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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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All sourcesNASA NTRSDOE OSTI
NASA NTRS2009

Flowability of JSC-1a

We have done a complete flowability characterization of the lunar soil simulant, JSC-1a, following closely the ASTM-6773 standard for the Schulze ring shear test. The measurements, which involve pre-shearing the material before each yield point, show JSC-1a to be cohesionless, with an angle of internal friction near 40 deg. We also measured yield loci after consolidating the material in a vibration table which show it to have significant cohesion (approximately equal to 1 kPa) and an angle of internal friction of about 60 deg. Hopper designs based on each type of flowability test differ significantly. These differences highlight the need to discern the condition of the lunar soil in the specific process where flowability is an issue. We close with a list not necessarily comprehensive of engineering rules of thumb that apply to powder flow in hoppers.

Rame, Enrique↗
NASA NTRSDate not supplied

Development and Optimization of Additively Manufactured NASA HR-1 for Space Applications

Metal additive manufacturing (AM) processes have been demonstrated to be effective at reducing costs and lead times associated with fabrication of complex propulsion component designs. Laser powder directed energy deposition (LP-DED) and laser powder bed fusion (L-PBF) are metal AM technologies that have effectively been used to produce a variety of parts for space applications. These technologies have enabled new designs and materials for these applications. The National Aeronautics and Space Administration (NASA) has identified the need to develop and advance new materials in unique space applications such as high-pressure hydrogen environments. One such metal alloy being developed for these applications is NASA HR-1. A high-strength Fe-Ni based superalloy, NASA HR-1 was designed to resist high pressure hydrogen environment embrittlement, oxidation, and corrosion. AM technologies have enabled the manufacturing of NASA HR-1 to be a feasible material for components in hydrogen environments. Development efforts for NASA HR-1 have completed build and heat treatment optimization, material characterization, thermophysical property testing, and mechanical testing in air and hydrogen environments to mature the understanding of the material. This presentation will summarize the development of NASA HR-1 for AM including composition and heat treatment optimization, microstructure characterization, and results of mechanical testing in air and high pressure hydrogen.

Additive Manufacturing↗
DOE OSTI2018

Efficient Recovery of Copper and Cobalt from the Matte–Slag Mixture of ISA Furnace by Injection of Coke and Pyrite

During ISA copper smelting process, ISASMELT furnace discharges a large amount of matte and slag mixture and the separation of them has an important influence on the recovery of valuable metals. This paper presented a reduction-sulfurization sedimentation process for recovering copper and cobalt from the matte–slag mixture of ISA furnace. Firstly, matte–slag mixture and traditional static sedimentation slag are characterized to determine their mineral composition and occurrence state. It indicates that Cu is primarily lost in slag in the form of sulfide, while Co is mostly lost in the form of oxide. With coke and pyrite as the reducing agent and vulcanizing agent, an orthogonal laboratory experiment was conducted to determine the effects of the smelting temperature and additive dosage on the recovery process. The optimum slag cleaning conditions were found to be: a coke dosage of 2 pct, a pyrite dosage of 2 pct, and a smelting temperature of 1260 °C lasting for 2 hours. In order to improve on the low utilization ratio of additives associated with the industrial sedimentation process, an innovative additive introducing method was put forward which enables the additives to mix and react with slag more adequately. A powder injection device was purpose-made to inject additives into molten slag in dispersion state, and a laboratory experiment was carried out to simulate this process. By injecting 2 pct coke and 2 pct pyrite, the contents of Cu and Co in cleaned slag decreased to 0.46 and 0.01 pct, respectively. It proves that the injection of additives into molten slag is an effective method to recover Cu and Co from the matte–slag mixture of ISA furnace.

36 MATERIALS SCIENCE↗
NASA NTRS1998

Imide Oligomers Containing Pendent and Terminal Phenylethynyl Groups-2

As part of a program to develop high-performance/high-temperature structural resins for aeronautical applications, imide oligomers containing pendent and terminal phenylethynyl groups were prepared, characterized and the cured resins evaluated as composite matrices. The oligomers were prepared at a calculated number-average molecular weight of 5000 g/mol and contained 15-20 mol% pendent phenylethynyl groups. In previous work, an oligomer containing pendent and terminal phenylethynyl groups exhibited a high glass transition temperature (approximately 313 C), and laminates therefrom exhibited high compressive properties, but processability, fracture toughness, microcrack resistance and damage tolerance were less than desired. In an attempt to improve these deficiencies, modifications in the oligomeric backbone involving the incorporation of 1,3-bis(3-aminophenoxy)benzene were investigated as a means of improving processability and toughness without detracting from the high glass transition temperature and high compressive properties. The amide acid oligomeric solutions were prepared in N-methyl-2-pyrrolidinone and were subsequently processed into imide powder, thin films, adhesive tape and carbon fiber prepreg. Neat resin plaques were fabricated from imide powder by compression moulding. The maximum processing pressure was 1.4 MPa and the cure temperature ranged from 350 to 371 C for 1 h for the mouldings, adhesives, films and composites. The properties of the 1,3-bis(3-aniinophenoxy)benzene modified cured imide oligomers containing pendent and terminal phenylethynyl groups are compared with those of previously prepared oligomers containing pendent and terminal phenylethynyl groups of similar composition and molecular weight.

Connell, J. W.↗
NASA NTRS2010

Fatigue Resistance of the Grain Size Transition Zone in a Dual Microstructure Superalloy Disk

Mechanical property requirements vary with location in nickel-based superalloy disks. To maximize the associated mechanical properties, heat treatment methods have been developed for producing tailored microstructures. In this study, a specialized heat treatment method was applied to produce varying grain microstructures from the bore to the rim portions of a powder metallurgy processed nickel-based superalloy disk. The bore of the contoured disk consisted of fine grains to maximize strength and fatigue resistance at lower temperatures. The rim microstructure of the disk consisted of coarse grains for maximum resistance to creep and dwell crack growth at high temperatures up to 704 C. However, the fatigue resistance of the grain size transition zone was unclear, and needed to be evaluated. This zone was located as a band in the disk web between the bore and rim. Specimens were extracted parallel and transverse to the transition zone, and multiple fatigue tests were performed at 427 and 704 C. Mean fatigue lives were lower at 427 C than for 704 C. Specimen failures often initiated at relatively large grains, which failed on crystallographic facets. Grain size distributions were characterized in the specimens, and related to the grains initiating failures as well as location within the transition zone. Fatigue life decreased with increasing maximum grain size. Correspondingly, mean fatigue resistance of the transition zone was slightly higher than that of the rim, but lower than that of the bore. The scatter in limited tests of replicates was comparable for all transition zone locations examined.

Gabb, T. P.↗
DOE OSTI2018

Superdislocations and point defects in pyrochlore Yb2Ti2O7 single crystals and implication on magnetic ground states

Abstract This study reports atomic-scale characterization of structural defects in Yb 2 Ti 2 O 7, a pyrochlore oxide whose subtle magnetic interactions is prone to small perturbations. Due to discrepancies in the reported magnetic ground states, it has become a pressing issue to determine the nature of defects in this system. In the present study, we use atomic resolution scanning transmission electron microscopy techniques to identify the type of defects in the ytterbium titanate single crystals grown by the conventional optical floating zone (FZ) method. In addition to the known point defects of substitution Yb on Ti B-sites, extended defects such as dissociated superdislocations and anti-phase boundaries were discovered for the first time in this material. Such defects were prevalently observed in the FZ grown single crystals (of a darker color), in contrast to the stoichiometric white polycrystalline powders or high quality colorless single crystals grown by the traveling solvent floating zone technique. The lattice strains from these extended defects result in distortions of Yb-tetrahedron. A change of Ti valance was not detected at the defects. Our findings provide new insights into understanding the nature of defects that are of great importance for the physical property studies of geometrically frustrated compounds. Furthermore, this work sheds light on the complicated core structure of superdislocations that have large Burgers vectors in oxides with complex unit cells.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
NASA NTRS2018

Hybrid Additive Manufacturing Deposition and Selective Laser Melting Techniques Applied to Copper-Alloy Liquid Rocket Engine Combustion Chambers

Virgin Orbit and the NASA Marshall Space Flight Center have partnered to fabricate a small, multi-metallic, regeneratively cooled thrust chamber by leveraging the strengths of two different types of additive manufacturing: Direct Metal Laser Sintering (DMLS) for the copper alloy liner and blown powder Directed Energy Deposition (DED) for the Inconel structural jacket. The DED is being developed using Virgin Orbit's DMG Mori Seiki hybrid additive/subtractive machining center to further enable unique processing and further cost savings. The materials chosen are preferred for high performance thrust chamber applications, representing a significant advancement from the compromises typically made in the production of metal 3D printed thrust chambers for rocket engines. The 1.2K-lbf thrust article is a 16" tall, 3" diameter design modified for this effort to be regeneratively cooled with water and hot fired using a RP-1/LOX pintle-style development injector from Virgin Orbit's NewtonFour upper stage engine. The thrust chamber was tested at Virgin Orbit's Necker test site in Mojave, California. Results from this test campaign are reported in addition to information characterizing the liner, jacket, and bimetallic diffusion layer materials. This paper will also highlight some of the future bimetallic thrust chamber developments that MSFC and Virgin Orbit will complete under a recently awarded NASA contract.

Zagorski, Kevin↗
NASA NTRSDate not supplied

Development of Laser Powder Bed Fusion NASA HR-2 for Hydrogen Sensitive Liquid Rocket Engine Applications

The National Aeronautics and Space Administration (NASA) has been involved in the development and maturation of metal additive manufacturing (AM) for space applications since the late 2000s. AM has provided new design and manufacturing opportunities to reduce cost and schedule, consolidate parts, and optimize performance. Laser Powder Bed Fusion (L-PBF) is one of the most commonly used AM processes to fabricate components of complex shape requiring fine feature resolution. Due to exposure to high-pressure gaseous hydrogen, mechanical property degradation caused by hydrogen environment embrittlement (HEE) is a critical concern for many materials in liquid hydrogen propulsion systems. NASA has identified the need to develop and advance new materials in unique engine applications using liquid hydrogen as a propellant. One such material being developed at NASA Marshall Space Flight Center is L-PBF NASA HR-2 (Hydrogen Resistant-2), a high-strength Fe-Ni-based superalloy resistant to HEE. The chemistry of NASA HR-2 was formulated to meet requirements for key liquid rocket engine (LRE) components that operate in high-pressure hydrogen environments. Initial development and material characterization found that NASA HR-2 has excellent L-PBF printability, and its microstructure evolves well after heat treatment. This new alloy has undergone fundamental metallurgical evaluations, heat treatment studies, detailed microstructure characterization, and mechanical testing across a range of temperatures. Tensile testing was performed in a pressurized gaseous hydrogen (GH2) environment to assess its resistance to HEE. L-PBF NASA HR-2 has an average yield stress of 95 ksi, an ultimate tensile stress of 165 ksi, and a very high fracture elongation of 34 - 36% when tested in a high-pressure (5 ksi) hydrogen environment. The tensile property data confirms hydrogen has little influence on HR-2’s ductility, strength, and fracture behavior. L-PBF NASA HR-2 is a promising option for many hydrogen-sensitive LRE components that require exceptional resistance to HEE. This paper will provide an overview of the L-PBF process development, material characterization, mechanical and thermophysical properties, and LRE hardware development for NASA HR-2.

Po S Chen↗
DOE OSTI2019

Effects of Lanthanum on Structural and Magnetic Properties of Sr{sub 1−x}La{sub (2/3)x}Fe{sub 12}O{sub 19} Compounds: Theoretical and Experimental Results

Pre-reacted powders of M-type strontium hexaferrites with chemical composition Sr{sub 1−x}La{sub (2/3)x}Fe{sub 12}O{sub 19} (x = 0.1, 0.2, 0.3 0.5, 0.6) were obtained from the conventional solid state reaction method. The final consolidation of these powders were performed by using the spark plasma sintering (SPS) technique. The influence of the La{sup 3+} content on the crystal structure and the magnetic properties of the samples were investigated firstly under the framework of a phenomenological model that predicted the cation substitution/distribution in the Sr and/or Fe sites. The theoretical results indicated that La{sup 3+} ion mostly occupies the Sr{sup 2+} site. It was also found that as La content increased, a certain amount of Fe{sup 2+} ions appear as a consequence of the Fe{sup 3+} to Fe{sup 2+} reduction. However, the Fe{sup 2+} occupied preferably the 12k and 4f1 iron sites. The magnetic properties of the obtained samples were assessed by measurements performed in a vibrating sample magnetometer. Also, X-ray diffraction (XRD) measurements were presented as a complementary characterization. We have found that the magnetic properties of the samples degraded as the La{sup 3+} content increased and the increase of the Fe{sub 2}O{sub 3} impurity phase.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2023

Prioritization of Existing Reactor Materials

The Advanced Materials and Manufacturing Technologies (AMMT) Program is aiming at the faster incorporation of new materials and manufacturing technologies into complex nuclear-related systems. An integrated approach, combining advanced characterization, high-throughput and accelerated testing, modeling and simulation, including machine learning and artificial intelligence, will be employed. Although 316H (Fe–[16–18]Cr–[10–14]Ni–[2–3]Mo–[0.04–0.1]C) has been identified as a key alloy to be integrated into the AMMT accelerated alloy qualification approach because of its relevance for many current and future nuclear energy reactors, many other alloys could be considered for the advanced fabrication of innovative, high-performance nuclear components. Argonne National Laboratory (ANL), Idaho National Laboratory (INL), Oak Ridge National Laboratory (ORNL), and Pacific Northwest National Laboratory (PNNL) are collaborating on identifying the most promising alloy candidates relevant for the AMMT Program. A selection criteria matrix was established to evaluate the alloys considering their relative importance and technological readiness levels for nuclear energy applications, with a focus on laser powder bed fusion (LPBF). Because of the broad range of potential candidate alloys, ORNL and INL focused on nickel-based alloys, and ANL and PNNL mainly evaluated iron-based alloys. PNNL previously published material scorecards reports on several key alloys, and this report provides a broader overview of iron- and nickel-based candidate alloys, expending beyond alloys well-known to the nuclear community.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2022

Fabrication of silicon-tipped fiber-optic temperature sensors using aerogel-assisted glass soldering with precise laser heating

We demonstrate the fabrication of fiber-optic Fabry–Perot interferometer (FPI) temperature sensors by bonding a small silicon diaphragm to the tip of an optical fiber using low melting point glass powders heated by a 980 nm laser on an aerogel substrate. The heating laser is delivered to the silicon FPI using an optical fiber, while the silicon temperature is being monitored using a 1550 nm white-light system, providing localized heating with precise temperature control. The use of an aerogel substrate greatly improves the heating efficiency by reducing the thermal loss of the bonding parts to the ambient environment. A desirable temperature for bonding can be achieved with relatively small heating laser power. The bonding process is carried out in an open space at room temperature for convenient optical alignment. The precise temperature control ensures minimum perturbation to the optical alignment and no induced thermal damage to the optical parts during the bonding process. For demonstration, we fabricated a low-finesse and high-finesse silicon FPI sensor and characterized their measurement resolution and temperature capability. The results show that the fabrication method has a good potential for high-precision fabrication of fiber-optic sensors.

Sheng, Qiwen↗
NASA NTRS2001

Thermal Performance of Biological Substance Systems in Vitro Under Static and Dynamic Conditions at the Cryogenic Test Laboratory, NASA Kennedy Space Center, USA

A unique research program, including a comprehensive study of thermal performance at cryogenic vacuum insulation systems, was performed at the NASA Kennedy Space Center. The main goal was to develop a new soft vacuum system (from 1 torr to 10 torr) that provides an intermediate level of performance (k-value below 4.8 mW/m-K). Liquid nitrogen boil-off methods were used to test conventional materials, novel materials, and certain combinations. The test articles included combinations of aluminum foil, fiberglass paper, polyester fabric, silica aerogel composite blanket, fumed silica, silica aerogel powder, and syntactic foam. A new LCI system was developed at the Cryogenics Test Laboratory. This system performs exceptionally well at soft vacuum levels and nearly as good as an MLI at high vacuum levels. Apparent thermal conductivities for the LCI range from 2 mW/m-K at soft vacuum to 0.1 mW/m-K at high vacuum. Several cryostats were designed, constructed, and calibrated by the Cryogenics Test Laboratory at KSC NASA as part of this research program. The cryostat test apparatus is a liquid nitrogen boil-off calorimeter system for direct measurement of the apparent thermal conductivity at a fixed vacuum level between 5 x 10(exp -5) and 760 torr. The apparatus is also used for transient measurements of temperature profiles. The development of efficient, robust cryogenic insulation systems has been a targeted area of research for a number of years. Improved methods of characterization, testing, and evaluation of complex biological substance systems for cryosurgery and cryobiology are the focus of this paper.

Augustynowicz, S. D.↗
DOE OSTI2021

Embedding Sensors in 3D Printed Metal Structures

The Transformational Challenge Reactor (TCR) program is leveraging recent advances in modeling and simulation, materials, and additive manufacturing (AM) technologies to design a modern nuclear reactor. Some of the main TCR technologies include in situ monitoring and the integration of sensors during the manufacturing of quality-significant nuclear reactor components. This report describes the general procedure and process optimization for embedding sensors within generic stainless steel 316 (SS316) components using laser powder bed fusion (LPBF). A more detailed, quality-significant test plan and supporting procedures are available upon request (ORNL/TM-2021/2127). LPBF involves the use of a scanning laser to selectively melt regions of a powder bed, additively building a part layer by layer. This report describes the LPBF processing technique and discusses the effects of LPBF processing parameters on the success of the sensor embedding process. Experiments used machined cavities in the form of channels in an SS316 base for the sensors to lay in while material is additively built over the top, thereby embedding them in an SS316 matrix. A preliminary investigation involved using empty SS316 sheaths as surrogates to explore the effects of various LPBF processing parameters and the dimensional requirements of the machined channels. Microstructural investigations showed that a smaller channel width/depth combination closer to the sensor’s diameter was best for the embedding process. After the desired parameters were selected, Type-K thermocouples were embedded and evaluated post-embedding using nondestructive thermal testing, as well as destructive sectioning and microscopy. Post-build characterization showed that the thermocouples were well-bonded to the SS316 matrix and were fully functional after embedding. During thermal testing to temperatures up to 500 °C, the embedded thermocouples read consistently with one another and deviated only slightly from the readings of a nonembedded thermocouple located within the furnace. This slight discrepancy was most likely due to differences in the thermal time constants for a nonembedded thermocouple vs. a thermocouple embedded in a solid SS316 block. The results presented in this report will serve as the foundation for future work that will focus on embedding sensors in relevant TCR reactor components and eventually testing those components under neutron irradiation.

36 MATERIALS SCIENCE↗
NASA NTRSDate not supplied

Metal Additive Manufacturing Process Selection and Development Lifecycle for Propulsion Components

Metal additive manufacturing (AM) is a generic term that captures a variety of fabrication processes. Each of these manufacturing process has unique advantages and challenges for use in aerospace propulsion applications. The most commonly used AM processes include Powder Bed Fusion (PBF), Directed Energy Deposition (DED), and solid-state processes as in Cold Spray, Ultrasonic Additive Manufacturing, and Additive Friction Stir Deposition. While detailed research has been conducted among many of the AM processes to mature processing parameters and material properties, navigating which processes are best to select is difficult as it is based on specific component requirements. The focus of this presentation is to provide an overview of considerations for each of metal AM process selection for aerospace components based on various key attributes. These key attributes include geometric considerations, metallurgical characteristics, cost basis, post-processing and maturity of the processes. The data for these trade selections are based on studies that NASA as performed internally and with academic and industry partners. These studies include multiple AM build experiments to evaluate (1) geometric variations and constraints within the processes, (2) alloy characterization and mechanical testing, (3) pathfinder component development and hot-fire evaluations, and (4) certification approaches. This presentation summarizes these results and is meant to introduce specific examples which show what to consider when designing a metal AM component for aerospace propulsion applications.

Paul Gradl↗
DOE OSTI2024

Antiferromagnetic Ordering in Quasi-One-Dimensional FeBi 4 S 7

Here, we report a detailed study of the synthesis, composition, magnetic structure, and transport properties of a quasi-one-dimensional antiferromagnet FeBi 4 S 7 that contains chains of edge-sharing FeS 6 octahedra. High-resolution powder X-ray diffraction (PXRD) analysis, aided by variation of synthetic conditions, suggests that the true formula of the material is Fe 1.2 Bi 3.8 S 7 , due to the minor substitution of Fe into Bi sites. This finding is in agreement with crystal structure refinement from neutron powder diffraction data as well as with the small band gap of 0.23 eV determined from electrical transport measurements. Analysis of the neutron diffraction pattern collected below the antiferromagnetic ordering temperature of 64 K revealed ferromagnetic coupling between the Fe moments in the chains of FeS 6 octahedra. The overall ordering, however, is antiferromagnetic due to the antiparallel arrangement of moments on neighboring chains. The collinear spin arrangement is described by a k-vector (1, 0, 1/2), which indicates doubling of the unit cell in the c direction and the loss of the C-centering translation as compared to the nuclear cell. The ferromagnetic nature of the sulfide-bridged chains of Fe 2+ ions in FeBi 4 S 7 , in contrast to the antiferromagnetic coupling between Fe moments in compounds with similar structural fragments, can be justified by the analysis of metric parameters that characterize the Fe–S bonding in these materials.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Design of Novel Hot Gas Component for Gas Turbine Engines Enabled by Materials and Additive Manufacturing Process Development

This CRADA project was the result of a project award under FOA-DOE-0001980. The overarching FOA project team consisted of researchers from Carpenter Technology Corporation (CTC), Solar Turbines Incorporated (Solar), Pennsylvania State University (PSU), University of California-Santa Barbara (UCSB), and Oak Ridge National Laboratory (ORNL). Evaluations were conducted on two high-γ’ superalloys that were designed by CTC and the UCSB. One alloy named GammaPrint-700 (GP-700) is a cobalt-base superalloy. The other alloy named GammaPrint-1100 (GP-1100) is a nickel-base (Ni-base) superalloy. PSU provided expertise and experimental testing of the thermal performance of AM micro-cooling architectures. ORNL provided expertise with the AM superalloy materials characterization and AM processing science. Solar provided turbine component design expertise. The focus of this CRADA report is to document the efforts between ORNL and CTC towards the development of superalloys designed for AM. The project goal was to use an AM processable high-temperature superalloy and design for Additive Manufacturing (DfAM) techniques to design an efficient turbine component (i.e. a turbine tip shoe) with enhanced cooling features that can only be fabricated through additive manufacturing (AM). The efficiencies of existing combined heat and power (CHP) engines are capped by both component design and materials limitations. However, AM of a tip shoe component from a γ’strengthened superalloy offers the design flexibility to increase the efficiency and power of an industrial gas turbine. This project brought about advancements in the DfAM tip shoe design space and in the area of high temperature superalloys processable through laser powder bed fusion (LPBF) AM. State of art computation design tools were utilized to optimize unique cooling features into a tip shoe component design. A two-prong materials development approach was taken to support development of the AM tip shoe geometry. The first approach centered on investigating the processability and the appropriate process science for the industry standard high-γ’ nickel-base (Ni-base) superalloy Mar-M247. This superalloy is typically cast and considered non-weldable by traditional welding standards. In the course of this work, the alloy was not deemed feasible for process scale-up due to significant cracking issues during printing. The second approach focused on the development and evaluation of a novel cobalt-base superalloy, GammaPrint™-700 (GP-700 and a Ni-base superalloy, GammaPrint™-1100 (GP-1100) designed to mitigate the significant AM processing issues with Mar-M247. The processability of these two alloys were investigated through electron beam melting (EBM) binder-jet AM (BJAM), and LPBF as a risk mitigation for manufacturability. To be considered a candidate material for down-selection to proceed to full-scale AM tip shoe engine testing trials, the high temperature creep rupture strength was required to achieve at a minimum, a Larsen Miller Parameter (LMP) increase of 10.9% over the baseline material LPBF AM Hastelloy X.

99 GENERAL AND MISCELLANEOUS↗
DOE OSTI2025

Design of Novel Hot Gas Component for Gas Turbine Engines Enabled by Materials and Additive Manufacturing Process Development

This CRADA project was the result of a project award under FOA-DOE-0001980. The overarching FOA project team consisted of researchers from Carpenter Technology Corporation (CTC), Solar Turbines Incorporated (Solar), Pennsylvania State University (PSU), University of California-Santa Barbara (UCSB), and Oak Ridge National Laboratory (ORNL). Evaluations were conducted on two high-γ’ superalloys that were designed by CTC and the UCSB. One alloy named GammaPrint-700 (GP-700) is a cobalt-base superalloy. The other alloy named GammaPrint-1100 (GP-1100) is a nickel-base (Ni-base) superalloy. PSU provided expertise and experimental testing of the thermal performance of AM micro-cooling architectures. ORNL provided expertise with the AM superalloy materials characterization and AM processing science. Solar provided turbine component design expertise. The focus of this CRADA report is to document the efforts between ORNL and CTC towards the development of superalloys designed for AM. The project goal was to use an AM processable high-temperature superalloy and design for Additive Manufacturing (DfAM) techniques to design an efficient turbine component (i.e. a turbine tip shoe) with enhanced cooling features that can only be fabricated through additive manufacturing (AM). The efficiencies of existing combined heat and power (CHP) engines are capped by both component design and materials limitations. However, AM of a tip shoe component from a γ’strengthened superalloy offers the design flexibility to increase the efficiency and power of an industrial gas turbine. This project brought about advancements in the DfAM tip shoe design space and in the area of high temperature superalloys processable through laser powder bed fusion (LPBF) AM. State of art computation design tools were utilized to optimize unique cooling features into a tip shoe component design. A two-prong materials development approach was taken to support development of the AM tip shoe geometry. The first approach centered on investigating the processability and the appropriate process science for the industry standard high-γ’ nickel-base (Ni-base) superalloy Mar-M247. This superalloy is typically cast and considered non-weldable by traditional welding standards. In the course of this work, the alloy was not deemed feasible for process scale-up due to significant cracking issues during printing. The second approach focused on the development and evaluation of a novel cobalt-base superalloy, GammaPrint™-700 (GP-700 and a Ni-base superalloy, GammaPrint™-1100 (GP-1100) designed to mitigate the significant AM processing issues with Mar-M247. The processability of these two alloys were investigated through electron beam melting (EBM) binder-jet AM (BJAM), and LPBF as a risk mitigation for manufacturability. To be considered a candidate material for down-selection to proceed to fullscale AM tip shoe engine testing trials, the high temperature creep rupture strength was required to achieve at a minimum, a Larsen Miller Parameter (LMP) increase of 10.9% over the baseline material LPBF AM Hastelloy X.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Moisture Stability of Sulfide Solid-State Electrolytes

In this report we detail a comprehensive study on the moisture stability of sulfide solid-state electrolytes in dry room environments. Although sulfide SSEs have many favorable attributes, this class of materials suffers from poor stability with water. Sulfide SSEs react with water to form gaseous H 2 S and a variety of solid byproducts like Li 3 PO 4 and LiOH, which go on to increase the interfacial impedance of solid-state batteries. Lab-scale research typically utilizes gloveboxes with <1 ppm water, however, the large-scale manufacturing of Li-ion batteries occurs in –40°C dewpoint dry rooms with around 126 ppm water. Consequently, the moisture stability of sulfide SSEs must be addressed if the manufacture of solid-state batteries based on sulfide SSEs is to be scaled up. Here, we are the first to characterize the moisture stability of sulfide SSEs according to both H 2 S and the degradation of ionic conductivity at different moisture setpoints ranging from –76°C to –40°C dewpoint. A variety of different SSE compositions are studied; namely, (Li 2 S) 75 (P 2 S 5 ) 25 , (Li 2 S) 70 (P 2 S 5 ) 30 , (Li 2 O) 7 (Li 2 S) 68 (P 2 S 5 ) 25 , (Li 2 O) 7 (Li 2 S) 63 (P 2 S 5 ) 30 , and (Li 2 S) 75 (P 2 S 5 ) 25 + 20 mol% LiI. We find that moisture stability improves with 75 mol% Li2S modifier content and the introduction of a Li 2 O co-modifier. After a 30 min exposure in a –40°C dewpoint dry room environment we found that (Li 2 S) 75 (P 2 S 5 ) 25 + 20 mol% LiI powder generated 0.1 cc/g H 2 S and its ionic conductivity decreased by over 50%. However, when SSE powder was exposed as a slurry in a dodecane carrier the same SSE composition generated 0 cc/g H 2 S and its ionic conductivity only dropped by 14%. Our results show that sulfide SSEs have acceptable moisture stability when appropriately processed in a dry room environment.

25 ENERGY STORAGE↗