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All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Conclusions • Multimaterial and isotopically-labeled specimens were successfully fabricated via FFF-AM • Raman spectroscopy, atomic force microscopy, and neutron scattering show promise for direct measurements of interlayer diffusion in the multimaterial and isotopically-labeled specimens • Although isotopically-labeled specimens offer the greatest potential for experimentally verifying FFF-AM process models, substituting hydrogen with deuterium alters the thermal and rheological properties of the HDPE polymer

Multimaterial and Isotopically Labeled Specimen Fabrication via Material Extrusion Additive Manufacturing for Interlayer Diffusion Analysis

Jones, Haley W. [Savannah River National Laborator↗
NASA NTRS1998

Friction Stir Weld Tooling Development for Application on the 2195 Al-Cu-Li Space Transportation System External Tank

Friction Stir Welding (FSW) is a new and innovative solid-state joining process which can be applied to difficult-to- weld aluminum alloys. However, the large forces involved with the process have posed a production tooling challenge. Lockheed Martin Michoud Space Systems has overcome many of these challenges on the Super Lightweight External Tank (ET) program. Utilizing Aluminum-Copper-Lithium alloy 2195 in the form of plate and extrusions, investigations of FSW process parameters have been completed. Major loading mechanisms are discussed in conjunction with deflection measurements. Since the ET program is a cryogenic application, a brief comparison of cryogenic material properties with room temperature material properties is offered for both FSW and fusion welds. Finally, a new approach to controlling the FSW process from a load perspective is introduced. Emphasis will be put on tooling development, as well as the impact of tooling design and philosophy on Friction Stir Weld success probability.

Loftus, Zachary↗
NASA NTRS1987

Preliminary investigation of inertia friction welding B2 aluminides

An attempt is made to achieve inertia friction-welding in FeAl and NiAl samples, taking into account their intermetallics' compositions, extrusion parameters, and microstructural data. The energy required for the weld is stored in a rotating flywheel mass attached to one of the two pieces to be joined; when enough energy is introduced, the flywheel is disconnected and an axial load is applied which forces the spinning piece against the stationary one, converting the energy into heat by means of friction. Due to the inherent brittleness of the aluminides, a step-load program was used in which an initial, low-pressure heat buildup increased the work pieces' ductility.

Whittenberger, J. Daniel↗
DOE OSTI2026

Design, characterization and shape recovery behavior of 3D/4D printed shape memory polymers (SMPs)

Shape memory polymers (SMPs) represent a paradigm shift in material science, uniquely capable of undergoing reversible shape transformations triggered by external stimuli, positioning them as pivotal in developing next-generation biomedical devices, aerospace components, and adaptive structures. Extensive research has been done on SMPs with a major focus on high-temperature programming methods, which can limit energy efficiency and applicability with temperature-sensitive materials. Additionally, while various SMP blends have demonstrated great potential, limited work has been done on the suitability for 3D printing these materials, particularly under high-strain and ambient temperature programming conditions. In this study, a three-component optimized SMP composition was evaluated by 3D printing via the Material Extrusion (MEX) technique and investigating its ambient temperature-programming behavior at high strains. The SMP formulation studied was a tailored blend of thermoplastic polyurethane (TPU), polycaprolactone (PCL), and an octadecane diol-based copolymer (OBC) that exhibits robust shape memory behavior, high strain tolerance, and efficient force generation. Rigorous thermal, mechanical, and shape recovery analyses, along with optimized printing parameters and consistent shape recovery rates of up to 90%, were achieved under dynamic mechanical analysis (DMA), even under ambient programming conditions. This work demonstrates the SMP composition’s potential for adaptive, self-deployable systems with 4D printing characteristics ideal for bio-inspired structures and artificial muscle fibers.

Sudan, Kavish [University of Louisville, KY]↗
DOE OSTI2021

Blending Polyurethane Thermosets Using Dynamic Urethane Exchange

Recycling crosslinked polyurethanes (PUs) is accomplished through mechanical or chemical processes that are energy-intensive or produce plastics of lesser value. Polymer recycling processes are notably intolerant of polymer mixtures, yet the ability to reprocess and compatibilize two or more crosslinked PUs together will make this process more amenable to mixed waste streams while offering an opportunity to tune the properties of the recycled polymer products. Here, we blend a rigid polyester PU and a soft polyether PU using twin-screw extrusion to yield materials with tunable mechanical properties based on the feed composition. Their material properties were compared to those of compression-molded reprocessed blends and blends where the monomers were mixed prior to synthesis. The extruded materials showed similar mechanical and thermal properties to newly prepared blends and had higher-value mechanical properties compared to the samples reprocessed via compression molding. The morphologies of the blends were observed using phase imaging via atomic force microscopy to show that there is less phase separation in the extruded materials compared to compression-molded blends. The mechanical properties of these materials were tunable from soft to elastomeric to rigid based on the feed composition, and this tunability was demonstrated through four consecutive reprocessing cycles, through which the mechanical properties were steadily varied from rigid to soft by incorporating increasing amounts of soft polyether PU material. Here, this blending method for reprocessing mixed waste compatibilizes different PUs and provides a means to tune the mechanical properties of a PU product, even if starting from waste streams of varying compositions. As such, this process represents an intriguing new approach for polymer reprocessing.

Extrusion↗
DOE OSTI2022

Processing of hollow sections

A system and method provide a material with uniform micro-structure. In an embodiment, an equal channel angular extrusion system includes an interior mandrel. The interior mandrel includes an expanding shear material section and a contracting shear material section. In addition, the system includes a material. The material is disposed about a portion of the interior mandrel. Moreover, the system includes a pressure application device. The pressure application device applies pressure to the material to force the material to contact the expanding shear material section to provide an expanded post-shear material section. Pressure from the pressure application device applies pressure to the material to force the expanded post-shear material section to contact the contracting shear material section to provide a contracted shear material section.

Barber, Robert E.↗
NASA NTRS1980

Physical chemistry and evolution of salt tolerance in halobacteria

The cellular constituents of extremely halophilic bacteria not only tolerate high salt concentration, but in many cases require it for optical functioning. The characteristics affected by salt include enzyme activity, stability, allosteric regulation, conformation and subunit association. The salt effects are of two major kinds: electrostatic shielding of negative charges by cations at low salt concentration, and hydrophobic stabilization by salting-out type salts at high salt concentration. The composition of halobacterial proteins shows an excess of acidic amino acids and a deficiency of nonpolar amino acids, which accounts for these effects. Since the cohesive forces are weaker and the repulsing forces are stronger in these proteins, preventing aggregation in salt, these structures are no longer suited for functioning in the absence of high salt concentrations. Unlike these nonspecific effects, ribosomes in halobacteria show marked preference for potassium over sodium ions. To ensure the proper intracellular ionic composition, powerful ion transport systems have evolved in the halobacteria, resulting in the extrusion of sodium ions and their replacement by potassium. It is likely that such membrane transport system for ionic movements is a necessary requisite for salt tolerance.

Lanyi, J. K.↗
NASA NTRS1979

Relationship between proton motive force and potassium ion transport in Halobacterium halobium envelope vesicles

The permeability of Halobacterium halobium vesicle membranes to potassium ions was investigated, and possible mechanisms for the regulation of the gradient of protons by the transmembrane movement of these ions were studied. The lack of a potassium ion diffusion potential in the absence of valinomycin, light-induced electrical potentials in excess of the chemical potential difference for potassium ions, and direct measurements of potassium ion influx during illumination show that the membranes are relatively impermeable to these ions. As a result of sodium ion extrusion during illumination, chlorine ions and water must be lost and the vesicles collapse. The light-induced collapse of vesicles is diminished only if the influx of potassium ions is increased.

Lanyi, J. K.↗
NASA NTRS1998

Mechanistic Models of Friction Stir Welding

Friction stir welding is a welding process developed at The Welding Institute (TWI) in England. The method uses very large strain plastic deformation of the material to join two pieces of metal together. The material is deformed using a tool which is forced between the two pieces which rotates causing a bond. Beyond this, very little is actually known although many people working in the field are willing to speculate on the detailed mechanisms involved. Some measurements made using sacrificial thermocouples at the weld joint indicate that the maximum temperature during the weld process is on the order of 370C - well below the melting temperature of the material. However, at this temperature, the material properties are highly temperature dependent, and the yield stress is approximately an order of magnitude less at this temperature than it is at room temperature. As expected, there are many interpretations of the physical mechanisms occurring during the weld process. Although there is very little published concerned with FSW, some of the anecdotal theories will be described. One describes the primary mechanism as frictional heating at the front of the tool caused by slip between the tool and the material. At elevated temperatures, the weld material becomes soft and deforms around the tool but not essentially altered by the tool rotation, similar to an extrusion. As the material meets again at the rear of the tool, the temperatures and pressures are sufficient to cause the material to bond. All other structures seen are secondary and unimportant. Another theory examined last summer at NASA's Marshall Space Flight Center (MSFC) was that there was no slip between the tool and the material resulting in a rotating mass of plastic weld material traveling at a variety of angular velocities - the greatest at the tool surface diminishing to zero at the outer edge of the plastic mass surrounding the tool. This conceptual model was followed by simplified calculations which showed that the balance of moments through the weld plug was not possible under steady state conditions and realistic temperature profiles. This led to some consideration of a quasi-steady oscillating process. Later when force measurements became available some models were modified and new ones were proposed.

Stewart, Michael B.↗
DOE OSTI2024

The effect of stretching on polyamide – 6: assessment of crystallinity, mechanical properties, and surface roughness

Polyamide-6 (PA6), or nylon-6, is a widely used low-cost polymer material for various applications. Manufacturing PA6 into fibers involves a spinning process such as melt extrusion, which orients the polymer chains into a semicrystalline structure. When stretching the produced fibers to high strains, the PA6 fibers transition the metastable gamma phase back into the stable gamma phase. The effects of these large stretches on mechanical properties have not been explored after the stretch has been released. In this study, the effects on mechanical properties were studied by stretching the PA6 fibers from 10% to 50% tensile strain and subsequently releasing the fibers. The stretched fibers were characterized by X-ray diffraction and atomic force microscopy to determine the changes to the crystal structure and surface roughness. The stretched fibers were then tensile tested to failure and the tensile properties were examined. The stress-strain curves on the post-stretched PA6 fibers showed clear softening in the fibers with lower initial moduli after 30% stretching. Furthermore, these results may hold a clue to softening of fibers in applications with repeated loading and have implications for mechanical stability and fatigue of this polymeric material.

36 MATERIALS SCIENCE↗
NASA NTRS2001

Extensional Rheology Experiment Developed to Investigate the Rheology of Dilute Polymer Solutions in Microgravity

A fundamental characteristic of fluid is viscosity; that is, the fluid resists forces that cause it to flow. This characteristic, or parameter, is used by manufacturers and end-users to describe the physical properties of a specific material so that they know what to expect when a material, such as a polymer, is processed through an extruder, a film blower, or a fiber-spinning apparatus. Normally, researchers will report a shear viscosity that depends on the rate of an imposed shearing flow. Although this type of characterization is sufficient for some processes, simple shearing experiments do not provide a complete picture of what a processor may expect for all materials. Extensional stretching flows are common in many polymer-processing operations such as extrusion, blow molding, and fiber spinning. Therefore, knowledge of the complete rheological (ability to flow and be deformed) properties of the polymeric fluid being processed is required to accurately predict and account for the flow behavior. In addition, if numerical simulations are ever able to serve as a priori design tools for optimizing polymer processing operations such as those described above, an accurate knowledge of the extensional viscosity of a polymer system and its variation with temperature, concentration, molecular weight, and strain rate is critical.

Logsdon, Kirk A.↗
DOE OSTI2022

Large-scale reactive thermoset printing: Complex interactions between temperature evolution, viscosity, and cure shrinkage

Thermoset composites are strong candidates for large-scale material extrusion additive manufacturing (AM). However, uncured thermoset composites become unstable as print height increases. Here, chemical initiation of vinyl ester immediately before deposition was used to suppress collapse and enable large-scale thermoset printing. Structural stability was assessed by printing thin walls at various layer times and monitoring thermal gradients with an infrared camera. Stable printing was observed at a layer time of 4.50 min, approximately half the gel time of the material (8 min). Self-weight collapse occurred at short layer time (0.68 min), whereas warpage occurred at long layer time (6.50 min). Here, a new behavior was discovered at intermediate layer time (2.25 min) where the heat generated by the reaction causes new, un-gelled layers to flow. Forced convection eliminates this behavior, stabilizing the 2.25-min layer time print. These findings motivated development of a less exothermic material system, which was used to print a large-scale mold and demonstrate the value of this understanding. By presenting these challenges of large-scale reactive thermoset AM for the first time, this work motivates focused studies of the complex interplay between rheological, thermal, and chemical behaviors to improve the feasibility of large-scale thermoset AM. Tensile properties of the printed material were also measured. Longitudinal and transverse elastic moduli are 3.79 and 2.95 GPa, respectively, and corresponding tensile strengths are 36.11 and 18.83 MPa. The glass transition temperature is 93.13 °C.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Effects of soybean 7S protein on the quality and digestibility of dry rice noodles under twin‐screw extrusion process

Summary Starch and protein are important components of food, the mixed system formed between them (complexes, gels, mixtures, etc.) can improve the physical and chemical properties of starch and protein, and its potential application in the food industry has also attracted widespread attention. In this study, indica rice flour and soybean 7S protein (β‐Conglycinin) were used as the experimental materials to explore the effect of soybean 7S protein addition on the quality and digestibility of rice noodles. Aims to develop rice noodles with high protein and low GI, so that people can take care of their health while satisfying their appetites. The results showed that with the increase of soybean 7S protein addition, the starch digestibility decreased, resulting in the estimated glycaemic index (eGI) and glycaemic load (GL) decreasing. However, the cooking loss rate and breakage rate of rice noodles gradually increased, the water absorption first increased and then decreased, and the taste of rice noodles is acceptable when the 7S protein addition amount is within 9%. The interaction between starch and soybean 7S protein was mediated by weak interactions such as hydrogen bonds and hydrophobic forces indicated by Fourier transform infrared spectroscopy (FTIR) and X‐ray diffraction (XRD).

Qiao, Fan↗
NASA NTRS1994

Interactions between nested sunspots. 1: The formation and breakup of a delta-type sunspot

We investigate a nest of sunspots in which three ordinary bipolar pairs of sunspots are aligned collinearly. The usual spreading action of the growing regions brings two spots of leading polarity together (p-p collision) and forces the leading and trailing spots of the two interior regions to overlap inot a single penumbra (p-f collision), thus forming a delta-spot. We examine digitally processed images from the Ottawa River Solar Observatory of two related events inside the delta-spot 5 days after the p-f collision begins: the violent disruption of the f-umbra, and the formation in less than a day of an hydrogen-alpha filament. The evolutionary changes in shape, area, relative motions, and brightness that we measure for each spot in the elongated nest are more compatible with Parker's (1979a) hypothesis of a sunspot as a cluster of flux tubes held together by downdrafts than with the notion of a sunspot as a monolithic plug of magnetic flux. From chromospheric developments over the delta-spot, we show that a shearing motion along a polarity inversion is more effective than convergence for creating a chromospheric filament. We invoke the release of an instability, triggered by a sequence of processes lasting 1 day or more, to explain the disruption of the f-umbra in this delta-spot. We show that the sequence is initiated when the colliding p-f umbrae reach a critical separation around 3200 +/- 200 km. We present a descriptive model in which the reconnected magnetic fields block vertical transport of convective heat flux just beneath the photosphere. We observe the formation of an unusual type of penumbra adjacent to the f-polarity portion of this delta-spot just before its disruption. A tangential penumbral band grows out of disordered matter connected to the f-umbra. We present this as evidence for the extrusion of umbral magnetic flux by thermal plumes rising through a loosely bound umbra.

Gaizauskas, V.↗