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All sources NASA NTRS DOE OSTI

DOE OSTI2024

Ink Casting and 3D‐Extrusion Printing of Yb 14 MnSb 11 for High‐Temperature Thermoelectric Material

Abstract Complex shapes are created from Yb 14 MnSb 11 , a high‐temperature thermoelectric Zintl phase, via a two‐step process: i) layer‐by‐layer 3D‐extrusion of ink containing partially‐reacted powders which are ball‐milled from a blend of Yb, MnSb, and Sb powders; ii) heat treatment to synthesize the ternary compound Yb 14 MnSb 11 and densify the extruded powders. A high phase purity for Yb 14 MnSb 11 (83–94%) is achieved in both cast and 3D‐extruded ink specimens via a solid‐state reaction between Yb, MnSb, and Yb 4 Sb 3 during reactive sintering. Pressure‐free sintering at temperatures of 1200–1400 °C densifies the powders to 82% relative density but can also induce the decomposition of the Yb 14 MnSb 11 phase due to Yb sublimation. A process window with optimized sintering temperature and time is identified, achieving both low porosity and high phase purity and reaching a maximum zT = 0.61 at 1000 °C, about half of the maximum zT value for bulk Yb 14 MnSb 11 made via conventional processes (pressure sintering of precursor powders). The present approach – direct ink writing of ball‐milled powders, combined with reactive sintering – is a scalable and affordable method to fabricate thermoelectric legs with intricate 3D shapes, for enhanced performances in high‐temperature thermoelectric applications.

Chen, Ming [Department of Materials Science &amp, ↗

DOE OSTI2023

Analytical Study and Experimental Verification of Shear-Thinning Ink Flow in Direct Ink Writing Process

Abstract Direct ink writing (DIW) process is a facile additive manufacturing technology to fabricate three-dimensional (3D) objects with various materials. Its versatility has attracted considerable interest in academia and industry in recent years. As such, upsurging endeavors are invested in advancing the ink flow behaviors in order to optimize the process resolution and the printing quality. However, so far, the physical phenomena during the DIW process are not revealed in detail, leaving a research gap between the physical experiments and its underlying theories. Here, we present a comprehensive analytical study of non-Newtonian ink flow behavior during the DIW process. Different syringe-nozzle geometries are modeled for the comparative case studies. By using the computational fluid dynamics (CFD) simulation method, we reveal the shear-thinning property during the ink extrusion process. Besides, we study the viscosity, shear stress, and velocity fields, and analyze the advantages and drawbacks of each syringe-nozzle model. On the basis of these investigations and analyses, we propose an improved syringe-nozzle geometry for stable extrusion and high printing quality. A set of DIW printing experiments and rheological characterizations are carried out to verify the simulation studies. The results developed in this work offer an in-depth understanding of the ink flow behavior in the DIW process, providing valuable guidelines for optimizing the physical DIW configuration toward high-resolution printing and, consequently, improving the performance of DIW-printed objects.

Engineering↗

DOE OSTI2024

Monodomain Liquid‐Crystal Elastomer Lattices for Broad Strain‐Rate Mechanical Damping

Designing structures that effectively dissipate energy across a broad range of mechanical loading rates, including those from compression, shock, and vibration, poses a significant engineering challenge. In this study, liquid‐crystal elastomers (LCEs), which possess anisotropic properties due to the alignment of their polymer backbone, are explored. As a result, LCEs exhibit a soft elastic response under mechanical loading, making them ideal for energy dissipation. Advances in additive manufacturing (AM) enable simple fabrication of foamlike dissipative structures with complex lattice geometries. Herein, direct ink write 3D printing, an extrusion AM method, is used to fabricate aligned, monodomain LCE lattice structures for broad strain‐rate mechanical damping. In this work, it is shown that these structures can dissipate strain energy in quasi‐static environments, comparable to traditional elastomeric lattices, and provide improved damping under high strain‐rate drop testing due to LCE soft elasticity. Additionally, under dynamic mechanical vibration, monodomain LCE lattices enhance damping at structural natural frequencies and provide high‐frequency attenuation. Finally, in these findings, a promising method is presented for fabricating mechanical damping devices that effectively dissipate energy across a broad range of loading rates.

3D printings↗

DOE OSTI2021

Utilizing computer vision and artificial intelligence algorithms to predict and design the mechanical compression response of direct ink write 3D printed foam replacement structures

Additive Manufacturing (AM) of porous polymeric materials, such as foams, recently became a topic of intensive research due their unique combination of low density, impressive mechanical properties, and stress dissipation capabilities. Conventional methods for fabricating foams rely on complex and stochastic processes, making it challenging to achieve precise architectural control of structured porosity. In contrast, AM provides access to a wide range of printable materials, where precise spatial control over structured porosity can be modulated during the fabrication process enabling the production of foam replacement structures (FRS). Current approaches for designing FRS are based on intuitive understanding of their properties or an extensive number of finite element method (FEM) simulations. These approaches, however, are computationally expensive and time consuming. As such, in this work, we present a novel methodology for determining the mechanical compression response of direct ink write (DIW) 3D printed FRS using a simple cross-sectional image. By obtaining measurement data for a relatively small number of samples, an artificial neural network (ANN) was trained, and a computer vision algorithm was used to make inferences about foam compression characteristics from a single cross-sectional image. Finally, a genetic algorithm (GA) was used to solve the inverse design problem, generating the AM printing parameters that an engineer should use to achieve a desired compression response from a DIW printed FRS. The methods developed herein present an avenue for entirely autonomous design and analysis of additively manufactured structures using artificial intelligence.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Evaluating Barcode Size and Metal Surface Treatment Options for a Global UF 6 Cylinder Identifier

A team at Oak Ridge National Laboratory tested various barcode sizes, materials, surface finishes, and marking techniques to determine suitable direct part marking techniques and barcode specifications for a new uranium hexafluoride (UF 6 ) cylinder global identifier. This paper describes testing those variables at different read distances and angles with several commercial off-the-shelf direct part mark or barcode readers. This research concluded that a 1.4 in. 2D Data Matrix barcode with a 0.1 in. quiet zone would be appropriate for the machine-readable feature on the proposed UF 6 cylinder global identifier. Testing suggests that this size barcode could be read from an angle of up to 30° over the range of 10–100 cm using multiple commercial off-the-shelf handheld direct part mark or barcode readers. Testing also suggested that barcodes marked on ball-blasted stainless steel with CerMark laser marking ink may be a good choice for the proposed UF 6 cylinder global identifier because they exhibited high contrast and were readable from a desirable range of distances and angles.

42 ENGINEERING↗

DOE OSTI2020

High temperature additive manufacturing print head

A system of 3D printing using a high temperature 3D print head that functions as a “modified ink jet” printer. The print head has the ability to print high temperature material such as metal, silicon carbide, and other high temperature material as opposed to inks or plastics. The print head is fabricated from a high temperature material to maintain structural integrity while operation at temperatures above the melting temperature for the material that is being printed.

36 MATERIALS SCIENCE↗

DOE OSTI2026

The Impact of Catalyst Layer Properties and Transport Layer Interactions on Rutile Iridium Oxide Anode Durability in Proton Exchange Membrane Electrolysis

The performance and durability of proton exchange membrane electrolyzers are governed by the interplay between catalyst inks and integration, the resulting catalyst layer (CL) structure, and the interface between the CL and porous transport layer (PTL). In this study, we examine the impact of these factors on cell performance and degradation using rutile IrO2 as the anode catalyst. The two commercial rutile IrO2 catalysts differ from each other and from the amorphous benchmark in agglomerate size and ink stability. This has implications for CL morphology and electronic connectivity. In the context of long-term pressurized operation for up to 1000 h, the selection of the PTL has a marginal effect on the durability of CLs with good structural and compositional properties, whereas poorly structured CLs demonstrate evident degradation when used with certain PTLs. Poor CL properties amplify the negative impact of non-ideal CL/PTL interfaces, demonstrating the importance of CL/PTL interface engineering.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Enhancing water and oxygen transport through electrode engineering for AEM water electrolyzers

Anion-exchange membrane water electrolyzers (AEMWEs) can accelerate the deployment of more efficient and affordable hydrogen production solutions. Here, electrode structure is shown to affect water back-diffusion and oxygen transport, which, in return, governs overpotential behaviors in AEMWEs. Measurements indicate that electrode with copious catalytic sites produces water close to the AEM, creating a higher water gradient and driving water back-diffusion, which improves membrane hydration and mass transport. In situ measurement reveals a high pH gradient near the anode surface, which affects anode kinetics. Operando measurement shows reduced oxygen accumulation when decoupling oxygen production and transport on anode. Catalyst ink rheology and stability are tuned with additives to realize scalable fabrication of electrodes with enhanced transport features, allowing AEMWE to operate at 2 A cm−2 for over 1,000+ h at a 2.3 μV h−1 degradation rate. Analysis during and post-durability provides insights into degradation mechanisms. This work demonstrates an electrode design strategy for efficient and durable AEMWEs.

AEM↗

DOE OSTI2024

Additive manufacturing of multiscale NiFeMn multi-principal element alloys with tailored composition

Nanostructured multi-principal element alloys (MPEAs) have been explored as next-generation engineering materials due to unique mechanical and functional properties which have significant advantages over traditional dilute alloys. However, the practical applications of nanostructured MPEAs are still limited due to the lack of scalable processing approaches to prepare a large quantity of nanostructured MPEAs, as well as lack of an efficient pathway for high-throughput discovery of better functional nanostructured MPEAs within their vast compositional space. Here we tackle these challenges by presenting an integrated approach by combining direct-ink-writing-based additive manufacturing, solid-state sintering, and chemical dealloying to manufacture hierarchically porous MPEAs. The hierarchical structure is comprised of macro- and micro-scale pores introduced via extrusion printing and polymer decomposition during sintering, as well as nanoscale pores formed via chemical dealloying. The macro- and micro-scale pores allow efficient dealloying of a large mass of material as the diffusion length that the corroding medium must penetrate remains at the scale of the ligaments formed after sintering (∼10 μm), despite the large volume of the 3D-printed samples. In addition, this integrated approach enables versatile control of the alloy composition via precisely tuning the ratio of elemental powders in the starting ink, thus offering a pathway for high-throughput discovery of novel functional MPEAs. As a case study, multiscale macro/micro/nanoporous NiFeMn MPEAs with three different compositions were investigated as catalysts to reduce the overpotential of oxygen evolution reaction (OER), where NiFeMn-based electrocatalysts display composition-dependent performance such that the overpotential measured at a current of 0.5 A g −1 for OER increases in the order of Ni 58 Fe 29 Mn 13 ⩽ Ni 64 Fe 26 Mn 10 < Ni 76 Fe 18 Mn 6 . This introduced manufacturing process offers new opportunities for scalable fabrication and rapid screening of nanostructured multi-component complex alloys.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Virtual Inspection of Advanced Manufacturing via Process-Scale Digital Twins (Abbreviated Report)

Inspection and certification comprise the most significant bottlenecks in advanced manufacturing for NNSA applications, often requiring far more time and resources than the fabrication of the parts themselves. Traditional methods, such as manual review and X-ray computed tomography, are not only slow and costly, but also struggle to provide a clear connection between manufacturing instructions and the final performance of critical components. This gap limits both the agility and assurance needed to support the modernization and safety of the United States nuclear stockpile. In response, our Strategic Initiative established a digital twin framework that integrates realtime process monitoring, automated data analysis, and immersive virtual reality collaboration into a unified inspection pipeline. By leveraging data from sensors, machine instructions, and imaging, we created high-fidelity virtual models of manufactured parts that could be rapidly analyzed and certified. This approach was first demonstrated with Direct Ink Write, and then extended to other manufacturing settings, including conventional (or “subtractive”) manufacturing and to predict the end of life performance of parts per the aging and lifetimes programs. The result is a transformational capability: inspection times have been reduced by a factor of 120,000 without loss of accuracy and while simultaneously improving traceability and confidence in part quality. This framework not only streamlines certification for critical applications, but also positions the national security enterprise to respond more flexibly to emerging challenges, supporting agile manufacturing and digital engineering practices across a broad range of mission-relevant domains.

42 ENGINEERING↗

DOE OSTI2023

Orthogonal luminescence lifetime encoding by intermetallic energy transfer in heterometallic rare-earth MOFs

Lifetime-encoded materials are particularly attractive as optical tags, however examples are rare and hindered in practical application by complex interrogation methods. Here, we demonstrate a design strategy towards multiplexed, lifetime-encoded tags via engineering intermetallic energy transfer in a family of heterometallic rare-earth metal-organic frameworks (MOFs). The MOFs are derived from a combination of a high-energy donor (Eu), a low-energy acceptor (Yb) and an optically inactive ion (Gd) with the 1,2,4,5 tetrakis(4-carboxyphenyl) benzene (TCPB) organic linker. Precise manipulation of the luminescence decay dynamics over a wide microsecond regime is achieved via control over metal distribution in these systems. Demonstration of this platform’s relevance as a tag is attained via a dynamic double encoding method that uses the braille alphabet, and by incorporation into photocurable inks patterned on glass and interrogated via digital high-speed imaging. This study reveals true orthogonality in encoding using independently variable lifetime and composition, and highlights the utility of this design strategy, combining facile synthesis and interrogation with complex optical properties.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Organic Nano-Junctions: Linking Nanomorphology and Charge Transport in Organic Semiconductor Nanoparticles for Organic Photovoltaic Devices

In this study, innovative nanoscale devices are developed to investigate the charge transport in organic semiconductor nanoparticles. Using different steps of lithography techniques and dielectrophoresis, planar organic nano-junctions are fabricated from which hole mobilities are extracted in a space charge-limited current regime. Subsequently, these devices are used to investigate the impact of the composition and morphology of organic semiconductor nanoparticles on the charge mobilities. Pure donor nanoparticles and composite donor:acceptor nanoparticles with different donor compositions in their shell are inserted in the nanogap electrode to form the nano-junctions. The results highlight that the hole mobilities in the composite nanoparticles decrease by two-fold compared to pure donor nanoparticles. However, no significant change between the two kinds of composite nanoparticle morphologies is observed, indicating that conduction pathways for the holes are as efficient for donor proportion in the shell from 40% to 60%. Organic photovoltaic (OPV) devices are fabricated from water-based colloidal inks containing the two composite nanoparticles (P3HT:eh-IDTBR and P3HT:o-IDTBR) and no significant change in the performances is observed in accordance with the mobility results. Through this study, the performance of OPV devices have been successfully correlated to the transport properties of nanoparticles having different morphology via innovative nanoscale devices.

42 ENGINEERING↗

DOE OSTI2021

Integrating helicoid channels for passive control of fiber alignment in direct-write 3D printing

3D printing of fiber-reinforced composites has been receiving increasing attention as an efficient additive approach enabling lightweight, functional, and high-performance components required for industrial applications. The properties of fiber composites significantly depend on internal microstructures, including fiber orientation, distribution, and degree of alignment. Although multiple strategies have been introduced for controlling the fiber composites microstructures, these strategies are mostly active approaches relying on additional control of mechatronics parts, external forces, or intentionally introduced unstable flows inside narrow nozzles. These methods suffer from higher risk of nozzle clogging and requiring extra parts in 3D printing. Here, we introduce helicoid channels into extrusion system as a passive approach to control the fiber alignment without any additional moving parts in direct-write 3D printing. The helicoid channels automatically guide the composite inks and align fibers before flowing into narrow nozzle space, avoiding clogging and improving printability. The analyses indicate that both helicoid surface to volume ratio and helix angle affect the pre-alignment of fibers, leading to tunable mechanical properties of printed fiber-reinforced composites with increased stiffness and strength up to 77.6% and 47.8%, respectively.

36 MATERIALS SCIENCE↗

NASA NTRS2019

Marshall Space Flight Center Faculty Fellowship Program

The 2018 Marshall Faculty Fellowship Program involved 16 faculty in the laboratories and departments at Marshall Space Flight Center. These faculty engineers and scientists worked with NASA collaborators on NASA projects, bringing new perspectives and solutions to bear. This Technical Memorandum is a compilation of the research reports of the 2018 Marshall Faculty Fellowship program, along with the Program Announcement (Appendix A) and the Program Description (Appendix B). The research affected the following five areas: (1) Materials (2) Propulsion (3) Spacecraft systems (4) Vehicle systems (5) Space science The materials investigations includes Lunar Regolith for habitats, friction stir welding, and composite joints. Propulsion studies included cryogenic tank pressurization, transmitted torque in a cryogenic environment, and condensation in presence of noncondensables, Europa Lander Deorbit Stage, and catalyst development for a hybrid rocket. Spacecraft systems include wireless sensor networks and printed electronic inks. Vehicle systems studies were performed on Mars ascent vehicle analysis, architecture models, and Space Launch System manual steering. Space science studies included planetary lava flow. Our goal is to continue the Marshall Faculty Fellowship Program funded by Center internal project offices. Faculty Fellows in this 2018 program represented the following minority-serving institutions: Alabama A&M University, Southern University, Delgado Community College, and Dillard University.

Six, N. F.↗

DOE OSTI2020

Cost-Effective Additive Manufacturing of Ambient Pressure-Dried Silica Aerogel

The conventional manufacturing processes for aerogel insulation materials mostly rely on the supercritical drying, which suffers from issues of massive energy consumption, high-cost equipment, and prolonged processing time. Considering the large market demand for the aerogel insulation material in the next decade, a cost-effective and scalable fabrication technique is highly desired. In this paper, a direct ink writing (DIW) method is used to three-dimensionally fabricate the silica aerogel insulation material, followed by room-temperature and ambient pressure drying. Compared with the supercritical drying and freeze-drying techniques, the reported method significantly reduces the fabrication time and costs. The cost-effective DIW technique offers the capability to print complex hollow internal structures, coupled with the porous aerogel structure, it is found to be beneficial for the thermal insulation property. In this work, the addition of fiber to the ink assures the durability of the fabricated product, without sacrificing the thermal insulation performance. The foam ink preparation methods and the printability are demonstrated in this paper, along with the printing of complex three-dimensional geometries. The thermal insulation performance of the printed objects is characterized, and the mechanical properties were also examined. The proposed approach is found to have a 56% reduction in the processing time. The printed silica aerogels exhibit a low thermal conductivity of 0.053 W m –1 K –1 .

36 MATERIALS SCIENCE↗

DOE OSTI2024

Vapor-induced phase-separation-enabled versatile direct ink writing

Abstract Versatile printing of polymers, metals, and composites always calls for simple, economic approaches. Here we present an approach to three-dimensional (3D) printing of polymeric, metallic, and composite materials at room conditions, based on the polymeric vapor-induced phase separation (VIPS) process. During VIPS 3D printing (VIPS-3DP), a dissolved polymer-based ink is deposited in an environment where nebulized non-solvent is present, inducing the low-volatility solvent to be extracted from the filament in a controllable manner due to its higher chemical affinity with the non-solvent used. The polymeric phase is hardened in situ as a result of the induced phase separation process. The low volatility of the solvent enables its reclamation after the printing process, significantly reducing its environmental footprint. We first demonstrate the use of VIPS-3DP for polymer printing, showcasing its potential in printing intricate structures. We further extend VIPS-3DP to the deposition of polymer-based metallic inks or composite powder-laden polymeric inks, which become metallic parts or composites after a thermal cycle is applied. Furthermore, spatially tunable porous structures and functionally graded parts are printed by using the printing path to set the inter-filament porosity as well as an inorganic space-holder as an intra-filament porogen.

42 ENGINEERING↗

DOE OSTI2025

Recent Advances in Scalable, High‐Mass Loaded Electrodes for Grid‐Scale Energy Storage

Abstract The increasing electrification of daily life as well as the intermittent characteristic of renewable energy sources require viable solutions for grid‐scale energy storage. Critical considerations for grid storage applications are electrode mass loading and electrode thickness as these features govern battery pack energy density, an important factor in determining manufacturing costs. For this reason, there is increased interest in finding new ways of creating electrodes with high mass loading. In this review, various high‐mass loading fabrication approaches are considered for positive electrode materials used in batteries. The benchmark used for high mass loading is above 20 mg cm −2 , which is higher than the practical limit of conventional tape‐cast electrodes. Several different electrode approaches are described including templating, laser patterning, direct ink writing, and electrodeposition. A variety of materials are covered with the most prominent being LiFe(PO 4 ) (LFP), LiCoO 2 (LCO), and MnO 2 . In research to date, scalable electrochemical performance has been achieved with mass loadings over 100 mg cm −2 . Areal capacities as high as 14.7 mAh cm −2 at 1.82 mA cm −2 have been achieved in non‐aqueous electrolytes and 9.8 mAh cm −2 at 10 mA cm −2 in aqueous electrolytes. These results establish that the mass loading of electrodes can be scaled up without compromising their electrochemical properties.

White, Makena [Department of Materials Science and↗

DOE OSTI2022

Laser strengthening of additive manufactured edge seal for vacuum insulated glazing with micro-size glass frit

Sealing of glass edge is a key step in developing cost-effective and durable vacuum insulated glazing for the drive towards net-zero energy buildings. In this study, to achieve a high-strength sealing with scalable and low-cost processing, we investigated a novel sealing method based on additive manufacturing and laser process and reported quantitative analysis of the laser assisted method sealing strength and the requirement of vacuum insulation glazing. Micro-size glass frits in printing ink and a continuous-wave laser curing were employed to allow the formation of a hermetic bonding layer with low thermal budget. Controlling various sealing parameters including laser traveling speed, spot diameter, and laser power, the water seepage and mechanical strength of the resulting glass-to-glass bonding were examined. Through the response surface methodology, we identified the optimized sealing condition where the bonding strength reached 5.68 MPa. A comparation of the bonding strength between thermal sealing method and laser-assisted method has been analyzed as well.

42 ENGINEERING↗