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Freeform thermoelectrics in single-step manufacturing: additive manufacturing of bismuth-telluride thermoelectrics

The project succeeded in producing crack-free Bismuth Telluride thermoelectric parts with density exceeding 98% through laser powder bed fusion (LPBF) additive manufacturing (AM). This greatly exceeded the highest previously reported density of 88% and is the highest among all semiconducting materials processed by LPBF. The additively manufactured material shows comparable Seebeck coefficient as conventional form and can be made into complex geometries with reduced material loss. On the other hand, measured properties are dramatically sensitive to the AM process parameters used, such that with identical composition, the Seebeck coefficient can be controllably tuned from +120 µV/K to -207 µV/K, which means the material switches between an n-type to a p-type semiconductor depending on processing. These changes are accompanied by significant differences in the as-processed microstructure due to rapid solidification. A machine learning protocol was developed and greatly reduced the experimental burden of the project, reducing the typical process optimization period of 2 years to 6 months. The project was fully successful in the objective of producing defect-free, complex geometry of bismuth-telluride parts through LPBF, but only partially successful in achieving performance goals. First, cost reduction of manufacturing, as measured by material waste, was successfully reduced by up to 70% compared to conventional manufacturing methods. This exceeded the proposed 30% reduction in materials waste needed to reach the 20% cost reduction goal of the project. On the other hand, the device performance, as measured by Seebeck coefficient, failed to reach the 40% improvement in efficiency. Rather, we observe comparable Seebeck coefficient between AM samples and conventionally processed counterparts. The device-level efficiency improvement does exceed 40% for complex geometry samples due to shape-induced increase in temperature gradients, but this was not the originally proposed metric. The machine learning approach developed in this project greatly accelerated the process optimization and can be adopted for fast development of AM processing parameters for other brittle and otherwise difficult-to-print materials. For the public, we deliver an efficient and widely adoptable process for incorporating waste-heat harvesting thermoelectric devices in both industrial and commercial heat exchangers. The geometric flexibility allows the capturing device to conform to the shape of the heat source to improve the system-level conversion efficiency. The technique can be deployed on any commercial LBPF systems with zero modifications, thus poses minimal adoption barrier for any manufacturer that already employed AM technology. Beyond bismuth-telluride, the machine-learning guided optimization protocol can be used in the future to reduce both the time and cost of process development for AM of other energy conversion and harvesting materials.

36 MATERIALS SCIENCE↗

Intrinsic fatigue crack growth rates for Al-Li-Cu-Mg alloys in vacuum

The influences of microstructure and deformation mode on inert environment intrinsic fatigue crack propagation were investigated for Al-Li-Cu-Mg alloys AA2090, AA8090, and X2095 compared to AA2024. The amount of coherent shearable delta-prime (Al3Li) precipitates and extent of localized planar slip deformation were reduced by composition (increased Cu/Li in X2095) and heat treatment (double aging of AA8090). Intrinsic growth rates, obtained at high constant K(max) to minimize crack closure and in vacuum to eliminate any environmental effect, were alloy dependent; da/dN varied up to tenfold based on applied Delta-K or Delta-K/E. When compared based on a crack tip cyclic strain or opening displacement parameter, growth rates were equivalent for all alloys except X2095-T8, which exhibited unique fatigue crack growth resistance. Tortuous fatigue crack profiles and large fracture surface facets were observed for each Al-Li alloy independent of the precipitates present, particularly delta-prime, and the localized slip deformation structure. Reduced fatigue crack propagation rates for X2095 in vacuum are not explained by either residual crack closure or slip reversibility arguments; the origin of apparent slip band facets in a homogeneous slip alloy is unclear.

Slavik, D. C.↗

Characterization of Ceramic Matrix Composite Combustor Components: Pre and Post Exposure

The pursuit of lower emissions and higher performance from gas turbine engines requires the development of innovative concepts and the use of advanced materials for key engine components. One key engine component is the combustor, where innovative design and material improvements have the potential to lower emissions. Efforts to develop a High Speed Civil Transport with low emissions were focused on the evaluation of combustor concepts with liners fabricated from a ceramic matrix composite of silicon carbide fibers in a silicon carbide matrix (SiC/SiC). The evaluation of SiC/SiC composites progressed from simple coupons (to establish a first-order database and identify operant failure mechanisms and damage accumulation processes), to feature-based subelements (to assess fabricability and in situ material response), to actual components (to assess structural integrity, dimensional, and compositional fidelity) tested under simulated engine conditions. As in the case of all evolutionary material and process work, a key element to resolving fabrication issues is the evaluation of witness areas taken from fabricated components before testing the actual component. The witness material from these components allowed microstructural and mechanical testing to be performed and compared to the ideal, flat panel, conditions and data that are typical of basic characterization. This also allowed samples of similar design to be taken from components after 115 hours of combustion exposure. Testing consisted of tensile, double notch shear, ring burst, and thermal conductivity that sampled various regions of the components. The evaluation of the witness material allowed an understanding of the fabrication process, highlighting critical issues, in an early phase of the learning curve development of these configuration and material unique parts. Residual property testing, after exposure, showed if degradation of the material under actual service conditions was occurring. This paper will present the results of this critical testing. Evaluations that consider the degree of complexity of the fabricated part were established to relate in situ performance to that of flat panel based coupons. Nondestructive evaluation was used throughout the evaluation process. These results will also be discussed as an aid in understanding the test results.

Ojard, G.↗

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↗

Investigation of interfacial strength in nacre-mimicking tungsten heavy alloys for nuclear fusion applications

Abstract Tungsten heavy alloys have been proposed as plasma facing material components in nuclear fusion reactors and require experimental investigation in their confirmation. For this purpose, a 90W–7Ni–3Fe alloy has been selected and microstructurally manipulated to present a multiphase brick-and-mortar structure of W-phase ‘bricks’ surrounded by a ductile ‘mortar’. This work draws inspiration from nature to artificially imitate the extraordinary combination of strength and stiffness exhibited by mollusks and produce a nacre-mimicking metal matrix composite capable of withstanding the extremely hostile environment of the reactor interior and maintaining structural integrity. The underlying mechanisms behind this integrity have been probed through high-resolution structural and chemical characterization techniques and have revealed chemically diffuse phase boundaries exhibiting unexpected lattice coherency. These features have been attributed to an increase in the energy required for interfacial decohesion in these systems and the simultaneous expression of high strength and toughness in tungsten heavy alloys.

36 MATERIALS SCIENCE↗

Exploiting the Temperature/Concentration Dependence of Magnetic Susceptibility to Control Convection in Fundamental Studies of Solidification Phenomena

The objective of this new research project is to demonstrate by experiment, supplemented by mathematical modeling and physical property measurement, that the effects of buoyancy driven convection can be largely eliminated in ground-based experiments, and further reduced in flight, by applying a new technique. That technique exploits the dependence of magnetic susceptibility on composition or temperature. It is emphasized at the outset that the phenomenon to be exploited is fundamentally and practically different from the magnetic damping of convection in conducting liquids that has been the subject of much prior research. The concept suggesting this research is that all materials, even non-conductors, when placed in a magnetic field gradient, experience a force. Of particular interest here are paramagnetic and diamagnetic materials, classes which embrace the "model alloys", such as succinonitrile-acetone, that have been used by others investigating the fundamentals of solidification. Such alloys will exhibit a dependence of susceptibility on composition. The consequence is that, with a properly oriented field (gradient) a force will arise that can be made to be equal to, but opposite, the buoyancy force arising from concentration (or temperature) gradients. In this way convection can be stilled. The role of convection in determining the microstructure, and thereby properties, of materials is well known. Elimination of that convection has both scientific and technological consequences. Our knowledge of diffusive phenomena in solidification, phenomena normally hidden by the dominance of convection, is enhanced if we can study solidification of quiescent liquids. Furthermore, the microstructure, microchemistry and properties of materials (thereby practical value) are affected by the convection occurring during their solidification. Hitherto the method of choice for elimination of convection has been experimentation in microgravity. However, even in low Earth orbit, residual convection has effects. That residual convection arises from acceleration (drag on the spacecraft), displacement from the center of mass or transients in the gravitational field (g-jitter). There is therefore a need for both further reducing buoyancy driven flow in flight and allowing the simulation of microgravity during ground based experiments. Previous investigations, the research project description, theory behind the study and experimental methods as well as plots of magnetic fields and forces are presented.

Evans, J. W.↗

Fabrication and Evaluation of Titanium and Zirconium based Wires for use during Extended, Deep Space, Missions

Novel materials and designs are necessary for transport vessels and propulsion systems to fulfill NASA's vision of easier access to space and the expansion of human exploration beyond low-earth orbit. Spacecraft components must necessarily be lighter and stronger than their predecessors and will likely be required to serve new purposes. Furthermore, they must be resilient to the thermal, vacuum, and radiation environment of space for extended periods of time and may need to perform in the near proximity of a nuclear fuel source. To this end research has been initiated to fabricate novel, composite, wires based on titanium and zirconium pearlitic alloys. It is expected that the fabricated wire will well endure in the space environment with application as tethers, sail components, fasteners, and a myriad of other (including earth-based) uses. A background on pearlitic wire, novel alloy development, microstructural characterization, and initial mechanical testing results will be presented and discussed.

Grugel, Richard N.↗

Oxygen Generation from Carbon Dioxide for Advanced Life Support

The partial electrochemical reduction of CO2 using ceramic oxygen generators (COGs) is well known and has been studied. Conventional COGs use yttria-stabilized zirconia (YSZ) electrolytes and operate at temperatures greater than 700 C (1, 2). Operating at a lower temperature has the advantage of reducing the mass of the ancillary components such as insulation. Moreover, complete reduction of metabolically produced CO2 (into carbon and oxygen) has the potential of reducing oxygen storage weight if the oxygen can be recovered. Recently, the University of Florida developed ceramic oxygen generators employing a bilayer electrolyte of gadolinia-doped ceria and erbia-stabilized bismuth oxide (ESB) for NASA s future exploration of Mars (3). The results showed that oxygen could be reliably produced from CO2 at temperatures as low as 400 C. These results indicate that this technology could be adapted to CO2 removal from a spacesuit and other applications in which CO2 removal is an issue. This strategy for CO2 removal in advanced life support systems employs a catalytic layer combined with a COG so that the CO2 is reduced completely to solid carbon and oxygen. First, to reduce the COG operating temperature, a thin, bilayer electrolyte was employed. Second, to promote full CO2 reduction while avoiding the problem of carbon deposition on the COG cathode, a catalytic carbon deposition layer was designed and the cathode utilized materials shown to be coke resistant. Third, a composite anode was used consisting of bismuth ruthenate (BRO) and ESB that has been shown to have high performance (4). The inset of figure 1 shows the conceptual design of the tubular COG and the rest of the figure shows schematically the test apparatus. Figure 2 shows the microstructure of a COG tube prior to testing. During testing, current is applied across the cell and initially CuO is reduced to copper metal by electrochemical pumping. Then the oxygen source becomes the CO/CO2. This presentation details the results of testing the COG.

Bishop, s. R.↗

Direct-write laser-assisted patterning of form birefringence in wave plates fabricated by glancing-angle deposition

The development of optics that provide spatial control of birefringence could enable better control of laser beam polarization, but available solutions are limited. Here we demonstrate a method to locally modify the birefringence of wave plates fabricated by glancing-angle deposition. The method employs localized melting of the anisotropic microstructure in a vacuum environment to alter the local birefringence. We demonstrate that this process is only possible under high vacuum to avoid trapping air within the melt zone. The direct-write method presented here can be readily utilized for coatings exhibiting form birefringence of virtually any chemical composition, size, and format.

42 ENGINEERING↗

The metallic microstructures and thermal histories of severely reheated chondrites

The metallographic structures of eight severely reheated chondrites - Farmington, Ramsdorf, Orvinio, Wickenburg, Lubbock, Rose City, Arapahoe, and Tadjera - were studied using optical, SEM and electron microprobe techniques. The following metallographic criteria were used to estimate the post-shock residual temperature of the chondrites: melted metal-troilite appearance, presence of martensite, phosphorus enrichment of metal and averaging of central metal grain compositions. The presence of phosphides and secondary kamacite are due to slow post-shock cooling rates. Ni rim gradients indicate both extensive remelting of metal grains and relatively fast cooling.

Smith, B. A.↗

Development of Methods of Characterizing Coal in Its Plastic State

Coal in its plastic state (typically 400-460 C) was examined by the isothermal Gieseler plastometry of seven selected coals of widely varying plastic properties. Kinetic models were proposed for the isothermal plastometric curves. Plastic behavior was compared with a variety of laboratory analyses and characterizations of these coals, including classical coal analysis; mineral analysis; microstructural analysis (extractable fractions, surface area measurement, and petrographic analysis); and thermal analysis (thermogravimetric analysis, thermomechanical analysis, and differential scanning calorimetry). The phenomenon of a sharp, large, poorly reproducible exotherm in the differential scanning calorimetric analysis of coking coals was examined. Several coal extrudates show mineral distribution, organic maceral composition and overall calorific value to be little affected by 800 F extrusion. Volatile matter and plastic properties are moderately reduced, and the network structure (as gauged by extractables) appears to be slightly degraded in the extrusion process.

Lloyd, W. G.↗

INEL Spray-forming Research

Spray forming is a near-net-shape fabrication technology in which a spray of finely atomized liquid droplets is deposited onto a suitably shaped substrate or mold to produce a coherent solid. The technology offers unique opportunities for simplifying materials processing without sacrificing, and oftentimes substantially improving, product quality. Spray forming can be performed with a wide range of metals and nonmetals, and offers property improvements resulting from rapid solidification (e.g., refined microstructures, extended solid solubilities and reduced segregation). Economic benefits result from process simplification and the elimination of unit operations. Researchers at the Idaho National Engineering Laboratory (INEL) are developing spray-forming technology for producing near-net-shape solids and coatings of a variety of metals, polymers, and composite materials. Results from several spray forming programs are presented to illustrate the range of capabilities of the technique as well as the accompanying technical and economic benefits. Low-carbon steel strip greater than 0.75 mm thick and polymer membranes for gas/gas and liquid/liquid separations that were spray formed are discussed; recent advances in spray forming molds, dies, and other tooling using low-melting-point metals are described.

Mchugh, Kevin M.↗

Sol-gel Technology and Advanced Electrochemical Energy Storage Materials

Advanced materials play an important role in the development of electrochemical energy devices such as batteries, fuel cells, and electrochemical capacitors. The sol-gel process is a versatile solution for use in the fabrication of ceramic materials with tailored stoichiometry, microstructure, and properties. This processing technique is particularly useful in producing porous materials with high surface area and low density, two of the most desirable characteristics for electrode materials. In addition,the porous surface of gels can be modified chemically to create tailored surface properties, and inorganic/organic micro-composites can be prepared for improved material performance device fabrication. Applications of several sol-gel derived electrode materials in different energy storage devices are illustrated in this paper. V2O5 gels are shown to be a promising cathode material for solid state lithium batteries. Carbon aerogels, amorphous RuO2 gels and sol-gel derived hafnium compounds have been studied as electrode materials for high energy density and high power density electrochemical capacitors.

Chung-tse Chu↗

High-Energy All-Solid-State Organic–Lithium Batteries Based on Ceramic Electrolytes

Recent studies have identified unique properties of organic battery electrode materials such as moderate redox potentials and mechanical softness which are uniquely beneficial for all-solid-state batteries based on ceramic electrolytes. Here, we further explore the promise of organic materials and demonstrate a sulfide electrolyte- based organic-lithium battery with a specific energy of 828 Wh kg –1 , rivaling the state-of- the-art of all-solid-state batteries. Two innovation steps are responsible for the accomplishment. First, the combination of lithium anode and the high-capacity cathode material pyrene-4,5,9,10-tetraone ensures a high theoretical specific energy. Second, the microstructure of the organic cathode is optimized with the introduction of cryomilling, a technique common to processing soft materials but not familiar to electrode fabrication. The cathode material utilization increases to 99.5% as a result, up from the 55–89% previously reported for ceramic electrolyte-based solid-state organic batteries. In conclusion, the improvement highlights the special requirements of solid-state organic electrodes for microstructural engineering while preserving the chemical integrity of components.

25 ENERGY STORAGE↗

The role of nickel content and the magnetic remanence in iron-nickel alloys of lunar composition

Lunar samples are magnetic primarily due to the body centered cubic (BCC) iron and iron-nickel alloys they contain. Presented for the first time are results which demonstrate that the magnitude of the martensitic thermal remanence (MTRM) induced on quenching iron-nickel alloy in the geomagnetic field depends on the nickel content of the alloy. High magnetic stability is due to the increasing dislocation density and increasingly complex microstructures associated with increasing nickel content in the alloys. The results agree with the mechanical and structural properties of the alloys. The characteristic quench martensite microstructure observed on metallographic examination provides a recognition criterion for the MTRM mechanism. These results are important for lunar and meteoritic research intending to ascertain the paleofield responsible for the observed remanent magnetization.-

Wasilewski, P.↗

Effects of carbonitrides and carbides on microstructure and properties of castable nanostructured alloys

In this work, to develop advanced reduced-activation ferritic-martensitic (RAFM) steels for fusion reactor structural applications, both carbonitride- and carbide-strengthened castable nanostructured alloys (CNAs) were explored for higher densities of MX (M = Ti/Ta/V/etc. and X = C/N) nanoprecipitates. Additionally, systematic comparisons between the two types of CNAs indicated generally similar microstructures and comparable tensile properties and creep resistance. However, the carbide-CNAs did show some advantages over the carbonitride-CNAs in terms of the uniformly distributed higher density of MC nanoprecipitates, greater Charpy impact upper shelf energies, less deuterium retention and swelling, and potentially less transmutation-induced composition changes and consequently thermodynamically more stable carbides. The carbide-CNAs showed the best-balanced high performance in the examined properties, in contrast to the significantly varied performance of oxide-dispersion-strengthened alloys and the generally lower performance of current RAFM steels.

36 MATERIALS SCIENCE↗

Atomically Resolved Electrically Active Intragrain Interfaces in Perovskite Semiconductors

Deciphering the atomic and electronic structures of interfaces is key to developing state-of-the-art perovskite semiconductors. However, conventional characterization techniques have limited previous studies mainly to grain-boundary interfaces, whereas the intragrain-interface microstructures and their electronic properties have been much less revealed. Herein using scanning transmission electron microscopy, we resolved the atomic-scale structural information on three prototypical intragrain interfaces, unraveling intriguing features clearly different from those from previous observations based on standalone films or nanomaterial samples. These intragrain interfaces include composition boundaries formed by heterogeneous ion distribution, stacking faults resulted from wrongly stacked crystal planes, and symmetrical twinning boundaries. The atomic-scale imaging of these intragrain interfaces enables us to build unequivocal models for the ab initio calculation of electronic properties. Our results suggest that these structure interfaces are generally electronically benign, whereas their dynamic interaction with point defects can still evoke detrimental effects. This work paves the way toward a more complete fundamental understanding of the microscopic structure-property-performance relationship in metal halide perovskites.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Deformation and fracture of thin sheet aluminum-lithium alloys: The effect of cryogenic temperatures

The objective is to characterize the fracture behavior and to define the fracture mechanisms for new Al-Li-Cu alloys, with emphasis on the role of indium additions and cryogenic temperatures. Three alloys were investigated in rolled product form: 2090 baseline and 2090 + indium produced by Reynolds Metals, and commercial AA 2090-T81 produced by Alcoa. The experimental 2090 + In alloy exhibited increases in hardness and ultimate strength, but no change in tensile yield strength, compared to the baseline 2090 composition in the unstretched T6 condition. The reason for this behavior is not understood. Based on hardness and preliminary Kahn Tear fracture experiments, a nominally peak-aged condition was employed for detailed fracture studies. Crack initiation and growth fracture toughness were examined as a function of stress state and microstructure using J(delta a) methods applied to precracked compact tension specimens in the LT orientation. To date, J(delta a) experiments have been limited to 23 C. Alcoa 2090-T81 exhibited the highest toughness regardless of stress state. Fracture was accompanied by extensive delamination associated with high angle grain boundaries normal to the fatigue precrack surface and progressed microscopically by a transgranular shear mechanism. In contrast the two peak-aged Reynolds alloys had lower toughness and fracture was intersubgranular without substantial delamination. The influences of cryogenic temperature, microstructure, boundary precipitate structure, and deformation mode in governing the competing fracture mechanisms will be determined in future experiments. Results contribute to the development of predictive micromechanical models for fracture modes in Al-Li alloys, and to fracture resistant materials.

Wagner, John A.↗