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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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At least 433 records · Page 24

Cellulose Nanofibers as Rheological Modifiers to Improve Biomass Slurry Processing and Fermentation

This study investigates the enhancement of biomass slurry processability through the addition of rheological modifiers, focusing on carboxymethyl cellulose (CMC) and TEMPO-mediated oxidized cellulose nanofibrils (TCNF). Three sets of experiments were conducted to assess the effects of these additives on slurry processing and fermentation. Initial experiments evaluated the slurry extrudability, concluding that TCNF aids extrusion similarly to CMC. Subsequent experiments explored slurry viscosity reduction mechanisms, revealing that while CMC significantly reduced the viscosity, TCNF’s impact is negligible. Additionally, TCNF performed comparably to CMC in water retention tests across different conditions, which suggests that TCNF have potential as an effective additive for maintaining slurry fluidity at high solid concentrations through enhanced water retention. Lastly, both additives were investigated to ensure that they did not impact hydrolyzed biomass fermentation. The findings suggest that TCNF’s mechanisms differ from those of traditional water-soluble polymers like CMC, offering insights into novel approaches to improve the biomass processing efficiency and subsequent fermentation.

Jamieson, Zachary↗

A VISCOELASTIC MODEL FOR EVALUATING EXTRUSION-BASED PRINT CONDITIONS

Extrusion-based printing systems have improved significantly over the past several years, allowing for higher throughput, higher temperatures, and larger components. At the same time, advanced materials are being introduced on the market that can provide improved performance over a range of operating conditions. Often these materials incorporate fiber reinforcements, reactive resins, and additives to control reaction kinetics, flow rheology, or thermal stability. This study presents a general framework for evaluating the printability of various candidate materials based on a basic viscoelastic model. The model addresses fundamental requirements for extrusion-based printing, including pressure-driven flow, bead formation, bead functionality, and component-level functionality. The effectiveness of this model for evaluating the impact of compositional variations and identifying appropriate processing conditions has been demonstrated for specific materials on direct write, fused filament fabrication, and large-scale extrusion platforms.

Duty, Chad↗

Preparation of Low-Density Microcellular Foams from Recycled PET Modified by Solid State Polymerization and Chain Extension

Recycled polyethylene-terephthalate (RPET) bottle regrinds were physically foamed after two types of industrially feasible molecular weight increasing processes. Intrinsic viscosity (IV) of initial waste (0.71 dL/g) increased both after reactive extrusion carried out using a multifunctional epoxy-based chain extender (0.74 dL/g) and after solid state polycondensation (SSP) (0.78 dL/g), while capillary rheometry revealed higher degree of branching in the chain extended PET material. Despite the relatively low IV values (below 0.80 dL/g), physical foaming, a mild and cost-efficient way, was successful in both cases, uniform microcellular foam structures with void fractions ranging between 75 and 83% were achieved. During the experiments morphology change in the materials was tracked by differential scanning calorimetry (DSC) besides recording IV values. The IV drop during foaming was between 0.03 and 0.10 depending on the pre-processing technology. Structure of foams produced from the two different modified RPET materials was compared with each other based on scanning electron microscopic imaging of cryogenic fracture surfaces. The average cell diameters were measured to be 213 and 360 µm in the case of chain extended and SSP-modified materials, respectively.

36 MATERIALS SCIENCE↗

Extrusion control for high quality printing on Big Area Additive Manufacturing (BAAM) systems

Big Area Additive Manufacturing (BAAM) is a large format additive manufacturing (AM) process. The size scale has enabled many new applications for AM. However, at this scale, lack of high print resolution and extruder flowrate control lead to potentially significant geometric deviations in the printed part. This paper examines strategies to improve geometric quality in BAAM parts. Multi-resolution printing, extrusion diversion, and feedforward extruder control are examined herein. Furthermore, these methods were all found to be effective in mitigating phenomena detrimental to geometric part quality on the BAAM process.

36 MATERIALS SCIENCE↗

Influence of processing on the microstructure and mechanical properties of 14YWT

The investigation of the mechanical alloying (MA) conditions for producing the advanced oxide dispersion strengthened (ODS) 14YWT ferritic alloy led to significant improvements in balancing the strength, ductility and fracture toughness properties while still maintaining the salient microstructural features consisting of ultra-fine grains and high concentration of Y-, Ti- and O-enriched nanoclusters. The implemented changes to the processing conditions included reducing the contamination of the powder during ball milling, applying a pre-extrusion annealing treatment on the ball milled powder and exploring different extrusion temperatures at 850 C (SM170 heat), 1000 C (SM185) and 1150 C (SM200). The microstructural studies of the three 14YWT heats showed similarities in the dispersion of nanoclusters and sub-micron size grains, indicating the microstructure was insensitive to the different extrusion conditions. Compared to past 14YWT heats, the three new heats showed lower strength, but higher ductility levels between 25 and 800 C and significantly higher fracture toughness values between 25 C and 700 C. The lower contamination levels of O, C and N achieved with improved ball milling conditions plus the slightly larger grain size were identified as important factors for improving the balance in mechanical properties of the three heats of 14YWT.

Hoelzer, D. T.↗

Solid Phase Processing of Lead-Free Brass with Carbon Additives

Currently, “lead-free” brass alloys (like C27450/C27451/C6930), used extensively in drinking water fixtures and automotive, electrical, and electronic applications contain maximum 0.25% lead to maintain mechanical performance and machinability. Adding graphite to brass as an alternative to lead, using casting, powder metallurgy, and extrusion methods, has been explored previously. However, all these methods have proven to be energy-, time-, and resource-intensive, while not enabling performance equivalent to that of C36000 brass. In this project, we developed a one-step approach using friction extrusion and ShAPE to make lead-free brass/graphite components such as wires, rods and tubes with mechanical performance equivalent to commercial lead-free brass alloys. Manufacturing temperatures were maintained ~550-730 °C with feed rates ranging between 4 – 25 mm/min. Results show larger grains at the center of the rods and wires with smaller grains developing at the edges. Graphite particles were sheared in the direction of extrusion with higher strains observed towards the edges. Hardness of the brass/graphite samples was over 25% higher than that of the corresponding brass-only samples (rods and wires), also friction extruded. Our results show that the sub-micron graphite plays an important role in limiting process temperature and restraining grain growth during friction extrusion, thus reducing grain size in composites.

36 MATERIALS SCIENCE↗

Effect of reprocessing cycles on the degradation of polypropylene copolymer filled with talc or montmorillonite during injection molding process

Mechanical recycling of polymeric materials is a favorable technique resulting in economic and environmental benefits, especially in the case of polymers with a high production volume as the polypropylene copolymer (PP). However, recycling by reprocessing techniques can lead to thermal, mechanical or thermo-oxidative degradation that can affect the structure of the polymer and subsequently the material properties. PP filled with montmorillonite (MMT) or talc are widely produced and studied, however, its degradation reactions by reprocessing cycles are poorly studied so far. In this study, the effects of reprocessing cycles in the structure and in the properties of the PP/MMT and PP/Talc were evaluated. The samples were mixed with 5% talc or MMT Cloisite C15A in a twin-screw extrusion. After extrusion, this filled material was submitted to five reprocessing cycles through an injection molding process. In order to evaluate the changes induced by reprocessing techniques, the samples were characterized by DSC, FT-IR, Izod impact and tensile strength tests. The study showed that Young modulus, elongation at brake and Izod impact were not affected by reprocessing cycles, except when using talc. In this case, the elongation at brake reduced until the fourth cycle, showing rigidity increase. The DSC results showed that melting and crystallization temperature were not affected. A comparison of FT-IR spectra of the reprocessed indicated that in both samples, between the first and the fifth cycle, no noticeable change has occurred. Thus, there is no evidence of thermo oxidative degradation. In general, these results suggest that PP reprocessing cycles using MMT or talc does not change the material properties until the fifth cycle.

36 MATERIALS SCIENCE↗

Thermokinetic mixing compounding for polymer composites – a comprehensive review

High-speed thermokinetic mixers (K-mixers) represent an advanced compounding technology that employs intense shear and friction to convert kinetic energy directly into thermal energy. This mechanism enables rapid mixing cycles, often under one minute, facilitating exceptional filler dispersion while minimizing the material’s thermal history. This is particularly effective for compounding challenging materials, including heat-sensitive biopolymers, wet filler feedstocks, and nanofillers prone to agglomeration. As the first comprehensive review of this technology, this article synthesizes the fundamental principles of thermokinetic mixing (K-mixing) and surveys recent advances in polymer composite fabrication. We contrast the working principles of K-mixers with conventional twin-screw extrusion, highlighting distinct advantages in dispersing nanoscale fillers, exfoliating layered materials, and processing wet cellulosic feedstocks and ultra-high filler loadings (e.g., 85 wt%). Furthermore, strategies to optimize filler–matrix interfacial bonding under rapid-processing constraints, such as the kinetic selection of compatibilizers and fiber surface treatments, are evaluated. Finally, we analyze key structure-processing-property relationships and outline future directions in scaling up, reactive processing, and hybrid material development.

Zhang, Xuefeng [University of Maine]↗

Macro copper-graphene composites with enhanced electrical conductivity

Composites demonstrating simultaneously enhanced-electrical conductivity, current density and lowered-temperature coefficient of resistance (TCR) compared to copper have been highly sought after for their advantages in efficient energy transport behavior. While such conductors have been demonstrated in 1D (nanowires) and 2D (films) samples, achieving similar behavior in 3D has been challenging owing to the limitations of the synthesis techniques used. In this paper, novel macro-scale 3D copper conductors were demonstrated with simultaneously increased electrical conductivity and decreased temperature coefficient of resistance (TCR) through the addition of graphene. Hot-extrusion was used to manufacture over 1-m-long, 2-mm-diameter copper-graphene composites with varying graphene content and defect density. Results showed that the electrical conductivity and current density in composites with low defect density graphene increased monotonically as a function of graphene content. They also demonstrated a significant decrease of over 17% in TCR with the addition of only 15 ppm graphene along with over 52% improvement in current density. Comparatively composites with high defect density graphene demonstrated lower electrical conductivity and current density. This study provides first-of-its-kind evidence of 3D metal composites whose bulk electrical performance has been enhanced using graphene additive in minute quantities. Further developments in this area are essential to achieve high performance composite conductors that can improve energy transport efficiency and pave way for industrial adoption of such materials in the future.

36 MATERIALS SCIENCE↗

Hybrid printing of wearable piezoelectric sensors

Piezoelectricity provides an ideal electromechanical mechanism with emerging applications in wearable devices due to its simplicity and self-powered nature. However, the 3D printing of piezoelectric devices still faces many challenges, including material printability, high energy poling process, and low dimensional accuracy. This study demonstrates, for the first time, a tellurium nanowire-based piezoelectric device fabricated by a hybrid printing method integrating highly complementary aerosol jet printing and extrusion printing in a single printing platform. The aerosol-jet-printed tellurium nanowire demonstrates piezoelectric properties without the need for any poling processing due to the unique properties of the tellurium nanowires. The silver nanowire electrodes printed by aerosol jet printing demonstrate excellent conductivity and stretchability without the need for sintering. An extrusion method is employed to print the silicone films, which serve as the stretchable substrate and the electrical insulation layers between the printed tellurium and silver. The printed wearable piezoelectric devices were attached to a human wrist to detect different hand gestures and to a human neck to detect heartbeat without using an external power source. In conclusion, the fully printed, sintering-free and poling-free, and stretchable piezoelectric device opens enormous opportunities for facile integration with a broad range of printed electronics and wearable devices.

47 OTHER INSTRUMENTATION↗

Influence of powder metallurgy route on precipitation processes in MgTbNd alloy

Solution treated MgTb3Nd2 alloy (nominal composition in wt.%) (ST) and the alloy prepared by hot extrusion of isostatically pressed powder (PM) were isochronally heat treated and studied by electrical resistivity and hardness measurements and by differential scanning calorimetry. Microstructure development was investigated in transmission electron microscopy. Successive precipitation of transient phases in the sequence β″ (D0{sub 19} plates) → β′(cbco) → β{sub 1} (Mg{sub 3}Gd type, fcc) → β (Mg{sub 5}Gd type, fcc) known from the ST alloy was identified also in the PM alloy. The early precipitation stage (D0{sub 19} clusters) revealed in the ST alloy as well as precipitation of equilibrium β{sub e} phase Mg{sub 41}(Tb,Nd){sub 5} manifest themselves only slightly in the PM alloy. Powder metallurgy route does not change the values of activation energies but shifts the temperature ranges of these processes. Vickers hardness of the as prepared state is higher in the PM alloy and is very resistant against the heat treatment up to 510 °C. Contrary to the ST alloy precipitation due to isochronal annealing does not lead to pronounced hardness changes in the PM alloy. - Highlights: • Powder metallurgy (PM) does not change precipitation sequence in MgTbNd alloy. • Temperature ranges of transient phase precipitations are shifted in PM alloy. • Hardness is resistant against isochronal heat treatment up to 510 °C in the PM alloy. • PM procedure does not change activation energies of precipitation.

36 MATERIALS SCIENCE↗

The Cell Utilized Partitioning Model as a Predictive Tool for Optimizing Counter-Current Chromatography Processes

Counter-current chromatography (CCC) is capable of unique elution modes that isolate analytes using the movement of the stationary phase in addition to moving the mobile phase. These modes include elution-extrusion CCC (EECCC) and dual-mode CCC (DM CCC) that are not possible in traditional solid-liquid chromatography systems. Although EECCC and DM CCC are widely used to recover highly retained components, to our knowledge, optimizing the elution process in these modes with predictive models has not been reported. To address this gap, we developed a predictive model for CCC dubbed the Cell Utilized Partitioning (CUP) model. The CUP model accurately predicts the effluents of multicomponent separations in EECCC and DM CCC modes when compared to experimental data. Furthermore, CUP model simulations were extended to investigate the influence of operating and intrinsic parameters on the yield and productivity, and to compare the separation performances of EECCC and DM CCC in various conditions. The results demonstrate that low distribution constants, usually a KD less than 1, and a selectivity > 1.3, under specific flowrate ranges, increase both productivity and yield. From these results, generalized optimization and scaleup guidelines are proposed that can apply to research settings and to industrial processes to maximize preparative CCC performance.

BIOMASS FUELS,INORGANIC, ORGANIC, PHYSICAL, AND AN↗

Evacuated Spheres for Closed-Cell Vacuum Insulation

Insulation materials with a thermal resistance per inch higher than 6h∙ft 2 ∙°F/Btu∙in or R6/in (42m∙K/W) are needed for building envelope retrofits in which solutions with slim profiles are required because of minimal available space or because real estate has a premium cost. These insulation materials will also be of benefit to prefabricated construction given that slim designs either reduce shipping costs or increase the floor space provided to the customer. Vacuum insulation panels (VIPs) are the current state-of-the-art insulation material with a resistance of about R35/in (243m∙K/W); however, their use in buildings is hindered by the fact that damages to their protective film decrease their performance to ≤R8/in (56m∙K/W). Given the lack of robust, highly-insulating materials, we are exploring methods to develop evacuated spheres that can act as a closed-cell vacuum insulation. The evacuated spheres could be assembled into boards that could attain ~R14/in (97m∙K/W). Advantages that evacuated spheres will offer over VIPs are that they will likely be more suitable for construction because punctures will only cause localized damage, and that the boards could be cut into customized shapes. We are currently investigating two processes to evacuate spheres to produce polymeric vacuum insulation spheres (PVISs) and coated and evacuated insulation spheres (CEISs). PVISs involve the extrusion of economical polymers, blowing agents, and gas barriers. CEISs use naturally-occurring or synthesized hollow particles with porous shells that are evacuated and coated with a gas impermeable thin film. Both manufacturing processes aim for very large throughputs to ensure cost-effectiveness and adoption by the construction industry. This paper discusses the manufacturing techniques that we are exploring and our progress to date.

Hun, Diana E.↗

Advanced Methods for Direct Ink Write Additive Manufacturing

Lawrence Livermore National Laboratory is one of the world’s premier labs for research and development of additive manufacturing processes. Out of these many processes, direct ink write (DIW) is arguably one of the most relevant for the manufacture of architected polymeric materials, components and hardware. However, a bottleneck in this pipeline that has largely been ignored to date is the lack of advanced software implementation with respect to toolpath execution. There remains to be a convenient, automated method to design and produce complex parts that is user-friendly and enabling for the realization of next generation designs and structures. For a material to be suitable as a DIW ink it must possess the appropriate rheological properties for this process. Most importantly, the material must exhibit shear-thinning in order to extrude through a print head and have a rapid recovery of its static shear modulus. This makes it possible for the extrudate to be self-supporting upon exiting the print head. While this and other prerequisites narrow the scope of ‘offthe- shelf’ printable materials directly amenable to DIW, the process still tolerates a wide range of potential feedstock materials. These include metallic alloys, inorganic solvent borne dispersions, polymeric melts, filler stabilized monomer compositions, pre-elastomeric feedstocks and thermoset resins each of which requires custom print conditions tailored to the individual ink. As such, an ink perfectly suited for DIW may be prematurely determined to be undesirable for the process if printed under the wrong conditions. Defining appropriate print conditions such as extrusion rate, layer height, and maximum bridge length is a vital first step in validating an ink’s DIW capability.

36 MATERIALS SCIENCE↗

Process innovations to enable viable enzymatic poly(ethylene terephthalate) recycling

Enzymatic depolymerization of poly(ethylene terephthalate) (PET) has received considerable attention for closed-loop polyester recycling. However, current approaches for enzymatic PET recycling face challenges to achieve commercial viability with lower environmental impacts compared with virgin polyester manufacturing. Here, in this study, we present multiple process innovations for enzymatic PET recycling that enable economic and environmental feasibility. We show that substrate amorphization through extrusion and quenching is energy-efficient and enables near-quantitative enzymatic conversion in 50 h. Using ammonium hydroxide for pH control and thermolysis of the isolated diammonium terephthalate salt reduces the acid and base consumption by >99%, lowering annual operating expenses by 74%. Fed-batch processing increased ethylene glycol concentration, leading to a 65% reduction in energy consumption for ethylene glycol recovery. These improvements were modeled in an optimal process, with recycled PET estimated to be US$\$$1.51 kg -1 relative to US domestic virgin PET at US$\$$1.87 kg -1 and eliminating key life cycle obstacles to scale this technology.

36 MATERIALS SCIENCE↗