Recently developed coatings for tantalum, columbium and TD alloys
Protective coatings of Ta, Nb and TD alloys for high performance thermal protection systems, discussing space shuttle reentry heat shield
Shoemaker, H. E.↗
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Development of advanced high strength tantalum base alloys. Part 1: Screening investigation
Five experimental tantalum alloy compositions containing 13-18% W+Re+Hf solid solution solute additions with dispersed phase strengthening achieved by carbon or nitrogen additions were prepared as 1.4 inch diameter ingot processed to 3/8 inch diameter rod and evaluated. Elevated temperature tensile and creep strength increased monotonically with increasing solute content. Room temperature elongation decreased for 20% to less than 2% as the solute content was increased above 16%. Phase identification indicated that the precipitating phase in the carbide containing alloys was Ta2C.
Buckman, R. W., Jr.↗
Development of advanced high strength tantalum base alloys. Phase 3: Influence of metallurgical condition on the mechanical properties of ASTAR-811C sheet
Metallurgical condition was shown to have a significant effect on the creep properties of ASTAR-811C (Ta-8W-1Re-0.7Hf-0.025C) sheet. Cold worked material exhibited creep rates 30 times higher than solution annealed material and 10 times greater than for recrystallized material. Both grain size and the carbide morphology changes as the final annealing temperature was raised from 3000 F to 3600 F. However, the lowest creep rates were achieved for material which retained the high temperature form of the Ta2C precipitate. Samples with GTA weldments had essentially identical properties as recrystallized base metal. Cooling rates from 3600 F of 5, 50, and 800 F deg/min. had little effect on the 2000 and 2400 F creep behavior of ASTAR-811C.
Ammon, R. L.↗
Development of ductile high-strength chromium alloys, phase 2
Strength and ductility were evaluated for chromium alloys dispersion hardened with the putative TaC, TaB, CbC, and CbB compounds. TaC and TaB proved to be the most potent strengtheners, but when combined, their effect far outweighed that produced individually. Tests at 1422 K (2100 F) on an alloy containing these two compounds at the combined level of 0.5 m/o revealed a 495 MN/sq m (70 ksi) tensile strength for wrought material, and a 100 hour rupture strength of 208 MN/sq m (30 ksi) when solution annealed and aged to maximize creep resistance. These levels of high temperature strength greatly exceed that reported for any other chromium-base alloy. The ductile-to-brittle transition temperature (DBTT) of the two phase strengthened alloy occurred at approximately 588 K (600 F) when heat treated to optimize creep strength and was not improved by fabrication to produce a wrought and recovered microstructure. The lowest DBTT measured on any of the alloys investigated was 422 K (300 F). Strengthening phases actually formed in Cr-Ta-B and Cr-Cb-B compositions are probable M2CrB2 (M=Ta or Cb) compounds of tetragonal crystal structure. The likely habit relationship between these compounds and chromium is postulated. Cube habit coherency was identified for TaC precipitation in chromium by electron microscopy. In another study, the maximum solubility of carbon in chromium was indicated to lie between 3/4 and 1 a/o and that of boron to be 1/2 a/o.
Filippi, A. M.↗
Development of advanced high strength tantalum base alloys. Part 2: Scale-up investigation
Three experimental tantalum alloy compositions containing 14-16% W, 1% Re, 0.7% Hf, 0.025% C or 0.015% C and 0.015% N were prepared as two inch diameter ingots by consumable electrode vacuum arc melting. The as-cast ingots were processed by extrusion and swaging to one inch and 0.4 inch diameter rod and evaluated. Excellent high temperature forging behavior was exhibited by all three compositions. Creep strength at 2000 F to 2400 F was enhanced by higher tungsten additions as well as substitution of nitrogen for carbon. Weldability of all three compositions was determined to be adequate. Room temperature ductility was retained in the advanced tantalum alloy compositions as well as a notched/unnotched strength ratio of 1.4 for a notched bar having a K sub t = 2.9.
Ammon, R. L.↗
Development of a dispersion strengthened nickel base alloy using the high intensity arc process
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Mccullogh, H. M.↗
Development of oxide dispersion strengthened turbine blade alloy by mechanical alloying
There were three nickel-base alloys containing up to 18 wt. % of refractory metal examined initially for oxide dispersion strengthening. To provide greater processing freedom, however, a leaner alloy was finally selected. This base alloy, alloy D, contained 0.05C/15Cr / 2Mo/4W/2Ta/4.5Al/2.Ti/015Zr/0.01-B/Bal. Ni. Following alloy selection, the effect of extrusion, heat treatment, and oxide volume fraction and size on microstructure and properties were examined. The optimum structure was achieved in zone annealed alloy D which contained 2.5 vol. % of 35 mm Y2O3 and which was extruded 16:1 at 1038 C.
Merrick, H. F.↗
Development of powder metallurgy 2XXX series Al alloys for high temperature aircraft structural applications
The objective of the present investigation was to improve the strength and fracture toughness combination of P/M 2124 Al alloys in accordance with NASA program goals for damage tolerance and fatigue resistance. Two (2) P/M compositions based on Al-3.70 Cu-1.85 Mg-0.20 Mn with 0.12 and 0.60 wt. pct. Zr were selected for investigation. The rapid solidification rates produced by atomization were observed to prohibit the precipitation of coarse, primary Al3Zr in both alloys. A major portion of the Zr precipitated as finely distributed, coherent Al3Zr phases during vacuum preheating and solution heat treatment. The proper balance between Cu and Mg contents eliminated undissolved, soluble constituents such as Al2CuMg and Al2Cu during atomization. The resultant extruded microstructures produced a unique combination of strength and fracture toughness. An increase in the volume fraction of coherent Al3Zr, unlike incoherent Al20Cu2Mn3 dispersoids, strengthened the P/M Al base alloy either directly by dislocation-precipitate interactions, indirectly by a retardation of recrystallization, or a combination of both mechanisms. Furthermore, coherent Al3Zr does not appear to degrade toughness to the extent that incoherent Al20Cu2Mn3 does. Consequently, the addition of 0.60 wt. pct. Zr to the base alloy, incorporated with a 774K (935 F) solution heat treatment temperature, produces an alloy which exceeds all tensile property and fracture toughness goals for damage tolerant and fatigue resistant applications in the naturally aged condition.
Chellman, D. J.↗
Development of powder metallurgy 2XXX series Al alloy plate and sheet materials for high temperature aircraft structural applications, FY 1983/1984
The objective of this investigation is to fabricate and evaluate PM 2124 Al alloy plate and sheet materials according to NASA program goals for damage tolerance and fatigue resistance. Previous research has indicated the outstanding strength-toughness relationship available with PM 2124 Al-Zr modified alloy compositions in extruded product forms. The range of processing conditions was explored in the fabrication of plate and sheet gage materials, as well as the resultant mechanical and metallurgical properties. The PM composition based on Al-3.70 Cu-1.85 Mg-0.20 Mn with 0.60 wt. pct. Zr was selected. Flat rolled material consisting of 0.250 in. thick plate was fabricated using selected thermal mechanical treatments (TMT). The schedule of TMT operations was designed to yield the extreme conditions of grain structure normally encountered in the fabrication of flat rolled products, specifically recrystallized and unrecrystallized. The PM Al alloy plate and sheet materials exhibited improved strength properties at thin gages compared to IM Al alloys, as a consequence of their enhanced ability to inhibit recrystallization and grain growth. In addition, the PM 2124 Al alloys offer much better combinations of strength and toughnessover equivalent IM Al. The alloy microstructures were examined by optical metallographic texture techniques in order to establish the metallurgical basis for these significant property improvements.
Chellman, D. J.↗
Effect of melt-solid interface shape on lateral compositional distribution of unidirectionally solidified 2-6 semiconducting alloys
A computer code developed previously has been used to simulate lateral compositional distributions for several 2-6 semiconducting systems. The code is based on analytical results obtained previously. The system under study is an azimuthal symmetric cylindrical system with a curved melt-solid interface shape during an unidirectional solidification process. It is assumed that the system is under a steady state diffusion limited growth condition.
Wang, Jai-Ching↗
Microsample Characterization of Coatings for Grcop-84 for High Heat Flux Applications
A multidisciplinary Johns Hopkins University-NASA Glenn team is undertaking a collaborative research program to elucidate and model the thermal stability and mechanical integrity of candidate coatings for GRCop-84. GRCop-84 is a high conductivity, high strength copper alloy that was recently developed at NASA Glenn for use in high temperature, high heat flux applications. With potential applications in rocket motor combustion chamber liners, nozzle ramps and other actively cooled structures, this new material offers great potential for decreasing weight and increasing reliability of third generation reusable launch vehicles. Current emphasis has turned toward the development of environmentally resistant and thermal barrier coatings for this alloy. Metallic coatings such as NiCrAlY and Cu-8-30%Cr have shown promise in: prohibiting blanching, reducing dog-house failures, increasing operating temperatures and decreasing cooling requirements. The focus of this research program is to develop a fundamental understanding of the substrate-coating interactions that occur during thermal cycling (inter-diffusion, viscoplasticity, morphological evolution, crack formation, etc.) and to derive a science-based protocol for future coating selection, optimization and reliability assurance. The microsample tensile testing approach adopted for this study allows us to characterize small-scale and highly scale-specific coatings and properties in a way not possible by conventional means. In addition to providing much needed design data, the integration of microsample testing with detailed microstructural observations provides a mechanistic foundation for coating optimization and life prediction modeling.
Hemker, Kevin↗
Analytical study of space processing of immiscible materials for superconductors and electrical contacts
The results of a study conducted to determine the role space processing or materials research in space plays in the superconductor and electrical contact industries are presented. Visits were made to manufacturers, users, and research organizations connected with these products to provide information about the potential benefits of the space environment and to exchange views on the utilization of space facilities for manufacture, process development, or research. In addition, space experiments were suggested which could result in improved terrestrial processes or products. Notable examples of these are, in the case of superconductors, the development of Nb-bronze alloys (Tsuei alloys) and, in the electrical contact field, the production of Ag-Ni or Ag-metal oxide alloys with controlled microstructure for research and development activities as well as for product development. A preliminary experimental effort to produce and evaluate rapidly cooled Pb-Zn and Cu-Nb-Sn alloys in order to understand the relationship between microstructure and superconducting properties and to simulate the fine structure potentially achievable by space processing was also described.
Gelles, S. H.↗
Robust Low Cost Liquid Rocket Combustion Chamber by Advanced Vacuum Plasma Process
Next-generation, regeneratively cooled rocket engines require materials that can meet high temperatures while resisting the corrosive oxidation-reduction reaction of combustion known as blanching, the main cause of engine failure. A project was initiated at NASA-Marshal Space Flight Center (MSFC) to combine three existing technologies to build and demonstrate an advanced liquid rocket engine combustion chamber that would provide a 100 mission life. Technology developed in microgravity research to build cartridges for space furnaces was utilized to vacuum plasma spray (VPS) a functional gradient coating on the hot wall of the combustion liner as one continuous operation, eliminating any bondline between the coating and the liner. The coating was NiCrAlY, developed previously as durable protective coatings on space shuttle high pressure fuel turbopump (HPFTP) turbine blades. A thermal model showed that 0.03 in. NiCrAlY applied to the hot wall of the combustion liner would reduce the hot wall temperature 200 F, a 20% reduction, for longer life. Cu-8Cr-4Nb alloy, which was developed by NASA-Glenn Research Center (GRC), and which possesses excellent high temperature strength, creep resistance, and low cycle fatigue behavior combined with exceptional thermal stability, was utilized as the liner material in place of NARloy-Z. The Cu-8Cr-4Nb material exhibits better mechanical properties at 650 C (1200 F) than NARloy-Z does at 538 C (1000 F). VPS formed Cu-8Cr-4Nb combustion chamber liners with a protective NiCrAlY functional gradient coating have been hot fire tested, successfully demonstrating a durable coating for the first time. Hot fire tests along with tensile and low cycle fatigue properties of the VPS formed combustion chamber liners and witness panel specimens are discussed.
Holmes, Richard↗
Having a Come-Apart: Lessons Learned from Additively Manufactured Hardware Failures
NASA has been engaged with additively manufactured (AM) process and component development since the 2000’s. AM offers various technical advantages, such as enhanced hardware design complexity, part consolidation, and processing of novel alloys in addition to programmatic advantages for reduction in processing time and cost. The focus of much of the AM development at NASA has been to mature the various processes, characterize material properties, develop standards, produce demonstrator parts, and integrate AM hardware in liquid rocket engines. These aspects have been demonstrated through process and design iterations using a methodical characterization, test-fail-fix cycles, as well as application and dissemination of lessons learned. In addition to these fundamental demonstrations of the AM process and hardware development, alloys that provide performance advantages in the high temperature and high-pressure environments have been matured for use in rocket engines. These environments are challenging for any alloy and any design, and the AM process is required to fully meet the intended design requirements. The importance of proper AM process was made evident in the failure of a Laser Powder Bed Fusion (L-PBF) copper-alloy combustion chamber during a hot-fire test due to a degraded material quality resulted from an AM process issue. The hot-fire test aimed to demonstrate high duty cycle under a risk-tolerant development project, where consequences of component failure would be minimal. However, the unintentional component failure emphasized the necessity of robust material characterization and rigorous process control procedures for the safe use of AM components in critical applications. In part, such concerns motivate the AM certification approach that NASA has recently adopted in NASA-STD-6030 “Additive Manufacturing Requirements for Spaceflight Systems”. This presentation provides an overview of the previously mentioned failure, a discussion on the evaluation of the failed chamber and supplemental chambers produced at the same time, a representative material samples that included intentional build witness lines, and a summary of the key results and recommendations from the evaluations. NASA continues to approach AM processes and designs with a level of risk and acceptance of failures that is appropriate for the project objectives, with the overall goal of safe implementation of AM technology and transferring AM technology into commercial space applications. The objective of this presentation is to provide awareness to the community working critical and non-critical AM components and the lessons learned on proper implementation of AM.
Additive Manufacturing↗
Dentritic morphology and microsegregation in directionally solidified superalloy, PWA-1480, single crystal: Effect of gravity; center director's discretionary fund report
Primary dendrite spacings, secondary dendrite spacings, and microsegregation have been examined in PWA-1480 single crystal specimens which were directionally solidified during parabolic maneuvers on the KC-135 aircraft. Experimentally observed growth rate and thermal gradient dependence of primary dendrite spacings are in good agreement with predictions from dendrite growth models for binary alloys. Secondary dendrite coarsening kinetics show a reasonable fit with the predictions from an analytical model proposed by Kirkwood for a binary alloy. The partition coefficients of tantalum, titanium, and aluminum are observed to be less than unity, while that for tungsten and cobalt are greater than unity. This is qualitatively similar to the nickel base binaries. Microsegregation profiles experimentally observed for PWA-1480 superalloy show a good fit with Bower, Brody, and Flemings model developed for binary alloys. Transitions in gravity levels do not appear to affect primary dendrite spacings. A trend of decreased secondary arm spacings with transition from high gravity to the low gravity period was observed at a growth speed of 0.023 cm s(exp -1). However, definite conclusions can only be drawn by experiments at lower growth speeds which make it possible to examine the side-branch coarsening kinetics over a longer duration. Such experiments, not possible due to the insufficient low-gravity time of the KC-135, may be carried out in the low-gravity environment of space.
Tewari, S. N.↗
Development of high-cycle fatigue design curves for a cast aluminum alloy
Life prediction curves for rocket engine pump parts were developed from the results of high-cycle fatigue tests run on cast-aluminum specimens. Notched and smooth specimens were cyclically tested at different mean stress levels at -320 F (78 K). The notch size and mean stress enveloped the design operating conditions. Local stress computed in the groove of the notched specimen was used to represent its fatigue strength. The von Mises criterion was used to determine effective cyclic stresses. The Goodman rule was applied to determine equivalent reversed alternating stresses. The procedure permitted the notched and smooth data sets to each be described by a single curve. High-cycle fatigue life curves were provided for the stress state, mean stress, and stress concentration spanned by the data.
Cooper, R. A.↗
Assessment of Shape Memory Alloys - From Atoms To Actuators - Via In Situ Neutron Diffraction
As shape memory alloys (SMAs) become an established actuator technology, it is important to identify the fundamental mechanisms responsible for their performance by understanding microstructure performance relationships from processing to final form. Yet, microstructural examination of SMAs at stress and temperature is often a challenge since structural changes occur with stress and temperature and microstructures cannot be preserved through quenching or after stress removal, as would be the case for conventional materials. One solution to this dilemma is in situ neutron diffraction, which has been applied to the investigation of SMAs and has offered a unique approach to reveal the fundamental micromechanics and microstructural aspects of bulk SMAs in a non-destructive setting. Through this technique, it is possible to directly correlate the micromechanical responses (e.g., internal residual stresses, lattice strains), microstructural evolutions (e.g., texture, defects) and phase transformation properties (e.g., phase fractions, kinetics) to the macroscopic actuator behavior. In this work, in situ neutron diffraction was systematically employed to evaluate the deformation and transformation behavior of SMAs under typical actuator conditions. Austenite and martensite phases, yield behavior, variant selection and transformation temperatures were characterized for a polycrystalline NiTi (49.9 at. Ni). As the alloy transforms under thermomechanical loading, the measured textures and lattice plane-level variations were directly related to the cyclic actuation-strain characteristics and the dimensional instability (strain ratcheting) commonly observed in this alloy. The effect of training on the shape memory characteristics of the alloy and the development of two-way shape memory effect (TWSME) were also assessed. The final conversion from a material to a useful actuator, typically termed shape setting, was also investigated in situ during constrained heatingcooling and subsequent shape recovery experiments. Neutron diffraction techniques are also being applied to the investigation of novel high temperature SMAs with the objective of designing alloys with better stability, higher transition temperatures and ultimately superior durability.
Shape Memory Alloys↗
GRCop-42 Development and Hot-fire Testing Using Additive Manufacturing Powder Bed Fusion for Channel-Cooled Combustion Chambers
GRCop-42 is a high conductivity, high-strength dispersion strengthened copper-alloy for use in high heat flux applications such as liquid rocket engine combustion devices. This alloy is part of the family of NASA-developed GRCop, copper-chrome-niobium alloys. GRCop alloys were developed for harsh environments specific to regeneratively-cooled combustion chambers and nozzles with good oxidation resistance. Significant development was completed on the GRCop-84 and GRCop-42 alloys in the extruded wrought form demonstrating feasibility for combustion chambers. NASA has recently developed a process for additive manufacturing, specifically Powder Bed Fusion (PBF) or Selective Laser Melting (SLM), of GRCop-42 to establish parameters, characterize the material, and complete testing of components with complex internal features. This evolution of the GRCop-42 was based on the successful predecessor development work using GRCop-84 with the motivation of establishing a new copper-alloy option for use in NASA, government, and industry programs with SLM. A few advantages have been shown with the GRCop-42 that include higher conductivity and faster build speeds over the GRCop-84, and a simplified powder supply chain. Initial property development has shown that it is possible to produce high density builds with strengths equivalent to wrought GRCop-42 and a conductivity greater than GRCop-84. The GRCop-42 has completed process development and initial properties have been established. Several demonstrator combustion chambers have also been fabricated with the SLM GRCop-42 that include integral channels and closeouts. Additional test units have been fabricated and are completing substantial hot-fire testing to demonstrate performance of the material, process, and design.
Gradl, Paul R.↗