage initiation occurred very early in cyclic life (N less than 0.1Nf) for both the IP and OP TMF loadings. IP TMF damage was found to be dominated by fiber breakage with a physical damage progression in the microstructure which was difficult to quantify. OP TMF loadings produced matrix cracking exclusively associated with surface initiations. Here, damage progression was easily distinguished in terms of both the number of cracks and their relative inward progressions toward the outer fiber rows with increased cycling. The point at which the leading cracks reached the outer fiber rows (when localized fiber/matrix de-bonding and matrix crack bridging occurred) appeared to be reflected in the macroscopic property degradation curves.

Castelli, Michael G.↗

NASA NTRS2001

Fabrication and Testing of Ceramic Matrix Composite Rocket Propulsion Components

NASA has established goals for Second and Third Generation Reusable Launch Vehicles. Emphasis has been placed on significantly improving safety and decreasing the cost of transporting payloads to orbit. Ceramic matrix composites (CMC) components are being developed by NASA to enable significant increases in safety and engineer performance, while reducing costs. The development of the following CMC components are being pursued by NASA: (1) Simplex CMC Blisk; (2) Cooled CMC Nozzle Ramps; (3) Cooled CMC Thrust Chambers; and (4) CMC Gas Generator. These development efforts are application oriented, but have a strong underpinning of fundamental understanding of processing-microstructure-property relationships relative to structural analyses, nondestructive characterization, and material behavior analysis at the coupon and component and system operation levels. As each effort matures, emphasis will be placed on optimizing and demonstrating material/component durability, ideally using a combined Building Block Approach and Build and Bust Approach.

Effinger, M. R.↗

NASA NTRS1998

Single-Transducer, Ultrasonic Imaging Method for High-Temperature Structural Materials Eliminates the Effect of Thickness Variation in the Image

NASA Lewis Research Center's Life Prediction Branch, in partnership with Sonix, Inc., and Cleveland State University, recently advanced the development of, refined, and commercialized an advanced nondestructive evaluation (NDE) inspection method entitled the Single Transducer Thickness-Independent Ultrasonic Imaging Method. Selected by R&D Magazine as one of the 100 most technologically significant new products of 1996, the method uses a single transducer to eliminate the superimposing effects of thickness variation in the ultrasonic images of materials. As a result, any variation seen in the image is due solely to microstructural variation. This nondestructive method precisely and accurately characterizes material gradients (pore fraction, density, or chemical) that affect the uniformity of a material's physical performance (mechanical, thermal, or electrical). Advantages of the method over conventional ultrasonic imaging include (1) elimination of machining costs (for precision thickness control) during the quality control stages of material processing and development and (2) elimination of labor costs and subjectivity involved in further image processing and image interpretation. At NASA Lewis, the method has been used primarily for accurate inspections of high temperature structural materials including monolithic ceramics, metal matrix composites, and polymer matrix composites. Data were published this year for platelike samples, and current research is focusing on applying the method to tubular components. The initial publicity regarding the development of the method generated 150 requests for further information from a wide variety of institutions and individuals including the Federal Bureau of Investigation (FBI), Lockheed Martin Corporation, Rockwell International, Hewlett Packard Company, and Procter & Gamble Company. In addition, NASA has been solicited by the 3M Company and Allison Abrasives to use this method to inspect composite materials that are manufactured by these companies.

Roth, Don J.↗

NASA NTRS2010

Improvement in the Shape Memory Response of Ti50.5Ni24.5Pd25 High-Temperature Shape Memory Alloy with Scandium Microalloying

A Ti(50.5)Ni(24.5)Pd25 high-temperature shape memory alloy (HTSMA) is microalloyed with 0.5 at. pct scandium (Sc) to enhance its shape-memory characteristics, in particular, dimensional stability under repeated thermomechanical cycles. For both Ti(50.5)Ni(24.5)Pd25 and the Sc-alloyed material, differential scanning calorimetry is conducted for multiple cycles to characterize cyclic stability of the transformation temperatures. The microstructure is evaluated using electron microscopy, X-ray diffractometry, and wavelength dispersive spectroscopy. Isobaric thermal cycling experiments are used to determine transformation temperatures, dimensional stability, and work output as a function of stress. The Sc-doped alloy displays more stable shape memory response with smaller irrecoverable strain and narrower thermal hysteresis than the baseline ternary alloy. This improvement in performance is attributed to the solid solution hardening effect of Sc.

Atli, K. C.↗

NASA NTRS2018

Freeze Casting of LAGP for 3D Textured Solid-State Structural Electrolytes

In this study, all-solid-state structural lithium-ion batteries, a type of load bearing electrochemical energy storage that provides systems-level weight savings is being pursued for the realization of inherently safe next generation hybrid-electric and all-electric green aerospace propulsion systems. Currently investigated all-solid-state batteries do not meet the requirements for specific power and mechanical stability. To address these issues, freeze casting of lithium aluminum germanium phosphate (LAGP) electrolyte material has been explored for the creation of a textured 3D electrolyte scaffold with large interfacial surface area for high power discharge and hierarchical porosity for accommodation of active material volume changes during electrochemical cycling. We report the effects of freeze casting processing parameters on the microstructural development and mechanical performance of the scaffolds, characterized through scanning electron microscopy and ring-on-ring mechanical testing. Slurry composition and casting parameters such as solids loading, casting speed, tape angle, and temperature gradients have been modified to determine the impact on density, lamellar morphology, and final load-bearing performance.

ceramics↗

NASA NTRS1997

Low Temperature Synthesis, Chemical and Electrochemical Characterization of LiNi(x)Co(1-x)O2 (0 less than x less than 1)

A new method of synthesis for the solid solution cathode materials LiNi(x)Co(1-x)O2 (0 less than x less than 1) involving enhanced reactions at temperatures less than or equal to 700 deg. C, between metal oxy-hydroxide precursors MOOH (M = Ni, Co) and Li-salts (Li2CO3, LiOH, and LiNO3) has been investigated. The effects of synthesis conditions and sources of Li, on phase purity, microstructure, and theoretical electrochemical capacity (total M(3+) content) are characterized by powder X-ray diffraction analysis, scanning electron microscopy, chemical analysis and room temperature magnetic susceptibility. An attempt has been made to correlate the electrochemical properties with the synthesis conditions and microstructure.

Nanjundaswamy, K. S.↗

NASA NTRS1991

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.↗

NASA NTRS1978

Characterization and properties of controlled nucleation thermochemical deposited (CNTD) silicon carbide

The microstructure of controlled nucleation thermochemical deposition (CNTD) - SiC material was studied and the room temperature and high temperature bend strength and oxidation resistance was evaluated. Utilizing the CNTD process, ultrafine grained (0.01-0.1 mm) SiC was deposited on W - wires (0.5 mm diameter by 20 cm long) as substrates. The deposited SiC rods had superior surface smoothness and were without any macrocolumnar growth commonly found in conventional CVD material. At both room and high temperature (1200 - 1380 C), the CNTD - SiC exhibited bend strength approximately 200,000 psi (1380 MPa), several times higher than that of hot pressed, sintered, or CVD SiC. The excellent retention of strength at high temperature was attributed to the high purity and fine grain size of the SiC deposit and the apparent absence of grain growth at elevated temperatures. The rates of weight change for CNTD - SiC during oxidation were lower than for NC-203 (hot pressed SiC), higher than for GE's CVD - SiC, and considerably below those for HS-130 (hot pressed Si3N4). The high purity, fully dense, and stable grain size CNTD - SiC material shows potential for high temperature structural applications; however problem areas might include: scaling the process to make larger parts, deposition on removable substrates, and the possible residual tensile stress.

Dutta, S.↗

NASA NTRS2010

The Smallest Lunar Grains: Analytical TEM Characterization of the Sub-micron Size Fraction of a Mare Soil

The chemical composition, mineralogical type, and morphology of lunar regolith grains changes considerably with decreasing size, and below the approx.25 m size range the correlation between these parameters and remotely-sensed lunar surface properties connected to space weathering increases significantly. Although trends for these parameters across grain size intervals greater than 20 m are now well established, the 0 to 20 m size interval remains relatively un-subdivided with respect to variations in grain modal composition, chemistry and microstructure. Of particular interest in this size range are grains in the approximate < 1 m diameter class, whose fundamental properties are now the focus of lunar research pertaining to electrostatic grain transport, dusty plasmas, and lunar dust effects on crew health and exploration systems. In this study we have used analytical transmission electron microscopy (TEM) to characterize the mineralogy, microstructure and major element composition of grains below the 1 m size threshold in lunar soil 10084.

Thompson, M.↗